# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Tapas Maji' _publ_contact_author_email TMAJI@JNCASR.AC.IN _publ_section_title ; A flexible supramolecular porous host with a crowned chair octameric water cluster and highly selective sorption properties ; loop_ _publ_author_name 'Tapas Maji' 'Arpan Hazra' 'Prakash Kanoo' 'Sudip Mohapatra' 'Golam Mostafa' # Attachment 'compound1.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 743895' #TrackingRef 'compound1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H43 Fe N12 O8' _chemical_formula_weight 827.67 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.7496(10) _cell_length_b 10.3079(5) _cell_length_c 11.9451(6) _cell_angle_alpha 114.920(2) _cell_angle_beta 110.933(4) _cell_angle_gamma 91.374(3) _cell_volume 995.02(12) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 25.1 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 433 _exptl_absorpt_coefficient_mu 0.445 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8312 _exptl_absorpt_correction_T_max 0.9871 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14096 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0778 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.08 _reflns_number_total 6721 _reflns_number_gt 5346 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker,2000)' _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Mercury 1.4.1' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0288P)^2^+0.6029P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.26(2) _refine_ls_number_reflns 6721 _refine_ls_number_parameters 515 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1028 _refine_ls_wR_factor_gt 0.0935 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 0.93048(12) -0.22534(13) 0.81645(11) 0.01675(14) Uani 1 1 d . . . N1 N 0.9642(6) 0.1066(6) 0.9091(6) 0.0291(15) Uani 1 1 d . . . N2 N 1.0288(6) -0.2485(6) 0.5903(5) 0.0230(13) Uani 1 1 d . . . N3 N 1.2594(6) -0.1851(6) 1.0022(6) 0.0274(14) Uani 1 1 d . . . N4 N 0.8963(6) -0.5567(7) 0.7262(6) 0.0261(14) Uani 1 1 d . . . N5 N 0.8266(5) -0.2056(6) 1.0403(5) 0.0251(14) Uani 1 1 d . . . N6 N 0.5973(6) -0.2692(6) 0.6257(5) 0.0268(14) Uani 1 1 d . . . N7 N 0.7110(6) -0.4225(6) 0.1889(6) 0.0269(14) Uani 1 1 d . . . H1 H 0.7998 -0.4207 0.1902 0.032 Uiso 1 1 d R . . N8 N -0.0164(7) -0.4331(7) 0.1820(6) 0.0304(15) Uani 1 1 d . . . N9 N 0.8640(5) -0.0246(5) 0.4383(5) 0.0140(12) Uani 1 1 d . . . H2 H 0.9519 -0.0265 0.4378 0.017 