# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Anne F. Richards' _publ_contact_author_email a.richards@latrobe.edu.au loop_ _publ_author_name A.Zavras J.A.Fry G.N.Talbo A.F.Richards data_1cbsav _database_code_depnum_ccdc_archive 'CCDC 805028' #TrackingRef '- 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (((2PyHCH2PO3H)Mn(H2O))(ClO4))N _chemical_melting_point ? _chemical_formula_moiety 'C12 H18 Mn N2 O8 P2, 2(Cl O4) ' _chemical_formula_sum 'C12 H18 Cl2 Mn N2 O16 P2' _chemical_formula_weight 634.06 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.3278(17) _cell_length_b 8.2658(10) _cell_length_c 10.1631(13) _cell_angle_alpha 90.00 _cell_angle_beta 97.450(2) _cell_angle_gamma 90.00 _cell_volume 1110.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 2216 _cell_measurement_theta_min 4.079 _cell_measurement_theta_max 28.1915 _exptl_crystal_description chunk _exptl_crystal_colour colorless _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.015 _exptl_crystal_size_min 0.011 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.897 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 642 _exptl_absorpt_coefficient_mu 1.064 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9759 _exptl_absorpt_correction_T_max 0.9780 _exptl_absorpt_process_details 'SADABS: SAINT+, 2001' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <0.01 _diffrn_reflns_number 9359 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 28.32 _reflns_number_total 2645 _reflns_number_gt 2197 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v. 5.626' _computing_cell_refinement 'Bruker SAINT+ v. 6.36a' _computing_data_reduction 'Bruker SAINT+ v. 6.36a' _computing_structure_solution 'XS, Bruker SHELXTL v. 6.12' _computing_structure_refinement 'XL, Bruker SHELXTL v. 6.12' _computing_molecular_graphics 'XP, Bruker SHELXTL v. 6.12' _computing_publication_material 'XCIF, Bruker SHELXTL v. 6.12' _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. The hydrogens were geometrically placed upon and refined as riding on all carbon atoms with Ueq(H) = 1.2* Ueq(C). The hydrogen atom on N1, H1py, was found in the difference map, and refined freely. The hydrogen atoms on the axial water molecule, O4, were found in the difference map, and were refined using a simularity restraint on their distances from O4, and their Ueq values were allowed to refine, as they were physically reasonable. The largest peak in the difference map is near the phosphonate phosphorous, and we belive it to be an artifact of unresolved twinning. Multiple attempts to use rotational twin laws were unsuccessful, probably due to the twinning not resulting in a perfect overlap. This peak was not modeled as an alternate phosphorous position, because it does not make any chemical or packing sense, w ; _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^)+(0.0806P)^2^+17.0420P] 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 2645 _refine_ls_number_parameters 160 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0893 _refine_ls_R_factor_gt 0.0749 _refine_ls_wR_factor_ref 0.2525 _refine_ls_wR_factor_gt 0.2358 _refine_ls_goodness_of_fit_ref 1.169 _refine_ls_restrained_S_all 1.169 _refine_ls_shift/su_max 0.000 _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 Mn1 Mn 0.5000 0.5000 0.0000 0.0143(3) Uani 1 2 d S . . Cl1 Cl 0.17368(14) -0.0878(3) -0.26714(19) 0.0340(5) Uani 1 1 d . . . P1 P 0.45038(13) 0.31026(19) -0.29420(16) 0.0167(4) Uani 1 1 d . . . N1 N 0.2478(5) 0.2435(9) -0.5237(6) 0.0296(14) Uani 1 1 d . . . H1PY H 0.2998 0.1999 -0.5671 0.036 Uiso 1 1 d R . . O1 O 0.4244(4) 0.3365(6) -0.1562(4) 0.0196(10) Uani 1 1 d . . . O2 O 0.4459(3) 0.1387(5) -0.3429(4) 0.0171(9) Uani 1 1 d . . . O3 O 0.5609(4) 0.3729(6) -0.3049(5) 0.0273(11) Uani 1 1 d . . . O4 O 0.3600(4) 0.6373(7) -0.0153(6) 0.0316(12) Uani 1 1 d . . . H4WA H 0.3441 0.6732 -0.0840 0.047 Uiso 1 1 d R . . H4WB H 0.3201 0.6432 0.0340 0.047 Uiso 1 1 d R . . O5 O 0.0753(5) -0.0213(11) -0.2688(8) 0.059(2) Uani 1 1 d . . . O6 O 0.1829(6) -0.1614(10) -0.3925(7) 0.055(2) Uani 1 1 d . . . O7 O 0.2455(6) 0.0452(9) -0.2508(8) 0.0531(18) Uani 1 1 d . . . O8 O 0.1942(7) -0.1977(14) -0.1636(9) 0.086(3) Uani 1 1 d . . . C1 C 0.3702(6) 0.4318(9) -0.4139(7) 0.0289(16) Uani 1 1 d . . . H1A H 0.3684 0.5428 -0.3804 0.035 Uiso 1 1 calc R . . H1B H 0.4000 0.4350 -0.4971 0.035 Uiso 1 1 calc R . . C2 C 0.2649(6) 0.3694(10) -0.4414(7) 0.0282(16) Uani 1 1 d . . . C3 C 0.1834(8) 0.4325(13) -0.3867(9) 0.046(2) Uani 1 1 d . . . H3A H 0.1925 0.5211 -0.3284 0.056 Uiso 1 1 calc R . . C4 C 0.0892(8) 0.3646(18) -0.4183(11) 0.065(4) Uani 1 1 d . . . H4A H 0.0335 0.4090 -0.3828 0.078 Uiso 1 1 calc R . . C5 C 0.0755(8) 0.2344(19) -0.5001(11) 0.061(3) Uani 1 1 d . . . H5A H 0.0111 0.1870 -0.5198 0.073 Uiso 1 1 calc R . . C6 C 0.1572(7) 0.1726(14) -0.5537(9) 0.045(2) Uani 1 1 d . . . H6A H 0.1495 0.0824 -0.6104 0.054 Uiso 1 1 calc R . . 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 Mn1 0.0199(7) 0.0127(6) 0.0110(6) 0.0003(5) 0.0041(5) -0.0004(5) Cl1 0.0278(9) 0.0487(12) 0.0259(9) -0.0007(8) 0.0055(7) 0.0053(8) P1 0.0265(8) 0.0125(7) 0.0124(7) -0.0016(6) 0.0071(6) -0.0028(6) N1 0.026(3) 0.042(4) 0.022(3) 0.004(3) 0.006(2) 0.005(3) O1 0.028(2) 0.020(2) 0.012(2) -0.0055(17) 0.0071(17) -0.0043(19) O2 0.025(2) 0.012(2) 0.015(2) -0.0001(16) 0.0066(17) 0.0002(17) O3 0.032(3) 0.029(3) 0.024(2) -0.010(2) 0.014(2) -0.013(2) O4 0.030(3) 0.035(3) 0.032(3) 0.009(2) 0.013(2) 0.013(2) O5 0.036(4) 0.083(6) 0.063(5) 0.022(4) 0.024(3) 0.016(4) O6 0.053(4) 0.068(5) 0.050(4) -0.031(4) 0.026(3) -0.023(4) O7 0.049(4) 0.049(4) 0.061(5) -0.010(4) 0.005(3) -0.007(3) O8 0.073(6) 0.119(9) 0.065(6) 0.054(6) 0.009(5) 0.014(6) C1 0.047(4) 0.017(3) 0.023(3) 0.007(3) 0.005(3) 0.001(3) C2 0.035(4) 0.032(4) 0.019(3) 0.011(3) 0.007(3) 0.013(3) C3 0.058(6) 0.050(6) 0.035(5) 0.011(4) 0.023(4) 0.030(5) C4 0.038(5) 0.113(11) 0.047(6) 0.039(7) 0.020(4) 0.034(6) C5 0.033(5) 0.109(10) 0.039(5) 0.028(6) 0.001(4) 0.002(6) C6 0.033(4) 0.073(7) 0.028(4) 0.013(4) -0.002(3) -0.008(4) _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 Mn1 O2 2.164(4) 2_654 ? Mn1 O2 2.164(4) 4_566 ? Mn1 O4 2.172(5) 3_665 ? Mn1 O4 2.172(5) . ? Mn1 O1 2.224(4) 3_665 ? Mn1 O1 2.224(4) . ? Cl1 O8 1.390(8) . ? Cl1 O5 1.420(7) . ? Cl1 O6 1.432(7) . ? Cl1 O7 1.452(8) . ? P1 O2 1.501(5) . ? P1 O1 1.504(5) . ? P1 O3 1.579(5) . ? P1 C1 1.815(7) . ? N1 C2 1.336(11) . ? N1 C6 1.342(11) . ? N1 H1PY 0.9402 . ? O2 Mn1 2.164(4) 2_644 ? O4 H4WA 0.7629 . ? O4 H4WB 0.7780 . ? C1 C2 1.488(11) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 C3 1.384(11) . ? C3 C4 1.375(17) . ? C3 H3A 0.9400 . ? C4 C5 1.358(19) . ? C4 H4A 0.9400 . ? C5 C6 1.377(15) . ? C5 H5A 0.9400 . ? C6 H6A 0.9400 . ? 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 Mn1 O2 180.0 2_654 4_566 ? O2 Mn1 O4 87.94(19) 2_654 3_665 ? O2 Mn1 O4 92.06(19) 4_566 3_665 ? O2 Mn1 O4 92.06(19) 2_654 . ? O2 Mn1 O4 87.94(19) 4_566 . ? O4 Mn1 O4 180.0 3_665 . ? O2 Mn1 O1 92.35(16) 2_654 3_665 ? O2 Mn1 O1 87.65(16) 4_566 3_665 ? O4 Mn1 O1 87.8(2) 3_665 3_665 ? O4 Mn1 O1 92.2(2) . 3_665 ? O2 Mn1 O1 87.65(16) 2_654 . ? O2 Mn1 O1 92.35(16) 4_566 . ? O4 Mn1 O1 92.2(2) 3_665 . ? O4 Mn1 O1 87.8(2) . . ? O1 Mn1 O1 180.0 3_665 . ? O8 Cl1 O5 110.6(5) . . ? O8 Cl1 O6 111.4(6) . . ? O5 Cl1 O6 109.8(5) . . ? O8 Cl1 O7 110.2(6) . . ? O5 Cl1 O7 107.6(5) . . ? O6 Cl1 O7 107.0(4) . . ? O2 P1 O1 116.1(3) . . ? O2 P1 O3 106.5(3) . . ? O1 P1 O3 110.3(3) . . ? O2 P1 C1 107.9(3) . . ? O1 P1 C1 111.0(3) . . ? O3 P1 C1 104.2(3) . . ? C2 N1 C6 123.9(8) . . ? C2 N1 H1PY 121.1 . . ? C6 N1 H1PY 115.0 . . ? P1 O1 Mn1 128.0(3) . . ? P1 O2 Mn1 137.8(3) . 2_644 ? Mn1 O4 H4WA 113.7 . . ? Mn1 O4 H4WB 129.7 . . ? H4WA O4 H4WB 115.7 . . ? C2 C1 P1 113.2(5) . . ? C2 C1 H1A 108.9 . . ? P1 C1 H1A 108.9 . . ? C2 C1 H1B 108.9 . . ? P1 C1 H1B 108.9 . . ? H1A C1 H1B 107.8 . . ? N1 C2 C3 117.8(8) . . ? N1 C2 C1 117.9(7) . . ? C3 C2 C1 124.3(8) . . ? C4 C3 C2 119.5(10) . . ? C4 C3 H3A 120.2 . . ? C2 C3 H3A 120.2 . . ? C5 C4 C3 120.8(10) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C4 C5 C6 119.0(10) . . ? C4 C5 H5A 120.5 . . ? C6 C5 H5A 120.5 . . ? N1 C6 C5 118.9(11) . . ? N1 C6 H6A 120.6 . . ? C5 C6 H6A 120.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 P1 O1 Mn1 139.0(3) . . . . ? O3 P1 O1 Mn1 17.7(5) . . . . ? C1 P1 O1 Mn1 -97.3(4) . . . . ? O2 Mn1 O1 P1 22.8(4) 2_654 . . . ? O2 Mn1 O1 P1 -157.2(4) 4_566 . . . ? O4 Mn1 O1 P1 -65.0(4) 3_665 . . . ? O4 Mn1 O1 P1 115.0(4) . . . . ? O1 Mn1 O1 P1 -177(95) 3_665 . . . ? O1 P1 O2 Mn1 -163.5(4) . . . 2_644 ? O3 P1 O2 Mn1 -40.2(5) . . . 2_644 ? C1 P1 O2 Mn1 71.3(5) . . . 2_644 ? O2 P1 C1 C2 54.6(6) . . . . ? O1 P1 C1 C2 -73.6(6) . . . . ? O3 P1 C1 C2 167.6(5) . . . . ? C6 N1 C2 C3 -1.6(11) . . . . ? C6 N1 C2 C1 177.9(7) . . . . ? P1 C1 C2 N1 -78.8(7) . . . . ? P1 C1 C2 C3 100.7(8) . . . . ? N1 C2 C3 C4 0.0(12) . . . . ? C1 C2 C3 C4 -179.5(8) . . . . ? C2 C3 C4 C5 1.5(15) . . . . ? C3 C4 C5 C6 -1.4(16) . . . . ? C2 N1 C6 C5 1.7(13) . . . . ? C4 C5 C6 N1 -0.1(15) . . . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 26.25 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.190 _refine_diff_density_min -0.766 _refine_diff_density_rms 0.204 # Attachment '- 2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 805029' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (2PyCH2PO3Mn(H2O)(ClO4))N _chemical_melting_point ? _chemical_formula_moiety 'C12 H20 Co N2 O8 P2, 2(Cl O4)' _chemical_formula_sum 'C12 H20 Cl2 Co N2 O16 P2' _chemical_formula_weight 640.07 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.398(3) _cell_length_b 8.2442(19) _cell_length_c 10.040(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.348(4) _cell_angle_gamma 90.00 _cell_volume 1099.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 3024 _cell_measurement_theta_min 2.9075 _cell_measurement_theta_max 27.618 _exptl_crystal_description chunk _exptl_crystal_colour 'pale pink' _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.933 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 650 _exptl_absorpt_coefficient_mu 1.254 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9717 _exptl_absorpt_correction_T_max 0.9814 _exptl_absorpt_process_details 'SADABS: SAINT+, 2001' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <0.01 _diffrn_reflns_number 6462 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 28.29 _reflns_number_total 2546 _reflns_number_gt 1906 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART v. 5.626' _computing_cell_refinement 'Bruker SAINT+ v. 6.36a' _computing_data_reduction 'Bruker SAINT+ v. 6.36a' _computing_structure_solution 'XS, Bruker SHELXTL v. 6.12' _computing_structure_refinement 'XL, Bruker SHELXTL v. 6.12' _computing_molecular_graphics 'XP, Bruker SHELXTL v. 6.12' _computing_publication_material 'XCIF, Bruker SHELXTL v. 6.12' _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. The hydrogens were geometrically placed upon and refined as riding on all carbon atoms with Ueq(H) = 1.2* Ueq(C). The hydrogen atom on N1, H1py, was found in the difference map, and refined freely. The hydrogen atoms on the axial water molecule, O4, were found in the difference map, and were refined using a simularity restraint on their distances from O4, and their Ueq values refined as Ueq(H) = 1.5* Ueq(O). The hydrogen on the phosphonate oxygen was refined similarly. ; _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^)+(0.0671P)^2^+2.6022P] 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 2546 _refine_ls_number_parameters 174 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1396 _refine_ls_wR_factor_gt 0.1233 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.000 _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 Co1 Co 0.5000 0.0000 0.5000 0.0183(2) Uani 1 2 d S . . Cl1 Cl 0.82428(8) 0.09529(15) 0.26300(10) 0.0387(3) Uani 1 1 d . . . P1 P 0.45135(7) 0.30888(11) 0.70790(9) 0.0202(2) Uani 1 1 d . . . O1 O 0.44632(19) 0.1354(3) 0.6587(2) 0.0202(5) Uani 1 1 d . . . O2 O 0.5605(2) 0.3713(4) 0.6924(3) 0.0324(7) Uani 1 1 d D . . H2 H 0.572(4) 0.463(3) 0.722(6) 0.063(19) Uiso 1 1 d D . . O3 O 0.4269(2) 0.3360(3) 0.8487(3) 0.0248(6) Uani 1 1 d . . . O4 O 0.6355(2) 0.1306(4) 0.5160(3) 0.0363(8) Uani 1 1 d D . . H4WA H 0.672(4) 0.126(7) 0.466(5) 0.055 Uiso 1 1 d D . . H4WB H 0.649(4) 0.187(6) 0.573(5) 0.055 Uiso 1 1 d D . . O5 O 0.9218(3) 0.0278(6) 0.2668(5) 0.0747(14) Uani 1 1 d . . . O6 O 0.8029(4) 0.2044(7) 0.1598(5) 0.0877(16) Uani 1 1 d . . . O7 O 0.7548(3) -0.0421(5) 0.2437(4) 0.0588(10) Uani 1 1 d . . . O8 O 0.8109(3) 0.1613(5) 0.3904(4) 0.0606(11) Uani 1 1 d . . . N1 N 0.2485(3) 0.2376(5) 0.4808(4) 0.0360(9) Uani 1 1 d D . . H1PY H 0.305(2) 0.207(7) 0.448(5) 0.056(17) Uiso 1 1 d D . . C1 C 0.3693(4) 0.4300(5) 0.5893(4) 0.0328(10) Uani 1 1 d . . . H1A H 0.3673 0.5408 0.6241 0.039 Uiso 1 1 calc R . . H1B H 0.3982 0.4350 0.5045 0.039 Uiso 1 1 calc R . . C2 C 0.2650(4) 0.3676(5) 0.5619(4) 0.0340(10) Uani 1 1 d . . . C3 C 0.1840(4) 0.4327(7) 0.6139(5) 0.0539(15) Uani 1 1 d . . . H3B H 0.1927 0.5242 0.6701 0.065 Uiso 1 1 calc R . . C4 C 0.0907(5) 0.3650(10) 0.5844(7) 0.073(2) Uani 1 1 d . . . H4B H 0.0355 0.4099 0.6205 0.087 Uiso 1 1 calc R . . C5 C 0.0775(4) 0.2323(11) 0.5024(6) 0.073(2) Uani 1 1 d . . . H5B H 0.0135 0.1850 0.4824 0.087 Uiso 1 1 calc R . . C6 C 0.1587(4) 0.1687(8) 0.4497(5) 0.0517(14) Uani 1 1 d . . . H6B H 0.1509 0.0780 0.3925 0.062 Uiso 1 1 calc R . . 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 Co1 0.0235(4) 0.0159(3) 0.0160(3) -0.0004(2) 0.0039(3) 0.0004(3) Cl1 0.0314(6) 0.0577(7) 0.0269(5) -0.0031(5) 0.0028(4) 0.0072(5) P1 0.0310(5) 0.0138(4) 0.0174(5) -0.0004(3) 0.0087(4) -0.0028(4) O1 0.0283(14) 0.0134(11) 0.0189(12) -0.0008(9) 0.0039(10) -0.0012(10) O2 0.0406(17) 0.0314(16) 0.0284(15) -0.0123(12) 0.0175(13) -0.0158(14) O3 0.0352(15) 0.0218(13) 0.0196(13) -0.0021(10) 0.0118(11) -0.0053(11) O4 0.0334(17) 0.0395(18) 0.0379(19) -0.0158(14) 0.0115(14) -0.0089(14) O5 0.039(2) 0.111(4) 0.078(3) 0.035(3) 0.022(2) 0.022(2) O6 0.090(4) 0.105(4) 0.069(3) 0.041(3) 0.017(3) 0.023(3) O7 0.057(2) 0.056(2) 0.062(2) -0.014(2) 0.0041(19) -0.0028(19) O8 0.069(3) 0.070(3) 0.047(2) -0.0211(19) 0.0213(19) -0.022(2) N1 0.035(2) 0.047(2) 0.0259(18) 0.0070(16) 0.0040(15) 0.0088(18) C1 0.056(3) 0.0190(18) 0.025(2) 0.0082(15) 0.0102(19) 0.0044(18) C2 0.047(3) 0.033(2) 0.024(2) 0.0150(17) 0.0104(18) 0.015(2) C3 0.065(4) 0.058(3) 0.043(3) 0.016(2) 0.023(3) 0.036(3) C4 0.049(4) 0.115(6) 0.060(4) 0.037(4) 0.027(3) 0.043(4) C5 0.039(3) 0.129(7) 0.048(3) 0.048(4) -0.004(3) -0.001(4) C6 0.041(3) 0.076(4) 0.036(3) 0.016(3) -0.004(2) -0.004(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 Co1 O4 2.099(3) . ? Co1 O4 2.099(3) 3_656 ? Co1 O1 2.143(2) 3_656 ? Co1 O1 2.143(2) . ? Co1 O3 2.171(3) 2_646 ? Co1 O3 2.171(3) 4_565 ? Cl1 O6 1.374(5) . ? Cl1 O5 1.417(4) . ? Cl1 O8 1.422(4) . ? Cl1 O7 1.464(4) . ? P1 O3 1.508(3) . ? P1 O1 1.512(2) . ? P1 O2 1.576(3) . ? P1 C1 1.813(4) . ? O2 H2 0.823(10) . ? O3 Co1 2.171(3) 2_656 ? O4 H4WA 0.74(4) . ? O4 H4WB 0.74(4) . ? N1 C6 1.332(7) . ? N1 C2 1.347(6) . ? N1 H1PY 0.900(10) . ? C1 C2 1.482(7) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 C3 1.372(6) . ? C3 C4 1.366(10) . ? C3 H3B 0.9400 . ? C4 C5 1.367(11) . ? C4 H4B 0.9400 . ? C5 C6 1.373(9) . ? C5 H5B 0.9400 . ? C6 H6B 0.9400 . ? 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 O4 Co1 O4 180.0 . 3_656 ? O4 Co1 O1 87.41(11) . 3_656 ? O4 Co1 O1 92.59(11) 3_656 3_656 ? O4 Co1 O1 92.59(11) . . ? O4 Co1 O1 87.41(11) 3_656 . ? O1 Co1 O1 180.0 3_656 . ? O4 Co1 O3 87.56(13) . 2_646 ? O4 Co1 O3 92.44(13) 3_656 2_646 ? O1 Co1 O3 91.80(9) 3_656 2_646 ? O1 Co1 O3 88.21(9) . 2_646 ? O4 Co1 O3 92.44(13) . 4_565 ? O4 Co1 O3 87.56(13) 3_656 4_565 ? O1 Co1 O3 88.20(9) 3_656 4_565 ? O1 Co1 O3 91.80(9) . 4_565 ? O3 Co1 O3 180.0 2_646 4_565 ? O6 Cl1 O5 112.3(3) . . ? O6 Cl1 O8 113.0(3) . . ? O5 Cl1 O8 110.4(3) . . ? O6 Cl1 O7 109.8(3) . . ? O5 Cl1 O7 105.6(3) . . ? O8 Cl1 O7 105.3(2) . . ? O3 P1 O1 116.17(15) . . ? O3 P1 O2 111.08(16) . . ? O1 P1 O2 106.22(16) . . ? O3 P1 C1 110.36(18) . . ? O1 P1 C1 107.94(18) . . ? O2 P1 C1 104.32(19) . . ? P1 O1 Co1 136.94(15) . . ? P1 O2 H2 113(4) . . ? P1 O3 Co1 127.99(16) . 2_656 ? Co1 O4 H4WA 124(5) . . ? Co1 O4 H4WB 120(5) . . ? H4WA O4 H4WB 115(6) . . ? C6 N1 C2 123.7(5) . . ? C6 N1 H1PY 125(4) . . ? C2 N1 H1PY 112(4) . . ? C2 C1 P1 114.1(3) . . ? C2 C1 H1A 108.7 . . ? P1 C1 H1A 108.7 . . ? C2 C1 H1B 108.7 . . ? P1 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? N1 C2 C3 117.7(5) . . ? N1 C2 C1 117.8(4) . . ? C3 C2 C1 124.6(5) . . ? C4 C3 C2 120.3(6) . . ? C4 C3 H3B 119.9 . . ? C2 C3 H3B 119.9 . . ? C3 C4 C5 120.1(5) . . ? C3 C4 H4B 119.9 . . ? C5 C4 H4B 119.9 . . ? C4 C5 C6 119.3(6) . . ? C4 C5 H5B 120.3 . . ? C6 C5 H5B 120.3 . . ? N1 C6 C5 118.9(6) . . ? N1 C6 H6B 120.6 . . ? C5 C6 H6B 120.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 P1 O1 Co1 -162.8(2) . . . . ? O2 P1 O1 Co1 -38.8(3) . . . . ? C1 P1 O1 Co1 72.6(3) . . . . ? O4 Co1 O1 P1 37.0(2) . . . . ? O4 Co1 O1 P1 -143.0(2) 3_656 . . . ? O1 Co1 O1 P1 -88(7) 3_656 . . . ? O3 Co1 O1 P1 124.4(2) 2_646 . . . ? O3 Co1 O1 P1 -55.6(2) 4_565 . . . ? O1 P1 O3 Co1 140.22(18) . . . 2_656 ? O2 P1 O3 Co1 18.7(3) . . . 2_656 ? C1 P1 O3 Co1 -96.5(2) . . . 2_656 ? O3 P1 C1 C2 -74.4(3) . . . . ? O1 P1 C1 C2 53.5(3) . . . . ? O2 P1 C1 C2 166.2(3) . . . . ? C6 N1 C2 C3 -0.6(6) . . . . ? C6 N1 C2 C1 179.1(4) . . . . ? P1 C1 C2 N1 -76.2(4) . . . . ? P1 C1 C2 C3 103.5(4) . . . . ? N1 C2 C3 C4 0.7(7) . . . . ? C1 C2 C3 C4 -179.0(4) . . . . ? C2 C3 C4 C5 -0.2(8) . . . . ? C3 C4 C5 C6 -0.4(9) . . . . ? C2 N1 C6 C5 0.0(7) . . . . ? C4 C5 C6 N1 0.5(8) . . . . ? 