# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Mir Wais Hosseini' _publ_contact_author_email HOSSEINI@CHIMIE.U-STRASBG.FR _publ_section_title ; Molecular tectonics: crystal engineering of mixed valence Fe(II)/Fe(III) solid solutions ; loop_ _publ_author_name 'Mir Wais Hosseini' 'Pierre Dechambenoit' 'Sylvie Ferlay' 'Kyritsakas Nathalie' # Attachment '22-Fe_II__CN_6_686_.cif' data_e686a _database_code_depnum_ccdc_archive 'CCDC 748252' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C26 H44 N4), C6 Fe N6, 6(H2 O)' _chemical_formula_sum 'C58 H100 Fe N14 O6' _chemical_formula_weight 1145.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.1100(8) _cell_length_b 17.7957(11) _cell_length_c 18.0780(13) _cell_angle_alpha 70.187(3) _cell_angle_beta 83.944(3) _cell_angle_gamma 80.834(3) _cell_volume 3314.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1647 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 20.49 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.148 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.283 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9777 _exptl_absorpt_correction_T_max 0.9860 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30641 _diffrn_reflns_av_R_equivalents 0.0974 _diffrn_reflns_av_sigmaI/netI 0.2298 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.68 _reflns_number_total 15294 _reflns_number_gt 6087 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1135P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15294 _refine_ls_number_parameters 699 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2242 _refine_ls_R_factor_gt 0.0839 _refine_ls_wR_factor_ref 0.2613 _refine_ls_wR_factor_gt 0.2042 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5281(5) 0.3144(3) 0.7008(3) 0.0268(12) Uani 1 1 d . . . N1 N 0.5049(4) 0.2617(3) 0.6697(3) 0.0342(11) Uani 1 1 d . . . H1 H 0.4288 0.2607 0.6610 0.041 Uiso 1 1 calc R . . C2 C 0.6011(5) 0.2048(3) 0.6491(4) 0.0407(15) Uani 1 1 d . . . H2A H 0.6364 0.2304 0.5954 0.049 Uiso 1 1 calc R . . H2B H 0.5661 0.1570 0.6494 0.049 Uiso 1 1 calc R . . C3 C 0.7022(5) 0.1786(3) 0.7083(4) 0.0396(15) Uani 1 1 d . . . C4 C 0.7438(5) 0.2561(4) 0.7083(4) 0.0452(16) Uani 1 1 d . . . H4A H 0.8004 0.2434 0.7510 0.054 Uiso 1 1 calc R . . H4B H 0.7886 0.2806 0.6576 0.054 Uiso 1 1 calc R . . N2 N 0.6401(4) 0.3140(3) 0.7198(3) 0.0344(12) Uani 1 1 d . . . H2 H 0.6529 0.3502 0.7403 0.041 Uiso 1 1 calc R . . C5 C 0.8140(7) 0.1312(4) 0.6761(5) 0.0791(14) Uani 1 1 d . . . H5A H 0.8390 0.1657 0.6227 0.095 Uiso 1 1 calc R . . H5B H 0.8828 0.1220 0.7101 0.095 Uiso 1 1 calc R . . C6 C 0.7938(7) 0.0504(4) 0.6712(5) 0.0791(14) Uani 1 1 d . . . H6A H 0.7265 0.0590 0.6363 0.095 Uiso 1 1 calc R . . H6B H 0.7690 0.0152 0.7243 0.095 Uiso 1 1 calc R . . C7 C 0.9076(7) 0.0087(4) 0.6402(5) 0.0791(14) Uani 1 1 d . . . H7A H 0.9206 0.0361 0.5835 0.119 Uiso 1 1 calc R . . H7B H 0.8974 -0.0476 0.6495 0.119 Uiso 1 1 calc R . . H7C H 0.9783 0.0104 0.6674 0.119 Uiso 1 1 calc R . . C8 C 0.6518(8) 0.1309(5) 0.7892(4) 0.0889(16) Uani 1 1 d . . . H8A H 0.5817 0.1650 0.8053 0.107 Uiso 1 1 calc R . . H8B H 0.6206 0.0834 0.7852 0.107 Uiso 1 1 calc R . . C9 C 0.7418(8) 0.1024(5) 0.8524(4) 0.0889(16) Uani 1 1 d . . . H9A H 0.7675 0.1495 0.8609 0.107 Uiso 1 1 calc R . . H9B H 0.8152 0.0715 0.8354 0.107 Uiso 1 1 calc R . . C10 C 0.6855(8) 0.0494(5) 0.9292(4) 0.0889(16) Uani 1 1 d . . . H10A H 0.6309 0.0834 0.9548 0.133 Uiso 1 1 calc R . . H10B H 0.7504 0.0182 0.9642 0.133 Uiso 1 1 calc R . . H10C H 0.6389 0.0125 0.9180 0.133 Uiso 1 1 calc R . . C11 C 0.4289(5) 0.3737(3) 0.7159(3) 0.0257(12) Uani 1 1 d . . . C12 C 0.4300(4) 0.4016(3) 0.7791(3) 0.0267(12) Uani 1 1 d . . . H12 H 0.4958 0.3825 0.8131 0.032 Uiso 1 1 calc R . . C13 C 0.3348(5) 0.4572(3) 0.7924(3) 0.0272(12) Uani 1 1 d . . . H13 H 0.3366 0.4769 0.8350 0.033 Uiso 1 1 calc R . . C14 C 0.2367(4) 0.4844(3) 0.7436(3) 0.0238(12) Uani 1 1 d . . . C15 C 0.2390(5) 0.4577(3) 0.6793(3) 0.0262(12) Uani 1 1 d . . . H15 H 0.1745 0.4777 0.6443 0.031 Uiso 1 1 calc R . . C16 C 0.3323(4) 0.4032(3) 0.6660(3) 0.0275(12) Uani 1 1 d . . . H16 H 0.3316 0.3852 0.6223 0.033 Uiso 1 1 calc R . . C17 C 0.1316(4) 0.5401(3) 0.7589(3) 0.0247(12) Uani 1 1 d . . . N3 N 0.1442(4) 0.5939(3) 0.7923(2) 0.0299(11) Uani 1 1 d . . . H3 H 0.2179 0.5976 0.8032 0.036 Uiso 1 1 calc R . . C18 C 0.0414(5) 0.6474(3) 0.8117(3) 0.0336(14) Uani 1 1 d . . . H18A H 0.0704 0.6973 0.8111 0.040 Uiso 1 1 calc R . . H18B H 0.0073 0.6208 0.8655 0.040 Uiso 1 1 calc R . . C19 C -0.0589(5) 0.6689(3) 0.7534(3) 0.0279(12) Uani 1 1 d . . . C20 C -0.0877(5) 0.5894(3) 0.7499(3) 0.0347(14) Uani 1 1 d . . . H20A H -0.1328 0.5618 0.7994 0.042 Uiso 1 1 calc R . . H20B H -0.1412 0.6005 0.7060 0.042 Uiso 1 1 calc R . . N4 N 0.0227(4) 0.5361(2) 0.7388(2) 0.0274(10) Uani 1 1 d . . . H4 H 0.0158 0.4993 0.7175 0.033 Uiso 1 1 calc R . . C21 C -0.1733(5) 0.7093(3) 0.7873(3) 0.0362(14) Uani 1 1 d . . . H21A H -0.2404 0.7198 0.7517 0.043 Uiso 1 1 calc R . . H21B H -0.1983 0.6712 0.8388 0.043 Uiso 1 1 calc R . . C22 C -0.1578(6) 0.7888(4) 0.7989(4) 0.0491(17) Uani 1 1 d . . . H22A H -0.0933 0.7786 0.8363 0.059 Uiso 1 1 calc R . . H22B H -0.1314 0.8271 0.7480 0.059 Uiso 1 1 calc R . . C23 C -0.2739(7) 0.8253(4) 0.8297(4) 0.069(2) Uani 1 1 d . . . H23A H -0.3367 0.8381 0.7915 0.103 Uiso 1 1 calc R . . H23B H -0.2605 0.8747 0.8383 0.103 Uiso 1 1 calc R . . H23C H -0.3010 0.7870 0.8797 0.103 Uiso 1 1 calc R . . C24 C -0.0126(5) 0.7216(3) 0.6731(3) 0.0304(13) Uani 1 1 d . . . H24A H 0.0219 0.7664 0.6805 0.037 Uiso 1 1 calc R . . H24B H 0.0550 0.6890 0.6529 0.037 Uiso 1 1 calc R . . C25 C -0.1058(6) 0.7572(4) 0.6108(3) 0.0468(16) Uani 1 1 d . . . H25A H -0.1763 0.7877 0.6311 0.056 Uiso 1 1 calc R . . H25B H -0.1359 0.7132 0.5992 0.056 Uiso 1 1 calc R . . C26 C -0.0509(7) 0.8130(4) 0.5356(4) 0.066(2) Uani 1 1 d . . . H26A H -0.0267 0.8588 0.5462 0.099 Uiso 1 1 calc R . . H26B H -0.1115 0.8327 0.4954 0.099 Uiso 1 1 calc R . . H26C H 0.0210 0.7835 0.5167 0.099 Uiso 1 1 calc R . . C27 C 0.0602(5) 0.3731(3) 0.9326(3) 0.0272(13) Uani 1 1 d . . . N5 N -0.0253(4) 0.3534(3) 0.8990(2) 0.0318(11) Uani 1 1 d . . . H5 H -0.0991 0.3805 0.8974 0.038 Uiso 1 1 calc R . . C28 C -0.0024(5) 0.2883(3) 0.8644(3) 0.0349(14) Uani 1 1 d . . . H28A H 0.0117 0.3118 0.8066 0.042 Uiso 1 1 calc R . . H28B H -0.0754 0.2601 0.8747 0.042 Uiso 1 1 calc R . . C29 C 0.1087(5) 0.2273(3) 0.8983(3) 0.0297(13) Uani 1 1 d . . . C30 C 0.2101(5) 0.2757(3) 0.8955(3) 0.0340(14) Uani 1 1 d . . . H30A H 0.2810 0.2388 0.9219 0.041 Uiso 1 1 calc R . . H30B H 0.2364 0.3024 0.8399 0.041 Uiso 1 1 calc R . . N6 N 0.1723(4) 0.3365(2) 0.9338(3) 0.0279(11) Uani 1 1 d . . . H6 H 0.2264 0.3489 0.9584 0.033 Uiso 1 1 calc R . . C31 C 0.0808(5) 0.1765(3) 0.9842(3) 0.0355(14) Uani 1 1 d . . . H31A H 0.1577 0.1439 1.0059 0.043 Uiso 1 1 calc R . . H31B H 0.0533 0.2136 1.0147 0.043 Uiso 1 1 calc R . . C32 C -0.0150(6) 0.1199(4) 0.9976(4) 0.0541(18) Uani 1 1 d . . . H32A H 0.0131 0.0802 0.9701 0.065 Uiso 1 1 calc R . . H32B H -0.0924 0.1513 0.9754 0.065 Uiso 1 1 calc R . . C33 C -0.0375(7) 0.0750(4) 1.0871(4) 0.075(2) Uani 1 1 d . . . H33A H 0.0401 0.0470 1.1098 0.112 Uiso 1 1 calc R . . H33B H -0.0941 0.0357 1.0944 0.112 Uiso 1 1 calc R . . H33C H -0.0728 0.1140 1.1135 0.112 Uiso 1 1 calc R . . C34 C 0.1464(6) 0.1781(4) 0.8427(4) 0.0445(16) Uani 1 1 d . . . H34A H 0.0773 0.1499 0.8411 0.053 Uiso 1 1 calc R . . H34B H 0.1614 0.2157 0.7890 0.053 Uiso 1 1 calc R . . C35 C 0.2594(7) 0.1160(4) 0.8644(4) 0.064(2) Uani 1 1 d . . . H35A H 0.2429 0.0752 0.9161 0.077 Uiso 1 1 calc R . . H35B H 0.3279 0.1430 0.8694 0.077 Uiso 1 1 calc R . . C36 C 0.2963(8) 0.0739(4) 0.8031(4) 0.077(3) Uani 1 1 d . . . H36A H 0.2285 0.0474 0.7977 0.115 Uiso 1 1 calc R . . H36B H 0.3678 0.0335 0.8199 0.115 Uiso 1 1 calc R . . H36C H 0.3164 0.1137 0.7524 0.115 Uiso 1 1 calc R . . C37 C 0.0295(5) 0.4378(3) 0.9678(3) 0.0232(12) Uani 1 1 d . . . C38 C 0.1200(5) 0.4808(3) 0.9747(3) 0.0264(12) Uani 1 1 d . . . H38 H 0.2021 0.4674 0.9579 0.032 Uiso 1 1 calc R . . C39 C -0.0908(5) 0.4570(3) 0.9939(3) 0.0292(13) Uani 1 1 d . . . H39 H -0.1526 0.4274 0.9902 0.035 Uiso 1 1 calc R . . C40 C 0.5446(4) 0.3818(3) 0.4207(3) 0.0222(12) Uani 1 1 d . . . N7 N 0.4515(4) 0.3665(2) 0.3918(2) 0.0247(10) Uani 1 1 d . . . H7 H 0.3774 0.3885 0.4013 0.030 Uiso 1 1 calc R . . C41 C 0.4683(5) 0.3133(3) 0.3437(3) 0.0322(13) Uani 1 1 d . . . H41A H 0.4872 0.3449 0.2881 0.039 Uiso 1 1 calc R . . H41B H 0.3916 0.2907 0.3461 0.039 Uiso 1 1 calc R . . C42 C 0.5715(5) 0.2448(3) 0.3725(3) 0.0259(12) Uani 1 1 d . . . C43 C 0.6838(4) 0.2851(3) 0.3746(3) 0.0273(12) Uani 1 1 d . . . H43A H 0.7487 0.2432 0.4026 0.033 Uiso 1 1 calc R . . H43B H 0.7158 0.3107 0.3201 0.033 Uiso 1 1 calc R . . N8 N 0.6545(4) 0.3458(2) 0.4138(2) 0.0270(10) Uani 1 1 d . . . H8 H 0.7141 0.3586 0.4337 0.032 Uiso 1 1 calc R . . C44 C 0.5385(5) 0.1885(3) 0.4554(3) 0.0297(13) Uani 1 1 d . . . H44A H 0.6121 0.1503 0.4752 0.036 Uiso 1 1 calc R . . H44B H 0.5170 0.2214 0.4906 0.036 Uiso 1 1 calc R . . C45 C 0.4342(6) 0.1403(4) 0.4616(4) 0.0484(17) Uani 1 1 d . . . H45A H 0.4527 0.1087 0.4251 0.058 Uiso 1 1 calc R . . H45B H 0.3583 0.1777 0.4458 0.058 Uiso 1 1 calc R . . C46 C 0.4145(6) 0.0828(4) 0.5460(4) 0.062(2) Uani 1 1 d . . . H46A H 0.4898 0.0460 0.5620 0.094 Uiso 1 1 calc R . . H46B H 0.3484 0.0515 0.5479 0.094 Uiso 1 1 calc R . . H46C H 0.3926 0.1141 0.5819 0.094 Uiso 1 1 calc R . . C47 C 0.6000(5) 0.2013(3) 0.3107(3) 0.0343(14) Uani 1 1 d . . . H47A H 0.5260 0.1790 0.3062 0.041 Uiso 1 1 calc R . . H47B H 0.6183 0.2415 0.2590 0.041 Uiso 1 1 calc R . . C48 C 0.7064(6) 0.1331(4) 0.3284(4) 0.0501(17) Uani 1 1 d . . . H48A H 0.6906 0.0936 0.3810 0.060 Uiso 1 1 calc R . . H48B H 0.7820 0.1553 0.3298 0.060 Uiso 1 1 calc R . . C49 C 0.7248(7) 0.0904(4) 0.2668(4) 0.073(2) Uani 1 1 d . . . H49A H 0.6490 0.0702 0.2638 0.109 Uiso 1 1 calc R . . H49B H 0.7905 0.0452 0.2818 0.109 Uiso 1 1 calc R . . H49C H 0.7467 0.1284 0.2154 0.109 Uiso 1 1 calc R . . C50 C 0.5211(4) 0.4416(3) 0.4629(3) 0.0220(12) Uani 1 1 d . . . C51 C 0.4272(4) 0.5059(3) 0.4401(3) 0.0238(12) Uani 1 1 d . . . H51 H 0.3775 0.5101 0.3988 0.029 Uiso 1 1 calc R . . C52 C 0.4063(4) 0.5637(3) 0.4775(3) 0.0224(11) Uani 1 1 d . . . H52 H 0.3420 0.6069 0.4621 0.027 Uiso 1 1 calc R . . Fe1 Fe 0.0000 0.5000 0.5000 0.0220(3) Uani 1 2 d S . . C53 C 0.1461(5) 0.4301(3) 0.4917(3) 0.0235(12) Uani 1 1 d . . . N9 N 0.2316(4) 0.3850(3) 0.4830(3) 0.0371(12) Uani 1 1 d . . . C54 C -0.0853(4) 0.4215(3) 0.4826(3) 0.0243(12) Uani 1 1 d . . . N10 N -0.1333(4) 0.3732(3) 0.4721(3) 0.0327(11) Uani 1 1 d . . . C55 C 0.0248(4) 0.5533(3) 0.3901(3) 0.0241(12) Uani 1 1 d . . . N11 N 0.0431(4) 0.5844(3) 0.3229(3) 0.0328(11) Uani 1 1 d . . . Fe2 Fe 0.5000 0.5000 0.0000 0.0240(3) Uani 1 2 d S . . C56 C 0.5742(5) 0.5905(3) -0.0012(3) 0.0251(12) Uani 1 1 d . . . N12 N 0.6184(4) 0.6450(3) 0.0000(3) 0.0344(12) Uani 1 1 d . . . C57 C 0.3742(5) 0.5271(3) 0.0722(3) 0.0287(13) Uani 1 1 d . . . N13 N 0.2984(4) 0.5481(3) 0.1127(3) 0.0369(12) Uani 1 1 d . . . C58 C 0.5934(4) 0.4304(3) 0.0869(3) 0.0259(12) Uani 1 1 d . . . N14 N 0.6517(4) 0.3888(3) 0.1392(3) 0.0328(11) Uani 1 1 d . . . O1 O 0.8087(5) 0.2692(3) 0.0754(4) 0.0930(18) Uani 1 1 d . . . O2 O 0.2887(3) 0.5505(2) 0.2668(2) 0.0384(10) Uani 1 1 d . . . O3 O 0.9588(5) 0.7404(3) 0.3632(3) 0.0904(18) Uani 1 1 d . . . O4 O 0.2913(4) 0.2461(2) 0.6072(2) 0.0456(11) Uani 1 1 d . . . O5 O 0.2954(6) 0.7197(3) 0.0812(4) 0.103(2) Uani 1 1 d . . . O6 O 0.4806(6) 0.8015(4) 0.9898(6) 0.192(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.023(3) 0.031(3) 0.024(3) -0.007(3) -0.001(2) -0.001(2) N1 0.027(3) 0.039(3) 0.040(3) -0.016(2) -0.006(2) -0.005(2) C2 0.043(4) 0.038(4) 0.044(4) -0.021(3) -0.003(3) 0.001(3) C3 0.036(3) 0.034(4) 0.050(4) -0.020(3) -0.007(3) 0.008(3) C4 0.032(3) 0.045(4) 0.058(4) -0.023(3) -0.003(3) 0.010(3) N2 0.026(3) 0.041(3) 0.041(3) -0.021(2) -0.004(2) 0.000(2) C5 0.086(4) 0.055(3) 0.092(4) -0.031(3) 0.020(3) 0.004(3) C6 0.086(4) 0.055(3) 0.092(4) -0.031(3) 0.020(3) 0.004(3) C7 0.086(4) 0.055(3) 0.092(4) -0.031(3) 0.020(3) 0.004(3) C8 0.112(4) 0.079(4) 0.052(3) 0.003(3) -0.017(3) 0.010(3) C9 0.112(4) 0.079(4) 0.052(3) 0.003(3) -0.017(3) 0.010(3) C10 0.112(4) 0.079(4) 0.052(3) 0.003(3) -0.017(3) 0.010(3) C11 0.024(3) 0.027(3) 0.024(3) -0.005(2) 0.003(2) -0.008(2) C12 0.018(3) 0.034(3) 0.024(3) -0.004(3) -0.002(2) -0.003(2) C13 