Uiso 1 1 d R . . N10 N 0.1396(6) -0.0326(6) 0.4344(6) 0.0212(13) Uani 1 1 d . . . N11 N 1.0336(4) 0.2789(5) 0.3107(4) 0.0242(10) Uani 1 1 d . . . H3 H 1.1219 0.2796 0.3109 0.029 Uiso 1 1 d R . . N12 N 0.3097(5) 0.2781(5) 0.3090(5) 0.0214(11) Uani 1 1 d . . . C1 C 0.9522(7) -0.0187(8) 0.8748(6) 0.0226(16) Uani 1 1 d . . . C2 C 0.9925(6) -0.2403(7) 0.6736(7) 0.0190(15) Uani 1 1 d . . . C3 C 1.1383(7) -0.1996(7) 0.9339(6) 0.0194(17) Uani 1 1 d . . . C4 C 0.9110(6) -0.4332(7) 0.7596(6) 0.0169(14) Uani 1 1 d . . . C5 C 0.8643(7) -0.2120(7) 0.9558(6) 0.0166(14) Uani 1 1 d . . . C6 C 0.7236(7) -0.2537(7) 0.6969(6) 0.0207(17) Uani 1 1 d . . . C7 C 0.6865(8) -0.3970(8) 0.3012(7) 0.0313(18) Uani 1 1 d . . . H7 H 0.7695 -0.3791 0.3818 0.038 Uiso 1 1 calc R . . C8 C 0.5886(8) -0.4498(7) 0.0752(7) 0.0270(17) Uani 1 1 d . . . H8 H 0.6024 -0.4673 -0.0044 0.032 Uiso 1 1 calc R . . C9 C 0.5477(8) -0.3965(7) 0.3014(7) 0.0236(16) Uani 1 1 d . . . H9 H 0.5368 -0.3737 0.3832 0.028 Uiso 1 1 calc R . . C10 C 0.4487(8) -0.4529(8) 0.0712(7) 0.0285(18) Uani 1 1 d . . . H10 H 0.3673 -0.4721 -0.0108 0.034 Uiso 1 1 calc R . . C11 C 0.4198(8) -0.4287(7) 0.1845(7) 0.0228(17) Uani 1 1 d . . . C12 C 0.2686(8) -0.4333(7) 0.1842(7) 0.0225(16) Uani 1 1 d . . . C13 C 0.2475(8) -0.3913(8) 0.3024(7) 0.0306(18) Uani 1 1 d . . . H13 H 0.3311 -0.3636 0.3855 0.037 Uiso 1 1 calc R . . C14 C 0.1381(8) -0.4782(8) 0.0611(7) 0.0266(17) Uani 1 1 d . . . H14 H 0.1467 -0.5090 -0.0226 0.032 Uiso 1 1 calc R . . C15 C 0.1054(8) -0.3898(7) 0.2989(7) 0.0246(17) Uani 1 1 d . . . H15 H 0.0923 -0.3575 0.3809 0.030 Uiso 1 1 calc R . . C16 C 0.0038(8) -0.4756(8) 0.0675(8) 0.0309(19) Uani 1 1 d . . . H16 H -0.0825 -0.5057 -0.0143 0.037 Uiso 1 1 calc R . . C17 C 0.8500(7) 0.0153(7) 0.5545(7) 0.0198(15) Uani 1 1 d . . . H17 H 0.9360 0.0426 0.6359 0.024 Uiso 1 1 calc R . . C18 C 0.7455(7) -0.0623(7) 0.3230(7) 0.0217(16) Uani 1 1 d . . . H18 H 0.7595 -0.0888 0.2420 0.026 Uiso 1 1 calc R . . C19 C 0.7057(7) 0.0165(7) 0.5553(7) 0.0186(15) Uani 1 1 d . . . H19 H 0.6949 0.0452 0.6379 0.022 Uiso 1 1 calc R . . C20 C 0.6035(7) -0.0632(7) 0.3197(6) 0.0151(14) Uani 1 1 d . . . H20 H 0.5198 -0.0911 0.2366 0.018 Uiso 1 1 calc R . . C21 C 0.5812(7) -0.0229(7) 0.4388(6) 0.0154(15) Uani 1 1 d . . . C22 C 0.4264(7) -0.0244(7) 0.4374(6) 0.0136(14) Uani 1 1 d . . . C23 C 0.4028(6) -0.0113(7) 0.5492(7) 0.0173(15) Uani 1 1 d . . . H23 H 0.4841 0.0004 0.6285 0.021 Uiso 1 1 calc R . . C24 C 