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 H1PY O3 0.900(10) 2.050(15) 2.941(5) 170(5) 4_565 O4 H4WA O8 0.74(4) 2.12(4) 2.817(5) 157(6) . O4 H4WA Cl1 0.74(4) 3.08(4) 3.818(3) 178(6) . O2 H2 O1 0.823(10) 1.89(3) 2.650(4) 153(6) 2_656 O2 H2 O7 0.823(10) 2.52(5) 2.947(5) 114(5) 4_566 O4 H4WB O6 0.74(4) 2.31(5) 2.853(6) 131(6) 4_566 O4 H4WB O2 0.74(4) 2.35(5) 2.923(4) 135(6) . _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 26.25 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.312 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.113 # Attachment '- 3.cif' data_3cb2 _database_code_depnum_ccdc_archive 'CCDC 805030' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Fe4(PyHCH2PO3)4(H2O)12(Cl)(ClO4)7xH2O) _chemical_melting_point ? _chemical_formula_moiety 'C24 H52 Fe4 N4 O24 P4, Cl, 7(ClO4),(H2O)' _chemical_formula_sum 'C24 H54 Cl8 Fe4 N4 O53 P4 ' _chemical_formula_weight 1877.59 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 11.051(3) _cell_length_b 14.563(4) _cell_length_c 20.651(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.526(6) _cell_angle_gamma 90.00 _cell_volume 3320.4(17) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 6557 _cell_measurement_theta_min 2.4166 _cell_measurement_theta_max 29.2322 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.878 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1900 _exptl_absorpt_coefficient_mu 1.393 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9727 _exptl_absorpt_correction_T_max 0.9862 _exptl_absorpt_process_details 'SADABS: SAINT+, 2001' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.3281 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19115 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 29.15 _reflns_number_total 7772 _reflns_number_gt 5667 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlisPro, V. 1.171.34.40' _computing_cell_refinement 'CrysAlisPro, V. 171.34.40' _computing_data_reduction 'CrysAlisPro, V. 1.171.34.40' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL-97 _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. The hydrogens were geometrically placed upon and refined as riding on all carbon atoms with Ueq(H) = 1.2* Ueq(C). The hydrogen atom on N2, H2py, was found in the difference map, and allowed to refine its position, with Ueq(H)=1.2Ueq(N2). The hydrogen atoms on the ligeate water molecules were found in the difference map and were refined using a DFIX of d=0.84 on their distances from their oxygens, with their Ueq(H) = 1.5* Ueq(O). They hydrogen on N1, H1py, was placed geometrically, and refined as riding. It was not possible to find this hydrogen in the difference map, probably due to the large amount of thermal motion in this ring. Modeling of this ring as a split-site disordered group was attempted, but this was not stable. There is an solvated, 0.5 occupancy water molecule, O1W, for which no hydrogens could be located. This crystal suffers greatly from disorder. There are eight perchlorate sites, two of which are slightly off the 2-fold axis (Resi #11, 12), one which is on an inversion center (resi #13) with a disordered component (Resi #14), and two sites with two orientations(Resi #7 and 10, #8 and 9). To manage these percholrate ions, they were retrained to be similar using RESI-based SIMU and SADI commands, as shown below: SADI_ClO4 0.01 Cl1 O1 Cl1 O2 CL1 O3 Cl1 O4 SADI_ClO4 0.02 O1 O2 O1 O3 O1 O4 O2 O3 O2 O4 O3 O4 SIMU_ClO4 0.1 The sum of the charge from the percholrates is 3.5. There is an chloride ion that occupies a site upon the twofold, which completes the charge balance. ; _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^)+(0.1088P)^2^+14.1672P] 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 7772 _refine_ls_number_parameters 684 _refine_ls_number_restraints 2215 _refine_ls_R_factor_all 0.0971 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.2009 _refine_ls_wR_factor_gt 0.1756 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 1.082 _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 Fe1 Fe 0.91606(7) -0.27097(5) 0.67359(3) 0.01951(19) Uani 1 1 d . . . Fe2 Fe 0.60353(7) -0.02875(5) 0.65657(3) 0.01903(19) Uani 1 1 d . . . Cl1 Cl 0.7500 0.11072(15) 0.2500 0.0329(4) Uani 1 2 d S . . P1 P 0.87881(13) -0.25890(9) 0.83178(6) 0.0215(3) Uani 1 1 d U . . P2 P 0.89538(12) -0.04084(9) 0.68282(6) 0.0198(3) Uani 1 1 d U . . O1 O 0.9049(5) -0.2923(4) 0.7647(2) 0.0462(12) Uani 1 1 d U . . O1W O 0.766(2) -0.8219(7) 0.7332(10) 0.074(5) Uani 0.50 1 d P . 1 O2 O 0.9020(5) -0.1589(3) 0.8427(3) 0.0458(12) Uani 1 1 d U . . O3 O 0.7534(4) -0.2878(3) 0.8520(2) 0.0375(10) Uani 1 1 d U . . O4 O 0.7773(4) -0.0094(3) 0.64961(19) 0.0301(9) Uani 1 1 d U . . O5 O 0.9028(4) -0.0089(3) 0.75264(19) 0.0398(11) Uani 1 1 d U . . O6 O 0.9179(5) -0.1414(3) 0.6763(3) 0.0479(12) Uani 1 1 d U . . N1 N 1.0442(11) -0.4752(6) 0.8796(5) 0.103(3) Uani 1 1 d U . . H1PY H 1.1034 -0.4545 0.8574 0.124 Uiso 1 1 calc R . . N2 N 0.9800(6) 0.1760(4) 0.6178(3) 0.0386(12) Uani 1 1 d U . . H2PY H 0.950(7) 0.160(5) 0.585(4) 0.046 Uiso 1 1 d . . . C1 C 0.9849(7) -0.3179(5) 0.8869(4) 0.0456(16) Uani 1 1 d U . . H1A H 1.0654 -0.3137 0.8690 0.055 Uiso 1 1 calc R . . H1B H 0.9883 -0.2843 0.9280 0.055 Uiso 1 1 calc R . . C2 C 0.9619(9) -0.4137(6) 0.9010(4) 0.062(2) Uani 1 1 d U . . C3 C 0.8702(11) -0.4462(8) 0.9342(6) 0.089(3) Uani 1 1 d U . . H3A H 0.8142 -0.4058 0.9520 0.106 Uiso 1 1 calc R . . C4 C 0.8583(14) -0.5436(8) 0.9424(6) 0.105(3) Uani 1 1 d U . . H4A H 0.7891 -0.5684 0.9606 0.126 Uiso 1 1 calc R . . C5 C 0.9505(15) -0.6006(8) 0.9229(6) 0.108(3) Uani 1 1 d U . . H5A H 0.9491 -0.6636 0.9329 0.130 Uiso 1 1 calc R . . C6 C 1.0390(16) -0.5667(8) 0.8908(7) 0.118(3) Uani 1 1 d U . . H6A H 1.0992 -0.6056 0.8755 0.141 Uiso 1 1 calc R . . C7 C 1.0196(5) 0.0162(4) 0.6434(3) 0.0258(11) Uani 1 1 d U . . H7A H 1.0959 -0.0143 0.6565 0.031 Uiso 1 1 calc R . . H7B H 1.0077 0.0094 0.5963 0.031 Uiso 1 1 calc R . . C8 C 1.0293(5) 0.1153(4) 0.6595(3) 0.0263(11) Uani 1 1 d U . . C9 C 1.0853(6) 0.1502(4) 0.7155(3) 0.0381(14) Uani 1 1 d U . . H9A H 1.1210 0.1102 0.7465 0.046 Uiso 1 1 calc R . . C10 C 1.0886(7) 0.2445(5) 0.7258(4) 0.0477(16) Uani 1 1 d U . . H10A H 1.1255 0.2681 0.7641 0.057 Uiso 1 1 calc R . . C11 C 1.0385(7) 0.3031(5) 0.6804(4) 0.0503(17) Uani 1 1 d U . . H11A H 1.0427 0.3670 0.6867 0.060 Uiso 1 1 calc R . . C12 C 0.9821(8) 0.2677(5) 0.6258(4) 0.0529(18) Uani 1 1 d U . . H12A H 0.9456 0.3067 0.5943 0.063 Uiso 1 1 calc R . . O1_1 O 0.9459(5) -0.4101(3) 0.6659(3) 0.0434(11) Uani 1 1 d D . . H1_1 H 0.873(3) -0.425(6) 0.669(4) 0.065 Uiso 1 1 d D . . H2_1 H 0.968(6) -0.436(5) 0.632(2) 0.065 Uiso 1 1 d D . . O1_2 O 1.1039(4) -0.2676(3) 0.6809(3) 0.0409(11) Uani 1 1 d D . . H1_2 H 1.140(6) -0.227(3) 0.703(3) 0.061 Uiso 1 1 d D . . H2_2 H 1.143(6) -0.316(3) 0.688(4) 0.061 Uiso 1 1 d D . . O1_3 O 0.9456(5) -0.2707(4) 0.5748(2) 0.0440(12) Uani 1 1 d D . . H1_3 H 1.009(4) -0.247(6) 0.561(3) 0.066 Uiso 1 1 d D . . H2_3 H 0.893(5) -0.263(6) 0.545(3) 0.066 Uiso 1 1 d D . . O1_4 O 0.5834(5) -0.0304(4) 0.5572(2) 0.0442(12) Uani 1 1 d D . . H1_4 H 0.625(7) 0.008(4) 0.538(4) 0.066 Uiso 1 1 d D . . H2_4 H 0.591(8) -0.079(3) 0.536(3) 0.066 Uiso 1 1 d D . . O1_5 O 0.5882(4) 0.1134(3) 0.6437(3) 0.0397(11) Uani 1 1 d D . . H1_5 H 0.634(5) 0.144(4) 0.620(3) 0.060 Uiso 1 1 d D . . H2_5 H 0.524(4) 0.145(4) 0.644(4) 0.060 Uiso 1 1 d D . . O1_6 O 0.4130(4) -0.0223(3) 0.6502(2) 0.0339(9) Uani 1 1 d D . . H1_6 H 0.407(7) 0.028(2) 0.669(3) 0.051 Uiso 1 1 d D . . H2_6 H 0.370(6) -0.058(4) 0.671(3) 0.051 Uiso 1 1 d D . . Cl1_7 Cl 0.291(2) 0.2036(17) 0.5589(11) 0.065(4) Uani 0.173(10) 1 d PDU A 1 O1_7 O 0.261(4) 0.2974(17) 0.5679(19) 0.086(7) Uani 0.173(10) 1 d PDU A 1 O2_7 O 0.298(4) 0.159(3) 0.6201(13) 0.075(6) Uani 0.173(10) 1 d PDU A 1 O3_7 O 0.405(3) 0.197(3) 0.530(2) 0.074(7) Uani 0.173(10) 1 d PDU A 1 O4_7 O 0.200(3) 0.161(3) 0.5191(15) 0.080(6) Uani 0.173(10) 1 d PDU A 1 Cl1_8 Cl 0.2332(15) -0.1807(11) 0.5242(7) 0.052(3) Uani 0.242(8) 1 d PDU B 1 O1_8 O 0.298(2) -0.1491(19) 0.4709(10) 0.087(5) Uani 0.242(8) 1 d PDU B 1 O2_8 O 0.1110(16) -0.1500(19) 0.5194(14) 0.052(5) Uani 0.242(8) 1 d PDU B 1 O3_8 O 0.230(2) -0.2784(11) 0.5227(13) 0.081(6) Uani 0.242(8) 1 d PDU B 1 O4_8 O 0.288(2) -0.1518(17) 0.5836(9) 0.084(5) Uani 0.242(8) 1 d PDU B 1 Cl1_9 Cl 0.2388(5) -0.1664(4) 0.5150(2) 0.0563(12) Uani 0.758(8) 1 d PDU B 2 O1_9 O 0.2447(9) -0.2297(8) 0.5664(5) 0.107(3) Uani 0.758(8) 1 d PDU B 2 O2_9 O 0.1229(8) -0.1251(9) 0.5068(5) 0.089(4) Uani 0.758(8) 1 d PDU B 2 O3_9 O 0.3272(7) -0.0977(6) 0.5264(3) 0.079(3) Uani 0.758(8) 1 d PDU B 2 O4_9 O 0.2642(7) -0.2083(6) 0.4538(3) 0.075(3) Uani 0.758(8) 1 d PDU B 2 Cl1_10 Cl 0.3038(4) 0.1904(3) 0.55705(18) 0.0525(9) Uani 0.827(10) 1 d PDU A 2 O1_10 O 0.2423(8) 0.1049(5) 0.5559(4) 0.091(3) Uani 0.827(10) 1 d PDU A 2 O2_10 O 0.3489(8) 0.2091(6) 0.6211(3) 0.073(2) Uani 0.827(10) 1 d PDU A 2 O3_10 O 0.4058(7) 0.1835(8) 0.5163(4) 0.074(3) Uani 0.827(10) 1 d PDU A 2 O4_10 O 0.2259(9) 0.2612(7) 0.5344(5) 0.107(3) Uani 0.827(10) 1 d PDU A 2 Cl1_11 Cl 0.7579(8) -0.5169(3) 1.2410(5) 0.090(2) Uani 0.50 1 d PDU . 1 O1_11 O 0.7274(15) -0.5434(12) 1.1764(6) 0.136(5) Uani 0.50 1 d PDU . 1 O2_11 O 0.8835(8) -0.5011(9) 1.2479(7) 0.094(4) Uani 0.50 1 d PDU . 1 O3_11 O 0.6968(12) -0.4376(7) 1.2604(8) 0.117(5) Uani 0.50 1 d PDU . 1 O4_11 O 0.7264(12) -0.5907(7) 1.2840(6) 0.098(4) Uani 0.50 1 d PDU . 1 Cl1_12 Cl 0.7448(10) -0.5718(3) 0.7430(6) 0.094(2) Uani 0.50 1 d PDU . 1 O1_12 O 0.6640(14) -0.5017(8) 0.7219(9) 0.114(4) Uani 0.50 1 d PDU . 1 O2_12 O 0.7267(14) -0.6512(6) 0.7037(7) 0.094(4) Uani 0.50 1 d PDU . 1 O3_12 O 0.7212(16) -0.5938(11) 0.8088(7) 0.120(5) Uani 0.50 1 d PDU . 1 O4_12 O 0.8669(10) -0.5420(9) 0.7419(9) 0.102(4) Uani 0.50 1 d PDU . 1 Cl1_13 Cl 0.5000 -0.5000 1.0000 0.086(4) Uani 0.322(18) 2 d SPDU . 1 O1_13 O 0.574(3) -0.511(2) 1.0577(10) 0.088(4) Uani 0.161(9) 1 d PDU . 1 O2_13 O 0.435(3) -0.4165(13) 1.0048(16) 0.083(5) Uani 0.161(9) 1 d PDU . 1 O3_13 O 0.418(3) -0.5746(17) 0.9933(18) 0.092(5) Uani 0.161(9) 1 d PDU . 1 O4_13 O 0.576(3) -0.497(2) 0.9464(12) 0.085(4) Uani 0.161(9) 1 d PDU . 1 Cl1_14 Cl 0.5495(13) -0.5145(6) 1.0033(4) 0.080(3) Uani 0.339(9) 1 d PDU . -1 O1_14 O 0.491(2) -0.4819(11) 1.0591(7) 0.081(4) Uani 0.339(9) 1 d PDU . -1 O2_14 O 0.609(2) -0.5984(9) 1.0193(9) 0.092(4) Uani 0.339(9) 1 d PDU . -1 O3_14 O 0.6306(17) -0.4492(11) 0.9793(10) 0.090(4) Uani 0.339(9) 1 d PDU . -1 O4_14 O 0.4582(18) -0.5353(14) 0.9541(9) 0.094(4) Uani 0.339(9) 1 d PDU . -1 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 Fe1 0.0200(4) 0.0174(3) 0.0214(4) -0.0032(3) 0.0038(3) -0.0004(3) Fe2 0.0220(4) 0.0189(3) 0.0159(3) 0.0019(3) -0.0018(3) -0.0007(3) Cl1 0.0229(9) 0.0453(11) 0.0306(9) 0.000 0.0032(7) 0.000 P1 0.0219(7) 0.0214(6) 0.0213(6) 0.0038(5) 0.0009(5) 0.0053(5) P2 0.0203(6) 0.0175(6) 0.0214(6) 0.0029(5) -0.0013(5) -0.0039(5) O1 0.054(3) 0.060(3) 0.025(2) 0.001(2) 0.006(2) 0.008(2) O1W 0.065(12) 0.037(5) 0.12(2) -0.009(7) 0.018(10) 0.004(6) O2 0.054(3) 0.020(2) 0.064(3) 0.005(2) 0.004(2) 0.0037(19) O3 0.023(2) 0.045(2) 0.044(2) 0.016(2) 0.0035(18) 0.0057(18) O4 0.022(2) 0.039(2) 0.0293(19) 0.0080(17) -0.0019(15) -0.0016(17) O5 0.039(2) 0.057(3) 0.0229(19) 0.0101(19) -0.0003(17) -0.020(2) O6 0.043(3) 0.0188(19) 0.082(4) 0.003(2) 0.005(3) -0.0027(18) N1 0.159(7) 0.061(4) 0.093(5) 0.011(4) 0.025(5) 0.037(5) N2 0.044(3) 0.030(2) 0.041(3) 0.004(2) -0.008(2) -0.003(2) C1 0.041(4) 0.042(3) 0.052(4) 0.019(3) -0.012(3) 0.005(3) C2 0.090(5) 0.046(4) 0.048(4) 0.014(3) -0.010(4) 0.017(4) C3 0.097(6) 0.071(5) 0.097(6) 0.038(5) -0.014(5) -0.009(5) C4 0.136(8) 0.070(5) 0.106(7) 0.032(5) -0.025(6) -0.007(6) C5 0.180(9) 0.046(5) 0.099(7) 0.015(5) 0.004(7) 0.006(6) C6 0.184(9) 0.057(5) 0.113(7) 0.006(5) 0.022(7) 0.032(6) C7 0.025(3) 0.026(3) 0.027(3) 0.004(2) 0.006(2) -0.001(2) C8 0.023(2) 0.027(2) 0.029(2) 0.004(2) 0.005(2) -0.007(2) C9 0.039(3) 0.038(3) 0.037(3) 0.005(3) -0.003(3) -0.013(3) C10 0.052(4) 0.042(3) 0.049(4) -0.012(3) 0.002(3) -0.021(3) C11 0.052(4) 0.027(3) 0.072(4) -0.005(3) 0.003(3) -0.010(3) C12 0.059(4) 0.030(3) 0.068(4) 0.010(3) -0.013(4) 0.000(3) O1_1 0.047(3) 0.025(2) 0.059(3) -0.013(2) 0.008(2) 0.005(2) O1_2 0.023(2) 0.042(3) 0.058(3) -0.010(2) 0.001(2) 0.0002(19) O1_3 0.039(3) 0.068(3) 0.025(2) 0.001(2) 0.0065(19) -0.010(2) O1_4 0.041(3) 0.072(3) 0.019(2) 0.007(2) -0.0030(18) -0.013(3) O1_5 0.034(2) 0.021(2) 0.064(3) 0.012(2) 0.000(2) 0.0025(18) O1_6 0.023(2) 0.044(2) 0.035(2) 0.0110(19) -0.0021(17) -0.0044(19) Cl1_7 0.060(6) 0.085(6) 0.051(6) -0.011(5) 0.013(5) 0.016(6) O1_7 0.080(12) 0.099(12) 0.078(12) -0.015(12) -0.011(12) 0.035(12) O2_7 0.073(11) 0.103(11) 0.052(10) 0.002(10) 0.016(10) 0.005(10) O3_7 0.062(12) 0.099(13) 0.062(12) -0.012(12) 0.016(11) -0.005(12) O4_7 0.065(11) 0.112(11) 0.063(10) -0.004(10) -0.004(10) 0.009(11) Cl1_8 0.040(5) 0.069(5) 0.046(5) 0.019(4) -0.002(4) -0.012(4) O1_8 0.077(10) 0.114(11) 0.071(10) 0.018(10) 0.020(9) -0.038(10) O2_8 0.028(9) 0.074(11) 0.055(10) 0.022(9) 0.010(8) -0.012(8) O3_8 0.084(11) 0.082(11) 0.078(11) -0.009(10) 0.000(10) -0.029(10) O4_8 0.088(10) 0.108(11) 0.052(9) 0.005(9) -0.036(9) -0.018(10) Cl1_9 0.0390(16) 0.094(3) 0.0354(15) 0.0189(16) -0.0042(12) -0.0366(17) O1_9 0.089(6) 0.144(8) 0.086(6) 0.063(6) -0.006(5) -0.035(6) O2_9 0.078(7) 0.134(9) 0.055(6) -0.027(6) -0.009(5) 0.002(6) O3_9 0.078(5) 0.122(6) 0.036(4) 0.003(4) -0.003(3) -0.063(5) O4_9 0.048(4) 0.107(7) 0.070(5) -0.003(5) 0.003(4) -0.023(4) Cl1_10 0.0396(14) 0.090(2) 0.0278(11) -0.0012(13) 0.0031(10) 0.0139(14) O1_10 0.074(5) 0.121(7) 0.082(5) -0.012(5) 0.030(4) -0.022(5) O2_10 0.090(6) 0.095(6) 0.034(3) -0.006(4) 0.003(3) -0.004(5) O3_10 0.068(5) 0.100(6) 0.056(5) -0.025(4) 0.031(4) -0.013(4) O4_10 0.095(6) 0.131(7) 0.090(6) -0.011(6) -0.035(5) 0.060(6) Cl1_11 0.045(3) 0.071(2) 0.152(6) -0.053(4) -0.035(3) 0.013(4) O1_11 0.080(8) 0.160(10) 0.165(11) -0.048(9) -0.030(8) -0.026(8) O2_11 0.050(6) 0.082(7) 0.144(9) -0.016(7) -0.048(7) -0.004(6) O3_11 0.083(8) 0.085(8) 0.181(10) 0.002(8) -0.002(9) 0.044(7) O4_11 0.068(7) 0.042(6) 0.185(11) -0.020(7) 0.007(8) -0.009(6) Cl1_12 0.074(3) 0.0406(17) 0.171(6) -0.008(4) 0.048(3) 0.028(4) O1_12 0.095(8) 0.059(7) 0.188(11) -0.018(8) -0.001(8) 0.039(7) O2_12 0.112(9) 0.037(5) 0.134(9) -0.005(6) 0.015(8) 0.023(6) O3_12 0.096(9) 0.107(9) 0.159(11) -0.007(9) 0.013(9) -0.002(8) O4_12 0.072(7) 0.052(7) 0.186(11) 0.022(7) 0.054(8) 0.007(6) Cl1_13 0.157(10) 0.042(5) 0.060(4) 0.010(4) 0.036(6) -0.007(5) O1_13 0.150(10) 0.047(6) 0.069(6) 0.015(6) 0.037(7) 0.003(7) O2_13 0.154(12) 0.040(8) 0.059(8) 0.010(8) 0.041(9) -0.006(9) O3_13 0.161(12) 0.051(9) 0.068(9) 0.006(8) 0.029(9) -0.008(9) O4_13 0.150(10) 0.047(6) 0.062(6) 0.014(6) 0.038(7) 0.001(7) Cl1_14 0.138(8) 0.042(3) 0.063(3) 0.022(3) 0.041(5) 0.014(4) O1_14 0.152(10) 0.043(6) 0.053(5) 0.016(5) 0.050(7) -0.003(6) O2_14 0.145(11) 0.054(7) 0.079(8) 0.018(7) 0.034(8) 0.010(8) O3_14 0.151(10) 0.051(6) 0.070(6) 0.020(6) 0.035(7) 0.002(7) O4_14 0.158(10) 0.059(6) 0.068(6) 0.006(6) 0.026(7) -0.007(7) _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 Fe1 O6 1.888(4) . ? Fe1 O1 1.917(4) . ? Fe1 O3 1.939(4) 2_656 ? Fe1 O1_1 2.061(4) . ? Fe1 O1_2 2.076(4) . ? Fe1 O1_3 2.081(4) . ? Fe2 O2 1.897(4) 2_656 ? Fe2 O5 1.901(4) 2_656 ? Fe2 O4 1.952(4) . ? Fe2 O1_4 2.055(4) . ? Fe2 O1_5 2.093(4) . ? Fe2 O1_6 2.106(4) . ? P1 O2 1.494(4) . ? P1 O1 1.507(4) . ? P1 O3 1.524(4) . ? P1 C1 1.814(6) . ? P2 O6 1.493(4) . ? P2 O5 1.514(4) . ? P2 O4 1.518(4) . ? P2 C7 1.826(5) . ? O1W O1W 0.79(3) 2_656 ? O2 Fe2 1.897(4) 2_656 ? O3 Fe1 1.939(4) 2_656 ? O5 Fe2 1.901(4) 2_656 ? N1 C6 1.353(14) . ? N1 C2 1.364(12) . ? N1 H1PY 0.8700 . ? N2 C8 1.334(8) . ? N2 C12 1.346(9) . ? N2 H2PY 0.77(8) . ? C1 C2 1.449(11) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 C3 1.335(15) . ? C3 C4 1.435(15) . ? C3 H3A 0.9400 . ? C4 C5 1.388(19) . ? C4 H4A 0.9400 . ? C5 C6 1.303(19) . ? C5 H5A 0.9400 . ? C6 H6A 0.9400 . ? C7 C8 1.485(7) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.383(8) . ? C9 C10 1.390(9) . ? C9 H9A 0.9400 . ? C10 C11 1.366(11) . ? C10 H10A 0.9400 . ? C11 C12 1.365(11) . ? C11 H11A 0.9400 . ? C12 H12A 0.9400 . ? O1_1 H1_1 0.836(11) . ? O1_1 H2_1 0.836(11) . ? O1_2 H1_2 0.840(11) . ? O1_2 H2_2 0.838(11) . ? O1_3 H1_3 0.837(11) . ? O1_3 H2_3 0.837(11) . ? O1_4 H1_4 0.839(11) . ? O1_4 H2_4 0.839(11) . ? O1_5 H1_5 0.838(11) . ? O1_5 H2_5 0.839(11) . ? O1_6 H1_6 0.837(11) . ? O1_6 H2_6 0.840(11) . ? Cl1_7 O2_7 1.418(8) . ? Cl1_7 O4_7 1.418(8) . ? Cl1_7 O3_7 1.420(8) . ? Cl1_7 O1_7 1.421(8) . ? Cl1_8 O4_8 1.410(8) . ? Cl1_8 O1_8 1.415(8) . ? Cl1_8 O2_8 1.422(8) . ? Cl1_8 O3_8 1.423(8) . ? Cl1_9 O1_9 1.405(6) . ? Cl1_9 O3_9 1.411(6) . ? Cl1_9 O2_9 1.418(6) . ? Cl1_9 O4_9 1.442(6) . ? Cl1_10 O4_10 1.409(6) . ? Cl1_10 O1_10 1.418(6) . ? Cl1_10 O2_10 1.418(6) . ? Cl1_10 O3_10 1.439(6) . ? Cl1_11 Cl1_11 0.42(2) 2_657 ? Cl1_11 O4_11 1.208(11) 2_657 ? Cl1_11 O3_11 1.259(10) 2_657 ? Cl1_11 O3_11 1.405(7) . ? Cl1_11 O2_11 1.408(7) . ? Cl1_11 O1_11 1.415(7) . ? Cl1_11 O4_11 1.446(7) . ? Cl1_11 O2_11 1.605(17) 2_657 ? Cl1_11 O1_11 1.751(19) 2_657 ? O1_11 O4_11 1.17(2) 2_657 ? O1_11 Cl1_11 1.751(19) 2_657 ? O2_11 O3_11 1.288(19) 2_657 ? O2_11 Cl1_11 1.605(17) 2_657 ? O3_11 Cl1_11 1.259(10) 2_657 ? O3_11 O3_11 1.27(3) 2_657 ? O3_11 O2_11 1.288(19) 2_657 ? O4_11 O1_11 1.17(2) 2_657 ? O4_11 Cl1_11 1.208(11) 2_657 ? O4_11 O4_11 1.52(3) 2_657 ? Cl1_12 Cl1_12 0.31(3) 2_656 ? Cl1_12 O3_12 1.19(2) 2_656 ? Cl1_12 O4_12 1.357(18) 2_656 ? Cl1_12 O1_12 1.412(7) . ? Cl1_12 O4_12 1.418(7) . ? Cl1_12 O2_12 1.421(7) . ? Cl1_12 O3_12 1.432(8) . ? Cl1_12 O1_12 1.587(18) 2_656 ? Cl1_12 O2_12 1.618(17) 2_656 ? O1_12 O4_12 1.02(2) 2_656 ? O1_12 Cl1_12 1.587(18) 2_656 ? O2_12 O3_12 1.05(2) 2_656 ? O2_12 Cl1_12 1.618(17) 2_656 ? O3_12 O2_12 1.05(2) 2_656 ? O3_12 Cl1_12 1.19(2) 2_656 ? O3_12 O4_12 1.59(2) 2_656 ? O4_12 O1_12 1.02(2) 2_656 ? O4_12 Cl1_12 1.357(18) 2_656 ? O4_12 O3_12 1.59(2) 2_656 ? Cl1_13 Cl1_14 0.587(14) . ? Cl1_13 O4_14 1.157(14) . ? Cl1_13 O1_14 1.257(12) . ? Cl1_13 O3_13 1.418(8) 3_647 ? Cl1_13 O2_13 1.418(8) . ? Cl1_13 O3_13 1.418(8) . ? Cl1_13 O2_13 1.418(8) 3_647 ? Cl1_13 O4_13 1.419(8) 3_647 ? Cl1_13 O4_13 1.419(8) . ? Cl1_13 O1_13 1.427(8) . ? Cl1_13 O1_13 1.427(8) 3_647 ? Cl1_13 O3_14 1.693(13) . ? O1_13 O1_14 1.02(4) . ? O1_13 Cl1_14 1.145(17) . ? O1_13 O2_14 1.55(4) . ? O1_13 O3_13 1.64(2) 3_647 ? O1_13 O4_13 1.66(2) 3_647 ? O1_13 O2_13 1.66(2) 3_647 ? O2_13 O1_14 1.58(3) . ? O2_13 O4_13 1.62(2) 3_647 ? O2_13 O3_13 1.63(2) 3_647 ? O2_13 O1_13 1.66(2) 3_647 ? O2_13 Cl1_14 1.908(16) . ? O3_13 O4_14 1.10(3) . ? O3_13 O4_13 1.63(2) 3_647 ? O3_13 O2_13 1.63(2) 3_647 ? O3_13 O1_13 1.64(2) 3_647 ? O3_13 Cl1_14 1.70(2) . ? O4_13 O3_14 1.13(4) . ? O4_13 Cl1_14 1.249(17) . ? O4_13 O4_14 1.43(3) . ? O4_13 O2_13 1.62(2) 3_647 ? O4_13 O3_13 1.63(2) 3_647 ? O4_13 O1_13 1.66(2) 3_647 ? Cl1_14 O3_14 1.411(7) . ? Cl1_14 O2_14 1.419(7) . ? Cl1_14 O1_14 1.426(7) . ? Cl1_14 O4_14 1.433(8) . ? 