0.028(3) 0.030(3) 0.023(3) -0.008(2) 0.001(2) -0.005(2) C14 0.024(3) 0.023(3) 0.022(3) -0.001(2) -0.004(2) -0.007(2) C15 0.026(3) 0.036(3) 0.017(3) -0.006(2) -0.004(2) -0.007(2) C16 0.024(3) 0.037(3) 0.024(3) -0.010(3) -0.005(2) -0.006(2) C17 0.024(3) 0.029(3) 0.019(3) -0.002(2) -0.001(2) -0.007(2) N3 0.023(2) 0.038(3) 0.030(3) -0.010(2) -0.007(2) -0.004(2) C18 0.029(3) 0.042(4) 0.035(3) -0.021(3) -0.004(3) 0.003(3) C19 0.027(3) 0.031(3) 0.026(3) -0.010(3) -0.007(2) 0.000(2) C20 0.023(3) 0.035(3) 0.042(4) -0.009(3) -0.002(3) -0.001(3) N4 0.020(2) 0.030(3) 0.035(3) -0.013(2) -0.001(2) -0.0033(19) C21 0.036(3) 0.039(4) 0.032(3) -0.012(3) 0.002(3) 0.000(3) C22 0.049(4) 0.042(4) 0.055(4) -0.021(3) 0.001(3) 0.006(3) C23 0.081(6) 0.055(5) 0.061(5) -0.022(4) 0.007(4) 0.015(4) C24 0.028(3) 0.031(3) 0.032(3) -0.010(3) -0.003(2) -0.002(2) C25 0.048(4) 0.049(4) 0.034(4) -0.004(3) -0.004(3) 0.004(3) C26 0.080(5) 0.061(5) 0.040(4) -0.005(4) -0.001(4) 0.013(4) C27 0.033(3) 0.022(3) 0.022(3) -0.001(2) 0.003(2) -0.009(3) N5 0.032(3) 0.031(3) 0.032(3) -0.006(2) -0.008(2) -0.008(2) C28 0.053(4) 0.026(3) 0.030(3) -0.012(3) -0.003(3) -0.011(3) C29 0.038(3) 0.022(3) 0.032(3) -0.013(3) 0.005(3) -0.008(3) C30 0.038(3) 0.029(3) 0.038(3) -0.018(3) 0.013(3) -0.008(3) N6 0.022(2) 0.026(3) 0.038(3) -0.014(2) -0.002(2) -0.004(2) C31 0.038(3) 0.029(3) 0.038(4) -0.013(3) 0.003(3) -0.002(3) C32 0.063(5) 0.039(4) 0.061(5) -0.017(4) 0.017(4) -0.019(3) C33 0.101(6) 0.044(4) 0.063(5) -0.008(4) 0.045(5) -0.018(4) C34 0.059(4) 0.036(4) 0.043(4) -0.020(3) 0.009(3) -0.015(3) C35 0.083(6) 0.048(4) 0.069(5) -0.033(4) 0.015(4) -0.012(4) C36 0.102(7) 0.052(5) 0.087(6) -0.045(5) 0.039(5) -0.019(4) C37 0.025(3) 0.022(3) 0.024(3) -0.007(2) -0.005(2) -0.007(2) C38 0.020(3) 0.026(3) 0.029(3) -0.003(3) 0.001(2) -0.003(2) C39 0.028(3) 0.032(3) 0.029(3) -0.009(3) -0.006(2) -0.008(2) C40 0.020(3) 0.024(3) 0.026(3) -0.012(2) -0.001(2) -0.004(2) N7 0.020(2) 0.027(2) 0.031(3) -0.016(2) -0.0050(19) 0.0029(19) C41 0.029(3) 0.036(3) 0.038(3) -0.019(3) -0.001(3) -0.007(3) C42 0.022(3) 0.028(3) 0.032(3) -0.016(3) 0.002(2) -0.005(2) C43 0.023(3) 0.025(3) 0.036(3) -0.016(3) 0.004(2) -0.001(2) N8 0.017(2) 0.029(3) 0.040(3) -0.019(2) 0.000(2) -0.0033(19) C44 0.028(3) 0.031(3) 0.031(3) -0.011(3) 0.003(2) -0.006(2) C45 0.053(4) 0.041(4) 0.051(4) -0.009(3) 0.003(3) -0.024(3) C46 0.067(5) 0.044(4) 0.072(5) -0.014(4) 0.029(4) -0.029(4) C47 0.037(3) 0.037(3) 0.038(3) -0.024(3) 0.003(3) -0.005(3) C48 0.047(4) 0.047(4) 0.069(5) -0.039(4) 0.002(3) -0.002(3) C49 0.076(6) 0.075(5) 0.083(6) -0.056(5) -0.002(4) 0.012(4) C50 0.018(3) 0.021(3) 0.025(3) -0.005(2) 0.002(2) -0.007(2) C51 0.024(3) 0.025(3) 0.023(3) -0.008(2) -0.001(2) -0.007(2) C52 0.020(3) 0.021(3) 0.025(3) -0.006(2) -0.001(2) -0.003(2) Fe1 0.0147(5) 0.0313(7) 0.0214(6) -0.0105(5) 0.0003(4) -0.0040(5) C53 0.021(3) 0.031(3) 0.021(3) -0.010(2) 0.004(2) -0.012(2) N9 0.025(3) 0.045(3) 0.045(3) -0.021(3) 0.002(2) -0.005(2) C54 0.015(3) 0.034(3) 0.023(3) -0.010(3) -0.001(2) 0.003(2) N10 0.023(2) 0.042(3) 0.040(3) -0.023(2) 0.001(2) -0.004(2) C55 0.014(3) 0.030(3) 0.031(3) -0.015(3) -0.002(2) -0.001(2) N11 0.031(3) 0.040(3) 0.028(3) -0.011(2) -0.001(2) -0.008(2) Fe2 0.0212(6) 0.0286(6) 0.0237(6) -0.0091(5) -0.0011(5) -0.0064(5) C56 0.025(3) 0.029(3) 0.022(3) -0.009(2) 0.000(2) -0.003(2) N12 0.033(3) 0.030(3) 0.042(3) -0.012(2) -0.006(2) -0.008(2) C57 0.024(3) 0.040(3) 0.027(3) -0.014(3) -0.002(2) -0.011(3) N13 0.031(3) 0.054(3) 0.033(3) -0.024(3) 0.006(2) -0.010(2) C58 0.021(3) 0.033(3) 0.028(3) -0.014(3) 0.004(2) -0.008(2) N14 0.027(3) 0.036(3) 0.033(3) -0.008(2) -0.004(2) -0.007(2) O1 0.087(4) 0.080(4) 0.109(5) -0.029(4) -0.015(4) -0.001(3) O2 0.027(2) 0.059(3) 0.036(2) -0.022(2) 0.0009(18) -0.0117(19) O3 0.100(5) 0.080(4) 0.090(4) -0.026(3) 0.012(4) -0.026(3) O4 0.046(3) 0.043(3) 0.055(3) -0.022(2) -0.014(2) -0.004(2) O5 0.102(5) 0.073(4) 0.128(5) -0.026(4) -0.022(4) 0.000(3) O6 0.098(5) 0.171(7) 0.392(13) -0.219(9) 0.153(7) -0.087(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.313(6) . ? C1 N2 1.323(6) . ? C1 C11 1.471(7) . ? N1 C2 1.461(7) . ? N1 H1 0.8800 . ? C2 C3 1.540(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.520(10) . ? C3 C4 1.523(8) . ? C3 C5 1.561(9) . ? C4 N2 1.465(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C6 1.523(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.517(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.499(10) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.526(11) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.393(7) . ? C11 C12 1.395(7) . ? C12 C13 1.389(7) . ? C12 H12 0.9500 . ? C13 C14 1.395(6) . ? C13 H13 0.9500 . ? C14 C15 1.393(6) . ? C14 C17 1.474(7) . ? C15 C16 1.363(7) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 N4 1.319(6) . ? C17 N3 1.323(6) . ? N3 C18 1.459(6) . ? N3 H3 0.8800 . ? C18 C19 1.528(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.521(7) . ? C19 C24 1.525(7) . ? C19 C21 1.534(7) . ? C20 N4 1.467(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? N4 H4 0.8800 . ? C21 C22 1.537(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.491(8) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.515(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.520(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 N6 1.310(6) . ? C27 N5 1.330(6) . ? C27 C37 1.473(7) . ? N5 C28 1.470(6) . ? N5 H5 0.8800 . ? C28 C29 1.536(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.511(7) . ? C29 C34 1.531(7) . ? C29 C31 1.536(7) . ? C30 N6 1.458(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? N6 H6 0.8800 . ? C31 C32 1.525(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.556(9) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.522(9) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.524(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.396(6) . ? C37 C39 1.399(7) . ? C38 C39 1.387(7) 2_567 ? C38 H38 0.9500 . ? C39 C38 1.387(7) 2_567 ? C39 H39 0.9500 . ? C40 N8 1.300(6) . ? C40 N7 1.311(6) . ? C40 C50 1.484(7) . ? N7 C41 1.467(6) . ? N7 H7 0.8800 . ? C41 C42 1.523(7) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C44 1.538(7) . ? C42 C47 1.544(7) . ? C42 C43 1.544(7) . ? C43 