0.3038(7) -0.0403(7) 0.3242(7) 0.0195(15) Uani 1 1 d . . . H24 H 0.3164 -0.0461 0.2471 0.023 Uiso 1 1 calc R . . C25 C 0.2560(7) -0.0158(7) 0.5423(7) 0.0195(16) Uani 1 1 d . . . H25 H 0.2398 -0.0062 0.6190 0.023 Uiso 1 1 calc R . . C26 C 0.1637(7) -0.0473(7) 0.3267(7) 0.0208(15) Uani 1 1 d . . . H26 H 0.0796 -0.0635 0.2475 0.025 Uiso 1 1 calc R . . C27 C 0.9141(7) 0.1781(7) 0.2017(6) 0.0334(17) Uani 1 1 d . . . H27 H 0.9288 0.1094 0.1257 0.040 Uiso 1 1 calc R . . C28 C 1.0121(7) 0.3761(7) 0.4174(6) 0.0301(16) Uani 1 1 d . . . H28 H 1.0957 0.4469 0.4930 0.036 Uiso 1 1 calc R . . C29 C 0.7755(6) 0.1743(6) 0.1999(6) 0.0299(15) Uani 1 1 d . . . H29 H 0.6941 0.1019 0.1231 0.036 Uiso 1 1 calc R . . C30 C 0.8748(6) 0.3764(6) 0.4208(6) 0.0276(14) Uani 1 1 d . . . H30 H 0.8632 0.4451 0.4986 0.033 Uiso 1 1 calc R . . C31 C 0.7487(5) 0.2738(5) 0.3077(5) 0.0212(12) Uani 1 1 d . . . C32 C 0.5955(5) 0.2723(5) 0.3081(5) 0.0145(12) Uani 1 1 d . . . C33 C 0.5751(6) 0.3209(7) 0.4262(7) 0.0226(14) Uani 1 1 d . . . H33 H 0.6598 0.3515 0.5092 0.027 Uiso 1 1 calc R . . C34 C 0.4695(6) 0.2233(6) 0.1891(6) 0.0212(13) Uani 1 1 d . . . H34 H 0.4793 0.1876 0.1055 0.025 Uiso 1 1 calc R . . C35 C 0.4343(5) 0.3262(6) 0.4267(5) 0.0182(13) Uani 1 1 d . . . H35 H 0.4238 0.3639 0.5101 0.022 Uiso 1 1 calc R . . C36 C 0.3284(6) 0.2262(6) 0.1914(5) 0.0179(13) Uani 1 1 d . . . H36 H 0.2425 0.1909 0.1086 0.021 Uiso 1 1 calc R . . O1W O 1.2320(5) 0.1871(6) 0.8690(5) 0.0440(14) Uani 1 1 d . . . H1W H 1.1574 0.1580 0.8852 0.066 Uiso 1 1 d R . . H2W H 1.2109 0.2322 0.8198 0.066 Uiso 1 1 d R . . O2W O 0.6186(5) -0.6495(6) 0.7423(5) 0.0425(14) Uani 1 1 d . . . H3W H 0.7000 -0.6195 0.7407 0.064 Uiso 1 1 d R . . H4W H 0.6441 -0.6893 0.7909 0.064 Uiso 1 1 d R . . O3W O 1.5310(5) -0.1273(6) 0.9816(6) 0.0532(16) Uani 1 1 d . . . H5W H 1.6043 -0.1870 0.9804 0.080 Uiso 1 1 d R . . H6W H 1.4493 -0.1577 0.9930 0.080 Uiso 1 1 d R . . O4W O 0.4662(5) 0.0468(6) 0.8551(5) 0.0449(14) Uani 1 1 d . . . H7W H 0.3915 0.0879 0.8628 0.067 Uiso 1 1 d R . . H8W H 0.4811 -0.0062 0.8968 0.067 Uiso 1 1 d R . . O5W O 1.1366(5) -0.7122(5) 0.6856(5) 0.0469(14) Uani 1 1 d . . . H9W H 1.0662 -0.6662 0.6980 0.070 Uiso 1 1 d R . . H10W H 1.2142 -0.6503 0.7067 0.070 Uiso 1 1 d R . . O6W O 0.7115(6) 0.2454(5) 0.9269(6) 0.0492(14) Uani 1 1 d . . . H11W H 0.7857 0.2037 0.9214 0.074 Uiso 1 1 d R . . H12W H 0.6348 0.1826 0.9044 0.074 Uiso 1 1 d R . . O7W O 0.3163(5) -0.3509(5) 0.6174(5) 0.0373(12) Uani 1 