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 O6 Fe1 O1 97.7(2) . . ? O6 Fe1 O3 98.2(2) . 2_656 ? O1 Fe1 O3 98.3(2) . 2_656 ? O6 Fe1 O1_1 169.7(2) . . ? O1 Fe1 O1_1 86.2(2) . . ? O3 Fe1 O1_1 90.6(2) 2_656 . ? O6 Fe1 O1_2 88.0(2) . . ? O1 Fe1 O1_2 92.3(2) . . ? O3 Fe1 O1_2 166.86(19) 2_656 . ? O1_1 Fe1 O1_2 82.3(2) . . ? O6 Fe1 O1_3 91.4(2) . . ? O1 Fe1 O1_3 169.4(2) . . ? O3 Fe1 O1_3 85.64(19) 2_656 . ? O1_1 Fe1 O1_3 83.9(2) . . ? O1_2 Fe1 O1_3 82.6(2) . . ? O2 Fe2 O5 98.1(2) 2_656 2_656 ? O2 Fe2 O4 100.2(2) 2_656 . ? O5 Fe2 O4 97.44(19) 2_656 . ? O2 Fe2 O1_4 89.6(2) 2_656 . ? O5 Fe2 O1_4 168.4(2) 2_656 . ? O4 Fe2 O1_4 89.52(18) . . ? O2 Fe2 O1_5 170.8(2) 2_656 . ? O5 Fe2 O1_5 88.2(2) 2_656 . ? O4 Fe2 O1_5 85.55(18) . . ? O1_4 Fe2 O1_5 83.1(2) . . ? O2 Fe2 O1_6 90.7(2) 2_656 . ? O5 Fe2 O1_6 88.54(18) 2_656 . ? O4 Fe2 O1_6 166.62(17) . . ? O1_4 Fe2 O1_6 82.80(18) . . ? O1_5 Fe2 O1_6 82.67(18) . . ? O2 P1 O1 114.5(3) . . ? O2 P1 O3 112.3(3) . . ? O1 P1 O3 112.1(3) . . ? O2 P1 C1 105.4(3) . . ? O1 P1 C1 106.2(3) . . ? O3 P1 C1 105.5(3) . . ? O6 P2 O5 112.7(3) . . ? O6 P2 O4 113.5(3) . . ? O5 P2 O4 110.3(3) . . ? O6 P2 C7 105.9(3) . . ? O5 P2 C7 105.9(3) . . ? O4 P2 C7 108.0(2) . . ? P1 O1 Fe1 150.8(3) . . ? P1 O2 Fe2 165.9(4) . 2_656 ? P1 O3 Fe1 140.3(3) . 2_656 ? P2 O4 Fe2 138.8(2) . . ? P2 O5 Fe2 152.8(3) . 2_656 ? P2 O6 Fe1 169.0(4) . . ? C6 N1 C2 123.9(12) . . ? C6 N1 H1PY 118.1 . . ? C2 N1 H1PY 118.1 . . ? C8 N2 C12 125.0(6) . . ? C8 N2 H2PY 121(6) . . ? C12 N2 H2PY 114(6) . . ? C2 C1 P1 117.9(6) . . ? C2 C1 H1A 107.8 . . ? P1 C1 H1A 107.8 . . ? C2 C1 H1B 107.8 . . ? P1 C1 H1B 107.8 . . ? H1A C1 H1B 107.2 . . ? C3 C2 N1 117.7(9) . . ? C3 C2 C1 126.0(9) . . ? N1 C2 C1 116.2(9) . . ? C2 C3 C4 119.1(13) . . ? C2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? C5 C4 C3 119.1(13) . . ? C5 C4 H4A 120.5 . . ? C3 C4 H4A 120.5 . . ? C6 C5 C4 119.8(11) . . ? C6 C5 H5A 120.1 . . ? C4 C5 H5A 120.1 . . ? C5 C6 N1 120.0(13) . . ? C5 C6 H6A 120.0 . . ? N1 C6 H6A 120.0 . . ? C8 C7 P2 113.0(4) . . ? C8 C7 H7A 109.0 . . ? P2 C7 H7A 109.0 . . ? C8 C7 H7B 109.0 . . ? P2 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? N2 C8 C9 116.8(5) . . ? N2 C8 C7 118.4(5) . . ? C9 C8 C7 124.7(5) . . ? C8 C9 C10 119.9(6) . . ? C8 C9 H9A 120.1 . . ? C10 C9 H9A 120.1 . . ? C11 C10 C9 120.3(7) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C12 C11 C10 119.2(6) . . ? C12 C11 H11A 120.4 . . ? C10 C11 H11A 120.4 . . ? N2 C12 C11 118.7(7) . . ? N2 C12 H12A 120.6 . . ? C11 C12 H12A 120.6 . . ? Fe1 O1_1 H1_1 95(6) . . ? Fe1 O1_1 H2_1 125(6) . . ? H1_1 O1_1 H2_1 105(4) . . ? Fe1 O1_2 H1_2 121(5) . . ? Fe1 O1_2 H2_2 120(5) . . ? H1_2 O1_2 H2_2 104(4) . . ? Fe1 O1_3 H1_3 120(5) . . ? Fe1 O1_3 H2_3 126(5) . . ? H1_3 O1_3 H2_3 105(4) . . ? Fe2 O1_4 H1_4 115(6) . . ? Fe2 O1_4 H2_4 122(6) . . ? H1_4 O1_4 H2_4 104(4) . . ? Fe2 O1_5 H1_5 123(5) . . ? Fe2 O1_5 H2_5 127(5) . . ? H1_5 O1_5 H2_5 104(4) . . ? Fe2 O1_6 H1_6 96(5) . . ? Fe2 O1_6 H2_6 122(5) . . ? H1_6 O1_6 H2_6 105(4) . . ? O2_7 Cl1_7 O4_7 109.0(11) . . ? O2_7 Cl1_7 O3_7 109.2(11) . . ? O4_7 Cl1_7 O3_7 110.6(11) . . ? O2_7 Cl1_7 O1_7 108.9(11) . . ? O4_7 Cl1_7 O1_7 109.5(11) . . ? O3_7 Cl1_7 O1_7 109.6(11) . . ? O4_8 Cl1_8 O1_8 111.6(11) . . ? O4_8 Cl1_8 O2_8 109.8(10) . . ? O1_8 Cl1_8 O2_8 110.6(10) . . ? O4_8 Cl1_8 O3_8 109.1(10) . . ? O1_8 Cl1_8 O3_8 108.6(10) . . ? O2_8 Cl1_8 O3_8 107.0(10) . . ? O1_9 Cl1_9 O3_9 109.3(6) . . ? O1_9 Cl1_9 O2_9 112.3(6) . . ? O3_9 Cl1_9 O2_9 109.6(7) . . ? O1_9 Cl1_9 O4_9 112.3(7) . . ? O3_9 Cl1_9 O4_9 106.6(5) . . ? O2_9 Cl1_9 O4_9 106.5(5) . . ? O4_10 Cl1_10 O1_10 110.6(6) . . ? O4_10 Cl1_10 O2_10 110.7(6) . . ? O1_10 Cl1_10 O2_10 109.4(6) . . ? O4_10 Cl1_10 O3_10 109.9(6) . . ? O1_10 Cl1_10 O3_10 108.4(5) . . ? O2_10 Cl1_10 O3_10 107.8(5) . . ? Cl1_11 Cl1_11 O4_11 117.0(9) 2_657 2_657 ? Cl1_11 Cl1_11 O3_11 101.6(14) 2_657 2_657 ? O4_11 Cl1_11 O3_11 137.8(15) 2_657 2_657 ? Cl1_11 Cl1_11 O3_11 61.4(11) 2_657 . ? O4_11 Cl1_11 O3_11 159.0(12) 2_657 . ? O3_11 Cl1_11 O3_11 56.6(13) 2_657 . ? Cl1_11 Cl1_11 O2_11 111(3) 2_657 . ? O4_11 Cl1_11 O2_11 91.6(10) 2_657 . ? O3_11 Cl1_11 O2_11 57.4(10) 2_657 . ? O3_11 Cl1_11 O2_11 108.7(8) . . ? Cl1_11 Cl1_11 O1_11 139(3) 2_657 . ? O4_11 Cl1_11 O1_11 52.2(11) 2_657 . ? O3_11 Cl1_11 O1_11 107.8(14) 2_657 . ? O3_11 Cl1_11 O1_11 113.4(9) . . ? O2_11 Cl1_11 O1_11 109.4(9) . . ? Cl1_11 Cl1_11 O4_11 48.1(6) 2_657 . ? O4_11 Cl1_11 O4_11 69.2(12) 2_657 . ? O3_11 Cl1_11 O4_11 143.3(13) 2_657 . ? O3_11 Cl1_11 O4_11 107.7(8) . . ? O2_11 Cl1_11 O4_11 108.7(9) . . ? O1_11 Cl1_11 O4_11 108.9(9) . . ? Cl1_11 Cl1_11 O2_11 55(2) 2_657 2_657 ? O4_11 Cl1_11 O2_11 110.4(9) 2_657 2_657 ? O3_11 Cl1_11 O2_11 105.2(9) 2_657 2_657 ? O3_11 Cl1_11 O2_11 50.1(8) . 2_657 ? O2_11 Cl1_11 O2_11 157.4(9) . 2_657 ? O1_11 Cl1_11 O2_11 89.0(9) . 2_657 ? O4_11 Cl1_11 O2_11 75.9(8) . 2_657 ? Cl1_11 Cl1_11 O1_11 32(2) 2_657 2_657 ? O4_11 Cl1_11 O1_11 102.2(10) 2_657 2_657 ? O3_11 Cl1_11 O1_11 101.8(11) 2_657 2_657 ? O3_11 Cl1_11 O1_11 85.8(10) . 2_657 ? O2_11 Cl1_11 O1_11 83.6(9) . 2_657 ? O1_11 Cl1_11 O1_11 150.1(13) . 2_657 ? O4_11 Cl1_11 O1_11 41.6(8) . 2_657 ? O2_11 Cl1_11 O1_11 86.6(9) 2_657 2_657 ? O4_11 O1_11 Cl1_11 54.7(7) 2_657 . ? O4_11 O1_11 Cl1_11 55.1(8) 2_657 2_657 ? Cl1_11 O1_11 Cl1_11 9.1(6) . 2_657 ? O3_11 O2_11 Cl1_11 55.5(6) 2_657 . ? O3_11 O2_11 Cl1_11 56.8(7) 2_657 2_657 ? Cl1_11 O2_11 Cl1_11 14.1(8) . 2_657 ? Cl1_11 O3_11 O3_11 67.5(8) 2_657 2_657 ? Cl1_11 O3_11 O2_11 67.1(7) 2_657 2_657 ? O3_11 O3_11 O2_11 126.7(12) 2_657 2_657 ? Cl1_11 O3_11 Cl1_11 17.0(9) 2_657 . ? O3_11 O3_11 Cl1_11 55.9(7) 2_657 . ? O2_11 O3_11 Cl1_11 73.0(9) 2_657 . ? O1_11 O4_11 Cl1_11 73.1(8) 2_657 2_657 ? O1_11 O4_11 Cl1_11 83.3(11) 2_657 . ? Cl1_11 O4_11 Cl1_11 14.9(8) 2_657 . ? O1_11 O4_11 O4_11 119.3(14) 2_657 2_657 ? Cl1_11 O4_11 O4_11 62.8(9) 2_657 2_657 ? Cl1_11 O4_11 O4_11 48.0(5) . 2_657 ? Cl1_12 Cl1_12 O3_12 137(4) 2_656 2_656 ? Cl1_12 Cl1_12 O4_12 95(4) 2_656 2_656 ? O3_12 Cl1_12 O4_12 128.1(18) 2_656 2_656 ? Cl1_12 Cl1_12 O1_12 120(2) 2_656 . ? O3_12 Cl1_12 O1_12 97.9(13) 2_656 . ? O4_12 Cl1_12 O1_12 43.2(9) 2_656 . ? Cl1_12 Cl1_12 O4_12 72(4) 2_656 . ? O3_12 Cl1_12 O4_12 74.4(11) 2_656 . ? O4_12 Cl1_12 O4_12 141.4(11) 2_656 . ? O1_12 Cl1_12 O4_12 111.3(8) . . ? Cl1_12 Cl1_12 O2_12 125.2(7) 2_656 . ? O3_12 Cl1_12 O2_12 46.5(10) 2_656 . ? O4_12 Cl1_12 O2_12 106.5(11) 2_656 . ? O1_12 Cl1_12 O2_12 110.0(9) . . ? O4_12 Cl1_12 O2_12 110.5(9) . . ? Cl1_12 Cl1_12 O3_12 35(3) 2_656 . ? O3_12 Cl1_12 O3_12 150.3(15) 2_656 . ? O4_12 Cl1_12 O3_12 69.4(11) 2_656 . ? O1_12 Cl1_12 O3_12 108.4(9) . . ? O4_12 Cl1_12 O3_12 107.2(9) . . ? O2_12 Cl1_12 O3_12 109.5(9) . . ? Cl1_12 Cl1_12 O1_12 51(2) 2_656 2_656 ? O3_12 Cl1_12 O1_12 111.3(13) 2_656 2_656 ? O4_12 Cl1_12 O1_12 104.8(10) 2_656 2_656 ? O1_12 Cl1_12 O1_12 93.2(12) . 2_656 ? O4_12 Cl1_12 O1_12 39.2(8) . 2_656 ? O2_12 Cl1_12 O1_12 148.7(11) . 2_656 ? O3_12 Cl1_12 O1_12 81.3(11) . 2_656 ? Cl1_12 Cl1_12 O2_12 45.9(7) 2_656 2_656 ? O3_12 Cl1_12 O2_12 111.0(10) 2_656 2_656 ? O4_12 Cl1_12 O2_12 102.9(11) 2_656 2_656 ? O1_12 Cl1_12 O2_12 145.9(11) . 2_656 ? O4_12 Cl1_12 O2_12 94.1(10) . 2_656 ? O2_12 Cl1_12 O2_12 79.9(10) . 2_656 ? O3_12 Cl1_12 O2_12 39.8(9) . 2_656 ? O1_12 Cl1_12 O2_12 92.8(12) 2_656 2_656 ? O4_12 O1_12 Cl1_12 65.5(10) 2_656 . ? O4_12 O1_12 Cl1_12 61.4(9) 2_656 2_656 ? Cl1_12 O1_12 Cl1_12 9.7(8) . 2_656 ? O3_12 O2_12 Cl1_12 55.3(12) 2_656 . ? O3_12 O2_12 Cl1_12 60.6(7) 2_656 2_656 ? Cl1_12 O2_12 Cl1_12 8.9(7) . 2_656 ? O2_12 O3_12 Cl1_12 78.2(14) 2_656 2_656 ? O2_12 O3_12 Cl1_12 79.6(12) 2_656 . ? Cl1_12 O3_12 Cl1_12 8.5(10) 2_656 . ? O2_12 O3_12 O4_12 122.6(18) 2_656 2_656 ? Cl1_12 O3_12 O4_12 59.2(9) 2_656 2_656 ? Cl1_12 O3_12 O4_12 53.1(8) . 2_656 ? O1_12 O4_12 Cl1_12 71.3(11) 2_656 2_656 ? O1_12 O4_12 Cl1_12 79.4(11) 2_656 . ? Cl1_12 O4_12 Cl1_12 12.5(11) 2_656 . ? O1_12 O4_12 O3_12 122.7(15) 2_656 2_656 ? Cl1_12 O4_12 O3_12 57.5(7) 2_656 2_656 ? Cl1_12 O4_12 O3_12 46.3(8) . 2_656 ? Cl1_14 Cl1_13 O4_14 105.8(13) . . ? Cl1_14 Cl1_13 O1_14 94.2(14) . . ? O4_14 Cl1_13 O1_14 147.5(12) . . ? Cl1_14 Cl1_13 O3_13 71.1(18) . 3_647 ? O4_14 Cl1_13 O3_13 130.7(16) . 3_647 ? O1_14 Cl1_13 O3_13 79.7(15) . 3_647 ? Cl1_14 Cl1_13 O2_13 140.5(18) . . ? O4_14 Cl1_13 O2_13 104.7(16) . . ? O1_14 Cl1_13 O2_13 72.0(16) . . ? O3_13 Cl1_13 O2_13 70.1(11) 3_647 . ? Cl1_14 Cl1_13 O3_13 108.9(18) . . ? O4_14 Cl1_13 O3_13 49.3(16) . . ? O1_14 Cl1_13 O3_13 100.3(15) . . ? O3_13 Cl1_13 O3_13 180.000(3) 3_647 . ? O2_13 Cl1_13 O3_13 109.9(11) . . ? Cl1_14 Cl1_13 O2_13 39.5(18) . 3_647 ? O4_14 Cl1_13 O2_13 75.3(16) . 3_647 ? O1_14 Cl1_13 O2_13 108.0(16) . 3_647 ? O3_13 Cl1_13 O2_13 109.9(11) 3_647 3_647 ? O2_13 Cl1_13 O2_13 180(3) . 3_647 ? O3_13 Cl1_13 O2_13 70.1(11) . 3_647 ? Cl1_14 Cl1_13 O4_13 118.6(15) . 3_647 ? O4_14 Cl1_13 O4_13 113.5(19) . 3_647 ? O1_14 Cl1_13 O4_13 34.3(16) . 3_647 ? O3_13 Cl1_13 O4_13 110.0(10) 3_647 3_647 ? O2_13 Cl1_13 O4_13 69.4(10) . 3_647 ? O3_13 Cl1_13 O4_13 70.0(10) . 3_647 ? O2_13 Cl1_13 O4_13 110.6(10) 3_647 3_647 ? Cl1_14 Cl1_13 O4_13 61.4(15) . . ? O4_14 Cl1_13 O4_13 66.5(18) . . ? O1_14 Cl1_13 O4_13 145.7(17) . . ? O3_13 Cl1_13 O4_13 70.0(10) 3_647 . ? O2_13 Cl1_13 O4_13 110.6(10) . . ? O3_13 Cl1_13 O4_13 110.0(10) . . ? O2_13 Cl1_13 O4_13 69.4(10) 3_647 . ? O4_13 Cl1_13 O4_13 180(3) 3_647 . ? Cl1_14 Cl1_13 O1_13 50.3(15) . . ? O4_14 Cl1_13 O1_13 145.8(14) . . ? O1_14 Cl1_13 O1_13 43.9(17) . . ? O3_13 Cl1_13 O1_13 70.5(10) 3_647 . ? O2_13 Cl1_13 O1_13 108.4(10) . . ? O3_13 Cl1_13 O1_13 109.5(10) . . ? O2_13 Cl1_13 O1_13 71.6(10) 3_647 . ? O4_13 Cl1_13 O1_13 71.6(11) 3_647 . ? O4_13 Cl1_13 O1_13 108.4(11) . . ? Cl1_14 Cl1_13 O1_13 129.7(15) . 3_647 ? O4_14 Cl1_13 O1_13 34.2(14) . 3_647 ? O1_14 Cl1_13 O1_13 136.1(17) . 3_647 ? O3_13 Cl1_13 O1_13 109.5(10) 3_647 3_647 ? O2_13 Cl1_13 O1_13 71.6(10) . 3_647 ? O3_13 Cl1_13 O1_13 70.5(10) . 3_647 ? O2_13 Cl1_13 O1_13 108.4(10) 3_647 3_647 ? O4_13 Cl1_13 O1_13 108.4(11) 3_647 3_647 ? O4_13 Cl1_13 O1_13 71.6(11) . 3_647 ? O1_13 Cl1_13 O1_13 180.0(19) . 3_647 ? Cl1_14 Cl1_13 O3_14 52.2(10) . . ? O4_14 Cl1_13 O3_14 107.6(10) . . ? O1_14 Cl1_13 O3_14 104.9(11) . . ? O3_13 Cl1_13 O3_14 30.8(14) 3_647 . ? O2_13 Cl1_13 O3_14 94.7(15) . . ? O3_13 Cl1_13 O3_14 149.2(14) . . ? O2_13 Cl1_13 O3_14 85.3(15) 3_647 . ? O4_13 Cl1_13 O3_14 138.4(15) 3_647 . ? O4_13 Cl1_13 O3_14 41.6(15) . . ? O1_13 Cl1_13 O3_14 78.2(15) . . ? O1_13 Cl1_13 O3_14 101.8(15) 3_647 . ? O1_14 O1_13 Cl1_14 82.4(14) . . ? O1_14 O1_13 Cl1_13 59.2(10) . . ? Cl1_14 O1_13 Cl1_13 23.3(7) . . ? O1_14 O1_13 O2_14 127(2) . . ? Cl1_14 O1_13 O2_14 61.4(15) . . ? Cl1_13 O1_13 O2_14 79.3(12) . . ? O1_14 O1_13 O3_13 76.6(18) . 3_647 ? Cl1_14 O1_13 O3_13 54.4(11) . 3_647 ? Cl1_13 O1_13 O3_13 54.5(6) . 3_647 ? O2_14 O1_13 O3_13 105.9(18) . 3_647 ? O1_14 O1_13 O4_13 21.1(18) . 3_647 ? Cl1_14 O1_13 O4_13 76.0(11) . 3_647 ? Cl1_13 O1_13 O4_13 54.0(6) . 3_647 ? O2_14 O1_13 O4_13 107.8(19) . 3_647 ? O3_13 O1_13 O4_13 89.3(11) 3_647 3_647 ? O1_14 O1_13 O2_13 105.3(16) . 3_647 ? Cl1_14 O1_13 O2_13 37.8(9) . 3_647 ? Cl1_13 O1_13 O2_13 54.0(6) . 3_647 ? O2_14 O1_13 O2_13 25.4(12) . 3_647 ? O3_13 O1_13 O2_13 89.3(11) 3_647 3_647 ? O4_13 O1_13 O2_13 89.0(11) 3_647 3_647 ? Cl1_13 O2_13 O1_14 49.3(7) . . ? Cl1_13 O2_13 O4_13 55.3(6) . 3_647 ? O1_14 O2_13 O4_13 29.1(13) . 3_647 ? Cl1_13 O2_13 O3_13 55.0(6) . 3_647 ? O1_14 O2_13 O3_13 64.8(13) . 3_647 ? O4_13 O2_13 O3_13 91.5(11) 3_647 3_647 ? Cl1_13 O2_13 O1_13 54.4(6) . 3_647 ? O1_14 O2_13 O1_13 100.3(10) . 3_647 ? O4_13 O2_13 O1_13 89.5(11) 3_647 3_647 ? O3_13 O2_13 O1_13 89.8(11) 3_647 3_647 ? Cl1_13 O2_13 Cl1_14 11.3(6) . . ? O1_14 O2_13 Cl1_14 47.1(5) . . ? O4_13 O2_13 Cl1_14 59.9(7) 3_647 . ? O3_13 O2_13 Cl1_14 43.9(7) 3_647 . ? O1_13 O2_13 Cl1_14 62.2(7) 3_647 . ? O4_14 O3_13 Cl1_13 52.9(8) . . ? O4_14 O3_13 O4_13 102.9(13) . 3_647 ? Cl1_13 O3_13 O4_13 55.0(6) . 3_647 ? O4_14 O3_13 O2_13 67.9(17) . 3_647 ? Cl1_13 O3_13 O2_13 55.0(6) . 3_647 ? O4_13 O3_13 O2_13 91.5(11) 3_647 3_647 ? O4_14 O3_13 O1_13 25.5(18) . 3_647 ? Cl1_13 O3_13 O1_13 55.0(6) . 3_647 ? O4_13 O3_13 O1_13 89.8(11) 3_647 3_647 ? O2_13 O3_13 O1_13 89.8(11) 3_647 3_647 ? O4_14 O3_13 Cl1_14 56.8(9) . . ? Cl1_13 O3_13 Cl1_14 19.1(5) . . ? O4_13 O3_13 Cl1_14 64.4(8) 3_647 . ? O2_13 O3_13 Cl1_14 36.1(7) 3_647 . ? O1_13 O3_13 Cl1_14 67.5(7) 3_647 . ? O3_14 O4_13 Cl1_14 72.5(16) . . ? O3_14 O4_13 Cl1_13 82.3(13) . . ? Cl1_14 O4_13 Cl1_13 24.4(7) . . ? O3_14 O4_13 O4_14 129.5(12) . . ? Cl1_14 O4_13 O4_14 64.3(11) . . ? Cl1_13 O4_13 O4_14 48.0(9) . . ? O3_14 O4_13 O2_13 99(2) . 3_647 ? Cl1_14 O4_13 O2_13 39.8(9) . 3_647 ? Cl1_13 O4_13 O2_13 55.3(6) . 3_647 ? O4_14 O4_13 O2_13 62.4(13) . 3_647 ? O3_14 O4_13 O3_13 30.5(14) . 3_647 ? Cl1_14 O4_13 O3_13 53.9(10) . 3_647 ? Cl1_13 O4_13 O3_13 55.0(6) . 3_647 ? O4_14 O4_13 O3_13 99.9(12) . 3_647 ? O2_13 O4_13 O3_13 91.4(11) 3_647 3_647 ? O3_14 O4_13 O1_13 119(2) . 3_647 ? Cl1_14 O4_13 O1_13 77.8(10) . 3_647 ? Cl1_13 O4_13 O1_13 54.4(6) . 3_647 ? O4_14 O4_13 O1_13 28.8(12) . 3_647 ? O2_13 O4_13 O1_13 89.4(11) 3_647 3_647 ? O3_13 O4_13 O1_13 89.8(11) 3_647 3_647 ? Cl1_13 Cl1_14 O1_13 106.4(18) . . ? Cl1_13 Cl1_14 O4_13 94.2(17) . . ? O1_13 Cl1_14 O4_13 149(2) . . ? Cl1_13 Cl1_14 O3_14 108.6(12) . . ? O1_13 Cl1_14 O3_14 101.0(19) . . ? O4_13 Cl1_14 O3_14 50.0(18) . . ? Cl1_13 Cl1_14 O2_14 139.1(13) . . ? O1_13 Cl1_14 O2_14 73.6(19) . . ? O4_13 Cl1_14 O2_14 105.3(16) . . ? O3_14 Cl1_14 O2_14 111.5(9) . . ? Cl1_13 Cl1_14 O1_14 61.6(11) . . ? O1_13 Cl1_14 O1_14 44.9(18) . . ? O4_13 Cl1_14 O1_14 145.9(17) . . ? O3_14 Cl1_14 O1_14 112.1(9) . . ? O2_14 Cl1_14 O1_14 108.7(8) . . ? Cl1_13 Cl1_14 O4_14 51.0(12) . . ? O1_13 Cl1_14 O4_14 147(2) . . ? O4_13 Cl1_14 O4_14 63.9(19) . . ? O3_14 Cl1_14 O4_14 109.3(9) . . ? O2_14 Cl1_14 O4_14 106.7(9) . . ? O1_14 Cl1_14 O4_14 108.3(9) . . ? Cl1_13 Cl1_14 O3_13 52.0(16) . . ? O1_13 Cl1_14 O3_13 107.8(15) . . ? O4_13 Cl1_14 O3_13 102.8(15) . . ? O3_14 Cl1_14 O3_13 148.8(14) . . ? O2_14 Cl1_14 O3_13 88.3(16) . . ? O1_14 Cl1_14 O3_13 81.7(15) . . ? O4_14 Cl1_14 O3_13 40.0(13) . . ? Cl1_13 Cl1_14 O2_13 28.2(13) . . ? O1_13 Cl1_14 O2_13 94.9(13) . . ? O4_13 Cl1_14 O2_13 92.9(12) . . ? O3_14 Cl1_14 O2_13 86.2(13) . . ? O2_14 Cl1_14 O2_13 160.2(13) . . ? O1_14 Cl1_14 O2_13 54.2(12) . . ? O4_14 Cl1_14 O2_13 74.0(13) . . ? O3_13 Cl1_14 O2_13 79.8(10) . . ? O1_13 O1_14 Cl1_13 76.9(12) . . ? O1_13 O1_14 Cl1_14 52.7(11) . . ? Cl1_13 O1_14 Cl1_14 24.2(6) . . ? O1_13 O1_14 O2_13 124.2(17) . . ? Cl1_13 O1_14 O2_13 58.7(11) . . ? Cl1_14 O1_14 O2_13 78.7(10) . . ? Cl1_14 O2_14 O1_13 45.1(7) . . ? Cl1_14 O2_14 Cl1_13 11.7(4) . . ? O1_13 O2_14 Cl1_13 47.5(5) . . ? O4_13 O3_14 Cl1_14 57.6(9) . . ? O4_13 O3_14 Cl1_13 56.2(8) . . ? Cl1_14 O3_14 Cl1_13 19.2(5) . . ? O3_13 O4_14 Cl1_13 77.8(15) . . ? O3_13 O4_14 O4_13 133(2) . . ? Cl1_13 O4_14 O4_13 65.6(13) . . ? O3_13 O4_14 Cl1_14 83.3(15) . . ? Cl1_13 O4_14 Cl1_14 23.2(6) . . ? O4_13 O4_14 Cl1_14 51.7(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 P1 O1 Fe1 -28.7(8) . . . . ? O3 P1 O1 Fe1 100.8(7) . . . . ? C1 P1 O1 Fe1 -144.5(7) . . . . ? O6 Fe1 O1 P1 16.2(7) . . . . ? O3 Fe1 O1 P1 -83.3(7) 2_656 . . . ? O1_1 Fe1 O1 P1 -173.4(7) . . . . ? O1_2 Fe1 O1 P1 104.5(7) . . . . ? O1_3 Fe1 O1 P1 165.5(8) . . . . ? O1 P1 O2 Fe2 72.9(15) . . . 2_656 ? O3 P1 O2 Fe2 -56.5(15) . . . 2_656 ? C1 P1 O2 Fe2 -170.8(14) . . . 2_656 ? O2 P1 O3 Fe1 68.5(5) . . . 2_656 ? O1 P1 O3 Fe1 -62.1(5) . . . 2_656 ? C1 P1 O3 Fe1 -177.2(5) . . . 2_656 ? O6 P2 O4 Fe2 63.9(5) . . . . ? O5 P2 O4 Fe2 -63.6(5) . . . . ? C7 P2 O4 Fe2 -179.0(4) . . . . ? O2 Fe2 O4 P2 -50.7(4) 2_656 . . . ? O5 Fe2 O4 P2 49.0(4) 2_656 . . . ? O1_4 Fe2 O4 P2 -140.3(4) . . . . ? O1_5 Fe2 O4 P2 136.6(4) . . . . ? O1_6 Fe2 O4 P2 165.0(6) . . . . ? O6 P2 O5 Fe2 -22.4(8) . . . 2_656 ? O4 P2 O5 Fe2 105.5(7) . . . 2_656 ? C7 P2 O5 Fe2 -137.8(7) . . . 2_656 ? O5 P2 O6 Fe1 76(2) . . . . ? O4 P2 O6 Fe1 -51(2) . . . . ? C7 P2 O6 Fe1 -169(2) . . . . ? O1 Fe1 O6 P2 -65(2) . . . . ? O3 Fe1 O6 P2 35(2) 2_656 . . . ? O1_1 Fe1 O6 P2 -176.7(14) . . . . ? O1_2 Fe1 O6 P2 -157(2) . . . . ? O1_3 Fe1 O6 P2 121(2) . . . . ? O2 P1 C1 C2 162.7(6) . . . . ? O1 P1 C1 C2 -75.4(7) . . . . ? O3 P1 C1 C2 43.7(7) . . . . ? C6 N1 C2 C3 -1.0(17) . . . . ? C6 N1 C2 C1 177.3(11) . . . . ? P1 C1 C2 C3 -67.8(12) . . . . ? P1 C1 C2 N1 114.0(9) . . . . ? N1 C2 C3 C4 -3.6(15) . . . . ? C1 C2 C3 C4 178.2(9) . . . . ? C2 C3 C4 C5 8.2(18) . . . . ? C3 C4 C5 C6 -8(2) . . . . ? C4 C5 C6 N1 4(2) . . . . ? C2 N1 C6 C5 1(2) . . . . ? O6 P2 C7 C8 -165.5(4) . . . . ? O5 P2 C7 C8 -45.5(5) . . . . ? O4 P2 C7 C8 72.6(5) . . . . ? C12 N2 C8 C9 1.0(10) . . . . ? C12 N2 C8 C7 -179.7(7) . . . . ? P2 C7 C8 N2 -97.7(6) . . . . ? P2 C7 C8 C9 81.6(7) . . . . ? N2 C8 C9 C10 -0.4(10) . . . . ? C7 C8 C9 C10 -179.7(6) . . . . ? C8 C9 C10 C11 -1.0(11) . . . . ? C9 C10 C11 C12 1.8(12) . . . . ? C8 N2 C12 C11 -0.1(12) . . . . ? C10 C11 C12 N2 -1.3(13) . . . . ? Cl1_11 Cl1_11 O1_11 O4_11 -89(2) 2_657 . . 2_657 ? O3_11 Cl1_11 O1_11 O4_11 137.3(16) 2_657 . . 2_657 ? O3_11 Cl1_11 O1_11 O4_11 -162.1(14) . . . 2_657 ? O2_11 Cl1_11 O1_11 O4_11 76.4(14) . . . 2_657 ? O4_11 Cl1_11 O1_11 O4_11 -42.3(16) . . . 2_657 ? O2_11 Cl1_11 O1_11 O4_11 -117.0(12) 2_657 . . 2_657 ? O1_11 Cl1_11 O1_11 O4_11 -35.7(14) 2_657 . . 2_657 ? O4_11 Cl1_11 O1_11 Cl1_11 89(2) 2_657 . . 2_657 ? O3_11 Cl1_11 O1_11 Cl1_11 -133(3) 2_657 . . 2_657 ? O3_11 Cl1_11 O1_11 Cl1_11 -73(2) . . . 2_657 ? O2_11 Cl1_11 O1_11 Cl1_11 166(2) . . . 2_657 ? O4_11 Cl1_11 O1_11 Cl1_11 47.2(17) . . . 