data_ba79cas _audit_creation_method SHELXL-97 _audit_update_record ; 2008-09-19 text and data added, mto ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H45 Fe2 N2 O3 P3 S2, 2(C H2 Cl2), 2(B F4)' _chemical_formula_sum 'C45 H49 B2 Cl4 F8 Fe2 N2 O3 P3 S2' _chemical_formula_structural ? _chemical_formula_weight 1250.01 _chemical_absolute_configuration . _chemical_formula_iupac ? _chemical_formula_analytical ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 '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' 'S' 'S' 0.1246 0.1234 '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' 'Cl' 'Cl' 0.1484 0.1585 '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 ' _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9738(13) _cell_length_b 13.2467(15) _cell_length_c 19.321(2) _cell_angle_alpha 77.934(7) _cell_angle_beta 72.938(7) _cell_angle_gamma 69.865(7) _cell_volume 2730.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 1117 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 16.94 _exptl_crystal_description 'platy' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_crystal_id ba79cas _exptl_crystal_preparation ; The data crystal was mounted using oil (Parantone-N, Exxon) to a 0.3 mm cryo-loop (Hampton Research) with the (-3 0 -2) scattering planes roughly normal to the spindle axis. ; _exptl_absorpt_coefficient_mu 0.959 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_correction_T_min 0.8015 _exptl_absorpt_correction_T_max 0.9819 _exptl_absorpt_process_details 'SHELXTL/XPREP V2005/2 (Bruker, 2005)' _exptl_special_details ; One distinct cell was identified using APEX2 (Bruker, 2001/4). Five frame series were integrated and filtered for statistical outliers using SAINT (Bruker, 2005) then corrected for absorption by integration using SHELXTL/XPREP V2005/2 (Bruker, 2005) before using SAINT/SADABS (Bruker, 2005) to sort, merge, and scale the combined data. No decay correction was applied. ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id ba79cas _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type ? _diffrn_measurement_device 'Bruker Kappa/ApexII CCD' _diffrn_measurement_method 'profile data from \f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30921 _diffrn_reflns_av_R_equivalents 0.2437 _diffrn_reflns_av_sigmaI/netI 0.3853 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.39 _reflns_number_total 9961 _reflns_number_gt 3056 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 V2.0-1 (Bruker, 2004)' _computing_cell_refinement 'SAINT V7.23A (Bruker, 2005)' _computing_data_reduction ; SAINT V7.23A, XPREP V2005/2, SADABS V2007/4 (Bruker, 2005 & 2007) ; _computing_structure_solution 'SHELXTL V6.12 (Bruker, 2005)' _computing_structure_refinement 'SHELXTL V6.12 (Bruker, 2005)' _computing_molecular_graphics 'SHELXTL V6.12 (Bruker, 2005)' _computing_publication_material 'XCIF V6.12 (Bruker, 2005)' _refine_special_details ; Structure was phased by dual space methods (Schneider, 2002). Systematic conditions suggested the ambiguous space group. The space group choice was confirmed by successful convergence of the full-matrix least-squares refinement (Sheldrick, 2008) on F^2^. The highest peak in the final difference Fourier map was located 2.6\%A from the nearest aromatic H atom. This residual density located in a void suggests the possibility of a partially occupied water solvate. The final map had no other significant features. A final analysis of variance between observed and calculated structure factors showed no dependence on amplitude or resolution. For the data crystal, mean I/\s(I) was less than 1 for reflections beyond 1.2\%A resolution. Reflections between 1.2 and 0.8\%A resolution were used for least-squares refinement to improve the data-to-variable ratio at the expense of