1 d . . . H13W H 0.3932 -0.3060 0.6180 0.056 Uiso 1 1 d R . . H14W H 0.2453 -0.3019 0.6090 0.056 Uiso 1 1 d R . . O8W O 1.3828(6) -0.5173(6) 0.7517(5) 0.0520(14) Uani 1 1 d . . . H15W H 1.3397 -0.4685 0.7064 0.078 Uiso 1 1 d R . . H16W H 1.4804 -0.5440 0.7491 0.078 Uiso 1 1 d 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 0.0138(3) 0.0211(3) 0.0143(3) 0.0065(2) 0.0065(2) 0.0050(2) N1 0.031(3) 0.017(4) 0.037(4) 0.008(3) 0.017(3) 0.001(3) N2 0.024(3) 0.025(3) 0.020(3) 0.010(3) 0.009(3) 0.009(2) N3 0.018(3) 0.038(4) 0.020(3) 0.012(3) 0.004(3) 0.005(3) N4 0.020(3) 0.038(4) 0.023(3) 0.014(3) 0.011(2) 0.013(3) N5 0.017(3) 0.033(4) 0.022(3) 0.007(3) 0.011(2) -0.002(2) N6 0.021(3) 0.041(4) 0.023(3) 0.015(3) 0.013(3) 0.008(3) N7 0.025(3) 0.033(4) 0.027(3) 0.015(3) 0.012(2) 0.014(3) N8 0.035(3) 0.039(4) 0.024(3) 0.018(3) 0.014(3) 0.013(3) N9 0.012(3) 0.015(3) 0.018(3) 0.008(2) 0.008(2) 0.002(2) N10 0.015(3) 0.020(3) 0.025(3) 0.009(3) 0.007(2) 0.005(2) N11 0.017(2) 0.032(3) 0.025(2) 0.017(2) 0.006(2) 0.010(2) N12 0.018(2) 0.027(2) 0.024(3) 0.012(2) 0.013(2) 0.0098(19) C1 0.019(3) 0.037(5) 0.015(3) 0.012(3) 0.010(3) 0.007(3) C2 0.005(3) 0.023(4) 0.022(4) 0.008(3) 0.000(3) 0.008(3) C3 0.013(4) 0.024(4) 0.026(4) 0.011(3) 0.013(3) 0.001(3) C4 0.011(3) 0.025(4) 0.016(3) 0.010(3) 0.006(2) 0.004(3) C5 0.020(3) 0.010(3) 0.010(3) -0.001(3) 0.002(3) 0.000(3) C6 0.033(5) 0.022(4) 0.005(4) 0.003(3) 0.010(3) 0.009(3) C7 0.053(5) 0.024(4) 0.013(4) 0.012(3) 0.006(3) 0.007(3) C8 0.036(4) 0.020(4) 0.016(3) 0.006(3) 0.003(3) 0.010(3) C9 0.037(4) 0.023(4) 0.014(3) 0.008(3) 0.014(3) 0.014(3) C10 0.035(4) 0.027(4) 0.017(4) 0.010(3) 0.004(3) 0.004(3) C11 0.036(4) 0.009(4) 0.020(4) 0.009(3) 0.005(3) 0.006(3) C12 0.035(4) 0.011(3) 0.021(4) 0.010(3) 0.009(3) 0.007(3) C13 0.044(5) 0.024(4) 0.018(4) 0.010(3) 0.007(3) 0.002(3) C14 0.026(4) 0.031(4) 0.014(3) 0.011(3) -0.002(3) 0.007(3) C15 0.036(4) 0.019(4) 0.023(4) 0.010(3) 0.015(3) 0.004(3) C16 0.028(4) 0.039(5) 0.022(4) 0.016(3) 0.005(3) 0.010(3) C17 0.017(3) 0.022(4) 0.023(4) 0.009(3) 0.012(3) 0.008(3) C18 0.029(4) 0.026(4) 0.018(4) 0.014(3) 0.013(3) 0.006(3) C19 0.022(3) 0.024(4) 0.012(3) 0.007(3) 0.011(3) 0.007(3) C20 0.015(3) 0.020(4) 0.012(3) 0.009(3) 0.004(2) 0.000(3) C21 0.012(3) 0.017(4) 0.018(3) 0.007(3) 0.008(3) 0.004(3) C22 0.018(3) 0.014(3) 0.004(3) 0.000(3) 0.005(2) 0.003(2) C23 0.006(3) 0.023(3) 0.021(4) 0.010(3) 0.004(2) 0.004(2) C24 0.017(3) 0.021(3) 0.026(4) 0.016(3) 0.008(3) 