2_657 ? O2_11 Cl1_11 O1_11 Cl1_11 -28(2) 2_657 . . 2_657 ? O1_11 Cl1_11 O1_11 Cl1_11 53.8(10) 2_657 . . 2_657 ? Cl1_11 Cl1_11 O2_11 O3_11 -90.7(12) 2_657 . . 2_657 ? O4_11 Cl1_11 O2_11 O3_11 149.5(17) 2_657 . . 2_657 ? O3_11 Cl1_11 O2_11 O3_11 -25.0(18) . . . 2_657 ? O1_11 Cl1_11 O2_11 O3_11 99.2(16) . . . 2_657 ? O4_11 Cl1_11 O2_11 O3_11 -142.0(14) . . . 2_657 ? O2_11 Cl1_11 O2_11 O3_11 -44(2) 2_657 . . 2_657 ? O1_11 Cl1_11 O2_11 O3_11 -108.4(13) 2_657 . . 2_657 ? O4_11 Cl1_11 O2_11 Cl1_11 -119.8(12) 2_657 . . 2_657 ? O3_11 Cl1_11 O2_11 Cl1_11 90.7(12) 2_657 . . 2_657 ? O3_11 Cl1_11 O2_11 Cl1_11 65.7(9) . . . 2_657 ? O1_11 Cl1_11 O2_11 Cl1_11 -170.0(11) . . . 2_657 ? O4_11 Cl1_11 O2_11 Cl1_11 -51.3(9) . . . 2_657 ? O2_11 Cl1_11 O2_11 Cl1_11 47(2) 2_657 . . 2_657 ? O1_11 Cl1_11 O2_11 Cl1_11 -17.7(8) 2_657 . . 2_657 ? O4_11 Cl1_11 O3_11 Cl1_11 91(4) 2_657 . . 2_657 ? O3_11 Cl1_11 O3_11 Cl1_11 -129(3) 2_657 . . 2_657 ? O2_11 Cl1_11 O3_11 Cl1_11 -104(3) . . . 2_657 ? O1_11 Cl1_11 O3_11 Cl1_11 134(3) . . . 2_657 ? O4_11 Cl1_11 O3_11 Cl1_11 14(2) . . . 2_657 ? O2_11 Cl1_11 O3_11 Cl1_11 67(3) 2_657 . . 2_657 ? O1_11 Cl1_11 O3_11 Cl1_11 -22(2) 2_657 . . 2_657 ? Cl1_11 Cl1_11 O3_11 O3_11 129(3) 2_657 . . 2_657 ? O4_11 Cl1_11 O3_11 O3_11 -139(4) 2_657 . . 2_657 ? O2_11 Cl1_11 O3_11 O3_11 25.3(17) . . . 2_657 ? O1_11 Cl1_11 O3_11 O3_11 -96.6(17) . . . 2_657 ? O4_11 Cl1_11 O3_11 O3_11 142.9(16) . . . 2_657 ? O2_11 Cl1_11 O3_11 O3_11 -164(2) 2_657 . . 2_657 ? O1_11 Cl1_11 O3_11 O3_11 107.1(15) 2_657 . . 2_657 ? Cl1_11 Cl1_11 O3_11 O2_11 -67(3) 2_657 . . 2_657 ? O4_11 Cl1_11 O3_11 O2_11 25(4) 2_657 . . 2_657 ? O3_11 Cl1_11 O3_11 O2_11 164(2) 2_657 . . 2_657 ? O2_11 Cl1_11 O3_11 O2_11 -170.8(9) . . . 2_657 ? O1_11 Cl1_11 O3_11 O2_11 67.3(12) . . . 2_657 ? O4_11 Cl1_11 O3_11 O2_11 -53.2(12) . . . 2_657 ? O1_11 Cl1_11 O3_11 O2_11 -89.0(12) 2_657 . . 2_657 ? Cl1_11 Cl1_11 O4_11 O1_11 -46(3) 2_657 . . 2_657 ? O4_11 Cl1_11 O4_11 O1_11 140.4(17) 2_657 . . 2_657 ? O3_11 Cl1_11 O4_11 O1_11 -4(2) 2_657 . . 2_657 ? O3_11 Cl1_11 O4_11 O1_11 -61.7(13) . . . 2_657 ? O2_11 Cl1_11 O4_11 O1_11 55.9(12) . . . 2_657 ? O1_11 Cl1_11 O4_11 O1_11 175.0(10) . . . 2_657 ? O2_11 Cl1_11 O4_11 O1_11 -101.0(13) 2_657 . . 2_657 ? O4_11 Cl1_11 O4_11 Cl1_11 -174(4) 2_657 . . 2_657 ? O3_11 Cl1_11 O4_11 Cl1_11 41(3) 2_657 . . 2_657 ? O3_11 Cl1_11 O4_11 Cl1_11 -16(3) . . . 2_657 ? O2_11 Cl1_11 O4_11 Cl1_11 102(3) . . . 2_657 ? O1_11 Cl1_11 O4_11 Cl1_11 -139(4) . . . 2_657 ? O2_11 Cl1_11 O4_11 Cl1_11 -55(3) 2_657 . . 2_657 ? O1_11 Cl1_11 O4_11 Cl1_11 46(3) 2_657 . . 2_657 ? Cl1_11 Cl1_11 O4_11 O4_11 174(4) 2_657 . . 2_657 ? O3_11 Cl1_11 O4_11 O4_11 -145(2) 2_657 . . 2_657 ? O3_11 Cl1_11 O4_11 O4_11 158.0(13) . . . 2_657 ? O2_11 Cl1_11 O4_11 O4_11 -84.4(12) . . . 2_657 ? O1_11 Cl1_11 O4_11 O4_11 34.7(12) . . . 2_657 ? O2_11 Cl1_11 O4_11 O4_11 118.6(12) 2_657 . . 2_657 ? O1_11 Cl1_11 O4_11 O4_11 -140.4(17) 2_657 . . 2_657 ? Cl1_12 Cl1_12 O1_12 O4_12 -63(4) 2_656 . . 2_656 ? O3_12 Cl1_12 O1_12 O4_12 139.6(19) 2_656 . . 2_656 ? O4_12 Cl1_12 O1_12 O4_12 -144.1(15) . . . 2_656 ? O2_12 Cl1_12 O1_12 O4_12 93.1(16) . . . 2_656 ? O3_12 Cl1_12 O1_12 O4_12 -26.5(16) . . . 2_656 ? O1_12 Cl1_12 O1_12 O4_12 -108(2) 2_656 . . 2_656 ? O2_12 Cl1_12 O1_12 O4_12 -9(2) 2_656 . . 2_656 ? O3_12 Cl1_12 O1_12 Cl1_12 -158(4) 2_656 . . 2_656 ? O4_12 Cl1_12 O1_12 Cl1_12 63(4) 2_656 . . 2_656 ? O4_12 Cl1_12 O1_12 Cl1_12 -81(4) . . . 2_656 ? O2_12 Cl1_12 O1_12 Cl1_12 156(4) . . . 2_656 ? O3_12 Cl1_12 O1_12 Cl1_12 36(4) . . . 2_656 ? O1_12 Cl1_12 O1_12 Cl1_12 -46(4) 2_656 . . 2_656 ? O2_12 Cl1_12 O1_12 Cl1_12 54(4) 2_656 . . 2_656 ? Cl1_12 Cl1_12 O2_12 O3_12 -124(5) 2_656 . . 2_656 ? O4_12 Cl1_12 O2_12 O3_12 127(2) 2_656 . . 2_656 ? O1_12 Cl1_12 O2_12 O3_12 81.8(17) . . . 2_656 ? O4_12 Cl1_12 O2_12 O3_12 -41.5(15) . . . 2_656 ? O3_12 Cl1_12 O2_12 O3_12 -159.3(14) . . . 2_656 ? O1_12 Cl1_12 O2_12 O3_12 -53(3) 2_656 . . 2_656 ? O2_12 Cl1_12 O2_12 O3_12 -132.1(19) 2_656 . . 2_656 ? O3_12 Cl1_12 O2_12 Cl1_12 124(5) 2_656 . . 2_656 ? O4_12 Cl1_12 O2_12 Cl1_12 -109(5) 2_656 . . 2_656 ? O1_12 Cl1_12 O2_12 Cl1_12 -154(5) . . . 2_656 ? O4_12 Cl1_12 O2_12 Cl1_12 82(5) . . . 2_656 ? O3_12 Cl1_12 O2_12 Cl1_12 -35(5) . . . 2_656 ? O1_12 Cl1_12 O2_12 Cl1_12 70(5) 2_656 . . 2_656 ? O2_12 Cl1_12 O2_12 Cl1_12 -8(5) 2_656 . . 2_656 ? Cl1_12 Cl1_12 O3_12 O2_12 -80(3) 2_656 . . 2_656 ? O3_12 Cl1_12 O3_12 O2_12 13(2) 2_656 . . 2_656 ? O4_12 Cl1_12 O3_12 O2_12 145.4(16) 2_656 . . 2_656 ? O1_12 Cl1_12 O3_12 O2_12 164.5(15) . . . 2_656 ? O4_12 Cl1_12 O3_12 O2_12 -75.3(15) . . . 2_656 ? O2_12 Cl1_12 O3_12 O2_12 44.5(18) . . . 2_656 ? O1_12 Cl1_12 O3_12 O2_12 -105.1(15) 2_656 . . 2_656 ? O3_12 Cl1_12 O3_12 Cl1_12 93(4) 2_656 . . 2_656 ? O4_12 Cl1_12 O3_12 Cl1_12 -135(3) 2_656 . . 2_656 ? O1_12 Cl1_12 O3_12 Cl1_12 -116(3) . . . 2_656 ? O4_12 Cl1_12 O3_12 Cl1_12 4(3) . . . 2_656 ? O2_12 Cl1_12 O3_12 Cl1_12 124(3) . . . 2_656 ? O1_12 Cl1_12 O3_12 Cl1_12 -25(3) 2_656 . . 2_656 ? O2_12 Cl1_12 O3_12 Cl1_12 80(3) 2_656 . . 2_656 ? Cl1_12 Cl1_12 O3_12 O4_12 135(3) 2_656 . . 2_656 ? O3_12 Cl1_12 O3_12 O4_12 -132(2) 2_656 . . 2_656 ? O1_12 Cl1_12 O3_12 O4_12 19.0(11) . . . 2_656 ? O4_12 Cl1_12 O3_12 O4_12 139.3(12) . . . 2_656 ? O2_12 Cl1_12 O3_12 O4_12 -100.9(11) . . . 2_656 ? O1_12 Cl1_12 O3_12 O4_12 109.5(8) 2_656 . . 2_656 ? O2_12 Cl1_12 O3_12 O4_12 -145.4(16) 2_656 . . 2_656 ? Cl1_12 Cl1_12 O4_12 O1_12 -48.4(19) 2_656 . . 2_656 ? O3_12 Cl1_12 O4_12 O1_12 160.0(19) 2_656 . . 2_656 ? O4_12 Cl1_12 O4_12 O1_12 27.4(17) 2_656 . . 2_656 ? O1_12 Cl1_12 O4_12 O1_12 67(2) . . . 2_656 ? O2_12 Cl1_12 O4_12 O1_12 -170.1(17) . . . 2_656 ? O3_12 Cl1_12 O4_12 O1_12 -51.0(17) . . . 2_656 ? O2_12 Cl1_12 O4_12 O1_12 -89.3(17) 2_656 . . 2_656 ? O3_12 Cl1_12 O4_12 Cl1_12 -151.7(16) 2_656 . . 2_656 ? O4_12 Cl1_12 O4_12 Cl1_12 76(2) 2_656 . . 2_656 ? O1_12 Cl1_12 O4_12 Cl1_12 115.8(17) . . . 2_656 ? O2_12 Cl1_12 O4_12 Cl1_12 -121.8(14) . . . 2_656 ? O3_12 Cl1_12 O4_12 Cl1_12 -2.6(14) . . . 2_656 ? O1_12 Cl1_12 O4_12 Cl1_12 48.4(19) 2_656 . . 2_656 ? O2_12 Cl1_12 O4_12 Cl1_12 -41.0(13) 2_656 . . 2_656 ? Cl1_12 Cl1_12 O4_12 O3_12 151.7(16) 2_656 . . 2_656 ? O4_12 Cl1_12 O4_12 O3_12 -133(2) 2_656 . . 2_656 ? O1_12 Cl1_12 O4_12 O3_12 -92.6(14) . . . 2_656 ? O2_12 Cl1_12 O4_12 O3_12 29.9(11) . . . 2_656 ? O3_12 Cl1_12 O4_12 O3_12 149.1(15) . . . 2_656 ? O1_12 Cl1_12 O4_12 O3_12 -160.0(18) 2_656 . . 2_656 ? O2_12 Cl1_12 O4_12 O3_12 110.7(9) 2_656 . . 2_656 ? Cl1_14 Cl1_13 O1_13 O1_14 177(3) . . . . ? O4_14 Cl1_13 O1_13 O1_14 -129(2) . . . . ? O3_13 Cl1_13 O1_13 O1_14 95(2) 3_647 . . . ? O2_13 Cl1_13 O1_13 O1_14 35(2) . . . . ? O3_13 Cl1_13 O1_13 O1_14 -85(2) . . . . ? O2_13 Cl1_13 O1_13 O1_14 -145(2) 3_647 . . . ? O4_13 Cl1_13 O1_13 O1_14 -25(2) 3_647 . . . ? O4_13 Cl1_13 O1_13 O1_14 155(2) . . . . ? O1_13 Cl1_13 O1_13 O1_14 -65(20) 3_647 . . . ? O3_14 Cl1_13 O1_13 O1_14 127(2) . . . . ? O4_14 Cl1_13 O1_13 Cl1_14 54(4) . . . . ? O1_14 Cl1_13 O1_13 Cl1_14 -177(3) . . . . ? O3_13 Cl1_13 O1_13 Cl1_14 -81(2) 3_647 . . . ? O2_13 Cl1_13 O1_13 Cl1_14 -141(2) . . . . ? O3_13 Cl1_13 O1_13 Cl1_14 99(2) . . . . ? O2_13 Cl1_13 O1_13 Cl1_14 39(2) 3_647 . . . ? O4_13 Cl1_13 O1_13 Cl1_14 159(2) 3_647 . . . ? O4_13 Cl1_13 O1_13 Cl1_14 -21(2) . . . . ? O1_13 Cl1_13 O1_13 Cl1_14 118(17) 3_647 . . . ? O3_14 Cl1_13 O1_13 Cl1_14 -50.2(15) . . . . ? Cl1_14 Cl1_13 O1_13 O2_14 -37.3(14) . . . . ? O4_14 Cl1_13 O1_13 O2_14 17(4) . . . . ? O1_14 Cl1_13 O1_13 O2_14 146(3) . . . . ? O3_13 Cl1_13 O1_13 O2_14 -119(2) 3_647 . . . ? O2_13 Cl1_13 O1_13 O2_14 -179(2) . . . . ? O3_13 Cl1_13 O1_13 O2_14 61(2) . . . . ? O2_13 Cl1_13 O1_13 O2_14 1(2) 3_647 . . . ? O4_13 Cl1_13 O1_13 O2_14 122(2) 3_647 . . . ? O4_13 Cl1_13 O1_13 O2_14 -58(2) . . . . ? O1_13 Cl1_13 O1_13 O2_14 81(19) 3_647 . . . ? O3_14 Cl1_13 O1_13 O2_14 -87.4(13) . . . . ? Cl1_14 Cl1_13 O1_13 O3_13 81(2) . . . 3_647 ? O4_14 Cl1_13 O1_13 O3_13 135(3) . . . 3_647 ? O1_14 Cl1_13 O1_13 O3_13 -95(2) . . . 3_647 ? O2_13 Cl1_13 O1_13 O3_13 -60.1(13) . . . 3_647 ? O3_13 Cl1_13 O1_13 O3_13 180.0 . . . 3_647 ? O2_13 Cl1_13 O1_13 O3_13 119.9(13) 3_647 . . 3_647 ? O4_13 Cl1_13 O1_13 O3_13 -120.0(13) 3_647 . . 3_647 ? O4_13 Cl1_13 O1_13 O3_13 60.0(13) . . . 3_647 ? O1_13 Cl1_13 O1_13 O3_13 -161(26) 3_647 . . 3_647 ? O3_14 Cl1_13 O1_13 O3_13 31.1(15) . . . 3_647 ? Cl1_14 Cl1_13 O1_13 O4_13 -159(2) . . . 3_647 ? O4_14 Cl1_13 O1_13 O4_13 -105(3) . . . 3_647 ? O1_14 Cl1_13 O1_13 O4_13 25(2) . . . 3_647 ? O3_13 Cl1_13 O1_13 O4_13 120.0(13) 3_647 . . 3_647 ? O2_13 Cl1_13 O1_13 O4_13 59.9(13) . . . 3_647 ? O3_13 Cl1_13 O1_13 O4_13 -60.0(13) . . . 3_647 ? O2_13 Cl1_13 O1_13 O4_13 -120.1(13) 3_647 . . 3_647 ? O4_13 Cl1_13 O1_13 O4_13 180.00(2) . . . 3_647 ? O1_13 Cl1_13 O1_13 O4_13 -41(29) 3_647 . . 3_647 ? O3_14 Cl1_13 O1_13 O4_13 151.1(15) . . . 3_647 ? Cl1_14 Cl1_13 O1_13 O2_13 -39(2) . . . 3_647 ? O4_14 Cl1_13 O1_13 O2_13 15(3) . . . 3_647 ? O1_14 Cl1_13 O1_13 O2_13 145(2) . . . 3_647 ? O3_13 Cl1_13 O1_13 O2_13 -119.9(13) 3_647 . . 3_647 ? O2_13 Cl1_13 O1_13 O2_13 179.998(15) . . . 3_647 ? O3_13 Cl1_13 O1_13 O2_13 60.1(13) . . . 3_647 ? O4_13 Cl1_13 O1_13 O2_13 120.1(13) 3_647 . . 3_647 ? O4_13 Cl1_13 O1_13 O2_13 -59.9(13) . . . 3_647 ? O1_13 Cl1_13 O1_13 O2_13 80(24) 3_647 . . 3_647 ? O3_14 Cl1_13 O1_13 O2_13 -88.9(16) . . . 3_647 ? Cl1_14 Cl1_13 O2_13 O1_14 -74(2) . . . . ? O4_14 Cl1_13 O2_13 O1_14 146.3(13) . . . . ? O3_13 Cl1_13 O2_13 O1_14 -85.3(17) 3_647 . . . ? O3_13 Cl1_13 O2_13 O1_14 94.7(17) . . . . ? O2_13 Cl1_13 O2_13 O1_14 22(7) 3_647 . . . ? O4_13 Cl1_13 O2_13 O1_14 36.3(17) 3_647 . . . ? O4_13 Cl1_13 O2_13 O1_14 -143.7(17) . . . . ? O1_13 Cl1_13 O2_13 O1_14 -25.0(18) . . . . ? O1_13 Cl1_13 O2_13 O1_14 155.0(18) 3_647 . . . ? O3_14 Cl1_13 O2_13 O1_14 -104.2(12) . . . . ? Cl1_14 Cl1_13 O2_13 O4_13 -110(2) . . . 3_647 ? O4_14 Cl1_13 O2_13 O4_13 110.0(19) . . . 3_647 ? O1_14 Cl1_13 O2_13 O4_13 -36.3(17) . . . 3_647 ? O3_13 Cl1_13 O2_13 O4_13 -121.6(13) 3_647 . . 3_647 ? O3_13 Cl1_13 O2_13 O4_13 58.4(13) . . . 3_647 ? O2_13 Cl1_13 O2_13 O4_13 -14(7) 3_647 . . 3_647 ? O4_13 Cl1_13 O2_13 O4_13 180.00(2) . . . 3_647 ? O1_13 Cl1_13 O2_13 O4_13 -61.3(13) . . . 3_647 ? O1_13 Cl1_13 O2_13 O4_13 118.7(13) 3_647 . . 3_647 ? O3_14 Cl1_13 O2_13 O4_13 -140.4(16) . . . 3_647 ? Cl1_14 Cl1_13 O2_13 O3_13 11(2) . . . 3_647 ? O4_14 Cl1_13 O2_13 O3_13 -128.4(18) . . . 3_647 ? O1_14 Cl1_13 O2_13 O3_13 85.3(17) . . . 3_647 ? O3_13 Cl1_13 O2_13 O3_13 180.000(2) . . . 3_647 ? O2_13 Cl1_13 O2_13 O3_13 107(7) 3_647 . . 3_647 ? O4_13 Cl1_13 O2_13 O3_13 121.6(13) 3_647 . . 3_647 ? O4_13 Cl1_13 O2_13 O3_13 -58.4(13) . . . 3_647 ? O1_13 Cl1_13 O2_13 O3_13 60.3(13) . . . 3_647 ? O1_13 Cl1_13 O2_13 O3_13 -119.7(13) 3_647 . . 3_647 ? O3_14 Cl1_13 O2_13 O3_13 -18.9(15) . . . 3_647 ? Cl1_14 Cl1_13 O2_13 O1_13 131(2) . . . 3_647 ? O4_14 Cl1_13 O2_13 O1_13 -8.7(19) . . . 3_647 ? O1_14 Cl1_13 O2_13 O1_13 -155.0(18) . . . 3_647 ? O3_13 Cl1_13 O2_13 O1_13 119.7(13) 3_647 . . 3_647 ? O3_13 Cl1_13 O2_13 O1_13 -60.3(13) . . . 3_647 ? O2_13 Cl1_13 O2_13 O1_13 -133(7) 3_647 . . 3_647 ? O4_13 Cl1_13 O2_13 O1_13 -118.7(13) 3_647 . . 3_647 ? O4_13 Cl1_13 O2_13 O1_13 61.3(13) . . . 3_647 ? O1_13 Cl1_13 O2_13 O1_13 180.001(17) . . . 3_647 ? O3_14 Cl1_13 O2_13 O1_13 100.8(15) . . . 3_647 ? O4_14 Cl1_13 O2_13 Cl1_14 -140(2) . . . . ? O1_14 Cl1_13 O2_13 Cl1_14 74(2) . . . . ? O3_13 Cl1_13 O2_13 Cl1_14 -11(2) 3_647 . . . ? O3_13 Cl1_13 O2_13 Cl1_14 169(2) . . . . ? O2_13 Cl1_13 O2_13 Cl1_14 96(7) 3_647 . . . ? O4_13 Cl1_13 O2_13 Cl1_14 110(2) 3_647 . . . ? O4_13 Cl1_13 O2_13 Cl1_14 -70(2) . . . . ? O1_13 Cl1_13 O2_13 Cl1_14 49(2) . . . . ? O1_13 Cl1_13 O2_13 Cl1_14 -131(2) 3_647 . . . ? O3_14 Cl1_13 O2_13 Cl1_14 -30.0(19) . . . . ? Cl1_14 Cl1_13 O3_13 O4_14 -95(2) . . . . ? O1_14 Cl1_13 O3_13 O4_14 167(2) . . . . ? O3_13 Cl1_13 O3_13 O4_14 102(19) 3_647 . . . ? O2_13 Cl1_13 O3_13 O4_14 93(2) . . . . ? O2_13 Cl1_13 O3_13 O4_14 -87(2) 3_647 . . . ? O4_13 Cl1_13 O3_13 O4_14 151(3) 3_647 . . . ? O4_13 Cl1_13 O3_13 O4_14 -29(3) . . . . ? O1_13 Cl1_13 O3_13 O4_14 -148(2) . . . . ? O1_13 Cl1_13 O3_13 O4_14 32(2) 3_647 . . . ? O3_14 Cl1_13 O3_13 O4_14 -48(4) . . . . ? Cl1_14 Cl1_13 O3_13 O4_13 114.5(17) . . . 3_647 ? O4_14 Cl1_13 O3_13 O4_13 -151(3) . . . 3_647 ? O1_14 Cl1_13 O3_13 O4_13 16.4(18) . . . 3_647 ? O3_13 Cl1_13 O3_13 O4_13 -49(28) 3_647 . . 3_647 ? O2_13 Cl1_13 O3_13 O4_13 -58.1(13) . . . 3_647 ? O2_13 Cl1_13 O3_13 O4_13 121.9(13) 3_647 . . 3_647 ? O4_13 Cl1_13 O3_13 O4_13 179.998(3) . . . 3_647 ? O1_13 Cl1_13 O3_13 O4_13 60.9(13) . . . 3_647 ? O1_13 Cl1_13 O3_13 O4_13 -119.1(13) 3_647 . . 3_647 ? O3_14 Cl1_13 O3_13 O4_13 161(3) . . . 3_647 ? Cl1_14 Cl1_13 O3_13 O2_13 -7.5(17) . . . 3_647 ? O4_14 Cl1_13 O3_13 O2_13 87(2) . . . 3_647 ? O1_14 Cl1_13 O3_13 O2_13 -105.6(17) . . . 3_647 ? O3_13 Cl1_13 O3_13 O2_13 -171(27) 3_647 . . 3_647 ? O2_13 Cl1_13 O3_13 O2_13 180.003(1) . . . 3_647 ? O4_13 Cl1_13 O3_13 O2_13 -121.9(13) 3_647 . . 3_647 ? O4_13 Cl1_13 O3_13 O2_13 58.1(13) . . . 3_647 ? O1_13 Cl1_13 O3_13 O2_13 -61.0(13) . . . 3_647 ? O1_13 Cl1_13 O3_13 O2_13 119.0(13) 3_647 . . 3_647 ? O3_14 Cl1_13 O3_13 O2_13 39(3) . . . 3_647 ? Cl1_14 Cl1_13 O3_13 O1_13 -126.5(16) . . . 3_647 ? O4_14 Cl1_13 O3_13 O1_13 -32(2) . . . 3_647 ? O1_14 Cl1_13 O3_13 O1_13 135.4(17) . . . 3_647 ? O3_13 Cl1_13 O3_13 O1_13 70(29) 3_647 . . 3_647 ? O2_13 Cl1_13 O3_13 O1_13 61.0(13) . . . 3_647 ? O2_13 Cl1_13 O3_13 O1_13 -119.0(13) 3_647 . . 3_647 ? O4_13 Cl1_13 O3_13 O1_13 119.1(13) 3_647 . . 3_647 ? O4_13 Cl1_13 O3_13 O1_13 -60.9(13) . . . 3_647 ? O1_13 Cl1_13 O3_13 O1_13 180.000(1) . . . 3_647 ? O3_14 Cl1_13 O3_13 O1_13 -80(3) . . . 3_647 ? O4_14 Cl1_13 O3_13 Cl1_14 95(2) . . . . ? O1_14 Cl1_13 O3_13 Cl1_14 -98.1(15) . . . . ? O3_13 Cl1_13 O3_13 Cl1_14 -163(9) 3_647 . . . ? O2_13 Cl1_13 O3_13 Cl1_14 -172.5(17) . . . . ? O2_13 Cl1_13 O3_13 Cl1_14 7.5(17) 3_647 . . . ? O4_13 Cl1_13 O3_13 Cl1_14 -114.5(17) 3_647 . . . ? O4_13 Cl1_13 O3_13 Cl1_14 65.5(17) . . . . ? O1_13 Cl1_13 O3_13 Cl1_14 -53.5(16) . . . . ? O1_13 Cl1_13 O3_13 Cl1_14 126.5(16) 3_647 . . . ? O3_14 Cl1_13 O3_13 Cl1_14 46(3) . . . . ? Cl1_14 Cl1_13 O4_13 O3_14 -64(2) . . . . ? O4_14 Cl1_13 O4_13 O3_14 171(2) . . . . ? O1_14 Cl1_13 O4_13 O3_14 -15(4) . . . . ? O3_13 Cl1_13 O4_13 O3_14 15(2) 3_647 . . . ? O2_13 Cl1_13 O4_13 O3_14 73(2) . . . . ? O3_13 Cl1_13 O4_13 O3_14 -165(2) . . . . ? O2_13 Cl1_13 O4_13 O3_14 -107(2) 3_647 . . . ? O4_13 Cl1_13 O4_13 O3_14 -76(22) 3_647 . . . ? O1_13 Cl1_13 O4_13 O3_14 -46(2) . . . . ? O1_13 Cl1_13 O4_13 O3_14 134(2) 3_647 . . . ? O4_14 Cl1_13 O4_13 Cl1_14 -125.2(18) . . . . ? O1_14 Cl1_13 O4_13 Cl1_14 49(3) . . . . ? O3_13 Cl1_13 O4_13 Cl1_14 79(2) 3_647 . . . ? O2_13 Cl1_13 O4_13 Cl1_14 137(2) . . . . ? O3_13 Cl1_13 O4_13 Cl1_14 -101(2) . . . . ? O2_13 Cl1_13 O4_13 Cl1_14 -43(2) 3_647 . . . ? O4_13 Cl1_13 O4_13 Cl1_14 -12(21) 3_647 . . . ? O1_13 Cl1_13 O4_13 Cl1_14 18(2) . . . . ? O1_13 Cl1_13 O4_13 Cl1_14 -162(2) 3_647 . . . ? O3_14 Cl1_13 O4_13 Cl1_14 64(2) . . . . ? Cl1_14 Cl1_13 O4_13 O4_14 125.2(18) . . . . ? O1_14 Cl1_13 O4_13 O4_14 174(3) . . . . ? O3_13 Cl1_13 O4_13 O4_14 -156.1(18) 3_647 . . . ? O2_13 Cl1_13 O4_13 O4_14 -97.6(17) . . . . ? O3_13 Cl1_13 O4_13 O4_14 23.9(18) . . . . ? O2_13 Cl1_13 O4_13 O4_14 82.4(17) 3_647 . . . ? O4_13 Cl1_13 O4_13 O4_14 114(23) 3_647 . . . ? O1_13 Cl1_13 O4_13 O4_14 143.7(16) . . . . ? O1_13 Cl1_13 O4_13 O4_14 -36.3(16) 3_647 . . . ? O3_14 Cl1_13 O4_13 O4_14 -171(2) . . . . ? Cl1_14 Cl1_13 O4_13 O2_13 43(2) . . . 3_647 ? O4_14 Cl1_13 O4_13 O2_13 -82.4(17) . . . 3_647 ? O1_14 Cl1_13 O4_13 O2_13 92(3) . . . 3_647 ? O3_13 Cl1_13 O4_13 O2_13 121.6(14) 3_647 . . 3_647 ? O2_13 Cl1_13 O4_13 O2_13 179.999(18) . . . 3_647 ? O3_13 Cl1_13 O4_13 O2_13 -58.4(14) . . . 3_647 ? O4_13 Cl1_13 O4_13 O2_13 31(27) 3_647 . . 3_647 ? O1_13 Cl1_13 O4_13 O2_13 61.3(13) . . . 3_647 ? O1_13 Cl1_13 O4_13 O2_13 -118.7(13) 3_647 . . 3_647 ? O3_14 Cl1_13 O4_13 O2_13 107(3) . . . 3_647 ? Cl1_14 Cl1_13 O4_13 O3_13 -79(2) . . . 3_647 ? O4_14 Cl1_13 O4_13 O3_13 156.1(18) . . . 3_647 ? O1_14 Cl1_13 O4_13 O3_13 -30(3) . . . 3_647 ? O2_13 Cl1_13 O4_13 O3_13 58.4(14) . . . 3_647 ? O3_13 Cl1_13 O4_13 O3_13 180.000(3) . . . 3_647 ? O2_13 Cl1_13 O4_13 O3_13 -121.6(14) 3_647 . . 3_647 ? O4_13 Cl1_13 O4_13 O3_13 -90(27) 3_647 . . 3_647 ? O1_13 Cl1_13 O4_13 O3_13 -60.3(13) . . . 3_647 ? O1_13 Cl1_13 O4_13 O3_13 119.7(13) 3_647 . . 3_647 ? O3_14 Cl1_13 O4_13 O3_13 -15(2) . . . 3_647 ? Cl1_14 Cl1_13 O4_13 O1_13 162(2) . . . 3_647 ? O4_14 Cl1_13 O4_13 O1_13 36.3(16) . . . 3_647 ? O1_14 Cl1_13 O4_13 O1_13 -149(3) . . . 3_647 ? O3_13 Cl1_13 O4_13 O1_13 -119.7(13) 3_647 . . 3_647 ? O2_13 Cl1_13 O4_13 O1_13 -61.3(13) . . . 3_647 ? O3_13 Cl1_13 O4_13 O1_13 60.3(13) . . . 3_647 ? O2_13 Cl1_13 O4_13 O1_13 118.7(13) 3_647 . . 3_647 ? O4_13 Cl1_13 O4_13 O1_13 150(25) 3_647 . . 3_647 ? O1_13 Cl1_13 O4_13 O1_13 180.00(2) . . . 3_647 ? O3_14 Cl1_13 O4_13 O1_13 -134(2) . . . 