agreement factors. ; _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^)+(0.0919P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9961 _refine_ls_number_parameters 655 _refine_ls_number_restraints 268 _refine_ls_R_factor_all 0.2969 _refine_ls_R_factor_gt 0.0796 _refine_ls_wR_factor_ref 0.2443 _refine_ls_wR_factor_gt 0.1594 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.899 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1015(9) 0.8803(9) 0.2731(6) 0.036(3) Uani 1 1 d . . . C2 C 0.2061(12) 0.6526(10) 0.3591(6) 0.049(3) Uani 1 1 d . . . C3 C 0.1261(13) 0.5831(10) 0.3611(8) 0.080(5) Uani 1 1 d . . . H3A H 0.1044 0.5473 0.4107 0.120 Uiso 1 1 calc R . . H3B H 0.1714 0.5282 0.3276 0.120 Uiso 1 1 calc R . . H3C H 0.0512 0.6291 0.3462 0.120 Uiso 1 1 calc R . . C4 C 0.3705(10) 0.7122(9) 0.4535(7) 0.043(3) Uani 1 1 d . . . C5 C 0.4857(11) 0.8349(9) 0.3693(6) 0.045(3) Uani 1 1 d . . . C6 C -0.0800(11) 1.1318(10) 0.2302(7) 0.055(4) Uani 1 1 d . . . H6 H -0.1633 1.1741 0.2344 0.066 Uiso 1 1 calc R . . C7 C -0.0059(11) 1.1039(11) 0.1649(7) 0.066(4) Uani 1 1 d . A . H7 H -0.0375 1.1234 0.1226 0.080 Uiso 1 1 calc R . . C8 C -0.1339(5) 1.0372(6) 0.3768(3) 0.038(3) Uani 1 1 d G . . C9 C -0.2534(6) 1.1065(4) 0.3894(4) 0.047(3) Uani 1 1 d G . . H9 H -0.2705 1.1783 0.3652 0.056 Uiso 1 1 calc R . . C10 C -0.3477(5) 1.0707(6) 0.4374(4) 0.050(3) Uani 1 1 d G . . H10 H -0.4293 1.1180 0.4460 0.060 Uiso 1 1 calc R . . C11 C -0.3226(6) 0.9655(6) 0.4728(3) 0.042(3) Uani 1 1 d G . . H11 H -0.3871 0.9410 0.5056 0.051 Uiso 1 1 calc R . . C12 C -0.2032(7) 0.8962(5) 0.4602(4) 0.039(3) Uani 1 1 d G . . H12 H -0.1860 0.8244 0.4844 0.047 Uiso 1 1 calc R . . C13 C -0.1088(5) 0.9321(5) 0.4122(4) 0.034(3) Uani 1 1 d G . . H13 H -0.0272 0.8847 0.4036 0.040 Uiso 1 1 calc R . . C14 C -0.0408(6) 1.2123(5) 0.3435(5) 0.041(3) Uani 1 1 d G . . C15 C -0.0567(7) 1.3121(7) 0.3005(4) 0.062(4) Uani 1 1 d G . . H15 H -0.0606 1.3178 0.2514 0.074 Uiso 1 1 calc R . . C16 C -0.0669(7) 1.4034(5) 0.3294(7) 0.074(5) Uani 1 1 d G . . H16 H -0.0778 1.4716 0.3001 0.089 Uiso 1 1 calc R . . C17 C -0.0612(7) 1.3950(7) 0.4013(7) 0.084(5) Uani 1 1 d G . . H17 H -0.0682 1.4575 0.4211 0.101 Uiso 1 1 calc R . . C18 C -0.0453(8) 1.2953(10) 0.4443(4) 0.076(4) Uani 1 1 d G . . H18 H -0.0414 1.2896 0.4934 0.091 Uiso 1 1 calc R . . C19 C -0.0351(7) 1.2040(6) 0.4154(4) 0.050(3) Uani 1 1 d G . . H19 H -0.0242 1.1358 0.4448 0.060 Uiso 1 1 calc R . . C20 C 0.1767(10) 0.9228(7) 0.1033(3) 0.059(3) Uani 0.523(12) 1 d PGDU A 1 C21 C 0.2827(11) 0.8348(10) 0.0975(8) 0.060(3) Uani 0.523(12) 1 d PGDU A 1 H21 H 0.3428 0.8297 0.1221 0.072 Uiso 0.523(12) 1 calc PR A 1 C22 C 0.3007(13) 0.7544(10) 0.0557(9) 0.063(4) Uani 0.523(12) 1 d PGDU A 1 H22 H 0.3731 0.6944 0.0517 0.075 Uiso 0.523(12) 1 calc PR A 1 C23 C 0.2128(16) 0.7620(10) 0.0197(6) 0.065(4) Uani 0.523(12) 1 d PGDU A 1 H23 H 0.2251 0.7070 -0.0089 0.078 Uiso 0.523(12) 1 calc PR A 1 C24 C 0.1068(16) 0.8499(12) 0.0254(8) 0.065(4) Uani 0.523(12) 1 d PGDU A 1 H24 H 0.0467 0.8550 0.0008 0.078 Uiso 0.523(12) 1 calc PR A 1 C25 C 0.0888(13) 0.9303(9) 0.0672(8) 0.062(4) Uani 0.523(12) 1 d PGDU A 1 H25 H 0.0164 0.9903 0.0712 0.075 Uiso 0.523(12) 1 calc PR A 1 C26 C 0.2314(7) 1.1211(6) 0.0946(4) 0.043(3) Uani 1 1 d G A . C27 C 0.1655(6) 1.2264(7) 0.0732(4) 0.057(4) Uani 1 1 d G . . H27 H 0.0793 1.2514 0.0918 0.068 Uiso 1 1 calc R . . C28 C 0.2259(9) 1.2952(5) 0.0245(5) 0.075(4) Uani 1 1 d G . . H28 H 0.1809 1.3671 0.0099 0.089 Uiso 1 1 calc R . . C29 C 0.3522(9) 1.2586(7) -0.0027(4) 0.070(4) Uani 1 1 d G . . H29 H 0.3935 1.3056 -0.0359 0.084 Uiso 1 1 calc R . . C30 C 0.4180(6) 1.1533(8) 0.0188(4) 0.064(4) Uani 1 1 d G . . H30 H 0.5043 1.1283 0.0002 0.076 Uiso 1 1 calc R . . C31 C 0.3576(7) 1.0845(5) 0.0674(4) 0.048(3) Uani 1 1 d G . . H31 H 0.4026 