N8 1.461(6) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? N8 H8 0.8800 . ? C44 C45 1.522(7) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.538(8) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.527(7) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.529(8) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C52 1.382(6) 2_666 ? C50 C51 1.399(6) . ? C51 C52 1.390(6) . ? C51 H51 0.9500 . ? C52 C50 1.382(6) 2_666 ? C52 H52 0.9500 . ? Fe1 C55 1.901(5) 2_566 ? Fe1 C55 1.901(5) . ? Fe1 C53 1.907(5) 2_566 ? Fe1 C53 1.907(5) . ? Fe1 C54 1.932(5) 2_566 ? Fe1 C54 1.932(5) . ? C53 N9 1.175(6) . ? C54 N10 1.157(6) . ? C55 N11 1.163(6) . ? Fe2 C56 1.915(5) . ? Fe2 C56 1.915(5) 2_665 ? Fe2 C58 1.922(5) . ? Fe2 C58 1.922(5) 2_665 ? Fe2 C57 1.928(6) . ? Fe2 C57 1.928(6) 2_665 ? C56 N12 1.163(6) . ? C57 N13 1.157(6) . ? C58 N14 1.167(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 120.6(5) . . ? N1 C1 C11 120.0(4) . . ? N2 C1 C11 119.4(5) . . ? C1 N1 C2 122.2(4) . . ? C1 N1 H1 118.9 . . ? C2 N1 H1 118.9 . . ? N1 C2 C3 110.4(4) . . ? N1 C2 H2A 109.6 . . ? C3 C2 H2A 109.6 . . ? N1 C2 H2B 109.6 . . ? C3 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? C8 C3 C4 111.8(6) . . ? C8 C3 C2 109.8(5) . . ? C4 C3 C2 105.8(5) . . ? C8 C3 C5 113.6(6) . . ? C4 C3 C5 106.6(5) . . ? C2 C3 C5 108.9(5) . . ? N2 C4 C3 111.5(5) . . ? N2 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? N2 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C1 N2 C4 123.1(5) . . ? C1 N2 H2 118.4 . . ? C4 N2 H2 118.4 . . ? C6 C5 C3 116.0(6) . . ? C6 C5 H5A 108.3 . . ? C3 C5 H5A 108.3 . . ? C6 C5 H5B 108.3 . . ? C3 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? C5 C6 C7 112.1(7) . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C3 114.8(7) . . ? C9 C8 H8A 108.6 . . ? C3 C8 H8A 108.6 . . ? C9 C8 H8B 108.6 . . ? C3 C8 H8B 108.6 . . ? H8A C8 H8B 107.5 . . ? C8 C9 C10 110.6(8) . . ? C8 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 C12 119.1(5) . . ? C16 C11 C1 119.8(5) . . ? C12 C11 C1 121.1(4) . . ? C13 C12 C11 120.0(4) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 120.4(5) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C15 C14 C13 118.8(5) . . ? C15 C14 C17 119.8(4) . . ? C13 C14 C17 121.4(4) . . ? C16 C15 C14 120.9(4) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C11 120.8(5) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? N4 C17 N3 119.4(5) . . ? N4 C17 C14 119.1(4) . . ? N3 C17 C14 121.5(4) . . ? C17 N3 C18 123.0(4) . . ? C17 N3 H3 118.5 . . ? C18 N3 H3 118.5 . . ? N3 C18 C19 111.5(4) . . ? N3 C18 H18A 109.3 . . ? C19 C18 H18A 109.3 . . ? N3 C18 H18B 109.3 . . ? C19 C18 H18B 109.3 . . ? H18A C18 H18B 108.0 . . ? C20 C19 C24 111.3(4) . . ? C20 C19 C18 106.3(4) . . ? C24 C19 C18 109.3(4) . . ? C20 C19 C21 108.0(4) . . ? C24 C19 C21 113.5(4) . . ? C18 C19 C21 108.2(4) . . ? N4 C20 C19 112.4(4) . . ? N4 C20 H20A 109.1 . . ? C19 C20 H20A 109.1 . . ? N4 C20 H20B 109.1 . . ? C19 C20 H20B 109.1 . . ? H20A C20 H20B 107.9 . . ? C17 N4 C20 123.7(4) . . ? C17 N4 H4 118.2 . . ? C20 N4 H4 118.2 . . ? C22 C21 C19 114.8(5) . . ? C22 C21 H21A 108.6 . . ? C19 C21 H21A 108.6 . . ? C22 C21 H21B 108.6 . . ? C19 C21 H21B 108.6 . . ? H21A C21 H21B 107.6 . . ? C23 C22 C21 111.3(6) . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22B 109.4 . . ? C21 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C19 116.2(4) . . ? C25 C24 H24A 108.2 . . ? C19 C24 H24A 108.2 . . ? C25 C24 H24B 108.2 . . ? C19 C24 H24B 108.2 . . ? H24A C24 H24B 107.4 . . ? C24 C25 C26 111.2(5) . . ? C24 C25 H25A 109.4 . . ? C26 C25 H25A 109.4 . . ? C24 C25 H25B 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N6 C27 N5 120.6(5) . . ? N6 C27 C37 119.5(4) . . ? N5 C27 C37 119.9(5) . . ? C27 N5 C28 123.1(5) . . ? C27 N5 H5 118.5 . . ? C28 N5 H5 118.5 . . ? N5 C28 C29 111.9(4) . . ? N5 C28 H28A 109.2 . . ? C29 C28 H28A 109.2 . . ? N5 C28 H28B 109.2 . . ? C29 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? C30 C29 C34 108.4(5) . . ? C30 C29 C28 106.6(4) . . ? C34 C29 C28 107.1(4) . . ? C30 C29 C31 109.0(4) . . ? C34 C29 C31 114.3(4) . . ? C28 C29 C31 111.1(5) . . ? N6 C30 C29 112.1(4) . . ? N6 C30 H30A 109.2 . . ? C29 C30 H30A 109.2 . . ? N6 C30 H30B 109.2 . . ? C29 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? C27 N6 C30 122.0(4) . . ? C27 N6 H6 119.0 . . ? C30 N6 H6 119.0 . . ? C32 C31 C29 116.2(5) . . ? C32 C31 H31A 108.2 . . ? C29 C31 H31A 108.2 . . ? C32 C31 H31B 108.2 . . ? C29 C31 H31B 108.2 . . ? H31A C31 H31B 107.4 . . ? C31 C32 C33 110.6(5) . . ? C31 C32 H32A 109.5 . . ? C33 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 108.1 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C29 115.3(5) . . ? C35 C34 H34A 108.5 . . ? C29 C34 H34A 108.5 . . ? C35 C34 H34B 108.5 . . ? C29 C34 H34B 108.5 . . ? H34A C34 H34B 107.5 . . ? C34 C35 C36 112.1(6) . . ? C34 C35 H35A 109.2 . . ? C36 C35 H35A 109.2 . . ? C34 C35 H35B 109.2 . . ? C36 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C39 119.5(5) . . ? C38 C37 C27 120.3(5) . . ? C39 C37 C27 120.2(4) . . ? C39 C38 C37 120.4(5) 2_567 . ? C39 C38 H38 119.8 2_567 . ? C37 C38 H38 119.8 . . ? C38 C39 C37 120.1(5) 2_567 . ? C38 C39 H39 120.0 2_567 . ? C37 C39 H39 120.0 . . ? N8 C40 N7 121.8(4) . . ? N8 C40 C50 120.2(4) . . ? N7 C40 C50 117.9(4) . . ? C40 N7 C41 121.3(4) . . ? C40 N7 H7 119.3 . . ? C41 N7 H7 119.3 . . ? N7 C41 C42 111.0(4) . . ? N7 C41 H41A 109.4 . . ? C42 C41 H41A 109.4 . . ? N7 C41 H41B 109.4 . . ? C42 C41 H41B 109.4 . . ? H41A C41 H41B 108.0 . . ? C41 C42 C44 110.9(4) . . ? C41 C42 C47 108.1(4) . . ? C44 C42 C47 113.3(4) . . ? C41 C42 C43 106.1(4) . . ? C44 C42 C43 110.0(4) . . ? C47 C42 C43 108.2(4) . . ? N8 C43 C42 112.1(4) . . ? N8 C43 H43A 109.2 . . ? C42 C43 H43A 109.2 . . ? N8 C43 H43B 109.2 . . ? C42 C43 H43B 109.2 . . ? H43A C43 H43B 107.9 . . ? C40 N8 C43 123.2(4) . . ? C40 N8 H8 118.4 . . ? C43 N8 H8 118.4 . . ? C45 C44 C42 116.0(4) . . ? C45 C44 H44A 108.3 . . ? C42 C44 H44A 108.3 . . ? C45 C44 H44B 108.3 . . ? C42 C44 H44B 108.3 . . ? H44A C44 H44B 107.4 . . ? C44 C45 C46 111.4(5) . . ? C44 C45 H45A 109.4 . . ? C46 C45 H45A 109.4 . . ? C44 C45 H45B 109.4 . . ? C46 C45 H45B 109.4 . . ? H45A C45 H45B 108.0 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 C42 115.0(4) . . ? C48 C47 H47A 108.5 . . ? C42 C47 H47A 108.5 . . ? C48 C47 H47B 108.5 . . ? C42 C47 H47B 108.5 . . ? H47A C47 H47B 107.5 . . ? C47 C48 C49 111.8(5) . . ? C47 C48 H48A 109.3 . . ? C49 C48 H48A 109.3 . . ? C47 C48 H48B 109.3 . . ? C49 C48 H48B 109.3 . . ? H48A C48 H48B 107.9 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C52 C50 C51 119.6(4) 2_666 . ? C52 C50 C40 120.8(4) 2_666 . ? C51 C50 C40 119.6(4) . . ? C52 C51 C50 120.2(4) . . ? C52 C51 H51 119.9 . . ? C50 C51 H51 119.9 . . ? C50 C52 C51 120.2(5) 2_666 . ? C50 C52 H52 119.9 2_666 . ? C51 C52 H52 119.9 . . ? C55 Fe1 C55 179.999(1) 2_566 . ? C55 Fe1 C53 86.8(2) 2_566 2_566 ? C55 Fe1 C53 93.2(2) . 