3_647 ? O4_14 Cl1_13 Cl1_14 O1_13 -151.8(19) . . . . ? O1_14 Cl1_13 Cl1_14 O1_13 2(2) . . . . ? O3_13 Cl1_13 Cl1_14 O1_13 79.9(18) 3_647 . . . ? O2_13 Cl1_13 Cl1_14 O1_13 69(3) . . . . ? O3_13 Cl1_13 Cl1_14 O1_13 -100.1(18) . . . . ? O2_13 Cl1_13 Cl1_14 O1_13 -111(3) 3_647 . . . ? O4_13 Cl1_13 Cl1_14 O1_13 -23(2) 3_647 . . . ? O4_13 Cl1_13 Cl1_14 O1_13 157(2) . . . . ? O1_13 Cl1_13 Cl1_14 O1_13 180.00(2) 3_647 . . . ? O3_14 Cl1_13 Cl1_14 O1_13 108(2) . . . . ? O4_14 Cl1_13 Cl1_14 O4_13 51(2) . . . . ? O1_14 Cl1_13 Cl1_14 O4_13 -154.7(18) . . . . ? O3_13 Cl1_13 Cl1_14 O4_13 -77.1(14) 3_647 . . . ? O2_13 Cl1_13 Cl1_14 O4_13 -88(2) . . . . ? O3_13 Cl1_13 Cl1_14 O4_13 102.9(14) . . . . ? O2_13 Cl1_13 Cl1_14 O4_13 92(2) 3_647 . . . ? O4_13 Cl1_13 Cl1_14 O4_13 180.000(18) 3_647 . . . ? O1_13 Cl1_13 Cl1_14 O4_13 -157(2) . . . . ? O1_13 Cl1_13 Cl1_14 O4_13 23(2) 3_647 . . . ? O3_14 Cl1_13 Cl1_14 O4_13 -49.0(17) . . . . ? O4_14 Cl1_13 Cl1_14 O3_14 100.2(12) . . . . ? O1_14 Cl1_13 Cl1_14 O3_14 -105.7(10) . . . . ? O3_13 Cl1_13 Cl1_14 O3_14 -28.0(15) 3_647 . . . ? O2_13 Cl1_13 Cl1_14 O3_14 -39(2) . . . . ? O3_13 Cl1_13 Cl1_14 O3_14 152.0(15) . . . . ? O2_13 Cl1_13 Cl1_14 O3_14 141(2) 3_647 . . . ? O4_13 Cl1_13 Cl1_14 O3_14 -131.0(17) 3_647 . . . ? O4_13 Cl1_13 Cl1_14 O3_14 49.0(17) . . . . ? O1_13 Cl1_13 Cl1_14 O3_14 -108(2) . . . . ? O1_13 Cl1_13 Cl1_14 O3_14 72(2) 3_647 . . . ? O4_14 Cl1_13 Cl1_14 O2_14 -68(2) . . . . ? O1_14 Cl1_13 Cl1_14 O2_14 86.0(19) . . . . ? O3_13 Cl1_13 Cl1_14 O2_14 164(2) 3_647 . . . ? O2_13 Cl1_13 Cl1_14 O2_14 153(2) . . . . ? O3_13 Cl1_13 Cl1_14 O2_14 -16(2) . . . . ? O2_13 Cl1_13 Cl1_14 O2_14 -27(2) 3_647 . . . ? O4_13 Cl1_13 Cl1_14 O2_14 61(2) 3_647 . . . ? O4_13 Cl1_13 Cl1_14 O2_14 -119(2) . . . . ? O1_13 Cl1_13 Cl1_14 O2_14 84(2) . . . . ? O1_13 Cl1_13 Cl1_14 O2_14 -96(2) 3_647 . . . ? O3_14 Cl1_13 Cl1_14 O2_14 -168(2) . . . . ? O4_14 Cl1_13 Cl1_14 O1_14 -154.1(12) . . . . ? O3_13 Cl1_13 Cl1_14 O1_14 77.6(16) 3_647 . . . ? O2_13 Cl1_13 Cl1_14 O1_14 67(2) . . . . ? O3_13 Cl1_13 Cl1_14 O1_14 -102.4(16) . . . . ? O2_13 Cl1_13 Cl1_14 O1_14 -113(2) 3_647 . . . ? O4_13 Cl1_13 Cl1_14 O1_14 -25.3(18) 3_647 . . . ? O4_13 Cl1_13 Cl1_14 O1_14 154.7(18) . . . . ? O1_13 Cl1_13 Cl1_14 O1_14 -2(2) . . . . ? O1_13 Cl1_13 Cl1_14 O1_14 178(2) 3_647 . . . ? O3_14 Cl1_13 Cl1_14 O1_14 105.7(10) . . . . ? O1_14 Cl1_13 Cl1_14 O4_14 154.1(12) . . . . ? O3_13 Cl1_13 Cl1_14 O4_14 -128.2(17) 3_647 . . . ? O2_13 Cl1_13 Cl1_14 O4_14 -139(2) . . . . ? O3_13 Cl1_13 Cl1_14 O4_14 51.8(17) . . . . ? O2_13 Cl1_13 Cl1_14 O4_14 41(2) 3_647 . . . ? O4_13 Cl1_13 Cl1_14 O4_14 129(2) 3_647 . . . ? O4_13 Cl1_13 Cl1_14 O4_14 -51(2) . . . . ? O1_13 Cl1_13 Cl1_14 O4_14 151.8(19) . . . . ? O1_13 Cl1_13 Cl1_14 O4_14 -28.2(19) 3_647 . . . ? O3_14 Cl1_13 Cl1_14 O4_14 -100.2(12) . . . . ? O4_14 Cl1_13 Cl1_14 O3_13 -51.8(16) . . . . ? O1_14 Cl1_13 Cl1_14 O3_13 102.4(16) . . . . ? O3_13 Cl1_13 Cl1_14 O3_13 180.0 3_647 . . . ? O2_13 Cl1_13 Cl1_14 O3_13 169(2) . . . . ? O2_13 Cl1_13 Cl1_14 O3_13 -11(2) 3_647 . . . ? O4_13 Cl1_13 Cl1_14 O3_13 77.1(14) 3_647 . . . ? O4_13 Cl1_13 Cl1_14 O3_13 -102.9(14) . . . . ? O1_13 Cl1_13 Cl1_14 O3_13 100.1(18) . . . . ? O1_13 Cl1_13 Cl1_14 O3_13 -79.9(18) 3_647 . . . ? O3_14 Cl1_13 Cl1_14 O3_13 -152.0(15) . . . . ? O4_14 Cl1_13 Cl1_14 O2_13 139(2) . . . . ? O1_14 Cl1_13 Cl1_14 O2_13 -67(2) . . . . ? O3_13 Cl1_13 Cl1_14 O2_13 11(2) 3_647 . . . ? O3_13 Cl1_13 Cl1_14 O2_13 -169(2) . . . . ? O2_13 Cl1_13 Cl1_14 O2_13 180.005(5) 3_647 . . . ? O4_13 Cl1_13 Cl1_14 O2_13 -92(2) 3_647 . . . ? O4_13 Cl1_13 Cl1_14 O2_13 88(2) . . . . ? O1_13 Cl1_13 Cl1_14 O2_13 -69(3) . . . . ? O1_13 Cl1_13 Cl1_14 O2_13 111(3) 3_647 . . . ? O3_14 Cl1_13 Cl1_14 O2_13 39(2) . . . . ? O1_14 O1_13 Cl1_14 Cl1_13 -3(3) . . . . ? O2_14 O1_13 Cl1_14 Cl1_13 137.3(14) . . . . ? O3_13 O1_13 Cl1_14 Cl1_13 -82(2) 3_647 . . . ? O4_13 O1_13 Cl1_14 Cl1_13 17.6(19) 3_647 . . . ? O2_13 O1_13 Cl1_14 Cl1_13 124(3) 3_647 . . . ? O1_14 O1_13 Cl1_14 O4_13 127(3) . . . . ? Cl1_13 O1_13 Cl1_14 O4_13 130(4) . . . . ? O2_14 O1_13 Cl1_14 O4_13 -92(4) . . . . ? O3_13 O1_13 Cl1_14 O4_13 48(3) 3_647 . . . ? O4_13 O1_13 Cl1_14 O4_13 148(3) 3_647 . . . ? O2_13 O1_13 Cl1_14 O4_13 -105(4) 3_647 . . . ? O1_14 O1_13 Cl1_14 O3_14 110(2) . . . . ? Cl1_13 O1_13 Cl1_14 O3_14 113.3(16) . . . . ? O2_14 O1_13 Cl1_14 O3_14 -109.4(11) . . . . ? O3_13 O1_13 Cl1_14 O3_14 31.4(16) 3_647 . . . ? O4_13 O1_13 Cl1_14 O3_14 130.9(15) 3_647 . . . ? O2_13 O1_13 Cl1_14 O3_14 -122(2) 3_647 . . . ? O1_14 O1_13 Cl1_14 O2_14 -140(2) . . . . ? Cl1_13 O1_13 Cl1_14 O2_14 -137.3(14) . . . . ? O3_13 O1_13 Cl1_14 O2_14 140.8(19) 3_647 . . . ? O4_13 O1_13 Cl1_14 O2_14 -119.7(18) 3_647 . . . ? O2_13 O1_13 Cl1_14 O2_14 -13(3) 3_647 . . . ? Cl1_13 O1_13 Cl1_14 O1_14 3(3) . . . . ? O2_14 O1_13 Cl1_14 O1_14 140(2) . . . . ? O3_13 O1_13 Cl1_14 O1_14 -79(2) 3_647 . . . ? O4_13 O1_13 Cl1_14 O1_14 20.4(18) 3_647 . . . ? O2_13 O1_13 Cl1_14 O1_14 127(3) 3_647 . . . ? O1_14 O1_13 Cl1_14 O4_14 -45(4) . . . . ? Cl1_13 O1_13 Cl1_14 O4_14 -42(3) . . . . ? O2_14 O1_13 Cl1_14 O4_14 96(3) . . . . ? O3_13 O1_13 Cl1_14 O4_14 -124(4) 3_647 . . . ? O4_13 O1_13 Cl1_14 O4_14 -24(3) 3_647 . . . ? O2_13 O1_13 Cl1_14 O4_14 83(4) 3_647 . . . ? O1_14 O1_13 Cl1_14 O3_13 -57(2) . . . . ? Cl1_13 O1_13 Cl1_14 O3_13 -54.6(18) . . . . ? O2_14 O1_13 Cl1_14 O3_13 82.7(19) . . . . ? O3_13 O1_13 Cl1_14 O3_13 -136.5(11) 3_647 . . . ? O4_13 O1_13 Cl1_14 O3_13 -37.1(14) 3_647 . . . ? O2_13 O1_13 Cl1_14 O3_13 69.8(16) 3_647 . . . ? O1_14 O1_13 Cl1_14 O2_13 23(2) . . . . ? Cl1_13 O1_13 Cl1_14 O2_13 26.3(15) . . . . ? O2_14 O1_13 Cl1_14 O2_13 163.6(16) . . . . ? O3_13 O1_13 Cl1_14 O2_13 -55.6(11) 3_647 . . . ? O4_13 O1_13 Cl1_14 O2_13 43.8(11) 3_647 . . . ? O2_13 O1_13 Cl1_14 O2_13 150.7(16) 3_647 . . . ? O3_14 O4_13 Cl1_14 Cl1_13 110.8(18) . . . . ? O4_14 O4_13 Cl1_14 Cl1_13 -42.3(15) . . . . ? O2_13 O4_13 Cl1_14 Cl1_13 -119(3) 3_647 . . . ? O3_13 O4_13 Cl1_14 Cl1_13 83.5(18) 3_647 . . . ? O1_13 O4_13 Cl1_14 Cl1_13 -15.3(17) 3_647 . . . ? O3_14 O4_13 Cl1_14 O1_13 -22(5) . . . . ? Cl1_13 O4_13 Cl1_14 O1_13 -133(4) . . . . ? O4_14 O4_13 Cl1_14 O1_13 -175(4) . . . . ? O2_13 O4_13 Cl1_14 O1_13 108(4) 3_647 . . . ? O3_13 O4_13 Cl1_14 O1_13 -49(3) 3_647 . . . ? O1_13 O4_13 Cl1_14 O1_13 -148(3) 3_647 . . . ? Cl1_13 O4_13 Cl1_14 O3_14 -110.8(18) . . . . ? O4_14 O4_13 Cl1_14 O3_14 -153(2) . . . . ? O2_13 O4_13 Cl1_14 O3_14 130(3) 3_647 . . . ? O3_13 O4_13 Cl1_14 O3_14 -27(2) 3_647 . . . ? O1_13 O4_13 Cl1_14 O3_14 -126(2) 3_647 . . . ? O3_14 O4_13 Cl1_14 O2_14 -105.5(15) . . . . ? Cl1_13 O4_13 Cl1_14 O2_14 143.7(16) . . . . ? O4_14 O4_13 Cl1_14 O2_14 101.4(13) . . . . ? O2_13 O4_13 Cl1_14 O2_14 24(2) 3_647 . . . ? O3_13 O4_13 Cl1_14 O2_14 -132.8(18) 3_647 . . . ? O1_13 O4_13 Cl1_14 O2_14 128.4(16) 3_647 . . . ? O3_14 O4_13 Cl1_14 O1_14 69(4) . . . . ? Cl1_13 O4_13 Cl1_14 O1_14 -42(3) . . . . ? O4_14 O4_13 Cl1_14 O1_14 -84(3) . . . . ? O2_13 O4_13 Cl1_14 O1_14 -161(4) 3_647 . . . ? O3_13 O4_13 Cl1_14 O1_14 41(4) 3_647 . . . ? O1_13 O4_13 Cl1_14 O1_14 -57(4) 3_647 . . . ? O3_14 O4_13 Cl1_14 O4_14 153(2) . . . . ? Cl1_13 O4_13 Cl1_14 O4_14 42.3(15) . . . . ? O2_13 O4_13 Cl1_14 O4_14 -77(2) 3_647 . . . ? O3_13 O4_13 Cl1_14 O4_14 125.8(17) 3_647 . . . ? O1_13 O4_13 Cl1_14 O4_14 27.0(14) 3_647 . . . ? O3_14 O4_13 Cl1_14 O3_13 162.8(19) . . . . ? Cl1_13 O4_13 Cl1_14 O3_13 52.0(16) . . . . ? O4_14 O4_13 Cl1_14 O3_13 9.6(16) . . . . ? O2_13 O4_13 Cl1_14 O3_13 -67.4(15) 3_647 . . . ? O3_13 O4_13 Cl1_14 O3_13 135.5(10) 3_647 . . . ? O1_13 O4_13 Cl1_14 O3_13 36.7(13) 3_647 . . . ? O3_14 O4_13 Cl1_14 O2_13 83(2) . . . . ? Cl1_13 O4_13 Cl1_14 O2_13 -28.3(13) . . . . ? O4_14 O4_13 Cl1_14 O2_13 -70.6(14) . . . . ? O2_13 O4_13 Cl1_14 O2_13 -147.6(15) 3_647 . . . ? O3_13 O4_13 Cl1_14 O2_13 55.2(11) 3_647 . . . ? O1_13 O4_13 Cl1_14 O2_13 -43.6(11) 3_647 . . . ? O4_14 O3_13 Cl1_14 Cl1_13 72(2) . . . . ? O4_13 O3_13 Cl1_14 Cl1_13 -55.7(15) 3_647 . . . ? O2_13 O3_13 Cl1_14 Cl1_13 170(2) 3_647 . . . ? O1_13 O3_13 Cl1_14 Cl1_13 45.5(14) 3_647 . . . ? O4_14 O3_13 Cl1_14 O1_13 169(2) . . . . ? Cl1_13 O3_13 Cl1_14 O1_13 97.2(19) . . . . ? O4_13 O3_13 Cl1_14 O1_13 41.5(16) 3_647 . . . ? O2_13 O3_13 Cl1_14 O1_13 -93.2(18) 3_647 . . . ? O1_13 O3_13 Cl1_14 O1_13 142.7(11) 3_647 . . . ? O4_14 O3_13 Cl1_14 O4_13 -14(2) . . . . ? Cl1_13 O3_13 Cl1_14 O4_13 -85.3(17) . . . . ? O4_13 O3_13 Cl1_14 O4_13 -141.1(10) 3_647 . . . ? O2_13 O3_13 Cl1_14 O4_13 84.2(17) 3_647 . . . ? O1_13 O3_13 Cl1_14 O4_13 -39.8(15) 3_647 . . . ? O4_14 O3_13 Cl1_14 O3_14 12(4) . . . . ? Cl1_13 O3_13 Cl1_14 O3_14 -59(3) . . . . ? O4_13 O3_13 Cl1_14 O3_14 -115(3) 3_647 . . . ? O2_13 O3_13 Cl1_14 O3_14 110(3) 3_647 . . . ? O1_13 O3_13 Cl1_14 O3_14 -14(3) 3_647 . . . ? O4_14 O3_13 Cl1_14 O2_14 -119(2) . . . . ? Cl1_13 O3_13 Cl1_14 O2_14 169.4(15) . . . . ? O4_13 O3_13 Cl1_14 O2_14 113.6(16) 3_647 . . . ? O2_13 O3_13 Cl1_14 O2_14 -21(2) 3_647 . . . ? O1_13 O3_13 Cl1_14 O2_14 -145.1(15) 3_647 . . . ? O4_14 O3_13 Cl1_14 O1_14 132(2) . . . . ? Cl1_13 O3_13 Cl1_14 O1_14 60.2(13) . . . . ? O4_13 O3_13 Cl1_14 O1_14 4.5(15) 3_647 . . . ? O2_13 O3_13 Cl1_14 O1_14 -130(2) 3_647 . . . ? O1_13 O3_13 Cl1_14 O1_14 105.7(15) 3_647 . . . ? Cl1_13 O3_13 Cl1_14 O4_14 -72(2) . . . . ? O4_13 O3_13 Cl1_14 O4_14 -128(2) 3_647 . . . ? O2_13 O3_13 Cl1_14 O4_14 98(3) 3_647 . . . ? O1_13 O3_13 Cl1_14 O4_14 -26(2) 3_647 . . . ? O4_14 O3_13 Cl1_14 O2_13 77(2) . . . . ? Cl1_13 O3_13 Cl1_14 O2_13 5.3(12) . . . . ? O4_13 O3_13 Cl1_14 O2_13 -50.4(11) 3_647 . . . ? O2_13 O3_13 Cl1_14 O2_13 174.9(11) 3_647 . . . ? O1_13 O3_13 Cl1_14 O2_13 50.8(10) 3_647 . . . ? O1_14 O2_13 Cl1_14 Cl1_13 96(3) . . . . ? O4_13 O2_13 Cl1_14 Cl1_13 63(2) 3_647 . . . ? O3_13 O2_13 Cl1_14 Cl1_13 -167(3) 3_647 . . . ? O1_13 O2_13 Cl1_14 Cl1_13 -44(2) 3_647 . . . ? Cl1_13 O2_13 Cl1_14 O1_13 -116(3) . . . . ? O1_14 O2_13 Cl1_14 O1_13 -20(2) . . . . ? O4_13 O2_13 Cl1_14 O1_13 -53.1(15) 3_647 . . . ? O3_13 O2_13 Cl1_14 O1_13 77.1(17) 3_647 . . . ? O1_13 O2_13 Cl1_14 O1_13 -160.2(12) 3_647 . . . ? Cl1_13 O2_13 Cl1_14 O4_13 94(3) . . . . ? O1_14 O2_13 Cl1_14 O4_13 -170(2) . . . . ? O4_13 O2_13 Cl1_14 O4_13 156.6(12) 3_647 . . . ? O3_13 O2_13 Cl1_14 O4_13 -73.2(16) 3_647 . . . ? O1_13 O2_13 Cl1_14 O4_13 49.6(15) 3_647 . . . ? Cl1_13 O2_13 Cl1_14 O3_14 143(2) . . . . ? O1_14 O2_13 Cl1_14 O3_14 -120.9(14) . . . . ? O4_13 O2_13 Cl1_14 O3_14 -153.8(17) 3_647 . . . ? O3_13 O2_13 Cl1_14 O3_14 -23.6(18) 3_647 . . . ? O1_13 O2_13 Cl1_14 O3_14 99.1(16) 3_647 . . . ? Cl1_13 O2_13 Cl1_14 O2_14 -63(5) . . . . ? O1_14 O2_13 Cl1_14 O2_14 33(5) . . . . ? O4_13 O2_13 Cl1_14 O2_14 0(5) 3_647 . . . ? O3_13 O2_13 Cl1_14 O2_14 130(4) 3_647 . . . ? O1_13 O2_13 Cl1_14 O2_14 -107(4) 3_647 . . . ? Cl1_13 O2_13 Cl1_14 O1_14 -96(3) . . . . ? O4_13 O2_13 Cl1_14 O1_14 -32.9(17) 3_647 . . . ? O3_13 O2_13 Cl1_14 O1_14 97(2) 3_647 . . . ? O1_13 O2_13 Cl1_14 O1_14 -140(2) 3_647 . . . ? Cl1_13 O2_13 Cl1_14 O4_14 32(2) . . . . ? O1_14 O2_13 Cl1_14 O4_14 127.7(14) . . . . ? O4_13 O2_13 Cl1_14 O4_14 94.8(17) 3_647 . . . ? O3_13 O2_13 Cl1_14 O4_14 -135.0(19) 3_647 . . . ? O1_13 O2_13 Cl1_14 O4_14 -12.3(15) 3_647 . . . ? Cl1_13 O2_13 Cl1_14 O3_13 -9(2) . . . . ? O1_14 O2_13 Cl1_14 O3_13 87.0(17) . . . . ? O4_13 O2_13 Cl1_14 O3_13 54.1(12) 3_647 . . . ? O3_13 O2_13 Cl1_14 O3_13 -175.7(10) 3_647 . . . ? O1_13 O2_13 Cl1_14 O3_13 -52.9(11) 3_647 . . . ? Cl1_14 O1_13 O1_14 Cl1_13 1.3(12) . . . . ? O2_14 O1_13 O1_14 Cl1_13 -44(2) . . . . ? O3_13 O1_13 O1_14 Cl1_13 56.4(10) 3_647 . . . ? O4_13 O1_13 O1_14 Cl1_13 -69(3) 3_647 . . . ? O2_13 O1_13 O1_14 Cl1_13 -29.1(17) 3_647 . . . ? Cl1_13 O1_13 O1_14 Cl1_14 -1.3(12) . . . . ? O2_14 O1_13 O1_14 Cl1_14 -44.9(17) . . . . ? O3_13 O1_13 O1_14 Cl1_14 55.1(11) 3_647 . . . ? O4_13 O1_13 O1_14 Cl1_14 -71(3) 3_647 . . . ? O2_13 O1_13 O1_14 Cl1_14 -30.4(12) 3_647 . . . ? Cl1_14 O1_13 O1_14 O2_13 -35(3) . . . . ? Cl1_13 O1_13 O1_14 O2_13 -36.7(18) . . . . ? O2_14 O1_13 O1_14 O2_13 -80(4) . . . . ? O3_13 O1_13 O1_14 O2_13 20(2) 3_647 . . . ? O4_13 O1_13 O1_14 O2_13 -106(4) 3_647 . . . ? O2_13 O1_13 O1_14 O2_13 -66(3) 3_647 . . . ? Cl1_14 Cl1_13 O1_14 O1_13 -3(2) . . . . ? O4_14 Cl1_13 O1_14 O1_13 126(3) . . . . ? O3_13 Cl1_13 O1_14 O1_13 -72.5(19) 3_647 . . . ? O2_13 Cl1_13 O1_14 O1_13 -145(2) . . . . ? O3_13 Cl1_13 O1_14 O1_13 107.5(19) . . . . ? O2_13 Cl1_13 O1_14 O1_13 35(2) 3_647 . . . ? O4_13 Cl1_13 O1_14 O1_13 136(4) 3_647 . . . ? O4_13 Cl1_13 O1_14 O1_13 -44(4) . . . . ? O1_13 Cl1_13 O1_14 O1_13 180.00(2) 3_647 . . . ? O3_14 Cl1_13 O1_14 O1_13 -55(2) . . . . ? O4_14 Cl1_13 O1_14 Cl1_14 129(3) . . . . ? O3_13 Cl1_13 O1_14 Cl1_14 -69.9(18) 3_647 . . . ? O2_13 Cl1_13 O1_14 Cl1_14 -142.1(18) . . . . ? O3_13 Cl1_13 O1_14 Cl1_14 110.1(18) . . . . ? O2_13 Cl1_13 O1_14 Cl1_14 37.9(18) 3_647 . . . ? O4_13 Cl1_13 O1_14 Cl1_14 138(3) 3_647 . . . ? O4_13 Cl1_13 O1_14 Cl1_14 -42(3) . . . . ? O1_13 Cl1_13 O1_14 Cl1_14 3(2) . . . . ? O1_13 Cl1_13 O1_14 Cl1_14 -177(2) 3_647 . . . ? O3_14 Cl1_13 O1_14 Cl1_14 -51.9(11) . . . . ? Cl1_14 Cl1_13 O1_14 O2_13 142.1(18) . . . . ? O4_14 Cl1_13 O1_14 O2_13 -89(3) . . . . ? O3_13 Cl1_13 O1_14 O2_13 72.2(12) 3_647 . . . ? O3_13 Cl1_13 O1_14 O2_13 -107.8(12) . . . . ? O2_13 Cl1_13 O1_14 O2_13 180.001(19) 3_647 . . . ? O4_13 Cl1_13 O1_14 O2_13 -80(3) 3_647 . . . ? O4_13 Cl1_13 O1_14 O2_13 100(3) . . . . ? O1_13 Cl1_13 O1_14 O2_13 145(2) . . . . ? O1_13 Cl1_13 O1_14 O2_13 -35(2) 3_647 . . . ? O3_14 Cl1_13 O1_14 O2_13 90.2(17) . . . . ? Cl1_13 Cl1_14 O1_14 O1_13 177(3) . . . . ? O4_13 Cl1_14 O1_14 O1_13 -134(4) . . . . ? O3_14 Cl1_14 O1_14 O1_13 -83(3) . . . . ? O2_14 Cl1_14 O1_14 O1_13 40(3) . . . . ? O4_14 Cl1_14 O1_14 O1_13 156(2) . . . . ? O3_13 Cl1_14 O1_14 O1_13 126(2) . . . . ? O2_13 Cl1_14 O1_14 O1_13 -151(3) . . . . ? O1_13 Cl1_14 O1_14 Cl1_13 -177(3) . . . . ? O4_13 Cl1_14 O1_14 Cl1_13 49(3) . . . . ? O3_14 Cl1_14 O1_14 Cl1_13 99.9(13) . . . . ? O2_14 Cl1_14 O1_14 Cl1_13 -136.4(14) . . . . ? O4_14 Cl1_14 O1_14 Cl1_13 -20.9(11) . . . . ? O3_13 Cl1_14 O1_14 Cl1_13 -51.1(15) . . . . ? O2_13 Cl1_14 O1_14 Cl1_13 32.4(16) . . . . ? Cl1_13 Cl1_14 O1_14 O2_13 -32.4(16) . . . . ? O1_13 Cl1_14 O1_14 O2_13 151(3) . . . . ? O4_13 Cl1_14 O1_14 O2_13 17(4) . . . . ? O3_14 Cl1_14 O1_14 O2_13 67.5(17) . . . . ? O2_14 Cl1_14 O1_14 O2_13 -168.8(17) . . . . ? O4_14 Cl1_14 O1_14 O2_13 -53.3(16) . . . . ? O3_13 Cl1_14 O1_14 O2_13 -83.4(13) . . . . ? Cl1_13 O2_13 O1_14 O1_13 43(2) . . . . ? O4_13 O2_13 O1_14 O1_13 133(4) 3_647 . . . ? O3_13 O2_13 O1_14 O1_13 -21(3) 3_647 . . . ? O1_13 O2_13 O1_14 O1_13 63(3) 3_647 . . . ? Cl1_14 O2_13 O1_14 O1_13 28(2) . . . . ? O4_13 O2_13 O1_14 Cl1_13 90.1(19) 3_647 . . . ? O3_13 O2_13 O1_14 Cl1_13 -64.4(10) 3_647 . . . ? O1_13 O2_13 O1_14 Cl1_13 20.5(14) 3_647 . . . ? Cl1_14 O2_13 O1_14 Cl1_13 -14.9(8) . . . . ? Cl1_13 O2_13 O1_14 Cl1_14 14.9(8) . . . . ? O4_13 O2_13 O1_14 Cl1_14 105(2) 3_647 . . . ? O3_13 O2_13 O1_14 Cl1_14 -49.5(12) 3_647 . . . ? O1_13 O2_13 O1_14 Cl1_14 35.4(17) 3_647 . . . ? Cl1_13 Cl1_14 O2_14 O1_13 -96(2) . . . . ? O4_13 Cl1_14 O2_14 O1_13 148(2) . . . . ? O3_14 Cl1_14 O2_14 O1_13 96(2) . . . . ? O1_14 Cl1_14 O2_14 O1_13 -29(2) . . . . ? O4_14 Cl1_14 O2_14 O1_13 -145(2) . . . . ? O3_13 Cl1_14 O2_14 O1_13 -109.1(17) . . . . ? O2_13 Cl1_14 O2_14 O1_13 -56(4) . . . . ? O1_13 Cl1_14 O2_14 Cl1_13 96(2) . . . . ? O4_13 Cl1_14 O2_14 Cl1_13 -116(3) . . . . ? O3_14 Cl1_14 O2_14 Cl1_13 -168(2) . . . . ? O1_14 Cl1_14 O2_14 Cl1_13 67.8(19) . . . . ? O4_14 Cl1_14 O2_14 Cl1_13 -48.8(18) . . . . ? O3_13 Cl1_14 O2_14 Cl1_13 -12.8(19) . . . . ? O2_13 Cl1_14 O2_14 Cl1_13 40(4) . . . . ? O1_14 O1_13 O2_14 Cl1_14 53(2) . . . . ? Cl1_13 O1_13 O2_14 Cl1_14 15.8(6) . . . . ? O3_13 O1_13 O2_14 Cl1_14 -32.3(11) 3_647 . . . ? O4_13 O1_13 O2_14 Cl1_14 62.3(11) 3_647 . . . ? O2_13 O1_13 O2_14 Cl1_14 19(4) 3_647 . . . ? O1_14 O1_13 O2_14 Cl1_13 37.0(19) . . . . ? Cl1_14 O1_13 O2_14 Cl1_13 -15.8(6) . . . . ? O3_13 O1_13 O2_14 Cl1_13 -48.1(10) 3_647 . . . ? O4_13 O1_13 O2_14 Cl1_13 46.4(9) 3_647 . . . ? O2_13 O1_13 O2_14 Cl1_13 3(4) 3_647 . . . ? O4_14 Cl1_13 O2_14 Cl1_14 117(2) . . . . ? O1_14 Cl1_13 O2_14 Cl1_14 -96(2) . . . . ? O3_13 Cl1_13 O2_14 Cl1_14 -16(2) 3_647 . . . ? O2_13 Cl1_13 O2_14 Cl1_14 -68(6) . . . . ? O3_13 Cl1_13 O2_14 Cl1_14 164(2) . . . . ? O2_13 Cl1_13 O2_14 Cl1_14 112(6) 3_647 . . . ? O4_13 Cl1_13 O2_14 Cl1_14 -128(2) 3_647 . . . ? O4_13 Cl1_13 O2_14 Cl1_14 52(2) . . . . ? O1_13 Cl1_13 O2_14 Cl1_14 -73(2) . . . . ? O1_13 Cl1_13 O2_14 Cl1_14 107(2) 3_647 . . . ? O3_14 Cl1_13 O2_14 Cl1_14 9.3(18) . . . . ? Cl1_14 Cl1_13 O2_14 O1_13 73(2) . . . . ? O4_14 Cl1_13 O2_14 O1_13 -171(2) . . . . ? O1_14 Cl1_13 O2_14 O1_13 -23(2) . . . . ? O3_13 Cl1_13 O2_14 O1_13 57.0(17) 3_647 . . . ? O2_13 Cl1_13 O2_14 O1_13 4(6) . . . . ? O3_13 Cl1_13 O2_14 O1_13 -123.0(17) . . . . ? O2_13 Cl1_13 O2_14 O1_13 -176(6) 3_647 . . . ? O4_13 Cl1_13 O2_14 O1_13 -55.8(18) 3_647 . . . ? O4_13 Cl1_13 O2_14 O1_13 124.2(18) . . . . ? O1_13 Cl1_13 O2_14 O1_13 180.001(15) 3_647 . . . ? O3_14 Cl1_13 O2_14 O1_13 82.0(18) . . . . ? Cl1_13 O4_13 O3_14 Cl1_14 22.9(6) . . . . ? O4_14 O4_13 O3_14 Cl1_14 32(2) . . . . ? O2_13 O4_13 O3_14 Cl1_14 -29.9(10) 3_647 . . . ? O3_13 O4_13 O3_14 Cl1_14 47(3) 3_647 . . . ? O1_13 O4_13 O3_14 Cl1_14 64.6(16) 3_647 . . . ? Cl1_14 O4_13 O3_14 Cl1_13 -22.9(6) . . . . ? O4_14 O4_13 O3_14 Cl1_13 9(2) . . . . ? O2_13 O4_13 O3_14 Cl1_13 -52.8(8) 3_647 . . . ? O3_13 O4_13 O3_14 Cl1_13 24(3) 3_647 . . . ? O1_13 O4_13 O3_14 Cl1_13 41.7(14) 3_647 . . . ? Cl1_13 Cl1_14 O3_14 O4_13 -80(2) . . . . ? O1_13 Cl1_14 O3_14 O4_13 169(2) . . . . ? O2_14 Cl1_14 O3_14 O4_13 92(2) . . . . ? O1_14 Cl1_14 O3_14 O4_13 -146(2) . . . . ? O4_14 Cl1_14 O3_14 O4_13 -25(2) . . . . ? O3_13 Cl1_14 O3_14 O4_13 -34(4) . . . . ? O2_13 Cl1_14 O3_14 O4_13 -97(2) . . . . ? O1_13 Cl1_14 O3_14 Cl1_13 -112(2) . . . . ? O4_13 Cl1_14 O3_14 Cl1_13 80(2) . . . . ? O2_14 Cl1_14 O3_14 Cl1_13 171.8(16) . . . . ? O1_14 Cl1_14 O3_14 Cl1_13 -66.1(13) . . . . ? O4_14 Cl1_14 O3_14 Cl1_13 54.1(13) . . . . ? O3_13 Cl1_14 O3_14 Cl1_13 46(3) . . . . ? O2_13 Cl1_14 O3_14 Cl1_13 -17.4(13) . . . . ? Cl1_14 Cl1_13 O3_14 O4_13 88(2) . . . . ? O4_14 Cl1_13 O3_14 O4_13 -9(2) . . . . ? O1_14 Cl1_13 O3_14 O4_13 171(2) . . . . ? O3_13 Cl1_13 O3_14 O4_13 -152(4) 3_647 . . . ? O2_13 Cl1_13 O3_14 O4_13 -116(2) . . . . ? O3_13 Cl1_13 O3_14 O4_13 28(4) . . . . ? O2_13 Cl1_13 O3_14 O4_13 64(2) 3_647 . . . ? O4_13 Cl1_13 O3_14 O4_13 179.997(8) 3_647 . . . ? O1_13 Cl1_13 O3_14 O4_13 136(2) . . . . ? O1_13 Cl1_13 O3_14 O4_13 -44(2) 3_647 . . . ? O4_14 Cl1_13 O3_14 Cl1_14 -96.7(15) . . . . ? O1_14 Cl1_13 O3_14 Cl1_14 83.6(15) . . . . ? O3_13 Cl1_13 O3_14 Cl1_14 120(3) 3_647 . . . ? O2_13 Cl1_13 O3_14 Cl1_14 156.2(17) . . . . ? O3_13 Cl1_13 O3_14 Cl1_14 -60(3) . . . . ? O2_13 Cl1_13 O3_14 Cl1_14 -23.8(17) 3_647 . . . ? O4_13 Cl1_13 O3_14 Cl1_14 92(2) 3_647 . . . ? O4_13 Cl1_13 O3_14 Cl1_14 -88(2) . . . . ? O1_13 Cl1_13 O3_14 Cl1_14 48.4(17) . . . . ? O1_13 Cl1_13 O3_14 Cl1_14 -131.6(17) 3_647 . . . ? O4_13 O3_13 O4_14 Cl1_13 24.3(19) 3_647 . . . ? O2_13 O3_13 O4_14 Cl1_13 -62.0(11) 3_647 . . . ? O1_13 O3_13 O4_14 Cl1_13 85(2) 3_647 . . . ? Cl1_14 O3_13 O4_14 Cl1_13 -22.9(6) . . . . ? Cl1_13 