1.0125 0.0820 0.057 Uiso 1 1 calc R . . C32 C 0.4953(11) 0.5975(9) 0.2345(6) 0.057(4) Uani 1 1 d . . . H32A H 0.5679 0.5451 0.2087 0.085 Uiso 1 1 calc R . . H32B H 0.4684 0.6613 0.2003 0.085 Uiso 1 1 calc R . . H32C H 0.4293 0.5641 0.2555 0.085 Uiso 1 1 calc R . . C33 C 0.6720(10) 0.6711(9) 0.2611(7) 0.061(4) Uani 1 1 d . . . H33A H 0.7271 0.6141 0.2310 0.091 Uiso 1 1 calc R . . H33B H 0.7118 0.6768 0.2972 0.091 Uiso 1 1 calc R . . H33C H 0.6528 0.7404 0.2301 0.091 Uiso 1 1 calc R . . C34 C 0.5760(10) 0.5161(8) 0.3662(7) 0.059(4) Uani 1 1 d . . . H34A H 0.6436 0.4622 0.3383 0.088 Uiso 1 1 calc R . . H34B H 0.5058 0.4881 0.3872 0.088 Uiso 1 1 calc R . . H34C H 0.6025 0.5308 0.4055 0.088 Uiso 1 1 calc R . . C35 C 0.2617(9) 1.0462(8) 0.3629(5) 0.032(3) Uani 1 1 d . A . H35A H 0.2015 1.1088 0.3871 0.039 Uiso 1 1 calc R . . H35B H 0.3409 1.0312 0.3753 0.039 Uiso 1 1 calc R . . C36 C 0.3981(9) 1.0016(7) 0.2440(6) 0.032(3) Uani 1 1 d . A . H36A H 0.4617 0.9926 0.2698 0.038 Uiso 1 1 calc R . . H36B H 0.4228 1.0353 0.1934 0.038 Uiso 1 1 calc R . . C37 C 0.2573(9) 1.1872(8) 0.2564(6) 0.036(3) Uani 1 1 d . . . H37A H 0.1816 1.2293 0.2883 0.043 Uiso 1 1 calc R . . H37B H 0.2445 1.2018 0.2065 0.043 Uiso 1 1 calc R . . C38 C 0.3638(6) 1.2274(5) 0.2555(5) 0.035(3) Uani 1 1 d G . . C39 C 0.3747(7) 1.2532(6) 0.3189(3) 0.043(3) Uani 1 1 d G . . H39 H 0.3164 1.2452 0.3636 0.051 Uiso 1 1 calc R . . C40 C 0.4709(8) 1.2905(6) 0.3169(4) 0.056(4) Uani 1 1 d G . . H40 H 0.4784 1.3082 0.3602 0.067 Uiso 1 1 calc R . . C41 C 0.5562(6) 1.3021(6) 0.2515(6) 0.058(4) Uani 1 1 d G . . H41 H 0.6220 1.3277 0.2501 0.069 Uiso 1 1 calc R . . C42 C 0.5453(7) 1.2763(6) 0.1881(4) 0.073(4) Uani 1 1 d G . . H42 H 0.6035 1.2843 0.1434 0.087 Uiso 1 1 calc R . . C43 C 0.4490(8) 1.2389(6) 0.1902(4) 0.058(4) Uani 1 1 d G . . H43 H 0.4416 1.2213 0.1469 0.070 Uiso 1 1 calc R . . N1 N 0.2769(7) 1.0692(6) 0.2823(5) 0.031(2) Uani 1 1 d . . . N2 N 0.2650(8) 0.7038(7) 0.3545(5) 0.039(3) Uani 1 1 d . . . O1 O 0.0564(7) 0.8192(6) 0.2694(4) 0.049(2) Uani 1 1 d . . . O2 O 0.3663(8) 0.6744(6) 0.5118(5) 0.060(3) Uani 1 1 d . . . O3 O 0.5536(7) 0.8728(6) 0.3775(5) 0.058(3) Uani 1 1 d . . . Fe1 Fe 0.17198(13) 0.97592(12) 0.27405(8) 0.0311(4) Uani 1 1 d . A . Fe2 Fe 0.37848(14) 0.77777(12) 0.36002(9) 0.0358(5) Uani 1 1 d . A . P1 P -0.0168(3) 1.0867(2) 0.30890(16) 0.0371(8) Uani 1 1 d . . . P2 P 0.1531(3) 1.0297(3) 0.15900(17) 0.0427(9) Uani 1 1 d D . . P3 P 0.5329(3) 0.6381(2) 0.30731(18) 0.0449(9) Uani 1 1 d . . . S1 S 0.2075(2) 0.9281(2) 0.39190(15) 0.0328(7) Uani 1 1 d . . . S2 S 0.3775(2) 0.8717(2) 0.24425(16) 0.0363(8) Uani 1 1 d . . . B1 B 0.2804(14) 0.3670(11) 0.5078(9) 0.048(4) Uani 1 1 d . . . F1 F 0.3058(7) 0.4635(6) 0.4747(4) 0.084(2) Uani 1 1 d . . . F2 F 0.2528(10) 0.3642(7) 0.5811(5) 0.127(4) Uani 1 1 d . . . F3 F 0.1800(8) 0.3677(6) 0.4877(5) 0.106(3) Uani 1 1 d . . . F4 F 0.3731(7) 0.2788(6) 0.4892(4) 0.091(3) Uani 1 1 d . . . B2 B 0.8102(16) 0.4214(13) 0.1071(10) 0.058(4) Uani 1 1 d . . . F5 F 0.7078(8) 0.4809(7) 0.0825(5) 0.109(3) Uani 1 1 d . . . F6 F 0.7957(10) 0.4369(9) 0.1757(6) 0.148(5) Uani 1 1 d . . . F7 F 0.8225(8) 0.3153(6) 0.1104(5) 0.098(3) Uani 1 1 d . . . F8 F 0.9130(9) 0.4379(8) 0.0632(7) 0.167(5) Uani 1 1 d . . . C44 C 0.0734(16) 0.5516(13) 0.1254(11) 0.124(7) Uani 1 1 d . . . H44A H 0.0189 0.5085 0.1279 0.148 Uiso 1 1 calc R . . H44B H 0.1034 0.5772 0.0735 0.148 Uiso 1 1 calc R . . Cl1 Cl 0.1957(6) 0.4713(5) 0.1603(4) 0.162(2) Uani 1 1 d . . . Cl2 Cl -0.0086(5) 0.6618(5) 0.1728(4) 0.168(3) Uani 1 1 d . . . C45 C 0.799(2) 0.931(3) 0.1458(9) 0.136(4) Uani 0.676(15) 1 d PDU B 1 H45A H 0.8628 0.8600 0.1394 0.163 Uiso 0.676(15) 1 calc PR B 1 H45B H 0.8366 0.9884 0.1204 0.163 Uiso 0.676(15) 1 calc PR B 1 Cl3 Cl 0.7442(12) 0.9453(12) 0.2382(5) 0.127(4) Uani 