2_566 ? C55 Fe1 C53 93.2(2) 2_566 . ? C55 Fe1 C53 86.8(2) . . ? C53 Fe1 C53 180.0(3) 2_566 . ? C55 Fe1 C54 92.1(2) 2_566 2_566 ? C55 Fe1 C54 87.9(2) . 2_566 ? C53 Fe1 C54 86.3(2) 2_566 2_566 ? C53 Fe1 C54 93.7(2) . 2_566 ? C55 Fe1 C54 87.9(2) 2_566 . ? C55 Fe1 C54 92.1(2) . . ? C53 Fe1 C54 93.7(2) 2_566 . ? C53 Fe1 C54 86.3(2) . . ? C54 Fe1 C54 180.000(2) 2_566 . ? N9 C53 Fe1 175.0(4) . . ? N10 C54 Fe1 178.1(4) . . ? N11 C55 Fe1 178.0(5) . . ? C56 Fe2 C56 180.0(3) . 2_665 ? C56 Fe2 C58 91.0(2) . . ? C56 Fe2 C58 89.0(2) 2_665 . ? C56 Fe2 C58 89.0(2) . 2_665 ? C56 Fe2 C58 91.0(2) 2_665 2_665 ? C58 Fe2 C58 180.000(1) . 2_665 ? C56 Fe2 C57 88.0(2) . . ? C56 Fe2 C57 92.0(2) 2_665 . ? C58 Fe2 C57 90.3(2) . . ? C58 Fe2 C57 89.7(2) 2_665 . ? C56 Fe2 C57 92.0(2) . 2_665 ? C56 Fe2 C57 88.0(2) 2_665 2_665 ? C58 Fe2 C57 89.7(2) . 2_665 ? C58 Fe2 C57 90.3(2) 2_665 2_665 ? C57 Fe2 C57 180.0 . 2_665 ? N12 C56 Fe2 178.3(5) . . ? N13 C57 Fe2 175.9(5) . . ? N14 C58 Fe2 178.9(5) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.68 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.327 _refine_diff_density_min -1.137 _refine_diff_density_rms 0.086 # Attachment 'Cs223-[Fe(CN)6]2(1181).cif' data_e1181a _database_code_depnum_ccdc_archive 'CCDC 748253' #TrackingRef 'Cs223-[Fe(CN)6]2(1181).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C26 H44 N4), 2(C6 Cs Fe N6)' _chemical_formula_sum 'C90 H132 Cs2 Fe2 N24' _chemical_formula_weight 1927.72 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' Cs Cs -0.3680 2.1192 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 _symmetry_space_group_name_Hall '-P 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 18.0456(6) _cell_length_b 18.0456(6) _cell_length_c 8.3728(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2361.26(18) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1588 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 27.47 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1002 _exptl_absorpt_coefficient_mu 1.123 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8320 _exptl_absorpt_correction_T_max 0.9155 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12284 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_sigmaI/netI 0.0918 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 30.05 _reflns_number_total 4624 _reflns_number_gt 3315 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0638P)^2^+0.1500P] 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 4624 _refine_ls_number_parameters 176 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0982 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1455 _refine_ls_wR_factor_gt 0.1257 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.001 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 0.9455(2) 0.5474(2) 0.7164(4) 0.0148(7) Uani 1 1 d . . . N1 N 0.8688(2) 0.5388(2) 0.7175(3) 0.0175(7) Uani 1 1 d . . . H1 H 0.8367 0.5172 0.8030 0.021 Uiso 1 1 calc R . . C2 C 0.8347(2) 0.5637(3) 0.5829(4) 0.0179(8) Uani 1 1 d . . . H2A H 0.7968 0.5845 0.6231 0.021 Uiso 1 1 calc R . . H2B H 0.8001 0.5131 0.5146 0.021 Uiso 1 1 calc R . . C3 C 0.9065(3) 0.6337(3) 0.4836(4) 0.0179(8) Uani 1 1 d . B . C4 C 0.9695(3) 0.6032(3) 0.4448(4) 0.0201(8) Uani 1 1 d . . . H4A H 0.9422 0.5536 0.3715 0.024 Uiso 1 1 calc R . . H4B H 1.0202 0.6496 0.3904 0.024 Uiso 1 1 calc R . . N2 N 0.9966(2) 0.5785(2) 0.5915(3) 0.0189(7) Uani 1 1 d . . . H2 H 1.0480 0.5845 0.5960 0.023 Uiso 1 1 calc R . . C5 C 0.9538(3) 0.7185(3) 0.5781(5) 0.0248(9) Uani 1 1 d . . . H5A H 0.9769 0.7075 0.6769 0.030 Uiso 1 1 calc R . . H5B H 1.0032 0.7598 0.5134 0.030 Uiso 1 1 calc R . . C6 C 0.9035(3) 0.7606(3) 0.6247(6) 0.0404(12) Uani 1 1 d . . . H6A H 0.8592 0.7238 0.7032 0.048 Uiso 1 1 calc R . . H6B H 0.8738 0.7653 0.5291 0.048 Uiso 1 1 calc R . . C7 C 0.9579(4) 0.8487(4) 0.6961(7) 0.0479(14) Uani 1 1 d . . . H7A H 0.9917 0.8455 0.7846 0.072 Uiso 1 1 calc R . . H7B H 0.9207 0.8698 0.7358 0.072 Uiso 1 1 calc R . . H7C H 0.9963 0.8878 0.6141 0.072 Uiso 1 1 calc R . . C8 C 0.8650(3) 0.6407(3) 0.3272(5) 0.0335(9) Uani 1 1 d . . . H8A H 0.8418 0.5850 0.2719 0.040 Uiso 1 1 calc R A 1 H8B H 0.8154 0.6467 0.3582 0.040 Uiso 1 1 calc R A 1 C9 C 0.9128(9) 0.7065(10) 0.2091(14) 0.0335(9) Uani 0.491(18) 1 d PD B 1 H9A H 0.9604 0.6991 0.1689 0.040 Uiso 0.491(18) 1 calc PR B 1 H9B H 0.9383 0.7632 0.2614 0.040 Uiso 0.491(18) 1 calc PR B 1 C10 C 0.8596(10) 0.7052(8) 0.0694(12) 0.0335(9) Uani 0.491(18) 1 d PD B 1 H10A H 0.8363 0.6502 0.0136 0.050 Uiso 0.491(18) 1 calc PR B 1 H10B H 0.8953 0.7517 -0.0042 0.050 Uiso 0.491(18) 1 calc PR B 1 H10C H 0.8124 0.7127 0.1079 0.050 Uiso 0.491(18) 1 calc PR B 1 C10A C 0.8936(10) 0.7109(8) 0.0524(12) 0.0335(9) Uani 0.509(18) 1 d PD B 2 H10D H 0.8601 0.6531 0.0081 0.050 Uiso 0.509(18) 1 calc PR B 2 H10E H 0.9377 0.7478 -0.0244 0.050 Uiso 0.509(18) 1 calc PR B 2 H10F H 0.8557 0.7341 0.0740 0.050 Uiso 0.509(18) 1 calc PR B 2 C9A C 0.9362(9) 0.7074(10) 0.2081(14) 0.0335(9) Uani 0.509(18) 1 d PD B 2 H9A1 H 0.9663 0.7648 0.2579 0.040 Uiso 0.509(18) 1 calc PR B 2 H9A2 H 0.9789 0.6896 0.1854 0.040 Uiso 0.509(18) 1 calc PR B 2 C11 C 0.9748(2) 0.5226(3) 0.8613(4) 0.0165(8) Uani 1 1 d . . . C12 C 0.9200(3) 0.4460(3) 0.9368(4) 0.0186(8) Uani 1 1 d . . . H12 H 0.8651 0.4093 0.8925 0.022 Uiso 1 1 calc R . . C13 C 1.0559(3) 0.5777(3) 0.9245(5) 0.0201(8) Uani 1 1 d . . . H13 H 1.0936 0.6303 0.8732 0.024 Uiso 1 1 calc R . . Cs1 Cs 0.6667 0.3333 0.69652(4) 0.02052(14) Uani 1 3 d S . . Fe1 