0.008(3) C25 0.012(3) 0.029(4) 0.015(3) 0.009(3) 0.005(2) -0.001(3) C26 0.016(3) 0.020(4) 0.021(4) 0.006(3) 0.006(3) 0.009(3) C27 0.045(4) 0.027(3) 0.016(3) 0.002(2) 0.010(3) 0.000(3) C28 0.046(4) 0.023(3) 0.015(3) 0.008(2) 0.006(3) 0.005(3) C29 0.038(3) 0.030(3) 0.016(3) 0.008(2) 0.009(3) 0.004(3) C30 0.025(3) 0.028(3) 0.019(3) 0.008(2) 0.003(2) -0.001(3) C31 0.025(3) 0.019(3) 0.014(2) 0.009(2) 0.002(2) 0.007(2) C32 0.019(3) 0.010(2) 0.014(3) 0.004(2) 0.007(2) 0.006(2) C33 0.014(3) 0.035(3) 0.022(3) 0.013(3) 0.011(2) 0.008(2) C34 0.013(3) 0.030(3) 0.024(3) 0.013(2) 0.010(2) 0.005(2) C35 0.006(3) 0.031(3) 0.013(3) 0.007(2) 0.003(2) 0.005(2) C36 0.016(3) 0.020(3) 0.009(3) 0.002(2) 0.002(2) 0.008(2) O1W 0.035(3) 0.065(4) 0.054(3) 0.038(3) 0.029(2) 0.012(3) O2W 0.031(3) 0.059(4) 0.037(3) 0.022(3) 0.014(2) 0.001(2) O3W 0.029(3) 0.060(3) 0.099(4) 0.051(3) 0.037(3) 0.019(2) O4W 0.043(3) 0.072(4) 0.035(3) 0.035(3) 0.020(2) 0.022(3) O5W 0.040(3) 0.055(3) 0.063(3) 0.030(3) 0.035(2) 0.025(2) O6W 0.044(3) 0.053(3) 0.065(4) 0.032(3) 0.029(2) 0.024(2) O7W 0.029(2) 0.056(3) 0.043(2) 0.035(2) 0.0168(19) 0.017(2) O8W 0.062(3) 0.056(3) 0.057(3) 0.040(3) 0.026(3) 0.031(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 C1 1.921(7) . ? Fe1 C4 1.937(7) . ? Fe1 C6 1.938(7) . ? Fe1 C3 1.943(7) . ? Fe1 C5 1.945(6) . ? Fe1 C2 1.955(7) . ? N1 C1 1.167(8) . ? N2 C2 1.142(8) . ? N3 C3 1.132(7) . ? N4 C4 1.150(8) . ? N5 C5 1.170(8) . ? N6 C6 1.180(7) . ? N7 C8 1.360(9) . ? N7 C7 1.364(9) . ? N7 H1 0.8600 . ? N8 C16 1.339(9) . ? N8 C15 1.351(9) . ? N9 C17 1.332(8) . ? N9 C18 1.332(8) . ? N9 H2 0.8598 . ? N10 C25 1.318(8) . ? N10 C26 1.336(9) . ? N11 C28 1.341(7) . ? N11 C27 1.361(7) . ? N11 H3 0.8599 . ? N12 C36 1.359(7) . ? N12 C35 1.365(7) . ? C7 C9 1.355(10) . ? C7 H7 0.9500 . ? C8 C10 1.347(9) . ? C8 H8 0.9500 . ? C9 C11 1.401(9) . ? C9 H9 0.9500 . ? C10 C11 1.402(10) . ? C10 H10 0.9500 . ? C11 C12 1.472(9) . ? C12 C13 1.386(10) . ? C12 C14 1.434(9) . ? C13 C15 1.372(10) . ? C13 H13 0.9500 . ? C14 C16 1.339(10) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C19 1.411(8) . ? C17 H17 0.9500 . ? C18 C20 1.371(9) . ? C18 H18 0.9500 . ? C19 C21 1.366(8) . ? C19 H19 0.9500 . ? C20 C21 1.404(9) . ? C20 H20 0.9500 . ? C21 C22 1.503(8) . ? C22 C23 1.387(9) . ? C22 C24 1.390(9) . ? C23 C25 1.402(8) . ? C23 H23 0.9500 . ? C24 C26 1.378(8) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C29 1.343(8) . ? C27 H27 0.9500 . ? C28 C30 1.353(8) . ? C28 