0.676(15) 1 d PDU B 1 Cl4 Cl 0.6810(10) 0.9384(12) 0.1062(6) 0.129(3) Uani 0.676(15) 1 d PDU B 1 C46 C 0.732(6) 1.013(3) 0.1410(15) 0.128(5) Uani 0.324(15) 1 d PDU B 2 H46A H 0.8101 1.0273 0.1133 0.154 Uiso 0.324(15) 1 calc PR B 2 H46B H 0.6642 1.0706 0.1243 0.154 Uiso 0.324(15) 1 calc PR B 2 Cl5 Cl 0.714(2) 1.013(2) 0.2341(12) 0.125(4) Uani 0.324(15) 1 d PDU B 2 Cl6 Cl 0.734(2) 0.8871(18) 0.1242(13) 0.131(4) Uani 0.324(15) 1 d PDU B 2 C47 C 0.1990(7) 0.9160(8) 0.1034(5) 0.060(3) Uani 0.477(12) 1 d PGDU A 2 C48 C 0.2593(14) 0.8117(9) 0.1301(7) 0.061(4) Uani 0.477(12) 1 d PGDU A 2 H48 H 0.2771 0.7983 0.1766 0.074 Uiso 0.477(12) 1 calc PR A 2 C49 C 0.2936(16) 0.7268(8) 0.0889(9) 0.064(4) Uani 0.477(12) 1 d PGDU A 2 H49 H 0.3349 0.6555 0.1071 0.077 Uiso 0.477(12) 1 calc PR A 2 C50 C 0.2676(14) 0.7464(11) 0.0209(8) 0.066(4) Uani 0.477(12) 1 d PGDU A 2 H50 H 0.2910 0.6884 -0.0073 0.080 Uiso 0.477(12) 1 calc PR A 2 C51 C 0.2072(19) 0.8507(13) -0.0058(7) 0.069(4) Uani 0.477(12) 1 d PGDU A 2 H51 H 0.1894 0.8641 -0.0523 0.083 Uiso 0.477(12) 1 calc PR A 2 C52 C 0.1729(16) 0.9355(10) 0.0355(7) 0.064(4) Uani 0.477(12) 1 d PGDU A 2 H52 H 0.1317 1.0069 0.0172 0.076 Uiso 0.477(12) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.033(7) 0.044(7) 0.038(8) -0.004(6) -0.010(6) -0.019(6) C2 0.059(9) 0.052(9) 0.040(9) 0.006(7) -0.023(7) -0.019(7) C3 0.100(12) 0.080(10) 0.094(12) 0.018(9) -0.054(10) -0.061(10) C4 0.044(8) 0.037(7) 0.054(9) 0.014(7) -0.023(7) -0.019(6) C5 0.039(8) 0.042(8) 0.044(8) 0.012(6) -0.014(6) -0.007(6) C6 0.041(8) 0.073(9) 0.048(9) 0.020(7) -0.025(7) -0.015(7) C7 0.035(8) 0.112(12) 0.042(9) 0.016(8) -0.015(7) -0.020(8) C8 0.041(7) 0.039(7) 0.040(8) -0.004(6) -0.009(6) -0.022(6) C9 0.028(7) 0.044(7) 0.064(9) 0.005(7) -0.017(7) -0.006(6) C10 0.020(7) 0.059(9) 0.068(10) -0.010(7) 0.004(6) -0.017(6) C11 0.030(7) 0.072(9) 0.038(8) -0.018(7) -0.005(6) -0.028(7) C12 0.050(8) 0.035(7) 0.044(8) 0.005(6) -0.013(6) -0.031(6) C13 0.030(7) 0.027(6) 0.045(8) -0.011(6) -0.006(6) -0.008(5) C14 0.036(7) 0.023(6) 0.058(9) 0.005(6) -0.003(6) -0.014(5) C15 0.023(7) 0.046(8) 0.098(12) 0.021(8) -0.013(7) -0.007(6) C16 0.041(9) 0.025(8) 0.141(16) 0.001(9) -0.003(10) -0.013(7) C17 0.052(10) 0.072(12) 0.128(16) -0.049(12) 0.006(10) -0.021(9) C18 0.051(9) 0.089(12) 0.093(13) -0.027(11) -0.005(8) -0.030(9) C19 0.052(9) 0.037(8) 0.067(10) -0.002(7) -0.020(7) -0.020(7) C20 0.073(7) 0.083(7) 0.038(6) -0.003(6) -0.021(6) -0.041(6) C21 0.074(7) 0.088(7) 0.038(7) -0.012(6) -0.023(6) -0.038(6) C22 0.080(7) 0.089(7) 0.038(7) -0.014(6) -0.025(6) -0.037(6) C23 0.083(8) 0.090(7) 0.043(7) -0.015(6) -0.027(6) -0.039(7) C24 0.081(8) 0.089(7) 0.041(7) -0.008(6) -0.027(6) -0.037(7) C25 0.076(8) 0.086(7) 0.042(7) -0.006(6) -0.025(6) -0.038(7) C26 0.040(8) 0.056(8) 0.028(7) 0.009(6) -0.011(6) -0.012(6) C27 0.069(10) 0.055(9) 0.037(8) 0.005(7) -0.013(7) -0.015(8) C28 0.109(13) 0.050(9) 0.051(10) 0.021(8) -0.014(9) -0.028(9) C29 0.084(12) 0.061(10) 0.059(10) 0.021(8) -0.017(9) -0.030(9) C30 0.056(9) 0.086(11) 0.040(9) -0.010(8) 0.010(7) -0.028(9) C31 0.048(8) 0.042(7) 0.050(9) 0.001(7) -0.014(7) -0.012(7) C32 0.074(10) 0.035(7) 0.068(10) -0.026(7) -0.024(8) -0.006(7) C33 0.048(8) 0.054(8) 0.066(10) -0.005(7) -0.003(7) -0.009(7) C34 0.051(9) 0.033(7) 0.084(11) -0.009(7) -0.019(8) 0.000(6) C35 0.022(6) 0.038(7) 0.036(8) -0.001(6) -0.002(5) -0.015(5) C36 0.026(6) 0.035(6) 0.030(7) 0.005(5) 0.000(5) -0.015(5) C37 0.037(7) 0.030(7) 0.039(8) 0.009(6) -0.011(6) -0.014(5) C38 0.033(7) 0.021(6) 0.046(8) 0.007(6) -0.010(6) -0.008(5) C39 0.063(9) 0.042(7) 0.028(8) 0.000(6) -0.008(6) -0.027(7) C40 0.059(9) 0.050(8) 0.068(10) 0.008(7) -0.024(8) -0.028(7) C41 0.043(8) 0.036(8) 0.100(12) -0.011(8) -0.021(9) -0.015(6) C42 0.068(10) 0.071(10) 0.076(12) -0.027(9) 0.025(8) -0.041(8) C43 