O3_13 O4_14 O4_13 39(2) . . . . ? O4_13 O3_13 O4_14 O4_13 63(4) 3_647 . . . ? O2_13 O3_13 O4_14 O4_13 -23(3) 3_647 . . . ? O1_13 O3_13 O4_14 O4_13 124(4) 3_647 . . . ? Cl1_14 O3_13 O4_14 O4_13 16(2) . . . . ? Cl1_13 O3_13 O4_14 Cl1_14 22.9(6) . . . . ? O4_13 O3_13 O4_14 Cl1_14 47(2) 3_647 . . . ? O2_13 O3_13 O4_14 Cl1_14 -39.1(11) 3_647 . . . ? O1_13 O3_13 O4_14 Cl1_14 108(2) 3_647 . . . ? Cl1_14 Cl1_13 O4_14 O3_13 102(2) . . . . ? O1_14 Cl1_13 O4_14 O3_13 -24(4) . . . . ? O3_13 Cl1_13 O4_14 O3_13 180.000(2) 3_647 . . . ? O2_13 Cl1_13 O4_14 O3_13 -103.8(17) . . . . ? O2_13 Cl1_13 O4_14 O3_13 76.2(17) 3_647 . . . ? O4_13 Cl1_13 O4_14 O3_13 -30(2) 3_647 . . . ? O4_13 Cl1_13 O4_14 O3_13 150(2) . . . . ? O1_13 Cl1_13 O4_14 O3_13 61(4) . . . . ? O1_13 Cl1_13 O4_14 O3_13 -119(4) 3_647 . . . ? O3_14 Cl1_13 O4_14 O3_13 156(2) . . . . ? Cl1_14 Cl1_13 O4_14 O4_13 -48.2(18) . . . . ? O1_14 Cl1_13 O4_14 O4_13 -174(3) . . . . ? O3_13 Cl1_13 O4_14 O4_13 30(2) 3_647 . . . ? O2_13 Cl1_13 O4_14 O4_13 106.4(13) . . . . ? O3_13 Cl1_13 O4_14 O4_13 -150(2) . . . . ? O2_13 Cl1_13 O4_14 O4_13 -73.6(13) 3_647 . . . ? O4_13 Cl1_13 O4_14 O4_13 180.002(8) 3_647 . . . ? O1_13 Cl1_13 O4_14 O4_13 -88(3) . . . . ? O1_13 Cl1_13 O4_14 O4_13 92(3) 3_647 . . . ? O3_14 Cl1_13 O4_14 O4_13 6.4(17) . . . . ? O1_14 Cl1_13 O4_14 Cl1_14 -126(3) . . . . ? O3_13 Cl1_13 O4_14 Cl1_14 78(2) 3_647 . . . ? O2_13 Cl1_13 O4_14 Cl1_14 154.6(18) . . . . ? O3_13 Cl1_13 O4_14 Cl1_14 -102(2) . . . . ? O2_13 Cl1_13 O4_14 Cl1_14 -25.4(18) 3_647 . . . ? O4_13 Cl1_13 O4_14 Cl1_14 -131.8(18) 3_647 . . . ? O4_13 Cl1_13 O4_14 Cl1_14 48.2(18) . . . . ? O1_13 Cl1_13 O4_14 Cl1_14 -40(3) . . . . ? O1_13 Cl1_13 O4_14 Cl1_14 140(3) 3_647 . . . ? O3_14 Cl1_13 O4_14 Cl1_14 54.7(11) . . . . ? O3_14 O4_13 O4_14 O3_13 -54(5) . . . . ? Cl1_14 O4_13 O4_14 O3_13 -20(3) . . . . ? Cl1_13 O4_13 O4_14 O3_13 -42(3) . . . . ? O2_13 O4_13 O4_14 O3_13 25(3) 3_647 . . . ? O3_13 O4_13 O4_14 O3_13 -62(4) 3_647 . . . ? O1_13 O4_13 O4_14 O3_13 -133(4) 3_647 . . . ? O3_14 O4_13 O4_14 Cl1_13 -12(3) . . . . ? Cl1_14 O4_13 O4_14 Cl1_13 22.0(8) . . . . ? O2_13 O4_13 O4_14 Cl1_13 66.7(10) 3_647 . . . ? O3_13 O4_13 O4_14 Cl1_13 -19.7(14) 3_647 . . . ? O1_13 O4_13 O4_14 Cl1_13 -91(2) 3_647 . . . ? O3_14 O4_13 O4_14 Cl1_14 -34(3) . . . . ? Cl1_13 O4_13 O4_14 Cl1_14 -22.0(8) . . . . ? O2_13 O4_13 O4_14 Cl1_14 44.7(11) 3_647 . . . ? O3_13 O4_13 O4_14 Cl1_14 -41.7(14) 3_647 . . . ? O1_13 O4_13 O4_14 Cl1_14 -113(2) 3_647 . . . ? Cl1_13 Cl1_14 O4_14 O3_13 -75(2) . . . . ? O1_13 Cl1_14 O4_14 O3_13 -19(4) . . . . ? O4_13 Cl1_14 O4_14 O3_13 165(2) . . . . ? O3_14 Cl1_14 O4_14 O3_13 -173(2) . . . . ? O2_14 Cl1_14 O4_14 O3_13 66(2) . . . . ? O1_14 Cl1_14 O4_14 O3_13 -51(2) . . . . ? O2_13 Cl1_14 O4_14 O3_13 -93.3(19) . . . . ? O1_13 Cl1_14 O4_14 Cl1_13 55(3) . . . . ? O4_13 Cl1_14 O4_14 Cl1_13 -120(2) . . . . ? O3_14 Cl1_14 O4_14 Cl1_13 -98.7(14) . . . . ? O2_14 Cl1_14 O4_14 Cl1_13 140.6(14) . . . . ? O1_14 Cl1_14 O4_14 Cl1_13 23.8(12) . . . . ? O3_13 Cl1_14 O4_14 Cl1_13 75(2) . . . . ? O2_13 Cl1_14 O4_14 Cl1_13 -18.7(13) . . . . ? Cl1_13 Cl1_14 O4_14 O4_13 120(2) . . . . ? O1_13 Cl1_14 O4_14 O4_13 175(3) . . . . ? O3_14 Cl1_14 O4_14 O4_13 21.5(18) . . . . ? O2_14 Cl1_14 O4_14 O4_13 -99.2(18) . . . . ? O1_14 Cl1_14 O4_14 O4_13 144.0(18) . . . . ? O3_13 Cl1_14 O4_14 O4_13 -165(2) . . . . ? O2_13 Cl1_14 O4_14 O4_13 101.4(13) . . . . ? 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 O1_1 H1_1 O3 0.836(11) 2.47(8) 2.845(7) 109(7) 2_656 O1_1 H2_1 O4_13 0.836(11) 1.90(5) 2.65(3) 148(7) 2_656 O1_1 H2_1 O1_14 0.836(11) 1.95(3) 2.770(14) 167(8) 4_645 O1_1 H2_1 O1_13 0.836(11) 2.12(4) 2.93(3) 163(7) 4_645 O1_1 H2_1 O4_14 0.836(11) 2.46(3) 3.29(2) 171(8) 2_656 O1_2 H1_2 Cl1 0.840(11) 2.275(18) 3.108(5) 171(8) 3_756 O1_2 H2_2 O4_11 0.838(11) 2.04(3) 2.861(13) 165(7) 3_747 O1_2 H2_2 O1_11 0.838(11) 2.27(3) 3.076(17) 162(7) 4_645 O1_3 H1_3 O2_8 0.837(11) 2.03(4) 2.82(2) 156(8) 1_655 O1_3 H1_3 O2_9 0.837(11) 2.48(4) 3.248(14) 153(7) 1_655 O1_3 H1_3 Cl1_8 0.837(11) 2.80(2) 3.634(16) 174(7) 1_655 O1_3 H2_3 O4_10 0.837(11) 2.05(2) 2.885(10) 172(9) 3_656 O1_3 H2_3 O4_7 0.837(11) 2.21(6) 2.94(4) 145(8) 3_656 O1_4 H1_4 O3_9 0.839(11) 1.95(3) 2.755(8) 161(9) 3_656 O1_4 H1_4 O1_8 0.839(11) 2.23(4) 2.99(2) 151(7) 3_656 O1_4 H2_4 O3_10 0.839(11) 1.865(18) 2.702(11) 175(9) 3_656 O1_4 H2_4 O3_7 0.839(11) 2.20(5) 3.03(5) 173(9) 3_656 O1_5 H1_5 O1_8 0.838(11) 2.06(5) 2.779(17) 143(8) 3_656 O1_5 H1_5 O4_9 0.838(11) 2.16(2) 2.986(9) 170(8) 3_656 O1_5 H2_5 O2_10 0.839(11) 2.19(3) 3.007(9) 165(8) . O1_5 H2_5 O2_7 0.839(11) 2.54(6) 3.29(4) 150(7) . O1_6 H1_6 O1_5 0.837(11) 2.43(7) 2.773(6) 106(5) . O1_6 H1_6 O2_7 0.837(11) 2.45(7) 2.99(3) 123(7) . O1_6 H2_6 O4_8 0.840(11) 2.41(7) 2.68(2) 99(5) . O1_6 H2_6 Cl1 0.840(11) 2.28(3) 3.078(4) 160(6) 3_656 N1 H1PY O1_11 0.87 2.02 2.84(2) 154.7 3_747 N1 H1PY O4_11 0.87 2.18 3.037(17) 167.9 4_645 N1 H1PY O2_11 0.87 2.28 2.805(18) 119.1 3_747 N1 H1PY Cl1_11 0.87 2.63 3.388(15) 146.1 3_747 N2 H2PY O2_9 0.77(8) 2.09(8) 2.864(12) 175(8) 3_656 N2 H2PY O2_8 0.77(8) 2.24(8) 2.99(3) 164(8) 3_656 N2 H2PY O4_9 0.77(8) 2.56(8) 3.055(10) 124(7) 3_656 N2 H2PY Cl1_9 0.77(8) 2.87(8) 3.577(8) 153(7) 3_656 N2 H2PY Cl1_8 0.77(8) 2.98(8) 3.681(16) 152(7) 3_656 _diffrn_measured_fraction_theta_max 0.867 _diffrn_reflns_theta_full 26.25 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.418 _refine_diff_density_min -1.050 _refine_diff_density_rms 0.136 # Attachment '- 4.CIF' data_g:\pych2p~1\cbrev~1\cb4sav _database_code_depnum_ccdc_archive 'CCDC 805031' #TrackingRef '- 4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (((2PyHCH2PO3H)Fe2)(ClO4))n _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 Cl3 Fe N3 O21 P3' _chemical_formula_weight 873.51 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' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 23.6196(7) _cell_length_b 23.6196(7) _cell_length_c 9.5024(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4591.0(2) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4753 _cell_measurement_theta_min 2.9202 _cell_measurement_theta_max 29.2623 _exptl_crystal_description cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.896 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2658 _exptl_absorpt_coefficient_mu 1.009 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.3281 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14286 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0476 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 29.33 _reflns_number_total 2581 _reflns_number_gt 1959 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, V. 1.171.34.40' _computing_cell_refinement 'CrysAlisPro, V. 171.34.40' _computing_data_reduction 'CrysAlisPro, V. 1.171.34.40' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Olex2 _computing_publication_material 'XCIF, Bruker SHELXTL v. 6.12' _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. The hydrogens were geometrically placed upon and refined as riding on all carbon atoms with Ueq(H) = 1.2* Ueq(C). The hydrogen atom on N1, H1py, was found in the difference map, and refined with Ueq(H) = 1.5* Ueq(N). The The hydrogen on the phosphonate oxygen wasfound in the difference map, and refined as Ueq(H) = 1.5* Ueq(O). ; _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^)+(0.0350P)^2^+15.7889P] 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 2581 _refine_ls_number_parameters 149 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.0904 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _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 Fe1 Fe 0.0000 0.0000 0.5000 0.01096(18) Uani 1 6 d S . . Fe2 Fe 0.0000 0.0000 0.0000 0.00994(18) Uani 1 6 d S . . Cl1 Cl 0.21721(3) -0.04952(4) -0.09742(7) 0.02963(18) Uani 1 1 d . . . P1 P 0.10372(3) 0.01317(3) 0.24197(6) 0.01257(15) Uani 1 1 d . . . N1 N 0.19576(12) -0.05775(12) 0.2874(3) 0.0276(5) Uani 1 1 d . . . H1PY H 0.2186 -0.0306 0.2160 0.033 Uiso 1 1 d R . . O1 O 0.07450(9) 0.01133(9) 0.38229(17) 0.0204(4) Uani 1 1 d . . . O2 O 0.07979(8) 0.03515(8) 0.11873(16) 0.0146(4) Uani 1 1 d . . . O3 O 0.17932(8) 0.05843(9) 0.25651(19) 0.0224(4) Uani 1 1 d . . . H3 H 0.1980 0.0828 0.1979 0.034 Uiso 1 1 d R . . O4 O 0.26525(13) -0.06743(16) -0.0836(4) 0.0832(11) Uani 1 1 d . . . O5 O 0.15364(10) -0.10634(10) -0.0740(2) 0.0334(5) Uani 1 1 d . . . O6 O 0.22780(14) -0.00138(12) 0.0070(3) 0.0619(8) Uani 1 1 d . . . O7 O 0.21894(13) -0.02266(13) -0.2311(2) 0.0594(8) Uani 1 1 d . . . C1 C 0.09396(13) -0.06601(13) 0.2068(3) 0.0208(6) Uani 1 1 d . . . H1A H 0.0470 -0.0994 0.2117 0.025 Uiso 1 1 calc R . . H1B H 0.1095 -0.0665 0.1103 0.025 Uiso 1 1 calc R . . C2 C 0.13113(14) -0.08300(13) 0.3096(3) 0.0229(6) Uani 1 1 d . . . C3 C 0.10433(15) -0.12090(15) 0.4265(3) 0.0305(7) Uani 1 1 d . . . H3A H 0.0591 -0.1389 0.4462 0.037 Uiso 1 1 calc R . . C4 C 0.14348(16) -0.13293(16) 0.5164(3) 0.0336(7) Uani 1 1 d . . . H4A H 0.1247 -0.1594 0.5974 0.040 Uiso 1 1 calc R . . C5 C 0.20853(16) -0.10718(16) 0.4897(3) 0.0338(7) Uani 1 1 d . . . H5A H 0.2352 -0.1158 0.5507 0.041 Uiso 1 1 calc R . . C6 C 0.23458(15) -0.06855(15) 0.3728(3) 0.0337(7) Uani 1 1 d . . . H6A H 0.2799 -0.0496 0.3526 0.040 Uiso 1 1 calc R . . 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 Fe1 0.0128(3) 0.0128(3) 0.0073(4) 0.000 0.000 0.00641(13) Fe2 0.0118(3) 0.0118(3) 0.0063(4) 0.000 0.000 0.00588(13) Cl1 0.0243(4) 0.0324(4) 0.0261(4) -0.0005(3) -0.0006(3) 0.0096(3) P1 0.0125(3) 0.0159(3) 0.0099(3) 0.0000(2) -0.0001(2) 0.0075(3) N1 0.0305(13) 0.0286(13) 0.0288(13) 0.0051(11) 0.0014(11) 0.0185(11) O1 0.0207(9) 0.0318(11) 0.0119(9) 0.0007(7) 0.0035(7) 0.0154(8) O2 0.0151(8) 0.0158(9) 0.0121(8) -0.0003(7) -0.0041(7) 0.0071(7) O3 0.0142(9) 0.0275(10) 0.0190(9) 0.0061(8) -0.0014(7) 0.0056(8) O4 0.0329(15) 0.082(2) 0.143(3) 0.014(2) 0.0044(18) 0.0352(16) O5 0.0253(11) 0.0289(11) 0.0379(12) 0.0029(9) -0.0023(9) 0.0075(9) O6 0.078(2) 0.0362(14) 0.0341(13) -0.0073(11) 0.0146(13) 0.0003(13) O7 0.0582(17) 0.0558(17) 0.0288(13) 0.0099(12) -0.0016(12) 0.0021(14) C1 0.0240(14) 0.0211(13) 0.0211(13) -0.0039(11) -0.0055(11) 0.0142(12) C2 0.0281(15) 0.0236(14) 0.0246(14) -0.0039(11) -0.0016(11) 0.0187(12) C3 0.0347(17) 0.0341(16) 0.0302(16) 0.0047(13) 0.0044(13) 0.0230(14) C4 0.0467(19) 0.0437(19) 0.0234(15) 0.0040(13) 0.0038(14) 0.0323(16) C5 0.0456(19) 0.0430(19) 0.0282(16) -0.0033(14) -0.0080(14) 0.0336(16) C6 0.0294(16) 0.0362(17) 0.0429(18) 0.0009(14) -0.0046(14) 0.0218(14) _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 Fe1 O1 1.9870(17) 12_556 ? Fe1 O1 1.9870(17) 2 ? Fe1 O1 1.9870(17) 3 ? Fe1 O1 1.9870(17) . ? Fe1 O1 1.9870(17) 11_556 ? Fe1 O1 1.9870(17) 10_556 ? Fe2 O2 1.9873(16) . ? Fe2 O2 1.9873(16) 12 ? Fe2 O2 1.9873(16) 10 ? Fe2 O2 1.9873(16) 2 ? Fe2 O2 1.9873(16) 11 ? Fe2 O2 1.9873(16) 3 ? Cl1 O4 1.402(3) . ? Cl1 O7 1.412(2) . ? Cl1 O6 1.433(3) . ? Cl1 O5 1.446(2) . ? P1 O1 1.4921(17) . ? P1 O2 1.5013(17) . ? P1 O3 1.5624(18) . ? P1 C1 1.798(3) . ? N1 C6 1.341(4) . ? N1 C2 1.349(4) . ? N1 H1PY 0.9040 . ? O3 H3 0.7630 . ? C1 C2 1.496(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.367(4) . ? C3 C4 1.388(4) . ? C3 H3A 0.9500 . ? C4 C5 1.364(5) . ? C4 H4A 0.9500 . ? C5 C6 1.372(4) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? 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 Fe1 O1 88.59(7) 12_556 2 ? O1 Fe1 O1 180.00 12_556 3 ? O1 Fe1 O1 91.42(7) 2 3 ? O1 Fe1 O1 88.59(7) 12_556 . ? O1 Fe1 O1 91.41(7) 2 . ? O1 Fe1 O1 91.41(7) 3 . ? O1 Fe1 O1 91.41(7) 12_556 11_556 ? O1 Fe1 O1 180.00 2 11_556 ? O1 Fe1 O1 88.59(7) 3 11_556 ? O1 Fe1 O1 88.59(7) . 11_556 ? O1 Fe1 O1 91.41(7) 12_556 10_556 ? O1 Fe1 O1 88.59(7) 2 10_556 ? O1 Fe1 O1 88.59(7) 3 10_556 ? O1 Fe1 O1 180.00 . 10_556 ? O1 Fe1 O1 91.41(7) 11_556 10_556 ? O2 Fe2 O2 89.05(7) . 12 ? O2 Fe2 O2 180.00 . 10 ? O2 Fe2 O2 90.95(7) 12 10 ? O2 Fe2 O2 90.95(7) . 2 ? O2 Fe2 O2 89.05(7) 12 2 ? O2 Fe2 O2 89.05(7) 10 2 ? O2 Fe2 O2 89.05(7) . 11 ? O2 Fe2 O2 90.95(7) 12 11 ? O2 Fe2 O2 90.95(7) 10 11 ? O2 Fe2 O2 180.00 2 11 ? O2 Fe2 O2 90.95(7) . 3 ? O2 Fe2 O2 180.00 12 3 ? O2 Fe2 O2 89.05(7) 10 3 ? O2 Fe2 O2 90.95(7) 2 3 ? O2 Fe2 O2 89.05(7) 11 3 ? O4 Cl1 O7 112.0(2) . . ? O4 Cl1 O6 109.1(2) . . ? O7 Cl1 O6 108.19(17) . . ? O4 Cl1 O5 109.08(16) . . ? O7 Cl1 O5 109.84(14) . . ? O6 Cl1 O5 108.54(14) . . ? O1 P1 O2 117.29(10) . . ? O1 P1 O3 107.14(10) . . ? O2 P1 O3 109.36(10) . . ? O1 P1 C1 108.60(12) . . ? O2 P1 C1 109.89(11) . . ? O3 P1 C1 103.68(12) . . ? C6 N1 C2 123.4(3) . . ? C6 N1 H1PY 111.5 . . ? C2 N1 H1PY 125.0 . . ? P1 O1 Fe1 150.76(12) . . ? P1 O2 Fe2 137.80(10) . . ? P1 O3 H3 118.9 . . ? C2 C1 P1 111.74(18) . . ? C2 C1 H1A 109.3 . . ? P1 C1 H1A 109.3 . . ? C2 C1 H1B 109.3 . . ? P1 C1 H1B 109.3 . . ? H1A C1 H1B 107.9 . . ? N1 C2 C3 117.9(3) . . ? N1 C2 C1 117.7(2) . . ? C3 C2 C1 124.4(3) . . ? C2 C3 C4 119.7(3) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C5 C4 C3 120.7(3) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C4 C5 C6 118.5(3) . . ? C4 C5 H5A 120.7 . . ? C6 C5 H5A 120.7 . . ? N1 C6 C5 119.7(3) . . ? N1 C6 H6A 120.2 . . ? C5 C6 H6A 120.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 P1 O1 Fe1 30.1(3) . . . . ? O3 P1 O1 Fe1 153.4(2) . . . . ? C1 P1 O1 Fe1 -95.2(3) . . . . ? O1 Fe1 O1 P1 -138.8(2) 12_556 . . . ? O1 Fe1 O1 P1 -50.2(2) 2 . . . ? O1 Fe1 O1 P1 41.2(2) 3 . . . ? O1 Fe1 O1 P1 129.8(2) 11_556 . . . ? O1 Fe1 O1 P1 93(70) 10_556 . . . ? O1 P1 O2 Fe2 -73.18(18) . . . . ? O3 P1 O2 Fe2 164.63(14) . . . . ? C1 P1 O2 Fe2 51.45(19) . . . . ? O2 Fe2 O2 P1 -176.03(16) 12 . . . ? O2 Fe2 O2 P1 49(36) 10 . . . ? O2 Fe2 O2 P1 94.93(10) 2 . . . ? O2 Fe2 O2 P1 -85.07(10) 11 . . . ? O2 Fe2 O2 P1 3.97(16) 3 . . . ? O1 P1 C1 C2 -64.1(2) . . . . ? O2 P1 C1 C2 166.39(18) . . . . ? O3 P1 C1 C2 49.6(2) . . . . ? C6 N1 C2 C3 0.8(4) . . . . ? C6 N1 C2 C1 179.0(3) . . . . ? P1 C1 C2 N1 -80.8(3) . . . . ? P1 C1 C2 C3 97.3(3) . . . . ? N1 C2 C3 C4 -0.9(4) . . . . ? C1 C2 C3 C4 -179.1(3) . . . . ? C2 C3 C4 C5 0.2(5) . . . . ? C3 C4 C5 C6 0.7(5) . . . . ? C2 N1 C6 C5 0.1(4) . . . . ? C4 C5 C6 N1 -0.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 26.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.469 _refine_diff_density_min -0.497 _refine_diff_density_rms 0.084 # Attachment '- 5.CIF' data_g:\pych2po\ar140f~1\ar140 _database_code_depnum_ccdc_archive 'CCDC 805032' #TrackingRef '- 5.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (((2PyHCH2PO3H)Fe(H2O))ClO4)n _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H20 Cl2 Fe N2 O16 P2' _chemical_formula_weight 636.99 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.5170(8) _cell_length_b 8.2636(4) _cell_length_c 10.3910(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.108(4) _cell_angle_gamma 90.00 _cell_volume 1151.75(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3262 _cell_measurement_theta_min 2.4597 _cell_measurement_theta_max 29.2873 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.837 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 1.107 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'not measured' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 10.3281 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8350 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 26.25 _reflns_number_total 2322 _reflns_number_gt 1790 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, V. 1.171.34.40' _computing_cell_refinement 'CrysAlisPro, V. 171.34.40' _computing_data_reduction 'CrysAlisPro, V. 1.171.34.40' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Olex2 _computing_publication_material 'XCIF, Bruker SHELXTL v. 6.12' _refine_special_details ; some twinning suspected but unable to solve when attempted. Thermal parameters of disordered perchlorate are quite high. 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^)+(0.1433P)^2^+8.7927P] 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 2322 _refine_ls_number_parameters 173 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1014 _refine_ls_R_factor_gt 0.0803 _refine_ls_wR_factor_ref 0.2536 _refine_ls_wR_factor_gt 0.2291 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.000 _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 Fe1 Fe 0.0000 0.0000 0.0000 0.0348(5) Uani 1 2 d SD . . Cl1 Cl -0.32842(12) -0.1169(2) 0.24342(14) 0.0328(5) Uani 1 1 d . . . P1 P -0.06557(11) 0.32196(18) 0.19943(13) 0.0182(4) Uani 1 1 d . . . O1 O -0.0631(3) 0.1478(5) 0.1578(4) 0.0186(9) Uani 1 1 d . . . O2 O 0.0400(4) 0.3935(7) 0.1846(5) 0.0430(15) Uani 1 1 d . . . H2A H 0.0508 0.4745 0.2331 0.064 Uiso 1 1 calc R . . O3 O -0.0935(3) 0.3527(5) 0.3332(3) 0.0177(9) Uani 1 1 d . . . O4 O 0.1419(4) 0.1633(6) 0.0022(5) 0.0301(11) Uani 1 1 d D . . O6 O -0.4115(5) -0.0201(11) 0.2519(7) 0.080(3) Uani 1 1 d . . . O7 O -0.3204(4) -0.1645(9) 0.1130(5) 0.0527(16) Uani 1 1 d . . . O8 O -0.238(3) -0.034(6) 0.290(3) 0.113(18) Uani 0.33 1 d P . . N1 N -0.2603(4) 0.2327(6) -0.0330(4) 0.0210(11) Uani 1 1 d . . . H1 H -0.2082 0.1995 -0.0686 0.025 Uiso 1 1 calc R . . C1 C -0.2486(5) 0.3578(8) 0.0486(5) 0.0265(14) Uani 1 1 d . . . C2 C -0.3310(8) 0.4117(12) 0.0995(7) 0.055(3) Uani 1 1 d . . . H2 H -0.3258 0.5025 0.1561 0.065 Uiso 1 1 calc R . . C3 C -0.4202(9) 0.337(2) 0.0699(11) 0.093(6) Uani 1 1 d . . . H3 H -0.4767 0.3745 0.1070 0.111 Uiso 1 1 calc R . . C4 C -0.4295(6) 0.209(2) -0.0118(10) 0.089(5) Uani 1 1 d . . . H4 H -0.4919 0.1562 -0.0332 0.107 Uiso 1 1 calc R . . C5 C -0.3456(6) 0.1557(11) -0.0633(7) 0.043(2) Uani 1 1 d . . . H5 H -0.3492 0.0650 -0.1199 0.052 Uiso 1 1 calc R . . C6 C -0.1468(6) 0.4293(8) 0.0772(6) 0.0325(16) Uani 1 1 d . . . H6B H -0.1532 0.5426 0.1060 0.039 Uiso 1 1 calc R . . H6A H -0.1153 0.4316 -0.0039 0.039 Uiso 1 1 calc R . . H4B H 0.187(3) 0.151(8) -0.049(6) 0.049 Uiso 1 1 d D . . H4A H 0.163(4) 0.226(9) 0.066(5) 0.049 Uiso 1 1 d D . . O8B O -0.2411(15) -0.084(2) 0.324(2) 0.028(4) Uiso 0.33 1 d P . . O8A O -0.2537(15) 0.028(2) 0.2506(18) 0.027(4) Uiso 0.33 1 d P . . O5B O -0.3668(10) -0.2735(16) 0.3038(12) 0.052(3) Uiso 0.50 1 d P . . O5A O -0.3024(13) -0.230(2) 0.3342(16) 0.074(4) 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 Fe1 0.0352(9) 0.0454(9) 0.0247(8) 0.0033(6) 0.0071(6) 0.0081(6) Cl1 0.0234(8) 0.0548(11) 0.0191(8) -0.0007(7) -0.0012(6) 0.0035(7) P1 0.0236(8) 0.0247(8) 0.0070(7) -0.0061(5) 0.0044(5) -0.0108(6) O1 0.025(2) 0.024(2) 0.0078(18) -0.0021(14) 0.0025(15) 0.0007(16) O2 0.043(3) 0.066(4) 0.024(2) -0.024(2) 0.023(2) -0.037(3) O3 0.019(2) 0.027(2) 0.0073(18) -0.0042(14) 0.0045(14) -0.0089(16) O4 0.028(3) 0.033(3) 0.030(2) -0.0014(19) 0.0085(19) -0.005(2) O6 0.051(4) 0.141(8) 0.053(4) 0.035(4) 0.030(3) 0.057(5) O7 0.041(3) 0.091(5) 0.028(3) -0.009(3) 0.012(2) -0.007(3) O8 0.08(2) 0.23(5) 0.035(18) -0.04(2) 0.023(15) -0.10(3) N1 0.023(3) 0.027(3) 0.013(2) 0.0016(19) 0.0038(19) 0.004(2) C1 0.042(4) 0.027(3) 0.011(3) 0.010(2) 0.006(2) 0.018(3) C2 0.065(6) 0.075(6) 0.028(4) 0.014(4) 0.024(4) 0.053(5) C3 0.064(8) 0.180(15) 0.042(6) 0.054(8) 0.037(5) 0.080(9) C4 0.016(4) 0.207(16) 0.043(6) 0.070(8) -0.004(4) -0.010(6) C5 0.033(4) 0.072(6) 0.021(3) 0.015(3) -0.011(3) -0.014(4) C6 0.065(5) 0.015(3) 0.015(3) 0.002(2) -0.003(3) -0.006(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 Fe1 O1 2.292(4) 3 ? Fe1 O1 2.292(4) . ? Fe1 O4 2.343(5) . ? Fe1 O4 2.343(5) 3 ? Fe1 O3 2.354(4) 2_545 ? Fe1 O3 2.354(4) 4_565 ? Cl1 O5A 1.344(16) . ? Cl1 O8B 1.39(2) . ? Cl1 O6 1.390(6) . ? Cl1 O7 1.428(6) . ? Cl1 O8 1.44(3) . ? Cl1 O5B 1.555(13) . ? Cl1 O8A 1.56(2) . ? P1 O1 1.504(4) . ? P1 O3 1.507(4) . ? P1 O2 1.570(5) . ? P1 C6 1.805(7) . ? O2 H2A 0.8400 . ? O3 Fe1 2.354(4) 2 ? O4 H4B 0.862(10) . ? O4 H4A 0.867(10) . ? N1 C5 1.320(9) . ? N1 C1 1.334(8) . ? N1 H1 0.8800 . ? C1 C2 1.366(10) . ? C1 C6 1.494(10) . ? C2 C3 1.357(19) . ? C2 H2 0.9500 . ? C3 C4 1.35(2) . ? C3 H3 0.9500 . ? C4 C5 1.383(15) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6B 0.9900 . ? C6 H6A 0.9900 . ? 