Fe 0.6667 0.3333 0.21439(9) 0.01136(19) Uani 1 3 d S . . C14 C 0.7036(2) 0.2739(2) 0.0745(4) 0.0149(7) Uani 1 1 d . . . C15 C 0.5996(2) 0.2327(2) 0.3429(4) 0.0140(7) Uani 1 1 d . . . N4 N 0.5570(2) 0.1722(2) 0.4205(4) 0.0201(7) Uani 1 1 d . . . N3 N 0.7260(2) 0.2434(2) -0.0225(4) 0.0217(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0123(18) 0.0163(19) 0.0163(15) -0.0007(14) -0.0019(13) 0.0076(16) N1 0.0137(16) 0.0223(18) 0.0147(13) 0.0055(12) 0.0001(12) 0.0077(15) C2 0.0157(19) 0.020(2) 0.0214(17) 0.0037(15) -0.0018(14) 0.0118(17) C3 0.018(2) 0.020(2) 0.0179(15) 0.0027(14) -0.0003(14) 0.0105(17) C4 0.023(2) 0.022(2) 0.0164(15) 0.0029(15) 0.0031(15) 0.0120(18) N2 0.0136(17) 0.0259(19) 0.0191(14) 0.0036(13) 0.0028(12) 0.0112(15) C5 0.023(2) 0.021(2) 0.0256(19) 0.0000(16) 0.0004(16) 0.0079(19) C6 0.039(3) 0.041(3) 0.051(3) -0.008(2) -0.013(2) 0.027(3) C7 0.054(4) 0.040(3) 0.054(3) -0.010(3) 0.001(3) 0.026(3) C8 0.034(2) 0.042(2) 0.0275(13) 0.0112(13) -0.0003(16) 0.022(2) C9 0.034(2) 0.042(2) 0.0275(13) 0.0112(13) -0.0003(16) 0.022(2) C10 0.034(2) 0.042(2) 0.0275(13) 0.0112(13) -0.0003(16) 0.022(2) C10A 0.034(2) 0.042(2) 0.0275(13) 0.0112(13) -0.0003(16) 0.022(2) C9A 0.034(2) 0.042(2) 0.0275(13) 0.0112(13) -0.0003(16) 0.022(2) C11 0.0166(19) 0.020(2) 0.0158(15) 0.0046(14) -0.0007(14) 0.0112(17) C12 0.015(2) 0.022(2) 0.0197(16) 0.0020(15) -0.0022(14) 0.0095(17) C13 0.015(2) 0.018(2) 0.0251(17) 0.0040(15) 0.0018(15) 0.0071(17) Cs1 0.02373(18) 0.02373(18) 0.01411(18) 0.000 0.000 0.01187(9) Fe1 0.0115(3) 0.0115(3) 0.0111(4) 0.000 0.000 0.00576(14) C14 0.0137(18) 0.0143(19) 0.0146(14) -0.0004(13) -0.0053(13) 0.0053(16) C15 0.0122(18) 0.0166(19) 0.0127(14) -0.0046(13) -0.0036(13) 0.0068(16) N4 0.0239(19) 0.0160(17) 0.0202(14) -0.0005(13) 0.0002(13) 0.0100(15) N3 0.0207(19) 0.0218(19) 0.0211(15) -0.0073(13) -0.0027(13) 0.0096(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.314(5) . ? C1 N2 1.319(5) . ? C1 C11 1.478(5) . ? N1 C2 1.458(4) . ? N1 H1 0.8800 . ? C2 C3 1.526(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.525(6) . ? C3 C8 1.545(5) . ? C3 C5 1.546(6) . ? C4 N2 1.471(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C6 1.497(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.513(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.451(14) . ? C8 C9A 1.596(14) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.507(11) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C10A C9A 1.531(11) . ? C10A H10D 0.9800 . ? C10A H10E 0.9800 . ? C10A H10F 0.9800 . ? C9A H9A1 0.9900 . ? C9A H9A2 0.9900 . ? C11 C12 1.386(5) . ? C11 C13 1.399(5) . ? C12 C13 1.380(5) 4_767 ? C12 H12 0.9500 . ? C13 C12 1.380(5) 4_767 ? C13 H13 0.9500 . ? Cs1 N3 3.325(3) 2_656 ? Cs1 N3 3.325(3) 3_666 ? Cs1 N3 3.325(3) 1_556 ? Cs1 C15 3.366(3) . ? Cs1 C15 3.366(3) 2_655 ? Cs1 C15 3.366(3) 3_665 ? Cs1 N4 3.458(3) 3_665 ? Cs1 N4 3.458(3) . ? Cs1 N4 3.458(3) 2_655 ? Cs1 C14 3.511(3) 2_656 ? Cs1 C14 3.511(3) 3_666 ? Cs1 C14 3.511(3) 1_556 ? Fe1 C14 1.919(4) 2_655 ? Fe1 C14 1.919(4) . ? Fe1 C14 1.919(4) 3_665 ? Fe1 C15 1.930(4) 2_655 ? Fe1 C15 1.930(4) 3_665 ? Fe1 C15 1.930(4) . ? Fe1 Cs1 4.3360(9) 1_554 ? C14 N3 1.162(5) . ? C14 Cs1 3.511(3) 1_554 ? C15 N4 1.168(5) . ? N3 Cs1 3.325(3) 1_554 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 121.7(3) . . ? N1 C1 C11 118.2(3) . . ? N2 C1 C11 120.0(3) . . ? C1 N1 C2 122.7(3) . . ? C1 N1 H1 118.7 . . ? C2 N1 H1 118.7 . . ? N1 C2 C3 111.2(3) . . ? N1 C2 H2A 109.4 . . ? C3 C2 H2A 109.4 . . ? N1 C2 H2B 109.4 . . ? C3 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C4 C3 C2 107.1(3) . . ? C4 C3 C8 109.2(3) . . ? C2 C3 C8 106.5(3) . . ? C4 C3 C5 108.9(3) . . ? C2 C3 C5 111.1(3) . . ? C8 C3 C5 113.8(4) . . ? N2 C4 C3 110.6(3) . . ? N2 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C1 N2 C4 121.6(3) . . ? C1 N2 H2 119.2 . . ? C4 N2 H2 119.2 . . ? C6 C5 C3 117.4(4) . . ? C6 C5 H5A 107.9 . . ? C3 C5 H5A 107.9 . . ? C6 C5 H5B 107.9 . . ? C3 C5 H5B 107.9 . . ? H5A C5 H5B 107.2 . . ? C5 C6 C7 113.4(4) . . ? C5 C6 H6A 108.9 . . ? C7 C6 H6A 108.9 . . ? C5 C6 H6B 108.9 . . ? C7 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C3 122.0(6) . . ? C9 C8 C9A 14.7(6) . . ? C3 C8 C9A 110.6(6) . . ? C9 C8 H8A 106.8 . . ? C3 C8 H8A 106.8 . . ? C9A C8 H8A 104.3 . . ? C9 C8 H8B 106.8 . . ? C3 C8 H8B 106.8 . . ? C9A C8 H8B 120.9 . . ? H8A C8 H8B 106.7 . . ? C8 C9 C10 113.7(9) . . ? C8 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? C8 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C9A C10A H10D 109.5 . . ? C9A C10A H10E 109.5 . . ? H10D C10A H10E 109.5 . . ? C9A C10A H10F 109.5 . . ? H10D C10A H10F 109.5 . . ? H10E C10A H10F 109.5 . . ? C10A C9A C8 109.3(8) . . ? C10A C9A H9A1 109.8 . . ? C8 C9A H9A1 109.8 . . ? C10A C9A H9A2 109.8 . . ? C8 C9A H9A2 109.8 . . ? H9A1 C9A H9A2 108.3 . . ? C12 C11 C13 120.5(3) . . ? C12 C11 C1 119.4(3) . . ? C13 C11 C1 120.1(3) . . ? C13 C12 C11 121.0(4) 4_767 . ? C13 C12 H12 119.5 4_767 . ? C11 C12 H12 119.5 . . ? C12 C13 C11 118.6(4) 4_767 . ? C12 C13 H13 120.7 4_767 . ? C11 C13 H13 120.7 . . ? N3 Cs1 N3 75.47(9) 2_656 3_666 ? N3 Cs1 N3 75.47(9) 2_656 1_556 ? N3 Cs1 N3 75.47(9) 3_666 1_556 ? N3 Cs1 C15 163.28(9) 2_656 . ? N3 Cs1 C15 115.70(9) 3_666 . ? N3 Cs1 C15 118.39(9) 1_556 . ? N3 Cs1 C15 118.39(9) 2_656 2_655 ? N3 Cs1 C15 163.28(9) 3_666 2_655 ? N3 Cs1 C15 115.70(8) 1_556 2_655 ? C15 Cs1 C15 48.68(11) . 2_655 ? N3 Cs1 C15 115.70(8) 2_656 3_665 ? N3 Cs1 C15 118.39(9) 3_666 3_665 ? N3 Cs1 C15 163.28(9) 1_556 3_665 ? C15 Cs1 C15 48.68(11) . 3_665 ? C15 Cs1 C15 48.68(11) 2_655 3_665 ? N3 Cs1 N4 99.85(8) 2_656 3_665 ? N3 Cs1 N4 104.54(8) 3_666 3_665 ? N3 Cs1 N4 175.21(8) 1_556 3_665 ? C15 Cs1 N4 66.05(9) . 3_665 ? C15 Cs1 N4 65.43(9) 2_655 3_665 ? C15 Cs1 N4 19.65(8) 3_665 3_665 ? N3 Cs1 N4 175.21(8) 2_656 . ? N3 Cs1 N4 99.85(8) 3_666 . ? N3 Cs1 N4 104.54(8) 1_556 . ? C15 Cs1 N4 19.65(8) . . ? C15 Cs1 N4 66.05(9) 2_655 . ? C15 Cs1 N4 65.43(9) 3_665 . ? N4 Cs1 N4 80.21(8) 3_665 . ? N3 Cs1 N4 104.54(8) 2_656 2_655 ? N3 Cs1 N4 175.21(8) 3_666 2_655 ? N3 Cs1 N4 99.85(8) 1_556 2_655 ? C15 Cs1 N4 65.43(9) . 2_655 ? C15 Cs1 N4 19.65(8) 2_655 2_655 ? C15 Cs1 N4 66.05(9) 3_665 2_655 ? N4 Cs1 N4 80.21(8) 3_665 2_655 ? N4 Cs1 N4 80.21(8) . 