H28 0.9500 . ? C29 C31 1.386(7) . ? C29 H29 0.9500 . ? C30 C31 1.415(7) . ? C30 H30 0.9500 . ? C31 C32 1.494(6) . ? C32 C33 1.375(7) . ? C32 C34 1.380(8) . ? C33 C35 1.377(6) . ? C33 H33 0.9500 . ? C34 C36 1.386(7) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? O1W H1W 0.8919 . ? O1W H2W 0.8673 . ? O2W H3W 0.8543 . ? O2W H4W 0.8183 . ? O3W H5W 0.9543 . ? O3W H6W 0.9234 . ? O4W H7W 0.8650 . ? O4W H8W 0.8655 . ? O5W H9W 0.8643 . ? O5W H10W 0.8649 . ? O6W H11W 0.8588 . ? O6W H12W 0.8585 . ? O7W H13W 0.8678 . ? O7W H14W 0.8684 . ? O8W H15W 0.8941 . ? O8W H16W 1.0043 . ? 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 C1 Fe1 C4 179.2(4) . . ? C1 Fe1 C6 89.4(3) . . ? C4 Fe1 C6 91.3(3) . . ? C1 Fe1 C3 91.2(3) . . ? C4 Fe1 C3 88.0(3) . . ? C6 Fe1 C3 179.0(4) . . ? C1 Fe1 C5 92.3(3) . . ? C4 Fe1 C5 87.5(3) . . ? C6 Fe1 C5 89.3(2) . . ? C3 Fe1 C5 91.3(3) . . ? C1 Fe1 C2 87.9(3) . . ? C4 Fe1 C2 92.3(3) . . ? C6 Fe1 C2 89.5(3) . . ? C3 Fe1 C2 89.9(2) . . ? C5 Fe1 C2 178.8(3) . . ? C8 N7 C7 117.0(6) . . ? C8 N7 H1 121.6 . . ? C7 N7 H1 121.4 . . ? C16 N8 C15 118.6(6) . . ? C17 N9 C18 121.7(6) . . ? C17 N9 H2 119.0 . . ? C18 N9 H2 119.3 . . ? C25 N10 C26 117.9(5) . . ? C28 N11 C27 119.3(4) . . ? C28 N11 H3 120.6 . . ? C27 N11 H3 120.1 . . ? C36 N12 C35 118.2(4) . . ? N1 C1 Fe1 179.3(7) . . ? N2 C2 Fe1 179.7(6) . . ? N3 C3 Fe1 179.7(6) . . ? N4 C4 Fe1 178.4(5) . . ? N5 C5 Fe1 178.6(6) . . ? N6 C6 Fe1 178.9(6) . . ? C9 C7 N7 122.1(6) . . ? C9 C7 H7 119.0 . . ? N7 C7 H7 119.0 . . ? C10 C8 N7 122.5(7) . . ? C10 C8 H8 118.7 . . ? N7 C8 H8 118.7 . . ? C7 C9 C11 121.8(7) . . ? C7 C9 H9 119.1 . . ? C11 C9 H9 119.1 . . ? C8 C10 C11 121.9(7) . . ? C8 C10 H10 119.0 . . ? C11 C10 H10 119.0 . . ? C9 C11 C10 114.6(7) . . ? C9 C11 C12 121.6(7) . . ? C10 C11 C12 123.8(6) . . ? C13 C12 C14 117.8(7) . . ? C13 C12 C11 121.5(6) . . ? C14 C12 C11 120.7(7) . . ? C15 C13 C12 119.7(7) . . ? C15 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C16 C14 C12 118.2(7) . . ? C16 C14 H14 120.9 . . ? C12 C14 H14 120.9 . . ? N8 C15 C13 121.7(7) . . ? N8 C15 H15 119.1 . . ? C13 C15 H15 119.1 . . ? C14 C16 N8 124.0(8) . . ? C14 C16 H16 118.0 . . ? N8 C16 H16 118.0 . . ? N9 C17 C19 119.1(6) . . ? N9 C17 H17 120.5 . . ? C19 C17 H17 120.5 . . ? N9 C18 C20 120.8(6) . . ? N9 C18 H18 119.6 . . ? C20 C18 H18 119.6 . . ? C21 C19 C17 120.9(6) . . ? C21 C19 H19 119.5 . . ? C17 C19 H19 119.5 . . ? C18 C20 C21 120.2(6) . . ? C18 