0.077(10) 0.055(9) 0.054(10) -0.007(7) -0.008(8) -0.039(8) N1 0.032(6) 0.035(5) 0.028(6) -0.004(5) -0.004(4) -0.015(4) N2 0.044(7) 0.025(6) 0.048(7) 0.003(5) -0.012(5) -0.014(5) O1 0.053(5) 0.045(5) 0.062(6) -0.009(4) -0.017(4) -0.027(4) O2 0.072(7) 0.058(6) 0.054(6) 0.020(5) -0.027(5) -0.029(5) O3 0.043(5) 0.054(6) 0.094(7) -0.006(5) -0.040(5) -0.017(5) Fe1 0.0302(10) 0.0319(9) 0.0328(10) 0.0019(8) -0.0098(8) -0.0128(8) Fe2 0.0367(10) 0.0294(9) 0.0432(12) 0.0026(8) -0.0157(8) -0.0115(8) P1 0.0338(18) 0.0411(19) 0.035(2) 0.0054(15) -0.0114(15) -0.0131(15) P2 0.039(2) 0.055(2) 0.035(2) 0.0012(17) -0.0112(16) -0.0179(17) P3 0.042(2) 0.0297(18) 0.061(2) 0.0014(17) -0.0173(18) -0.0083(15) S1 0.0341(17) 0.0350(17) 0.0303(18) 0.0003(14) -0.0075(14) -0.0143(14) S2 0.0307(17) 0.0358(17) 0.041(2) 0.0002(15) -0.0077(14) -0.0123(14) B1 0.050(10) 0.031(9) 0.047(11) 0.011(8) -0.006(9) -0.009(8) F1 0.093(6) 0.066(5) 0.104(7) 0.018(5) -0.033(5) -0.048(5) F2 0.208(11) 0.073(6) 0.077(7) -0.008(5) -0.044(7) -0.007(6) F3 0.103(7) 0.072(6) 0.170(9) 0.033(6) -0.084(7) -0.047(5) F4 0.079(6) 0.066(5) 0.091(7) 0.005(5) -0.004(5) 0.001(5) B2 0.066(13) 0.044(10) 0.062(13) 0.015(9) -0.022(10) -0.021(9) F5 0.094(7) 0.102(7) 0.112(8) 0.041(6) -0.056(6) -0.014(5) F6 0.139(10) 0.172(10) 0.135(10) -0.088(8) -0.077(8) 0.030(7) F7 0.108(7) 0.065(6) 0.130(8) 0.004(5) -0.048(6) -0.031(5) F8 0.078(7) 0.146(9) 0.232(14) 0.056(9) 0.002(8) -0.060(7) C44 0.115(15) 0.089(13) 0.17(2) -0.057(14) 0.024(14) -0.056(12) Cl1 0.185(6) 0.122(5) 0.174(6) -0.021(4) -0.043(5) -0.040(4) Cl2 0.117(4) 0.143(5) 0.245(7) -0.068(5) 0.006(5) -0.054(4) C45 0.107(8) 0.176(10) 0.147(6) -0.022(7) -0.028(6) -0.070(8) Cl3 0.112(7) 0.166(10) 0.135(5) 0.002(6) -0.042(4) -0.083(8) Cl4 0.096(7) 0.171(10) 0.138(6) -0.035(6) -0.029(4) -0.054(7) C46 0.103(8) 0.166(10) 0.143(7) -0.027(8) -0.028(6) -0.071(8) Cl5 0.105(8) 0.162(11) 0.140(7) -0.016(8) -0.033(6) -0.077(10) Cl6 0.109(9) 0.169(11) 0.145(7) -0.028(7) -0.028(6) -0.078(8) C47 0.073(7) 0.084(7) 0.039(6) -0.003(6) -0.020(6) -0.042(6) C48 0.074(7) 0.088(7) 0.038(7) -0.009(6) -0.020(6) -0.038(6) C49 0.077(8) 0.091(7) 0.040(7) -0.011(6) -0.023(6) -0.036(7) C50 0.081(8) 0.092(7) 0.044(7) -0.011(6) -0.028(7) -0.035(7) C51 0.084(8) 0.093(7) 0.044(7) -0.010(6) -0.029(7) -0.031(7) C52 0.078(8) 0.086(7) 0.042(7) -0.007(6) -0.024(6) -0.037(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 C1 O1 1.139(11) . ? C1 Fe1 1.753(11) . ? C2 N2 1.110(13) . ? C2 C3 1.529(17) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 O2 1.127(12) . ? C4 Fe2 1.823(13) . ? C5 O3 1.152(12) . ? C5 Fe2 1.765(13) . ? C6 C7 1.352(15) . ? C6 P1 1.795(11) . ? C6 H6 0.9500 . ? C7 P2 1.799(12) . ? C7 H7 0.9500 . ? C8 C9 1.3900 . ? C8 C13 1.3900 . ? C8 P1 1.819(6) . ? C9 C10 1.3900 . ? C9 H9 0.9500 . ? C10 C11 1.3900 . ? C10 H10 0.9500 . ? C11 C12 1.3900 . ? C11 H11 0.9500 . ? C12 C13 1.3900 . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.3900 . ? C14 C19 1.3900 . ? C14 P1 1.823(7) . ? C15 C16 1.3900 . ? C15 H15 0.9500 . ? C16 C17 1.3900 . ? C16 H16 0.9500 . ? C17 C18 1.3900 . ? C17 H17 0.9500 . ? C18 C19 1.3900 . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.3900 . ? C20 C25 1.3900 . ? C20 P2 1.852(8) . ? C21 C22 1.3900 . ? C21 H21 0.9500 . ? C22 C23 1.3900 . ? C22 H22 0.9500 . ? C23 C24 1.3900 . ? C23 H23 0.9500 . ? C24 C25 1.3900 . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.3900 . ? C26 C31 1.3900 . ? C26 P2 1.833(6) . ? C27 C28 1.3900 . ? C27 H27 0.9500 . ? C28 C29 1.3900 . ? C28 H28 0.9500 . ? C29 C30 1.3900 . ? C29 H29 0.9500 . ? C30 C31 1.3900 . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 P3 1.823(11) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 P3 1.797(11) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 P3 1.782(11) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 N1 1.490(12) . ? C35 S1 1.817(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 N1 1.486(12) . ? C36 S2 1.819(9) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 N1 1.496(11) . ? C37 C38 1.535(10) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.3900 . ? C38 C43 1.3900 . ? C39 C40 1.3900 . ? C39 H39 0.9500 . ? C40 C41 1.3900 . ? C40 H40 0.9500 . ? C41 C42 1.3900 . ? C41 H41 0.9500 . ? C42 C43 1.3900 . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? N1 Fe1 2.098(8) . ? N2 Fe2 1.965(10) . ? Fe1 P1 2.226(3) . ? Fe1 P2 2.241(3) . ? Fe1 S2 2.336(3) . ? Fe1 S1 2.355(3) . ? Fe2 P3 2.282(4) . ? Fe2 S2 2.323(3) . ? Fe2 S1 2.346(3) . ? P2 C47 1.866(8) . ? B1 F4 1.332(15) . ? B1 F2 1.353(16) . ? B1 F3 1.364(16) . ? B1 F1 1.396(14) . ? B2 F8 1.334(18) . ? B2 F6 1.335(18) . ? B2 F7 1.351(16) . ? B2 F5 1.367(17) . ? C44 Cl1 1.714(19) . ? C44 Cl2 1.725(15) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 Cl3 1.739(13) . ? C45 Cl4 1.756(13) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 Cl5 1.749(14) . ? C46 Cl6 1.753(14) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.3900 . ? C47 C52 1.3900 . ? C48 C49 1.3900 . ? C48 H48 0.9500 . ? C49 C50 1.3900 . ? C49 H49 0.9500 . ? C50 C51 1.3900 . ? C50 H50 0.9500 . ? C51 C52 1.3900 . ? C51 H51 0.9500 . ? C52 H52 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 C1 Fe1 177.1(10) . . ? N2 C2 C3 177.0(13) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O2 C4 Fe2 177.8(10) . . ? O3 C5 Fe2 178.0(11) . . ? C7 C6 P1 118.3(10) . . ? C7 C6 H6 120.9 . . ? P1 C6 H6 120.9 . . ? C6 C7 P2 119.2(10) . . ? C6 C7 H7 120.4 . . ? P2 C7 H7 120.4 . . ? C9 C8 C13 120.0 . . ? C9 C8 P1 117.6(4) . . ? C13 C8 P1 122.3(4) . . ? C8 C9 C10 120.0 . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C9 C10 C11 120.0 . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 120.0 . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C13 C12 C11 120.0 . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C8 120.0 . . ? C12 C13 H13 120.0 . . ? C8 C13 H13 120.0 . . ? C15 C14 C19 120.0 . . ? C15 C14 P1 123.2(6) . . ? C19 C14 P1 116.7(6) . . ? C16 C15 C14 120.0 . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C18 120.0 . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C19 C18 C17 120.0 . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C14 120.0 . . ? C18 C19 H19 120.0 . . ? C14 C19 H19 120.0 . . ? C21 C20 C25 120.0 . . ? C21 C20 P2 119.9(6) . . ? C25 C20 P2 120.1(6) . . ? C20 C21 C22 120.0 . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C21 C22 C23 120.0 . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 120.0 . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 120.0 . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C20 120.0 . . ? C24 C25 H25 120.0 . . ? C20 C25 H25 120.0 . . ? C27 C26 C31 120.0 . . ? C27 C26 P2 120.5(5) . . ? C31 C26 P2 119.5(5) . . ? C26 C27 C28 120.0 . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.0 . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 120.0 . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C26 120.0 . . ? C30 C31 H31 120.0 . . ? C26 C31 H31 120.0 . . ? P3 C32 H32A 109.5 . . ? P3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? P3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? P3 C33 H33A 109.5 . . ? P3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? P3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? P3 C34 H34A 109.5 . . ? P3 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? P3 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N1 C35 S1 106.4(6) . . ? N1 C35 H35A 110.4 . . ? S1 C35 H35A 110.4 . . ? N1 C35 H35B 110.4 . . ? S1 C35 H35B 110.4 . . ? H35A C35 H35B 108.6 . . ? N1 C36 S2 105.4(6) . . ? N1 C36 H36A 110.7 . . ? S2 C36 H36A 110.7 . . ? N1 C36 H36B 110.7 . . ? S2 C36 H36B 110.7 . . ? H36A C36 H36B 108.8 . . ? N1 C37 C38 114.0(7) . . ? N1 C37 H37A 108.7 . . ? C38 C37 H37A 108.7 . . ? N1 C37 H37B 108.7 . . ? C38 C37 H37B 108.7 . . ? H37A C37 H37B 107.6 . . ? C39 C38 C43 120.0 . . ? C39 C38 C37 120.8(7) . . ? C43 C38 C37 119.2(7) . . ? C40 C39 C38 120.0 . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C39 C40 C41 120.0 . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C42 C41 C40 120.0 . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C41 C42 C43 120.0 . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C42 C43 C38 120.0 . . ? C42 C43 H43 120.0 . . ? C38 C43 H43 120.0 . . ? C36 N1 C35 110.7(8) . . ? C36 N1 C37 111.8(8) . . ? C35 N1 C37 111.8(8) . . ? C36 N1 Fe1 97.4(5) . . ? C35 N1 Fe1 97.2(5) . . ? C37 N1 Fe1 126.4(6) . . ? C2 N2 Fe2 170.5(10) . . ? C1 Fe1 N1 170.7(4) . . ? C1 Fe1 P1 86.2(4) . . ? N1 Fe1 P1 100.9(2) . . ? C1 Fe1 P2 84.8(4) . . ? N1 Fe1 P2 101.4(2) . . ? P1 Fe1 P2 87.24(12) . . ? C1 Fe1 S2 99.9(4) . . ? N1 Fe1 S2 72.8(2) . . ? P1 Fe1 S2 173.23(13) . . ? P2 Fe1 S2 96.15(12) . . ? C1 Fe1 S1 100.7(4) . . ? N1 Fe1 S1 72.9(2) . . ? P1 Fe1 S1 95.12(12) . . ? P2 Fe1 S1 174.18(13) . . ? S2 Fe1 S1 80.97(11) . . ? C5 Fe2 C4 88.9(5) . . ? C5 Fe2 N2 175.4(4) . . ? C4 Fe2 N2 87.4(4) . . ? C5 Fe2 P3 90.9(4) . . ? C4 Fe2 P3 95.6(4) . . ? N2 Fe2 P3 86.8(3) . . ? C5 Fe2 S2 91.1(4) . . ? C4 Fe2 S2 175.9(4) . . ? N2 Fe2 S2 92.8(3) . . ? P3 Fe2 S2 88.45(12) . . ? C5 Fe2 S1 95.1(4) . . ? C4 Fe2 S1 94.5(4) . . ? N2 Fe2 S1 87.9(3) . . ? P3 Fe2 S1 168.33(13) . . ? S2 Fe2 S1 81.45(11) . . ? C6 P1 C8 103.0(5) . . ? C6 P1 C14 103.5(5) . . ? C8 P1 C14 99.9(4) . . ? C6 P1 Fe1 107.4(5) . . ? C8 P1 Fe1 120.5(3) . . ? C14 P1 Fe1 120.2(3) . . ? C7 P2 C26 102.5(5) . . ? C7 P2 C20 101.7(6) . . ? C26 P2 C20 102.8(3) . . ? C7 P2 C47 109.4(6) . . ? C26 P2 C47 100.2(4) . . ? C7 P2 Fe1 106.3(4) . . ? C26 P2 Fe1 123.6(3) . . ? C20 P2 Fe1 117.0(3) . . ? C47 P2 Fe1 113.9(4) . . ? C34 P3 C33 106.0(6) . . ? C34 P3 C32 104.7(5) . . ? C33 P3 C32 102.4(6) . . ? C34 P3 Fe2 116.2(4) . . ? C33 P3 Fe2 114.0(4) . . ? C32 P3 Fe2 112.2(4) . . ? C35 S1 Fe2 106.4(3) . . ? C35 S1 Fe1 80.3(3) . . ? Fe2 S1 Fe1 94.32(11) . . ? C36 S2 Fe2 107.7(4) . . ? C36 S2 Fe1 80.9(3) . . ? Fe2 S2 Fe1 95.46(12) . . ? F4 B1 F2 108.1(12) . . ? F4 B1 F3 110.1(13) . . ? F2 B1 F3 108.8(12) . . ? F4 B1 F1 113.4(12) . . ? F2 B1 F1 109.5(13) . . ? F3 B1 F1 106.7(11) . . ? F8 B2 F6 112.2(15) . . ? F8 B2 F7 107.0(14) . . ? F6 B2 F7 105.0(13) . . ? F8 B2 F5 113.2(14) . . ? F6 B2 F5 110.7(15) . . ? F7 B2 F5 108.3(13) . . ? Cl1 C44 Cl2 111.3(11) . . ? Cl1 C44 H44A 109.4 . . ? Cl2 C44 H44A 109.4 . . ? Cl1 C44 H44B 109.4 . . ? Cl2 C44 H44B 109.4 . . ? H44A C44 H44B 108.0 . . ? Cl3 C45 Cl4 111.7(13) . . ? Cl3 C45 H45A 109.3 . . ? Cl4 C45 H45A 109.3 . . ? Cl3 C45 H45B 109.3 . . ? Cl4 C45 H45B 109.3 . . ? H45A C45 H45B 107.9 . . ? Cl5 C46 Cl6 110.5(16) . . ? Cl5 C46 H46A 109.5 . . ? Cl6 C46 H46A 109.5 . . ? Cl5 C46 H46B 109.5 . . ? Cl6 C46 H46B 109.6 . . ? H46A C46 H46B 108.1 . . ? C48 C47 C52 120.0 . . ? C48 C47 P2 119.9(6) . . ? C52 C47 P2 120.1(6) . . ? C49 C48 C47 120.0 . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C48 C49 C50 120.0 . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C51 C50 C49 120.0 . . ? C51 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C52 C51 C50 120.0 . . ? C52 C51 H51 120.0 . . ? C50 C51 H51 120.0 . . ? C51 C52 C47 120.0 . . ? C51 C52 H52 120.0 . . ? C47 C52 H52 120.0 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.589 _refine_diff_density_min -0.690 _refine_diff_density_rms 0.111 _vrf_RINTA01_ba79cas ; PROBLEM: The value of Rint is greater than 0.20 RESPONSE: For the best availabe crystal, mean I/\s(I) was less than 1 for reflections beyond 1.2\%A resolution. Reflections between 1.2 and 0.8\%A resolution were used for least-squares refinement to improve the data-to-variable ratio at the expense of agreement factors. ; _vrf_PLAT020_ba79cas ; PROBLEM: The value of Rint is greater than 0.10 ......... 