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 Fe1 O1 180.0 3 . ? O1 Fe1 O4 86.41(15) 3 . ? O1 Fe1 O4 93.59(15) . . ? O1 Fe1 O4 93.59(15) 3 3 ? O1 Fe1 O4 86.41(15) . 3 ? O4 Fe1 O4 180.0 . 3 ? O1 Fe1 O3 92.17(13) 3 2_545 ? O1 Fe1 O3 87.83(13) . 2_545 ? O4 Fe1 O3 85.76(16) . 2_545 ? O4 Fe1 O3 94.24(16) 3 2_545 ? O1 Fe1 O3 87.83(13) 3 4_565 ? O1 Fe1 O3 92.17(13) . 4_565 ? O4 Fe1 O3 94.24(16) . 4_565 ? O4 Fe1 O3 85.76(16) 3 4_565 ? O3 Fe1 O3 180.0 2_545 4_565 ? O5A Cl1 O8B 65.2(11) . . ? O5A Cl1 O6 119.9(8) . . ? O8B Cl1 O6 118.9(9) . . ? O5A Cl1 O7 115.5(8) . . ? O8B Cl1 O7 117.9(8) . . ? O6 Cl1 O7 112.1(4) . . ? O5A Cl1 O8 87(2) . . ? O8B Cl1 O8 22.4(19) . . ? O6 Cl1 O8 111(2) . . ? O7 Cl1 O8 107.1(11) . . ? O5A Cl1 O5B 37.8(8) . . ? O8B Cl1 O5B 102.6(9) . . ? O6 Cl1 O5B 98.1(6) . . ? O7 Cl1 O5B 102.8(5) . . ? O8 Cl1 O5B 125.0(19) . . ? O5A Cl1 O8A 112.9(10) . . ? O8B Cl1 O8A 47.6(11) . . ? O6 Cl1 O8A 94.4(8) . . ? O7 Cl1 O8A 97.6(8) . . ? O8 Cl1 O8A 26(2) . . ? O5B Cl1 O8A 149.8(8) . . ? O1 P1 O3 116.3(2) . . ? O1 P1 O2 106.2(3) . . ? O3 P1 O2 111.2(2) . . ? O1 P1 C6 107.5(3) . . ? O3 P1 C6 111.5(3) . . ? O2 P1 C6 103.1(3) . . ? P1 O1 Fe1 137.6(2) . . ? P1 O2 H2A 109.5 . . ? P1 O3 Fe1 126.4(2) . 2 ? Fe1 O4 H4B 124(2) . . ? Fe1 O4 H4A 123(2) . . ? H4B O4 H4A 111(3) . . ? C5 N1 C1 123.9(6) . . ? C5 N1 H1 118.1 . . ? C1 N1 H1 118.1 . . ? N1 C1 C2 117.4(8) . . ? N1 C1 C6 117.9(6) . . ? C2 C1 C6 124.7(8) . . ? C3 C2 C1 120.5(10) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C4 C3 C2 120.7(8) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 118.2(10) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? N1 C5 C4 119.3(10) . . ? N1 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C1 C6 P1 114.2(4) . . ? C1 C6 H6B 108.7 . . ? P1 C6 H6B 108.7 . . ? C1 C6 H6A 108.7 . . ? P1 C6 H6A 108.7 . . ? H6B C6 H6A 107.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 P1 O1 Fe1 -163.9(3) . . . . ? O2 P1 O1 Fe1 -39.5(4) . . . . ? C6 P1 O1 Fe1 70.3(4) . . . . ? O1 Fe1 O1 P1 -77(100) 3 . . . ? O4 Fe1 O1 P1 34.7(4) . . . . ? O4 Fe1 O1 P1 -145.3(4) 3 . . . ? O3 Fe1 O1 P1 120.3(4) 2_545 . . . ? O3 Fe1 O1 P1 -59.7(4) 4_565 . . . ? O1 P1 O3 Fe1 125.0(3) . . . 2 ? O2 P1 O3 Fe1 3.2(4) . . . 2 ? C6 P1 O3 Fe1 -111.2(3) . . . 2 ? C5 N1 C1 C2 -2.4(9) . . . . ? C5 N1 C1 C6 177.9(6) . . . . ? N1 C1 C2 C3 1.7(11) . . . . ? C6 C1 C2 C3 -178.6(7) . . . . ? C1 C2 C3 C4 -0.9(14) . . . . ? C2 C3 C4 C5 0.5(15) . . . . ? C1 N1 C5 C4 2.0(10) . . . . ? C3 C4 C5 N1 -1.0(13) . . . . ? N1 C1 C6 P1 -82.1(6) . . . . ? C2 C1 C6 P1 98.3(7) . . . . ? O1 P1 C6 C1 54.4(5) . . . . ? O3 P1 C6 C1 -74.2(5) . . . . ? O2 P1 C6 C1 166.3(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 O4 H4A O2 0.867(10) 2.59(5) 3.122(7) 121(4) . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.25 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.935 _refine_diff_density_min -1.845 _refine_diff_density_rms 0.193 # Attachment '- 6.CIF' data_g:\pych2po\pych2p~2\ar560a _database_code_depnum_ccdc_archive 'CCDC 805033' #TrackingRef '- 6.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((2PyCH2PO3)AgPb(NO3))n _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H6 Ag N2 O6 P Pb' _chemical_formula_weight 548.16 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.9027(19) _cell_length_b 9.8255(14) _cell_length_c 7.9178(11) _cell_angle_alpha 90.00 _cell_angle_beta 104.871(2) _cell_angle_gamma 90.00 _cell_volume 1045.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 2162 _cell_measurement_theta_min 2.568 _cell_measurement_theta_max 28.2445 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 18.129 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7985 _exptl_absorpt_correction_T_max 0.8395 _exptl_absorpt_process_details 'SADABS: SAINT+, 2001' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <0.01 _diffrn_reflns_number 5763 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2384 _reflns_number_gt 1954 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v. 5.626' _computing_cell_refinement 'Bruker SAINT+ v. 6.36a' _computing_data_reduction 'Bruker SAINT+ v. 6.36a' _computing_structure_solution 'XS, Bruker SHELXTL v. 6.12' _computing_structure_refinement 'XL, Bruker SHELXTL v. 6.12' _computing_molecular_graphics 'XP, Bruker SHELXTL v. 6.12' _computing_publication_material 'XCIF, Bruker SHELXTL v. 6.12' _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^)+(0.0577P)^2^+0.7391P] 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 2384 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1080 _refine_ls_wR_factor_gt 0.0993 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.000 _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 Pb1 Pb 0.45330(3) 0.77920(3) 0.48718(4) 0.01396(14) Uani 1 1 d . . . Ag1 Ag 0.71307(7) 0.87239(8) 0.74762(10) 0.0261(2) Uani 1 1 d . . . P1 P 0.61336(19) 0.5448(2) 0.8153(3) 0.0117(5) Uani 1 1 d . . . O1 O 0.5684(6) 0.6762(8) 0.7291(9) 0.0237(16) Uani 1 1 d . . . O2 O 0.5626(5) 0.4145(7) 0.7352(8) 0.0180(15) Uani 1 1 d . . . O3 O 0.6121(5) 0.5475(7) 1.0104(8) 0.0173(15) Uani 1 1 d . . . O6 O 0.1765(7) 0.6041(9) 0.5677(12) 0.039(2) Uani 1 1 d . . . O5 O 0.2493(6) 0.7595(8) 0.4516(11) 0.0294(19) Uani 1 1 d . . . O4 O 0.3381(6) 0.6061(8) 0.6227(9) 0.0259(17) Uani 1 1 d . . . N1 N 0.8262(7) 0.7468(9) 0.9246(11) 0.0178(18) Uani 1 1 d . . . N2 N 0.2517(6) 0.6577(8) 0.5471(10) 0.0164(17) Uani 1 1 d . . . C1 C 0.7415(7) 0.5367(9) 0.7967(12) 0.0136(19) Uani 1 1 d . . . H1A H 0.7603 0.4405 0.7973 0.016 Uiso 1 1 calc R . . H1B H 0.7427 0.5738 0.6823 0.016 Uiso 1 1 calc R . . C2 C 0.8198(8) 0.6082(10) 0.9320(13) 0.018(2) Uani 1 1 d . . . C3 C 0.8880(9) 0.5375(12) 1.0589(14) 0.030(3) Uani 1 1 d . . . H3A H 0.8801 0.4431 1.0696 0.036 Uiso 1 1 calc R . . C4 C 0.9671(9) 0.6019(12) 1.1701(15) 0.030(3) Uani 1 1 d . . . H4A H 1.0140 0.5524 1.2544 0.035 Uiso 1 1 calc R . . C5 C 0.9762(9) 0.7417(12) 1.1550(15) 0.027(3) Uani 1 1 d . . . H5A H 1.0302 0.7894 1.2260 0.033 Uiso 1 1 calc R . . C6 C 0.9038(9) 0.8069(11) 1.0333(13) 0.023(2) Uani 1 1 d . . . H6A H 0.9091 0.9019 1.0252 0.027 Uiso 1 1 calc R . . 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 Pb1 0.0189(2) 0.0104(2) 0.0112(2) 0.00069(13) 0.00133(15) -0.00010(14) Ag1 0.0319(5) 0.0179(4) 0.0206(4) 0.0047(3) -0.0075(4) 0.0022(3) P1 0.0159(13) 0.0081(11) 0.0101(11) -0.0008(8) 0.0016(10) -0.0002(9) O1 0.021(4) 0.021(4) 0.024(4) 0.009(3) -0.002(3) 0.004(3) O2 0.025(4) 0.013(3) 0.015(3) -0.006(3) 0.003(3) -0.003(3) O3 0.023(4) 0.021(4) 0.007(3) -0.002(3) 0.000(3) -0.002(3) O6 0.025(5) 0.039(5) 0.051(5) -0.006(4) 0.008(4) -0.015(4) O5 0.032(5) 0.019(4) 0.035(5) 0.009(3) 0.006(4) -0.001(3) O4 0.030(5) 0.021(4) 0.024(4) -0.001(3) 0.001(3) -0.007(3) N1 0.020(5) 0.017(4) 0.012(4) 0.002(3) -0.003(4) -0.001(4) N2 0.020(5) 0.015(4) 0.015(4) -0.002(3) 0.005(4) -0.001(4) C1 0.012(5) 0.010(4) 0.019(5) -0.003(4) 0.003(4) 0.000(3) C2 0.017(5) 0.016(5) 0.021(5) -0.003(4) 0.001(4) -0.004(4) C3 0.024(6) 0.022(6) 0.033(6) 0.009(5) -0.011(5) 0.002(5) C4 0.031(7) 0.027(6) 0.028(6) 0.001(5) 0.002(5) 0.009(5) C5 0.026(7) 0.028(6) 0.023(6) 0.001(5) -0.001(5) -0.011(5) C6 0.026(6) 0.016(5) 0.019(5) 0.002(4) -0.007(5) -0.004(4) _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 Pb1 O1 2.383(7) . ? Pb1 O2 2.564(6) 3_666 ? Pb1 O2 2.626(7) 2_656 ? Pb1 O4 2.737(8) . ? Pb1 O3 2.757(7) 4_575 ? Ag1 O3 2.183(6) 4_575 ? Ag1 N1 2.197(9) . ? P1 O1 1.518(8) . ? P1 O2 1.519(7) . ? P1 O3 1.550(6) . ? P1 C1 1.826(10) . ? O2 Pb1 2.564(6) 3_666 ? O2 Pb1 2.626(7) 2_646 ? O3 Ag1 2.183(6) 4_576 ? O3 Pb1 2.757(7) 4_576 ? O6 N2 1.218(11) . ? O5 N2 1.249(11) . ? O4 N2 1.300(11) . ? N1 C6 1.334(14) . ? N1 C2 1.367(12) . ? C1 C2 1.493(13) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 C3 1.379(15) . ? C3 C4 1.374(16) . ? C3 H3A 0.9400 . ? C4 C5 1.387(16) . ? C4 H4A 0.9400 . ? C5 C6 1.362(16) . ? C5 H5A 0.9400 . ? C6 H6A 0.9400 . ? 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 Pb1 O2 99.1(3) . 3_666 ? O1 Pb1 O2 74.1(2) . 2_656 ? O2 Pb1 O2 160.0(2) 3_666 2_656 ? O1 Pb1 O4 76.2(2) . . ? O2 Pb1 O4 81.5(2) 3_666 . ? O2 Pb1 O4 78.6(2) 2_656 . ? O1 Pb1 O3 81.2(2) . 4_575 ? O2 Pb1 O3 115.5(2) 3_666 4_575 ? O2 Pb1 O3 82.5(2) 2_656 4_575 ? O4 Pb1 O3 153.8(2) . 4_575 ? O3 Ag1 N1 161.5(3) 4_575 . ? O1 P1 O2 115.8(4) . . ? O1 P1 O3 109.0(4) . . ? O2 P1 O3 107.9(4) . . ? O1 P1 C1 107.4(4) . . ? O2 P1 C1 106.7(4) . . ? O3 P1 C1 110.0(4) . . ? P1 O1 Pb1 146.8(5) . . ? P1 O2 Pb1 149.4(4) . 3_666 ? P1 O2 Pb1 102.0(3) . 2_646 ? Pb1 O2 Pb1 100.8(2) 3_666 2_646 ? P1 O3 Ag1 134.0(4) . 4_576 ? P1 O3 Pb1 99.1(3) . 4_576 ? Ag1 O3 Pb1 99.3(2) 4_576 4_576 ? N2 O4 Pb1 98.1(5) . . ? C6 N1 C2 117.6(9) . . ? C6 N1 Ag1 119.4(7) . . ? C2 N1 Ag1 122.9(7) . . ? O6 N2 O5 122.4(9) . . ? O6 N2 O4 119.6(9) . . ? O5 N2 O4 118.0(8) . . ? C2 C1 P1 117.9(7) . . ? C2 C1 H1A 107.8 . . ? P1 C1 H1A 107.8 . . ? C2 C1 H1B 107.8 . . ? P1 C1 H1B 107.8 . . ? H1A C1 H1B 107.2 . . ? N1 C2 C3 119.6(10) . . ? N1 C2 C1 118.8(9) . . ? C3 C2 C1 121.6(9) . . ? C4 C3 C2 121.5(11) . . ? C4 C3 H3A 119.3 . . ? C2 C3 H3A 119.3 . . ? C3 C4 C5 118.5(11) . . ? C3 C4 H4A 120.8 . . ? C5 C4 H4A 120.8 . . ? C6 C5 C4 117.4(11) . . ? C6 C5 H5A 121.3 . . ? C4 C5 H5A 121.3 . . ? N1 C6 C5 125.2(10) . . ? N1 C6 H6A 117.4 . . ? C5 C6 H6A 117.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 P1 O1 Pb1 -10.0(10) . . . . ? O3 P1 O1 Pb1 -131.8(8) . . . . ? C1 P1 O1 Pb1 109.1(8) . . . . ? O2 Pb1 O1 P1 -21.8(9) 3_666 . . . ? O2 Pb1 O1 P1 138.9(9) 2_656 . . . ? O4 Pb1 O1 P1 57.0(8) . . . . ? O3 Pb1 O1 P1 -136.4(9) 4_575 . . . ? O1 P1 O2 Pb1 89.3(9) . . . 3_666 ? O3 P1 O2 Pb1 -148.3(7) . . . 3_666 ? C1 P1 O2 Pb1 -30.1(9) . . . 3_666 ? O1 P1 O2 Pb1 -133.2(4) . . . 2_646 ? O3 P1 O2 Pb1 -10.8(4) . . . 2_646 ? C1 P1 O2 Pb1 107.3(4) . . . 2_646 ? O1 P1 O3 Ag1 -86.1(6) . . . 4_576 ? O2 P1 O3 Ag1 147.4(5) . . . 4_576 ? C1 P1 O3 Ag1 31.4(7) . . . 4_576 ? O1 P1 O3 Pb1 26.3(4) . . . 4_576 ? O2 P1 O3 Pb1 -100.2(4) . . . 4_576 ? C1 P1 O3 Pb1 143.8(3) . . . 4_576 ? O1 Pb1 O4 N2 163.2(6) . . . . ? O2 Pb1 O4 N2 -95.1(5) 3_666 . . . ? O2 Pb1 O4 N2 87.0(5) 2_656 . . . ? O3 Pb1 O4 N2 131.9(6) 4_575 . . . ? O3 Ag1 N1 C6 126.6(10) 4_575 . . . ? O3 Ag1 N1 C2 -55.0(14) 4_575 . . . ? Pb1 O4 N2 O6 176.7(8) . . . . ? Pb1 O4 N2 O5 -1.5(9) . . . . ? O1 P1 C1 C2 84.7(8) . . . . ? O2 P1 C1 C2 -150.5(7) . . . . ? O3 P1 C1 C2 -33.7(8) . . . . ? C6 N1 C2 C3 5.3(16) . . . . ? Ag1 N1 C2 C3 -173.2(8) . . . . ? C6 N1 C2 C1 -172.0(9) . . . . ? Ag1 N1 C2 C1 9.5(13) . . . . ? P1 C1 C2 N1 -75.8(11) . . . . ? P1 C1 C2 C3 107.0(11) . . . . ? N1 C2 C3 C4 -5.1(18) . . . . ? C1 C2 C3 C4 172.1(10) . . . . ? C2 C3 C4 C5 1.5(19) . . . . ? C3 C4 C5 C6 1.9(18) . . . . ? C2 N1 C6 C5 -1.9(18) . . . . ? Ag1 N1 C6 C5 176.6(10) . . . . ? C4 C5 C6 N1 -1.7(19) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.25 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.251 _refine_diff_density_min -1.976 _refine_diff_density_rms 0.388 # Attachment '- 8A.CIF' data_g:\pych2po\2p112d~1\8a _database_code_depnum_ccdc_archive 'CCDC 805034' #TrackingRef '- 8A.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((2PyHCH2PO3)Ag3(SO3CF3)2)N _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H7 Ag3 F6 N O9 P S2' _chemical_formula_weight 793.85 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.144(10) _cell_length_b 9.394(8) _cell_length_c 16.244(13) _cell_angle_alpha 90.00 _cell_angle_beta 108.812(15) _cell_angle_gamma 90.00 _cell_volume 1899(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1719 _cell_measurement_theta_min 2.627 _cell_measurement_theta_max 22.509 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.777 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 3.470 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9530 _exptl_absorpt_correction_T_max 0.9595 _exptl_absorpt_process_details 'SADABS: SAINT+, 2001' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.01 _diffrn_reflns_number 11025 _diffrn_reflns_av_R_equivalents 0.0661 _diffrn_reflns_av_sigmaI/netI 0.0953 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4308 _reflns_number_gt 2091 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v. 5.626' _computing_cell_refinement 'Bruker SAINT+ v. 6.36a' _computing_data_reduction 'Bruker SAINT+ v. 6.36a' _computing_structure_solution 'XS, Bruker SHELXTL v. 6.12' _computing_structure_refinement 'XL, Bruker SHELXTL v. 6.12' _computing_molecular_graphics 'XP, Bruker SHELXTL v. 6.12' _computing_publication_material 'XCIF, Bruker SHELXTL v. 6.12' _refine_special_details ; O7 and c8 are part of the triflate group with higher thermal parameters than other atoms 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^)+(0.0343P)^2^+4.1854P] 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 4308 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1294 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1180 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.000 _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 Ag1 Ag 0.52438(7) 0.35428(8) 0.18204(5) 0.0579(3) Uani 1 1 d . . . Ag2 Ag 0.56788(8) 0.37037(8) 0.52456(5) 0.0614(3) Uani 1 1 d . . . Ag3 Ag 0.48603(7) 0.20701(7) 0.33967(5) 0.0533(2) Uani 1 1 d . . . S1 S 0.6555(2) -0.0014(2) 0.52999(14) 0.0405(6) Uani 1 1 d . . . S2 S 0.2403(2) 0.4154(3) 0.28867(15) 0.0499(7) Uani 1 1 d . . . P1 P 0.59095(19) 0.5442(2) 0.35817(13) 0.0301(5) Uani 1 1 d . . . O1 O 0.5927(5) 0.3971(5) 0.3978(3) 0.0340(14) Uani 1 1 d . . . O2 O 0.5061(5) 0.6418(6) 0.3728(3) 0.0388(15) Uani 1 1 d . . . O3 O 0.5848(5) 0.5369(5) 0.2633(3) 0.0343(13) Uani 1 1 d . . . O4 O 0.6315(6) 0.1223(7) 0.5720(4) 0.068(2) Uani 1 1 d . . . O5 O 0.6260(5) 0.0107(7) 0.4370(4) 0.0564(18) Uani 1 1 d . . . O6 O 0.6301(6) -0.1330(6) 0.5612(4) 0.061(2) Uani 1 1 d . . . O7 O 0.3272(7) 0.3658(9) 0.2615(5) 0.087(3) Uani 1 1 d . . . O8 O 0.2683(6) 0.4661(7) 0.3752(4) 0.073(2) Uani 1 1 d . . . O9 O 0.1486(6) 0.3253(8) 0.2635(5) 0.083(2) Uani 1 1 d . . . N1 N 0.8604(7) 0.5886(9) 0.3498(5) 0.058(2) Uani 1 1 d . . . H1 H 0.8374 0.6653 0.3208 0.070 Uiso 1 1 calc R . . F1 F 0.8397(5) 0.1173(7) 0.5431(5) 0.094(2) Uani 1 1 d . . . F2 F 0.8415(5) -0.1066(7) 0.5342(5) 0.097(2) Uani 1 1 d . . . F3 F 0.8401(6) -0.0089(8) 0.6507(4) 0.109(3) Uani 1 1 d . . . F4 F 0.1144(7) 0.6342(9) 0.2398(6) 0.140(4) Uani 1 1 d . . . F5 F 0.1554(8) 0.5377(10) 0.1406(5) 0.137(3) Uani 1 1 d . . . F6 F 0.2680(6) 0.6617(8) 0.2270(5) 0.115(3) Uani 1 1 d . . . C1 C 0.7203(7) 0.6238(8) 0.4158(5) 0.039(2) Uani 1 1 d . . . H1A H 0.7224 0.7196 0.3941 0.047 Uiso 1 1 calc R . . H1B H 0.7280 0.6307 0.4771 0.047 Uiso 1 1 calc R . . C2 C 0.8110(8) 0.5424(10) 0.4061(5) 0.042(2) Uani 1 1 d . . . C3 C 0.8495(8) 0.4204(10) 0.4511(6) 0.051(3) Uani 1 1 d . . . H3 H 0.8187 0.3865 0.4914 0.061 Uiso 1 1 calc R . . C4 C 0.9343(8) 0.3464(11) 0.4374(7) 0.060(3) Uani 1 1 d . . . H4 H 0.9577 0.2616 0.4669 0.072 Uiso 1 1 calc R . . C5 C 0.9836(9) 0.3973(13) 0.3806(7) 0.067(3) Uani 1 1 d . . . H5 H 1.0416 0.3498 0.3723 0.080 Uiso 1 1 calc R . . C6 C 0.9447(10) 0.5192(14) 0.3371(7) 0.074(4) Uani 1 1 d . . . H6 H 0.9763 0.5558 0.2980 0.089 Uiso 1 1 calc R . . C7 C 0.8024(9) 0.0010(10) 0.5665(7) 0.057(3) Uani 1 1 d . . . C8 C 0.1922(11) 0.5725(13) 0.2226(8) 0.067(3) 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 Ag1 0.0973(7) 0.0361(4) 0.0492(4) -0.0165(3) 0.0362(5) -0.0198(4) Ag2 0.0981(7) 0.0534(5) 0.0497(5) 0.0169(4) 0.0475(5) 0.0244(5) Ag3 0.0702(6) 0.0361(4) 0.0475(5) -0.0069(3) 0.0106(4) -0.0102(4) S1 0.0543(18) 0.0370(13) 0.0361(13) 0.0072(9) 0.0228(12) 0.0101(11) S2 0.066(2) 0.0417(13) 0.0416(14) 0.0021(11) 0.0167(13) 0.0056(14) P1 0.0455(15) 0.0237(10) 0.0236(11) 0.0013(8) 0.0145(10) 0.0025(11) O1 0.054(4) 0.020(3) 0.031(3) 0.000(2) 0.019(3) 0.002(3) O2 0.055(4) 0.032(3) 0.035(3) 0.006(3) 0.023(3) 0.010(3) O3 0.049(4) 0.027(3) 0.030(3) 0.003(2) 0.017(3) -0.002(3) O4 0.100(6) 0.049(4) 0.070(5) 0.004(3) 0.049(5) 0.022(4) O5 0.064(5) 0.072(5) 0.031(3) 0.009(3) 0.012(3) 0.006(4) O6 0.077(5) 0.039(4) 0.078(5) 0.019(3) 0.039(4) 0.009(4) O7 0.101(7) 0.092(6) 0.081(6) 0.017(5) 0.048(5) 0.055(5) O8 0.119(7) 0.065(5) 0.038(4) -0.009(3) 0.030(4) -0.008(5) O9 0.089(6) 0.066(5) 0.082(6) -0.003(4) 0.010(5) -0.031(5) N1 0.061(6) 0.075(6) 0.032(4) 0.002(4) 0.007(4) -0.022(5) F1 0.080(5) 0.075(5) 0.129(6) 0.010(4) 0.034(4) -0.022(4) F2 0.064(5) 0.085(5) 0.147(7) -0.014(5) 0.040(5) 0.018(4) F3 0.101(6) 0.138(7) 0.060(5) 0.018(4) -0.013(4) -0.007(5) F4 0.140(8) 0.123(7) 0.196(9) 0.086(6) 0.107(7) 0.093(6) F5 0.180(9) 0.148(8) 0.063(5) 0.035(5) 0.011(5) 0.039(7) F6 0.088(6) 0.096(6) 0.157(8) 0.060(5) 0.032(5) -0.006(5) C1 0.053(6) 0.027(4) 0.033(5) -0.006(4) 0.008(4) -0.002(4) C2 0.047(7) 0.044(5) 0.034(5) -0.001(4) 0.009(4) -0.009(5) C3 0.049(7) 0.046(6) 0.056(6) -0.002(5) 0.014(5) -0.015(5) C4 0.048(8) 0.050(6) 0.067(7) -0.006(5) 0.000(6) -0.023(6) C5 0.046(8) 0.081(9) 0.073(8) -0.030(7) 0.018(6) -0.004(7) C6 0.060(9) 0.101(10) 0.067(8) -0.019(7) 0.029(7) -0.017(8) C7 0.074(9) 0.039(6) 0.055(7) 0.010(5) 0.016(6) -0.005(6) C8 0.073(9) 0.068(8) 0.066(8) 0.025(6) 0.031(7) 0.014(7) _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 Ag1 O3 2.154(5) . ? Ag1 O2 2.170(5) 2_645 ? Ag1 Ag3 3.091(2) . ? Ag1 Ag3 3.330(3) 2_655 ? Ag2 O2 2.187(5) 3_666 ? Ag2 O1 2.200(5) . ? Ag2 O4 2.512(7) . ? Ag2 Ag2 2.972(2) 3_666 ? Ag2 Ag3 3.233(2) . ? Ag3 O1 2.279(5) . ? Ag3 O3 2.283(5) 2_645 ? Ag3 O7 2.547(7) . ? Ag3 Ag1 3.330(3) 2_645 ? S1 O6 1.416(6) . ? S1 O4 1.434(6) . ? S1 O5 1.438(6) . ? S1 C7 1.829(12) . ? S2 O8 1.416(6) . ? S2 O9 1.421(7) . ? S2 O7 1.429(7) . ? S2 C8 1.814(11) . ? P1 O3 1.518(5) . ? P1 O2 1.521(6) . ? P1 O1 1.522(5) . ? P1 C1 1.817(9) . ? O2 Ag1 2.170(5) 2_655 ? O2 Ag2 2.187(5) 3_666 ? O3 Ag3 2.283(5) 2_655 ? N1 C2 1.352(11) . ? N1 C6 1.358(13) . ? N1 H1 0.8600 . ? F1 C7 1.303(10) . ? F2 C7 1.317(11) . ? F3 C7 1.300(11) . ? F4 C8 1.282(12) . ? F5 C8 1.303(13) . ? F6 C8 1.286(13) . ? C1 C2 1.467(12) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.365(12) . ? C3 C4 1.391(13) . ? C3 H3 0.9300 . ? C4 C5 1.373(14) . ? C4 H4 0.9300 . ? C5 C6 1.356(15) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? 