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C19 C21 C20 117.3(6) . . ? C19 C21 C22 121.6(6) . . ? C20 C21 C22 121.1(5) . . ? C23 C22 C24 118.6(6) . . ? C23 C22 C21 120.4(5) . . ? C24 C22 C21 121.0(6) . . ? C22 C23 C25 118.3(6) . . ? C22 C23 H23 120.8 . . ? C25 C23 H23 120.8 . . ? C26 C24 C22 118.4(6) . . ? C26 C24 H24 120.8 . . ? C22 C24 H24 120.8 . . ? N10 C25 C23 123.1(6) . . ? N10 C25 H25 118.5 . . ? C23 C25 H25 118.5 . . ? N10 C26 C24 123.7(6) . . ? N10 C26 H26 118.2 . . ? C24 C26 H26 118.2 . . ? C29 C27 N11 121.0(6) . . ? C29 C27 H27 119.5 . . ? N11 C27 H27 119.5 . . ? N11 C28 C30 122.0(6) . . ? N11 C28 H28 119.0 . . ? C30 C28 H28 119.0 . . ? C27 C29 C31 121.4(6) . . ? C27 C29 H29 119.3 . . ? C31 C29 H29 119.3 . . ? C28 C30 C31 119.6(6) . . ? C28 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C29 C31 C30 116.7(5) . . ? C29 C31 C32 122.4(4) . . ? C30 C31 C32 120.8(4) . . ? C33 C32 C34 117.7(5) . . ? C33 C32 C31 121.6(5) . . ? C34 C32 C31 120.7(4) . . ? C32 C33 C35 121.3(6) . . ? C32 C33 H33 119.3 . . ? C35 C33 H33 119.3 . . ? C32 C34 C36 120.1(5) . . ? C32 C34 H34 120.0 . . ? C36 C34 H34 120.0 . . ? N12 C35 C33 120.9(5) . . ? N12 C35 H35 119.6 . . ? C33 C35 H35 119.6 . . ? N12 C36 C34 121.7(5) . . ? N12 C36 H36 119.1 . . ? C34 C36 H36 119.1 . . ? H1W O1W H2W 116.7 . . ? H3W O2W H4W 104.6 . . ? H5W O3W H6W 116.3 . . ? H7W O4W H8W 109.1 . . ? H9W O5W H10W 109.2 . . ? H11W O6W H12W 110.3 . . ? H13W O7W H14W 108.6 . . ? H15W O8W H16W 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 C4 Fe1 C1 N1 176(100) . . . . ? C6 Fe1 C1 N1 -17(51) . . . . ? C3 Fe1 C1 N1 162(100) . . . . ? C5 Fe1 C1 N1 -106(51) . . . . ? C2 Fe1 C1 N1 73(51) . . . . ? C1 Fe1 C2 N2 1(100) . . . . ? C4 Fe1 C2 N2 -178(100) . . . . ? C6 Fe1 C2 N2 90(100) . . . . ? C3 Fe1 C2 N2 -90(100) . . . . ? C5 Fe1 C2 N2 102(100) . . . . ? C1 Fe1 C3 N3 168(100) . . . . ? C4 Fe1 C3 N3 -12(100) . . . . ? C6 Fe1 C3 N3 -59(100) . . . . ? C5 Fe1 C3 N3 76(100) . . . . ? C2 Fe1 C3 N3 -104(100) . . . . ? C1 Fe1 C4 N4 122(25) . . . . ? C6 Fe1 C4 N4 -45(21) . . . . ? C3 Fe1 C4 N4 136(21) . . . . ? C5 Fe1 C4 N4 44(21) . . . . ? C2 Fe1 C4 N4 -134(21) . . . . ? C1 Fe1 C5 N5 -132(24) . . . . ? C4 Fe1 C5 N5 48(24) . . . . ? C6 Fe1 C5 N5 139(24) . . . . ? C3 Fe1 C5 N5 -40(24) . . . . ? C2 Fe1 C5 N5 127(21) . . . . ? C1 Fe1 C6 N6 -48(35) . . . . ? C4 Fe1 C6 N6 132(35) . . . . ? C3 Fe1 C6 N6 179(100) . . . . ? C5 Fe1 C6 N6 44(35) . . . . ? C2 Fe1 C6 N6 -136(35) . . . . ? C8 N7 C7 C9 -0.9(10) . . . . ? C7 N7 C8 C10 -0.4(11) . . . . ? N7 C7 C9 C11 2.9(12) . . . . ? N7 C8 C10 C11 -0.3(12) . . . . ? C7 C9 C11 C10 -3.4(11) . . . . ? C7 C9 C11 C12 177.7(6) . . . . ? C8 C10 C11 C9 2.1(10) . . . . ? C8 C10 C11 C12 -179.0(7) . . . . ? C9 C11 C12 C13 6.8(11) . . . . ? C10 C11 C12 C13 -172.0(7) . . . . ? C9 C11 C12 C14 -174.8(6) . . . . ? C10 C11 C12 C14 6.4(11) . . . . ? C14 C12 C13 C15 -1.8(10) . . . . ? C11 C12 C13 C15 176.6(6) . . . . ? C13 C12 C14 C16 0.7(11) . . . . ? C11 C12 C14 C16 -177.8(7) . . . . ? C16 N8 C15 C13 -1.3(11) . . . . ? C12 C13 C15 N8 2.2(11) . . . . ? C12 C14 C16 N8 0.2(13) . . . . ? C15 N8 C16 C14 0.1(12) . . . . ? C18 N9 C17 C19 0.6(10) . . . . ? C17 N9 C18 C20 -1.0(10) . . . . ? N9 C17 C19 C21 0.2(11) . . . . ? N9 C18 C20 C21 0.6(10) . . . . ? C17 C19 C21 C20 -0.5(10) . . . . ? C17 C19 C21 C22 179.1(6) . . . . ? C18 C20 C21 C19 0.1(10) . . . . ? C18 C20 C21 C22 -179.4(6) . . . . ? C19 C21 C22 C23 -11.7(10) . . . . ? C20 C21 C22 C23 167.9(6) . . . . ? C19 C21 C22 C24 168.9(6) . . . . ? C20 C21 C22 C24 -11.5(10) . . . . ? C24 C22 C23 C25 0.5(9) . . . . ? C21 C22 C23 C25 -178.9(6) . . . . ? C23 C22 C24 C26 -2.2(10) . . . . ? C21 C22 C24 C26 177.2(6) . . . . ? C26 N10 C25 C23 0.6(10) . . . . ? C22 C23 C25 N10 0.4(11) . . . . ? C25 N10 C26 C24 -2.5(10) . . . . ? C22 C24 C26 N10 3.4(10) . . . . ? C28 N11 C27 C29 -0.3(9) . . . . ? C27 N11 C28 C30 0.6(9) . . . . ? N11 C27 C29 C31 1.0(10) . . . . ? N11 C28 C30 C31 -1.5(9) . . . . ? C27 C29 C31 C30 -1.7(8) . . . . ? C27 C29 C31 C32 179.8(6) . . . . ? C28 C30 C31 C29 2.0(8) . . . . ? C28 C30 C31 C32 -179.5(5) . . . . ? C29 C31 C32 C33 151.0(6) . . . . ? C30 C31 C32 C33 -27.4(7) . . . . ? C29 C31 C32 C34 -29.8(7) . . . . ? C30 C31 C32 C34 151.8(5) . . . . ? C34 C32 C33 C35 -2.5(8) . . . . ? C31 C32 C33 C35 176.7(5) . . . . ? C33 C32 C34 C36 0.9(8) . . . . ? C31 C32 C34 C36 -178.3(5) . . . . ? C36 N12 C35 C33 -0.6(8) . . . . ? C32 C33 C35 N12 2.4(9) . . . . ? C35 N12 C36 C34 -1.0(8) . . . . ? C32 C34 C36 N12 0.8(9) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.284 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.060 # start Validation Reply Form _vrf_PLAT113 ; PROBLEM: ADDSYM Suggests Possible Pseudo/New Space-group. P-1 RESPONSE: The additional symmetry is pseudo symmetry. The crystal is a twin. No solution and wrong refinement in the centrosymmetric P-1. This pseudo symmetry is discussed in the text. ; # end Validation Reply Form