0.24 RESPONSE: For the best availabe crystal, mean I/\s(I) was less than 1 for reflections beyond 1.2\%A resolution. Reflections between 1.2 and 0.8\%A resolution were used for least-squares refinement to improve the data-to-variable ratio at the expense of agreement factors. ; # end Validation Reply Form _publ_requested_category FM _publ_section_references ; Allen, F.H., Kennard, O., Watson, D.G., Brammer, L., Orpen, A.G., and Taylor, R. (1987). J. Chem. Soc. Perkin Trans. II. S1-S19. Bruker (2004). APEX2. Bruker AXS, Inc., Madison, Wisconsin, USA. Bruker (2005). SAINT, SHELXTL, XCIF, XPREP. Bruker AXS, Inc., Madison, Wisconsin, USA. Bruker (2007). SADABS. Bruker AXS, Inc., Madison, Wisconsin, USA. Schneider, T.R. and Sheldrick, G.M. (2002). Acta Cryst. D58, 1772-1779. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122 ; _publ_section_figure_captions ; Figure 1. SHELXTL (Bruker, 2005) plot showing 35% probability ellipsoids for non-H atoms and circles of arbitrary size for H atoms. Minor site disordered phenyl atoms, anions, and solvate molecules were omitted for clarity. ; _publ_section_exptl_prep ; Crystals were grown by liquid diffusion of hexanes into methylene chloride solution at -30C. ; _publ_section_exptl_refinement ; The proposed model includes two disordered positions for phenyl ring C20-25 of the host cation and two disordered positions for one of two DCM solvate molecules. All phenyl rings were refined as rigid, idealized groups. A common geometry was imposed on the disordered DCM solvates using effective standard deviations of 0.01 and 0.02\%A for bond lengths and bond angles, respectively. This common geometry converged in satisfactory agreement with expected values (Allen et al, 1987). Rigid-bond restraints (esd 0.01) were imposed on displacement parameters for all disordered sites and similar displacement amplitudes (esd 0.01) were imposed on disordered sites overlapping by less than the sum of van der Waals radii. Methyl H atom positions, R-CH~3~, were optimized by rotation about R-C bonds with idealized C-H, R--H and H--H distances. Remaining H atoms were included as riding idealized contributors. Methyl H atom U's were assigned as 1.5 times U~eq~ of the carrier atom; remaining H atom U's were assigned as 1.2 times carrier U~eq~. ; _publ_contact_author ; Scott R. Wilson University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; _publ_contact_author_phone '1 217 244 1708' _publ_contact_author_fax '1 217 244 8068' _publ_contact_author_email srwilson@uiuc.edu _publ_contact_letter ; Please consider this CIF submission for publication as a structural paper in Acta Crystallographica E. ; _publ_requested_journal 'Acta Crystallographica E' _publ_requested_coeditor_name ? _publ_section_title ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_acknowledgements ; The Materials Chemistry Laboratory at the University of Illinois was supported in part by grants NSF CHE 95-03145 and NSF CHE 03-43032 from the National Science Foundation. ; loop_ _publ_author_name _publ_author_address 'Wilson, Scott R.' ; University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; 'Prussak-Wieckowska, Teresa' ; University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; 'Gao, Yi-Gui' ; University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; 'Ramesh, Maya' ; University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 1.00 0.00 0.0400 -1.00 -1.00 0.00 0.0100 2.00 -1.00 1.00 0.1800 -1.00 0.00 0.00 0.1300 3.00 1.00 2.00 0.1100 0.00 0.00 1.00 0.0100 0.00 0.00 -1.00 0.0100