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 O3 Ag1 O2 165.3(2) . 2_645 ? O3 Ag1 Ag3 88.57(14) . . ? O2 Ag1 Ag3 82.58(14) 2_645 . ? O3 Ag1 Ag3 42.85(14) . 2_655 ? O2 Ag1 Ag3 151.13(15) 2_645 2_655 ? Ag3 Ag1 Ag3 121.39(3) . 2_655 ? O2 Ag2 O1 162.9(2) 3_666 . ? O2 Ag2 O4 84.4(2) 3_666 . ? O1 Ag2 O4 104.95(19) . . ? O2 Ag2 Ag2 82.62(15) 3_666 3_666 ? O1 Ag2 Ag2 84.99(14) . 3_666 ? O4 Ag2 Ag2 162.61(17) . 3_666 ? O2 Ag2 Ag3 125.92(16) 3_666 . ? O1 Ag2 Ag3 44.77(14) . . ? O4 Ag2 Ag3 79.80(17) . . ? Ag2 Ag2 Ag3 98.53(6) 3_666 . ? O1 Ag3 O3 154.56(17) . 2_645 ? O1 Ag3 O7 92.5(3) . . ? O3 Ag3 O7 88.3(2) 2_645 . ? O1 Ag3 Ag1 75.52(13) . . ? O3 Ag3 Ag1 80.97(14) 2_645 . ? O7 Ag3 Ag1 69.61(17) . . ? O1 Ag3 Ag2 42.84(12) . . ? O3 Ag3 Ag2 161.42(13) 2_645 . ? O7 Ag3 Ag2 99.15(18) . . ? Ag1 Ag3 Ag2 117.57(6) . . ? O1 Ag3 Ag1 145.32(14) . 2_645 ? O3 Ag3 Ag1 39.92(13) 2_645 2_645 ? O7 Ag3 Ag1 122.1(2) . 2_645 ? Ag1 Ag3 Ag1 111.69(4) . 2_645 ? Ag2 Ag3 Ag1 124.11(4) . 2_645 ? O6 S1 O4 115.1(4) . . ? O6 S1 O5 115.4(4) . . ? O4 S1 O5 114.2(4) . . ? O6 S1 C7 103.9(4) . . ? O4 S1 C7 102.0(5) . . ? O5 S1 C7 103.8(4) . . ? O8 S2 O9 114.3(5) . . ? O8 S2 O7 116.0(5) . . ? O9 S2 O7 113.9(5) . . ? O8 S2 C8 104.1(5) . . ? O9 S2 C8 102.3(6) . . ? O7 S2 C8 104.1(5) . . ? O3 P1 O2 112.6(3) . . ? O3 P1 O1 112.2(3) . . ? O2 P1 O1 113.1(3) . . ? O3 P1 C1 106.0(4) . . ? O2 P1 C1 106.4(4) . . ? O1 P1 C1 105.8(4) . . ? P1 O1 Ag2 120.9(3) . . ? P1 O1 Ag3 127.8(3) . . ? Ag2 O1 Ag3 92.39(19) . . ? P1 O2 Ag1 122.6(3) . 2_655 ? P1 O2 Ag2 128.1(3) . 3_666 ? Ag1 O2 Ag2 107.0(2) 2_655 3_666 ? P1 O3 Ag1 123.1(3) . . ? P1 O3 Ag3 126.0(3) . 2_655 ? Ag1 O3 Ag3 97.2(2) . 2_655 ? S1 O4 Ag2 135.1(4) . . ? S2 O7 Ag3 130.2(4) . . ? C2 N1 C6 122.8(10) . . ? C2 N1 H1 118.6 . . ? C6 N1 H1 118.6 . . ? C2 C1 P1 112.8(6) . . ? C2 C1 H1A 109.0 . . ? P1 C1 H1A 109.0 . . ? C2 C1 H1B 109.0 . . ? P1 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? N1 C2 C3 117.1(9) . . ? N1 C2 C1 119.3(9) . . ? C3 C2 C1 123.6(8) . . ? C2 C3 C4 120.8(10) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 120.6(11) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C6 C5 C4 117.6(11) . . ? C6 C5 H5 121.2 . . ? C4 C5 H5 121.2 . . ? C5 C6 N1 121.0(11) . . ? C5 C6 H6 119.5 . . ? N1 C6 H6 119.5 . . ? F3 C7 F1 108.4(9) . . ? F3 C7 F2 107.4(9) . . ? F1 C7 F2 107.2(9) . . ? F3 C7 S1 110.1(8) . . ? F1 C7 S1 111.9(8) . . ? F2 C7 S1 111.6(8) . . ? F4 C8 F6 110.6(11) . . ? F4 C8 F5 106.1(12) . . ? F6 C8 F5 104.3(10) . . ? F4 C8 S2 112.9(8) . . ? F6 C8 S2 112.4(9) . . ? F5 C8 S2 110.1(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Ag1 Ag3 O1 -13.7(2) . . . . ? O2 Ag1 Ag3 O1 154.5(2) 2_645 . . . ? Ag3 Ag1 Ag3 O1 -42.77(15) 2_655 . . . ? O3 Ag1 Ag3 O3 176.07(11) . . . 2_645 ? O2 Ag1 Ag3 O3 -15.7(2) 2_645 . . 2_645 ? Ag3 Ag1 Ag3 O3 147.02(15) 2_655 . . 2_645 ? O3 Ag1 Ag3 O7 84.6(3) . . . . ? O2 Ag1 Ag3 O7 -107.2(3) 2_645 . . . ? Ag3 Ag1 Ag3 O7 55.5(2) 2_655 . . . ? O3 Ag1 Ag3 Ag2 -5.27(16) . . . . ? O2 Ag1 Ag3 Ag2 162.92(16) 2_645 . . . ? Ag3 Ag1 Ag3 Ag2 -34.32(5) 2_655 . . . ? O3 Ag1 Ag3 Ag1 -157.95(15) . . . 2_645 ? O2 Ag1 Ag3 Ag1 10.24(16) 2_645 . . 2_645 ? Ag3 Ag1 Ag3 Ag1 173.00(5) 2_655 . . 2_645 ? O2 Ag2 Ag3 O1 161.0(3) 3_666 . . . ? O4 Ag2 Ag3 O1 -123.6(3) . . . . ? Ag2 Ag2 Ag3 O1 73.9(2) 3_666 . . . ? O2 Ag2 Ag3 O3 -35.3(5) 3_666 . . 2_645 ? O1 Ag2 Ag3 O3 163.8(5) . . . 2_645 ? O4 Ag2 Ag3 O3 40.1(5) . . . 2_645 ? Ag2 Ag2 Ag3 O3 -122.3(4) 3_666 . . 2_645 ? O2 Ag2 Ag3 O7 77.2(3) 3_666 . . . ? O1 Ag2 Ag3 O7 -83.8(3) . . . . ? O4 Ag2 Ag3 O7 152.6(2) . . . . ? Ag2 Ag2 Ag3 O7 -9.84(19) 3_666 . . . ? O2 Ag2 Ag3 Ag1 148.88(18) 3_666 . . . ? O1 Ag2 Ag3 Ag1 -12.1(2) . . . . ? O4 Ag2 Ag3 Ag1 -135.70(17) . . . . ? Ag2 Ag2 Ag3 Ag1 61.85(7) 3_666 . . . ? O2 Ag2 Ag3 Ag1 -62.12(18) 3_666 . . 2_645 ? O1 Ag2 Ag3 Ag1 136.9(2) . . . 2_645 ? O4 Ag2 Ag3 Ag1 13.30(17) . . . 2_645 ? Ag2 Ag2 Ag3 Ag1 -149.15(5) 3_666 . . 2_645 ? O3 P1 O1 Ag2 -167.3(3) . . . . ? O2 P1 O1 Ag2 -38.6(5) . . . . ? C1 P1 O1 Ag2 77.5(4) . . . . ? O3 P1 O1 Ag3 -45.6(5) . . . . ? O2 P1 O1 Ag3 83.1(4) . . . . ? C1 P1 O1 Ag3 -160.8(4) . . . . ? O2 Ag2 O1 P1 74.0(8) 3_666 . . . ? O4 Ag2 O1 P1 -164.3(4) . . . . ? Ag2 Ag2 O1 P1 30.2(4) 3_666 . . . ? Ag3 Ag2 O1 P1 137.7(5) . . . . ? O2 Ag2 O1 Ag3 -63.7(7) 3_666 . . . ? O4 Ag2 O1 Ag3 58.0(3) . . . . ? Ag2 Ag2 O1 Ag3 -107.45(16) 3_666 . . . ? O3 Ag3 O1 P1 58.9(7) 2_645 . . . ? O7 Ag3 O1 P1 -32.3(4) . . . . ? Ag1 Ag3 O1 P1 35.9(3) . . . . ? Ag2 Ag3 O1 P1 -133.0(5) . . . . ? Ag1 Ag3 O1 P1 143.2(3) 2_645 . . . ? O3 Ag3 O1 Ag2 -168.0(4) 2_645 . . . ? O7 Ag3 O1 Ag2 100.8(2) . . . . ? Ag1 Ag3 O1 Ag2 168.95(18) . . . . ? Ag1 Ag3 O1 Ag2 -83.7(2) 2_645 . . . ? O3 P1 O2 Ag1 -47.6(5) . . . 2_655 ? O1 P1 O2 Ag1 -176.1(3) . . . 2_655 ? C1 P1 O2 Ag1 68.2(4) . . . 2_655 ? O3 P1 O2 Ag2 152.2(4) . . . 3_666 ? O1 P1 O2 Ag2 23.7(5) . . . 3_666 ? C1 P1 O2 Ag2 -92.1(5) . . . 3_666 ? O2 P1 O3 Ag1 -106.8(4) . . . . ? O1 P1 O3 Ag1 22.3(5) . . . . ? C1 P1 O3 Ag1 137.3(4) . . . . ? O2 P1 O3 Ag3 24.5(5) . . . 2_655 ? O1 P1 O3 Ag3 153.5(3) . . . 2_655 ? C1 P1 O3 Ag3 -91.4(4) . . . 2_655 ? O2 Ag1 O3 P1 -53.2(10) 2_645 . . . ? Ag3 Ag1 O3 P1 -0.2(4) . . . . ? Ag3 Ag1 O3 P1 142.2(5) 2_655 . . . ? O2 Ag1 O3 Ag3 164.6(7) 2_645 . . 2_655 ? Ag3 Ag1 O3 Ag3 -142.46(16) . . . 2_655 ? O6 S1 O4 Ag2 -145.4(5) . . . . ? O5 S1 O4 Ag2 -8.4(8) . . . . ? C7 S1 O4 Ag2 102.9(6) . . . . ? O2 Ag2 O4 S1 150.2(7) 3_666 . . . ? O1 Ag2 O4 S1 -15.3(7) . . . . ? Ag2 Ag2 O4 S1 108.1(6) 3_666 . . . ? Ag3 Ag2 O4 S1 22.1(6) . . . . ? O8 S2 O7 Ag3 44.4(8) . . . . ? O9 S2 O7 Ag3 -91.3(7) . . . . ? C8 S2 O7 Ag3 158.1(7) . . . . ? O1 Ag3 O7 S2 -92.5(7) . . . . ? O3 Ag3 O7 S2 112.9(7) 2_645 . . . ? Ag1 Ag3 O7 S2 -166.1(7) . . . . ? Ag2 Ag3 O7 S2 -50.0(7) . . . . ? Ag1 Ag3 O7 S2 90.5(7) 2_645 . . . ? O3 P1 C1 C2 -58.7(7) . . . . ? O2 P1 C1 C2 -178.8(6) . . . . ? O1 P1 C1 C2 60.6(7) . . . . ? C6 N1 C2 C3 0.0(14) . . . . ? C6 N1 C2 C1 -179.9(9) . . . . ? P1 C1 C2 N1 102.0(8) . . . . ? P1 C1 C2 C3 -77.9(10) . . . . ? N1 C2 C3 C4 -1.5(13) . . . . ? C1 C2 C3 C4 178.4(8) . . . . ? C2 C3 C4 C5 2.4(15) . . . . ? C3 C4 C5 C6 -1.8(15) . . . . ? C4 C5 C6 N1 0.4(16) . . . . ? C2 N1 C6 C5 0.5(16) . . . . ? O6 S1 C7 F3 -59.0(8) . . . . ? O4 S1 C7 F3 60.9(8) . . . . ? O5 S1 C7 F3 179.8(7) . . . . ? O6 S1 C7 F1 -179.7(8) . . . . ? O4 S1 C7 F1 -59.8(9) . . . . ? O5 S1 C7 F1 59.2(9) . . . . ? O6 S1 C7 F2 60.1(8) . . . . ? O4 S1 C7 F2 -180.0(7) . . . . ? O5 S1 C7 F2 -61.0(8) . . . . ? O8 S2 C8 F4 -56.6(12) . . . . ? O9 S2 C8 F4 62.7(11) . . . . ? O7 S2 C8 F4 -178.5(10) . . . . ? O8 S2 C8 F6 69.3(10) . . . . ? O9 S2 C8 F6 -171.4(9) . . . . ? O7 S2 C8 F6 -52.6(11) . . . . ? O8 S2 C8 F5 -174.9(9) . . . . ? O9 S2 C8 F5 -55.7(10) . . . . ? O7 S2 C8 F5 63.2(11) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.25 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.742 _refine_diff_density_min -1.118 _refine_diff_density_rms 0.163 # Attachment '- 7sav.CIF' data_g:\pych2po\2p8682~1\ar553 _database_code_depnum_ccdc_archive 'CCDC 805035' #TrackingRef '- 7sav.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((2PyHCH2PO3H2)Pb(NO3)2)N _chemical_melting_point ? _chemical_formula_moiety 'C6 H8 N P O3 Pb,(N O3)2 ' _chemical_formula_sum 'C6 H8 N3 O9 P Pb' _chemical_formula_weight 504.31 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 '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 5.4028(4) _cell_length_b 10.1360(8) _cell_length_c 11.8724(9) _cell_angle_alpha 73.6130(10) _cell_angle_beta 84.5320(10) _cell_angle_gamma 82.5930(10) _cell_volume 617.36(8) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 2419 _cell_measurement_theta_min 2.363 _cell_measurement_theta_max 28.14 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 13.844 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7887 _exptl_absorpt_correction_T_max 0.8515 _exptl_absorpt_process_details 'SADABS: SAINT+, 2001' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <0.01 _diffrn_reflns_number 3575 _diffrn_reflns_av_R_equivalents 0.0188 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 28.30 _reflns_number_total 2708 _reflns_number_gt 2474 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART v. 5.626' _computing_cell_refinement 'Bruker SAINT+ v. 6.36a' _computing_data_reduction 'Bruker SAINT+ v. 6.36a' _computing_structure_solution 'XS, Bruker SHELXTL v. 6.12' _computing_structure_refinement 'XL, Bruker SHELXTL v. 6.12' _computing_molecular_graphics 'XP, Bruker SHELXTL v. 6.12' _computing_publication_material 'XCIF, Bruker SHELXTL v. 6.12' _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^)+(0.0698P)^2^+0.0000P] 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 2708 _refine_ls_number_parameters 189 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0955 _refine_ls_wR_factor_gt 0.0922 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Pb1 Pb 0.78172(4) 0.01999(2) 0.33768(2) 0.01466(11) Uani 1 1 d . . . P1 P 0.8352(3) 0.32299(18) 0.09697(16) 0.0133(3) Uani 1 1 d . . . O1 O 1.1281(10) 0.3122(6) 0.0866(5) 0.0197(11) Uani 1 1 d . . . O2 O 0.7446(10) 0.2360(5) 0.2152(4) 0.0208(11) Uani 1 1 d . . . O3 O 0.7283(9) 0.4736(5) 0.0712(4) 0.0155(10) Uani 1 1 d . . . O4 O 0.2811(9) 0.0426(6) 0.2985(5) 0.0193(11) Uani 1 1 d . . . O5 O 0.5236(11) -0.0230(7) 0.1620(5) 0.0301(14) Uani 1 1 d . . . O6 O 1.1183(11) -0.0105(6) 0.1591(5) 0.0248(12) Uani 1 1 d . . . O7 O 0.9168(10) 0.1568(6) 0.4720(5) 0.0220(11) Uani 1 1 d . . . O8 O 0.6755(13) 0.2679(7) 0.5782(6) 0.0411(17) Uani 1 1 d . . . O9 O 0.5148(10) 0.1639(6) 0.4707(5) 0.0253(12) Uani 1 1 d . . . N1 N 0.6958(12) 0.4551(6) -0.1856(5) 0.0170(12) Uani 1 1 d . . . C3 C 1.0580(14) 0.3041(8) -0.1975(7) 0.0201(15) Uani 1 1 d . . . H3 H 1.1608 0.2222 -0.1659 0.024 Uiso 1 1 calc R . . N2 N 0.3085(11) 0.0029(6) 0.2048(5) 0.0162(12) Uani 1 1 d . . . N3 N 0.7007(12) 0.1987(7) 0.5087(6) 0.0219(14) Uani 1 1 d . . . C1 C 0.7514(14) 0.2530(8) -0.0181(6) 0.0188(15) Uani 1 1 d . . . H1A H 0.8290 0.1576 -0.0056 0.023 Uiso 1 1 calc R . . H1B H 0.5696 0.2518 -0.0138 0.023 Uiso 1 1 calc R . . C2 C 0.8351(13) 0.3372(7) -0.1368(6) 0.0157(14) Uani 1 1 d . . . C4 C 1.1267(16) 0.3935(9) -0.3054(8) 0.0272(18) Uani 1 1 d . . . H4 H 1.2757 0.3715 -0.3472 0.033 Uiso 1 1 calc R . . C5 C 0.9772(17) 0.5137(9) -0.3507(7) 0.0281(18) Uani 1 1 d . . . H5 H 1.0229 0.5747 -0.4232 0.034 Uiso 1 1 calc R . . C6 C 0.7583(16) 0.5436(8) -0.2880(7) 0.0222(16) Uani 1 1 d . . . H6 H 0.6543 0.6258 -0.3172 0.027 Uiso 1 1 calc R . . H12 H 0.554(16) 0.485(9) -0.141(8) 0.02(2) Uiso 1 1 d . . . H1 H 1.176(16) 0.376(10) 0.045(8) 0.02(2) Uiso 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 Pb1 0.01160(16) 0.01717(16) 0.01242(16) -0.00070(11) -0.00152(10) 0.00164(10) P1 0.0131(8) 0.0134(8) 0.0104(8) -0.0006(7) -0.0012(6) 0.0036(6) O1 0.013(2) 0.019(3) 0.021(3) 0.003(2) -0.001(2) 0.003(2) O2 0.024(3) 0.023(3) 0.011(2) 0.000(2) 0.001(2) 0.000(2) O3 0.015(2) 0.015(2) 0.014(2) -0.002(2) 0.0014(19) 0.0025(19) O4 0.013(3) 0.029(3) 0.016(2) -0.008(2) -0.0033(19) 0.002(2) O5 0.018(3) 0.044(4) 0.032(3) -0.020(3) 0.005(2) 0.002(2) O6 0.016(3) 0.033(3) 0.030(3) -0.014(3) -0.008(2) -0.002(2) O7 0.013(2) 0.028(3) 0.023(3) -0.005(2) -0.002(2) 0.001(2) O8 0.047(4) 0.044(4) 0.044(4) -0.034(4) 0.009(3) -0.005(3) O9 0.017(3) 0.031(3) 0.024(3) 0.001(2) -0.006(2) -0.002(2) N1 0.018(3) 0.019(3) 0.011(3) -0.003(2) -0.001(2) 0.007(2) C3 0.018(4) 0.023(4) 0.021(4) -0.012(3) -0.004(3) 0.004(3) N2 0.015(3) 0.016(3) 0.016(3) -0.005(2) 0.001(2) 0.003(2) N3 0.022(3) 0.021(3) 0.021(3) -0.004(3) -0.003(3) 0.005(3) C1 0.022(4) 0.018(3) 0.014(3) -0.004(3) -0.001(3) 0.004(3) C2 0.018(3) 0.015(3) 0.015(3) -0.005(3) -0.002(3) 0.000(3) C4 0.023(4) 0.036(5) 0.028(4) -0.021(4) 0.006(3) -0.003(3) C5 0.038(5) 0.033(4) 0.015(4) -0.010(3) 0.005(3) -0.011(4) C6 0.032(4) 0.018(4) 0.015(4) -0.005(3) -0.002(3) 0.006(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 Pb1 O2 2.257(5) . ? Pb1 O7 2.594(6) . ? Pb1 O9 2.651(6) . ? Pb1 O6 2.718(6) . ? Pb1 O4 2.722(5) 1_655 ? Pb1 O4 2.757(5) . ? P1 O2 1.506(5) . ? P1 O3 1.516(5) . ? P1 O1 1.568(5) . ? P1 C1 1.823(8) . ? O1 H1 0.76(9) . ? O4 N2 1.276(8) . ? O4 Pb1 2.722(5) 1_455 ? O5 N2 1.250(8) . ? O6 N2 1.247(9) 1_655 ? O7 N3 1.270(8) . ? O8 N3 1.214(9) . ? O9 N3 1.267(9) . ? N1 C6 1.335(10) . ? N1 C2 1.338(9) . ? N1 H12 0.96(9) . ? C3 C4 1.393(12) . ? C3 C2 1.396(10) . ? C3 H3 0.9400 . ? N2 O6 1.247(9) 1_455 ? C1 C2 1.489(10) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C4 C5 1.373(13) . ? C4 H4 0.9400 . ? C5 C6 1.383(12) . ? C5 H5 0.9400 . ? C6 H6 0.9400 . ? 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 Pb1 O7 79.93(18) . . ? O2 Pb1 O9 77.57(18) . . ? O7 Pb1 O9 48.76(17) . . ? O2 Pb1 O6 79.01(18) . . ? O7 Pb1 O6 115.42(17) . . ? O9 Pb1 O6 153.86(18) . . ? O2 Pb1 O4 83.96(18) . 1_655 ? O7 Pb1 O4 70.57(16) . 1_655 ? O9 Pb1 O4 118.53(16) . 1_655 ? O6 Pb1 O4 47.01(16) . 1_655 ? O2 Pb1 O4 81.19(18) . . ? O7 Pb1 O4 118.22(16) . . ? O9 Pb1 O4 69.85(16) . . ? O6 Pb1 O4 117.60(16) . . ? O4 Pb1 O4 160.8(2) 1_655 . ? O2 P1 O3 113.4(3) . . ? O2 P1 O1 110.3(3) . . ? O3 P1 O1 109.8(3) . . ? O2 P1 C1 109.4(3) . . ? O3 P1 C1 108.5(3) . . ? O1 P1 C1 105.1(3) . . ? P1 O1 H1 112(7) . . ? P1 O2 Pb1 143.1(3) . . ? N2 O4 Pb1 96.2(4) . 1_455 ? N2 O4 Pb1 97.0(4) . . ? Pb1 O4 Pb1 160.8(2) 1_455 . ? N2 O6 Pb1 97.2(4) 1_655 . ? N3 O7 Pb1 98.3(4) . . ? N3 O9 Pb1 95.7(4) . . ? C6 N1 C2 124.1(7) . . ? C6 N1 H12 116(5) . . ? C2 N1 H12 119(5) . . ? C4 C3 C2 119.5(7) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? O6 N2 O5 121.7(6) 1_455 . ? O6 N2 O4 118.7(6) 1_455 . ? O5 N2 O4 119.6(6) . . ? O8 N3 O9 121.9(7) . . ? O8 N3 O7 120.9(7) . . ? O9 N3 O7 117.2(6) . . ? C2 C1 P1 111.2(5) . . ? C2 C1 H1A 109.4 . . ? P1 C1 H1A 109.4 . . ? C2 C1 H1B 109.4 . . ? P1 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N1 C2 C3 117.9(7) . . ? N1 C2 C1 118.3(6) . . ? C3 C2 C1 123.8(7) . . ? C5 C4 C3 120.1(7) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 119.0(8) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? N1 C6 C5 119.5(7) . . ? N1 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 P1 O2 Pb1 -178.1(5) . . . . ? O1 P1 O2 Pb1 -54.4(6) . . . . ? C1 P1 O2 Pb1 60.7(6) . . . . ? O7 Pb1 O2 P1 121.6(6) . . . . ? O9 Pb1 O2 P1 171.3(6) . . . . ? O6 Pb1 O2 P1 3.0(5) . . . . ? O4 Pb1 O2 P1 50.3(6) 1_655 . . . ? O4 Pb1 O2 P1 -117.5(6) . . . . ? O2 Pb1 O4 N2 86.2(4) . . . . ? O7 Pb1 O4 N2 159.8(4) . . . . ? O9 Pb1 O4 N2 166.2(4) . . . . ? O6 Pb1 O4 N2 13.6(5) . . . . ? O4 Pb1 O4 N2 46.6(9) 1_655 . . . ? O2 Pb1 O4 Pb1 -140.3(7) . . . 1_455 ? O7 Pb1 O4 Pb1 -66.8(7) . . . 1_455 ? O9 Pb1 O4 Pb1 -60.4(6) . . . 1_455 ? O6 Pb1 O4 Pb1 147.1(6) . . . 1_455 ? O4 Pb1 O4 Pb1 180.0 1_655 . . 1_455 ? O2 Pb1 O6 N2 97.4(5) . . . 1_655 ? O7 Pb1 O6 N2 24.2(5) . . . 1_655 ? O9 Pb1 O6 N2 70.7(6) . . . 1_655 ? O4 Pb1 O6 N2 5.4(4) 1_655 . . 1_655 ? O4 Pb1 O6 N2 171.3(4) . . . 1_655 ? O2 Pb1 O7 N3 82.5(4) . . . . ? O9 Pb1 O7 N3 0.2(4) . . . . ? O6 Pb1 O7 N3 155.1(4) . . . . ? O4 Pb1 O7 N3 169.6(5) 1_655 . . . ? O4 Pb1 O7 N3 8.2(5) . . . . ? O2 Pb1 O9 N3 -87.7(4) . . . . ? O7 Pb1 O9 N3 -0.2(4) . . . . ? O6 Pb1 O9 N3 -60.8(6) . . . . ? O4 Pb1 O9 N3 -11.7(5) 1_655 . . . ? O4 Pb1 O9 N3 -172.7(5) . . . . ? Pb1 O4 N2 O6 9.6(7) 1_455 . . 1_455 ? Pb1 O4 N2 O6 175.7(6) . . . 1_455 ? Pb1 O4 N2 O5 -169.6(6) 1_455 . . . ? Pb1 O4 N2 O5 -3.5(7) . . . . ? Pb1 O9 N3 O8 -178.8(7) . . . . ? Pb1 O9 N3 O7 0.4(7) . . . . ? Pb1 O7 N3 O8 178.8(7) . . . . ? Pb1 O7 N3 O9 -0.4(7) . . . . ? O2 P1 C1 C2 179.4(5) . . . . ? O3 P1 C1 C2 55.2(6) . . . . ? O1 P1 C1 C2 -62.3(6) . . . . ? C6 N1 C2 C3 -0.8(11) . . . . ? C6 N1 C2 C1 175.7(7) . . . . ? C4 C3 C2 N1 -0.1(11) . . . . ? C4 C3 C2 C1 -176.5(7) . . . . ? P1 C1 C2 N1 -79.8(7) . . . . ? P1 C1 C2 C3 96.5(8) . . . . ? C2 C3 C4 C5 0.6(12) . . . . ? C3 C4 C5 C6 -0.3(13) . . . . ? C2 N1 C6 C5 1.2(12) . . . . ? C4 C5 C6 N1 -0.6(12) . . . . ? 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 H12 O3 0.96(9) 2.74(9) 3.130(8) 105(6) . _diffrn_measured_fraction_theta_max 0.884 _diffrn_reflns_theta_full 26.25 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 2.678 _refine_diff_density_min -3.558 _refine_diff_density_rms 0.283