2_655 ? N3 Cs1 C14 19.32(8) 2_656 2_656 ? N3 Cs1 C14 61.28(9) 3_666 2_656 ? N3 Cs1 C14 60.71(9) 1_556 2_656 ? C15 Cs1 C14 176.88(9) . 2_656 ? C15 Cs1 C14 134.41(9) 2_655 2_656 ? C15 Cs1 C14 132.85(9) 3_665 2_656 ? N4 Cs1 C14 114.96(8) 3_665 2_656 ? N4 Cs1 C14 157.47(8) . 2_656 ? N4 Cs1 C14 117.51(8) 2_655 2_656 ? N3 Cs1 C14 60.71(9) 2_656 3_666 ? N3 Cs1 C14 19.32(8) 3_666 3_666 ? N3 Cs1 C14 61.28(9) 1_556 3_666 ? C15 Cs1 C14 132.85(9) . 3_666 ? C15 Cs1 C14 176.88(9) 2_655 3_666 ? C15 Cs1 C14 134.41(9) 3_665 3_666 ? N4 Cs1 C14 117.51(8) 3_665 3_666 ? N4 Cs1 C14 114.96(8) . 3_666 ? N4 Cs1 C14 157.47(8) 2_655 3_666 ? C14 Cs1 C14 44.04(11) 2_656 3_666 ? N3 Cs1 C14 61.28(9) 2_656 1_556 ? N3 Cs1 C14 60.71(9) 3_666 1_556 ? N3 Cs1 C14 19.32(8) 1_556 1_556 ? C15 Cs1 C14 134.41(9) . 1_556 ? C15 Cs1 C14 132.85(9) 2_655 1_556 ? C15 Cs1 C14 176.88(9) 3_665 1_556 ? N4 Cs1 C14 157.47(8) 3_665 1_556 ? N4 Cs1 C14 117.51(8) . 1_556 ? N4 Cs1 C14 114.96(8) 2_655 1_556 ? C14 Cs1 C14 44.04(11) 2_656 1_556 ? C14 Cs1 C14 44.04(11) 3_666 1_556 ? C14 Fe1 C14 86.63(15) 2_655 . ? C14 Fe1 C14 86.63(15) 2_655 3_665 ? C14 Fe1 C14 86.63(15) . 3_665 ? C14 Fe1 C15 92.50(16) 2_655 2_655 ? C14 Fe1 C15 88.88(15) . 2_655 ? C14 Fe1 C15 175.47(15) 3_665 2_655 ? C14 Fe1 C15 88.88(15) 2_655 3_665 ? C14 Fe1 C15 175.47(15) . 3_665 ? C14 Fe1 C15 92.50(16) 3_665 3_665 ? C15 Fe1 C15 91.93(14) 2_655 3_665 ? C14 Fe1 C15 175.47(15) 2_655 . ? C14 Fe1 C15 92.50(16) . . ? C14 Fe1 C15 88.88(15) 3_665 . ? C15 Fe1 C15 91.92(14) 2_655 . ? C15 Fe1 C15 91.92(14) 3_665 . ? C14 Fe1 Cs1 127.61(10) 2_655 . ? C14 Fe1 Cs1 127.61(10) . . ? C14 Fe1 Cs1 127.61(10) 3_665 . ? C15 Fe1 Cs1 56.11(10) 2_655 . ? C15 Fe1 Cs1 56.11(10) 3_665 . ? C15 Fe1 Cs1 56.11(10) . . ? C14 Fe1 Cs1 52.39(10) 2_655 1_554 ? C14 Fe1 Cs1 52.39(10) . 1_554 ? C14 Fe1 Cs1 52.39(10) 3_665 1_554 ? C15 Fe1 Cs1 123.89(10) 2_655 1_554 ? C15 Fe1 Cs1 123.89(10) 3_665 1_554 ? C15 Fe1 Cs1 123.89(10) . 1_554 ? Cs1 Fe1 Cs1 180.0 . 1_554 ? N3 C14 Fe1 172.9(3) . . ? N3 C14 Cs1 71.2(2) . 1_554 ? Fe1 C14 Cs1 101.96(14) . 1_554 ? N4 C15 Fe1 178.0(3) . . ? N4 C15 Cs1 84.6(2) . . ? Fe1 C15 Cs1 95.47(13) . . ? C15 N4 Cs1 75.7(2) . . ? C14 N3 Cs1 89.4(3) . 1_554 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.801 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.123 # Attachment 'K223-[Fe(CN)6]2(332).cif' data_e332a _database_code_depnum_ccdc_archive 'CCDC 748254' #TrackingRef 'K223-[Fe(CN)6]2(332).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C26 H44 N4), 2(C6 Fe K N6)' _chemical_formula_sum 'C90 H132 Fe2 K2 N24' _chemical_formula_weight 1740.10 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 _symmetry_space_group_name_Hall '-P 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 19.0191(3) _cell_length_b 19.0191(3) _cell_length_c 7.1810(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2249.55(11) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2906 _cell_measurement_theta_min 3.27 _cell_measurement_theta_max 26.10 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 930 _exptl_absorpt_coefficient_mu 0.474 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9323 _exptl_absorpt_correction_T_max 0.9906 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15227 _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_av_sigmaI/netI 0.0756 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 3 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.29 _reflns_number_total 3334 _reflns_number_gt 2207 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0626P)^2^+0.6796P] 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 3334 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1127 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 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 0.95979(15) 0.55743(14) 0.6703(4) 0.0145(5) Uani 1 1 d . . . N1 N 0.88346(12) 0.53605(12) 0.6451(3) 0.0158(5) Uani 1 1 d . . . H1 H 0.8478 0.5083 0.7325 0.019 Uiso 1 1 calc R . . C2 C 0.85625(15) 0.55730(15) 0.4750(4) 0.0186(6) Uani 1 1 d . . . H2A H 0.8037 0.5547 0.4979 0.022 Uiso 1 1 calc R . . H2B H 0.8482 0.5179 0.3755 0.022 Uiso 1 1 calc R . . C3 C 0.91914(14) 0.64264(15) 0.4127(3) 0.0144(5) Uani 1 1 d . . . C4 C 0.99965(15) 0.64360(16) 0.3916(4) 0.0173(6) Uani 1 1 d . . . H4A H 0.9983 0.6150 0.2754 0.021 Uiso 1 1 calc R . . H4B H 1.0443 0.7005 0.3805 0.021 Uiso 1 1 calc R . . N2 N 1.01645(12) 0.60495(12) 0.5494(3) 0.0155(5) Uani 1 1 d . . . H2 H 1.0661 0.6137 0.5643 0.019 Uiso 1 1 calc R . . C5 C 0.89472(15) 0.65847(16) 0.2190(4) 0.0174(6) Uani 1 1 d . . . H5A H 0.9368 0.7131 0.1769 0.021 Uiso 1 1 calc R . . H5B H 0.8946 0.6185 0.1303 0.021 Uiso 1 1 calc R . . C6 C 0.81240(16) 0.65367(17) 0.2092(4) 0.0217(6) Uani 1 1 d . . . H6A H 0.7694 0.5984 0.2449 0.026 Uiso 1 1 calc R . . H6B H 0.8113 0.6925 0.2994 0.026 Uiso 1 1 calc R . . C7 C 0.79485(19) 0.67304(19) 0.0148(4) 0.0308(7) Uani 1 1 d . . . H7A H 0.8393 0.7261 -0.0247 0.046 Uiso 1 1 calc R . . H7B H 0.7440 0.6743 0.0164 0.046 Uiso 1 1 calc R . . H7C H 0.7899 0.6312 -0.0725 0.046 Uiso 1 1 calc R . . C8 C 0.92445(15) 0.70311(15) 0.5631(4) 0.0190(6) Uani 1 1 d . . . H8A H 0.8684 0.6897 0.5950 0.023 Uiso 1 1 calc R . . H8B H 0.9485 0.6940 0.6764 0.023 Uiso 1 1 calc R . . C9 C 0.97240(17) 0.79252(16) 0.5164(4) 0.0262(7) Uani 1 1 d . . . H9A H 0.9469 0.8036 0.4087 0.031 Uiso 1 1 calc R . . H9B H 1.0282 0.8069 0.4800 0.031 Uiso 1 1 calc R . . C10 C 0.97641(19) 0.84588(18) 0.6814(5) 0.0385(8) Uani 1 1 d . . . H10A H 0.9212 0.8313 0.7190 0.058 Uiso 1 1 calc R . . H10B H 1.0063 0.9031 0.6443 0.058 Uiso 1 1 calc R . . H10C H 1.0043 0.8372 0.7861 0.058 Uiso 1 1 calc R . . C11 C 0.98173(15) 0.52774(15) 0.8391(3) 0.0137(5) Uani 1 1 d . . . C12 C 0.92582(15) 0.45264(15) 0.9125(4) 0.0156(5) Uani 1 1 d . . . H12 H 0.8752 0.4203 0.8518 0.019 Uiso 1 1 calc R . . C13 C 0.94358(15) 0.42486(15) 1.0736(3) 0.0143(5) Uani 1 1 d . . . H13 H 0.9051 0.3738 1.1246 0.017 Uiso 1 1 calc R . . Fe1 Fe 0.6667 0.3333 0.20768(9) 0.01158(18) Uani 1 3 d S . . C14 C 0.73295(15) 0.42330(15) 0.0481(4) 0.0153(6) Uani 1 1 d . . . N3 N 0.76851(13) 0.47368(14) -0.0623(3) 0.0233(5) Uani 1 1 d . . . C15 C 0.75977(15) 0.35184(14) 0.3539(4) 0.0143(5) Uani 1 1 d . . . N4 N 0.81545(12) 0.36027(12) 0.4403(3) 0.0180(5) Uani 1 1 d . . . K1 K 0.6667 0.3333 -0.30652(14) 0.0237(3) Uani 1 3 d S . . 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 0.0193(13) 0.0135(12) 0.0119(14) 0.0005(10) 0.0004(10) 0.0090(11) N1 0.0136(11) 0.0199(11) 0.0103(11) 0.0082(9) 0.0017(9) 0.0057(9) C2 0.0164(13) 0.0194(14) 0.0153(14) 0.0049(11) -0.0035(11) 0.0054(11) C3 0.0154(13) 0.0169(13) 0.0124(14) 0.0018(10) -0.0010(10) 0.0092(11) C4 0.0186(13) 0.0214(14) 0.0134(14) 0.0075(11) 0.0046(11) 0.0112(11) N2 0.0123(10) 0.0222(11) 0.0133(12) 0.0067(9) 0.0014(9) 0.0097(9) C5 0.0180(13) 0.0206(13) 0.0136(14) 0.0040(11) 0.0011(11) 0.0097(11) C6 0.0221(14) 0.0272(15) 0.0169(15) 0.0049(12) -0.0024(12) 0.0131(12) C7 0.0332(17) 0.0354(17) 0.0258(17) 0.0076(14) -0.0060(13) 0.0185(14) C8 0.0189(13) 0.0238(14) 0.0164(14) -0.0021(12) -0.0029(11) 0.0122(12) C9 0.0240(15) 0.0224(15) 0.0313(18) -0.0016(13) -0.0016(13) 0.0110(13) C10 0.0331(18) 0.0290(17) 0.054(2) -0.0117(16) -0.0061(16) 0.0159(15) C11 0.0186(13) 0.0187(13) 0.0092(13) 0.0015(10) 0.0023(10) 0.0132(11) C12 0.0149(12) 0.0180(13) 0.0148(14) 0.0005(11) -0.0001(10) 0.0088(11) C13 0.0155(13) 0.0136(12) 0.0140(13) 0.0046(10) 0.0030(10) 0.0074(10) Fe1 0.0121(2) 0.0121(2) 0.0106(3) 0.000 0.000 0.00603(11) C14 0.0149(13) 0.0185(13) 0.0151(15) -0.0035(11) -0.0003(11) 0.0102(11) N3 0.0243(12) 0.0238(13) 0.0190(13) 0.0026(10) 0.0036(10) 0.0099(11) C15 0.0174(13) 0.0125(12) 0.0122(14) 0.0014(10) 0.0045(11) 0.0069(11) N4 0.0144(11) 0.0189(12) 0.0191(13) 0.0003(9) -0.0008(9) 0.0072(9) K1 0.0287(4) 0.0287(4) 0.0137(6) 0.000 0.000 0.01435(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.310(3) . ? C1 N2 1.326(3) . ? C1 C11 1.483(3) . ? N1 C2 1.460(3) . ? N1 H1 0.8800 . ? C2 C3 1.524(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.530(3) . ? C3 C5 1.543(3) . ? C3 C8 1.544(4) . ? C4 N2 1.470(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C6 1.524(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.523(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.512(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.537(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.389(3) . ? C11 C13 1.394(3) 4_767 ? C12 C13 1.382(3) . ? C12 H12 0.9500 . ? C13 C11 1.394(3) 4_767 ? C13 H13 0.9500 . ? Fe1 C14 1.916(3) 2_655 ? Fe1 C14 1.916(3) 3_665 ? Fe1 C14 1.916(3) . ? Fe1 C15 1.933(3) . ? Fe1 C15 1.933(3) 2_655 ? Fe1 C15 1.933(3) 3_665 ? Fe1 K1 3.4885(12) 1_556 ? Fe1 K1 3.6925(12) . ? C14 N3 1.165(3) . ? C14 K1 2.974(3) . ? N3 K1 2.963(2) . ? C15 N4 1.167(3) . ? C15 K1 2.930(3) 1_556 ? N4 K1 3.182(2) 1_556 ? K1 C15 2.930(3) 3_664 ? K1 C15 2.930(3) 2_654 ? K1 C15 2.930(3) 1_554 ? K1 N3 2.963(2) 3_665 ? K1 N3 2.963(2) 2_655 ? K1 C14 2.974(3) 3_665 ? K1 C14 2.974(3) 2_655 ? K1 N4 3.182(2) 3_664 ? K1 N4 3.182(2) 2_654 ? K1 N4 3.182(2) 1_554 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 121.2(2) . . ? N1 C1 C11 118.3(2) . . ? N2 C1 C11 120.5(2) . . ? C1 N1 C2 121.4(2) . . ? C1 N1 H1 119.3 . . ? C2 N1 H1 119.3 . . ? N1 C2 C3 110.00(19) . . ? N1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? N1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C2 C3 C4 106.8(2) . . ? C2 C3 C5 108.6(2) . . ? C4 C3 C5 107.8(2) . . ? C2 C3 C8 108.2(2) . . ? C4 C3 C8 111.6(2) . . ? C5 C3 C8 113.5(2) . . ? N2 C4 C3 112.6(2) . . ? N2 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? N2 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? C1 N2 C4 122.7(2) . . ? C1 N2 H2 118.7 . . ? C4 N2 H2 118.7 . . ? C6 C5 C3 115.5(2) . . ? C6 C5 H5A 108.4 . . ? C3 C5 H5A 108.4 . . ? C6 C5 H5B 108.4 . . ? C3 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? C7 C6 C5 111.8(2) . . ? C7 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? C7 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C3 117.4(2) . . ? C9 C8 H8A 107.9 . . ? C3 C8 H8A 107.9 . . ? C9 C8 H8B 107.9 . . ? C3 C8 H8B 107.9 . . ? H8A C8 H8B 107.2 . . ? C8 C9 C10 112.0(2) . . ? C8 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? C8 C9 H9B 109.2 . . ? C10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C13 120.2(2) . 4_767 ? C12 C11 C1 119.0(2) . . ? C13 C11 C1 120.8(2) 4_767 . ? C13 C12 C11 120.2(2) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C11 119.6(2) . 4_767 ? C12 C13 H13 120.2 . . ? C11 C13 H13 120.2 4_767 . ? C14 Fe1 C14 87.93(11) 2_655 3_665 ? C14 Fe1 C14 87.93(11) 2_655 . ? C14 Fe1 C14 87.93(11) 3_665 . ? C14 Fe1 C15 175.01(11) 2_655 . ? C14 Fe1 C15 87.09(10) 3_665 . ? C14 Fe1 C15 91.62(10) . . ? C14 Fe1 C15 91.62(10) 2_655 2_655 ? C14 Fe1 C15 175.01(11) 3_665 2_655 ? C14 Fe1 C15 87.09(10) . 2_655 ? C15 Fe1 C15 93.32(10) . 2_655 ? C14 Fe1 C15 87.09(10) 2_655 3_665 ? C14 Fe1 C15 91.62(10) 3_665 3_665 ? C14 Fe1 C15 175.01(11) . 3_665 ? C15 Fe1 C15 93.32(10) . 3_665 ? C15 Fe1 C15 93.32(10) 2_655 3_665 ? C14 Fe1 K1 126.72(8) 2_655 1_556 ? C14 Fe1 K1 126.72(8) 3_665 1_556 ? C14 Fe1 K1 126.72(8) . 1_556 ? C15 Fe1 K1 57.12(7) . 1_556 ? C15 Fe1 K1 57.12(7) 2_655 1_556 ? C15 Fe1 K1 57.12(7) 3_665 1_556 ? C14 Fe1 K1 53.28(8) 2_655 . ? C14 Fe1 K1 53.28(8) 3_665 . ? C14 Fe1 K1 53.28(8) . . ? C15 Fe1 K1 122.88(7) . . ? C15 Fe1 K1 122.88(7) 2_655 . ? C15 Fe1 K1 122.88(7) 3_665 . ? K1 Fe1 K1 180.0 1_556 . ? N3 C14 Fe1 173.6(2) . . ? N3 C14 K1 78.16(17) . . ? Fe1 C14 K1 95.62(9) . . ? C14 N3 K1 79.21(17) . . ? N4 C15 Fe1 177.6(2) . . ? N4 C15 K1 91.49(17) . 1_556 ? Fe1 C15 K1 89.23(9) . 1_556 ? C15 N4 K1 66.99(16) . 1_556 ? C15 K1 C15 57.36(9) 3_664 2_654 ? C15 K1 C15 57.36(9) 3_664 1_554 ? C15 K1 C15 57.36(9) 2_654 1_554 ? C15 K1 N3 159.70(7) 3_664 . ? C15 K1 N3 103.83(7) 2_654 . ? C15 K1 N3 107.50(6) 1_554 . ? C15 K1 N3 107.50(6) 3_664 3_665 ? C15 K1 N3 159.70(7) 2_654 3_665 ? C15 K1 N3 103.83(7) 1_554 3_665 ? N3 K1 N3 88.56(7) . 3_665 ? C15 K1 N3 103.83(7) 3_664 2_655 ? C15 K1 N3 107.50(6) 2_654 2_655 ? C15 K1 N3 159.70(7) 1_554 2_655 ? N3 K1 N3 88.56(7) . 2_655 ? N3 K1 N3 88.56(7) 3_665 2_655 ? C15 K1 C14 176.70(7) 3_664 . ? C15 K1 C14 123.58(7) 2_654 . ? C15 K1 C14 125.93(7) 1_554 . ? N3 K1 C14 22.63(6) . . ? N3 K1 C14 72.37(7) 3_665 . ? N3 K1 C14 72.89(7) 2_655 . ? C15 K1 C14 125.93(7) 3_664 3_665 ? C15 K1 C14 176.70(7) 2_654 3_665 ? C15 K1 C14 123.58(7) 1_554 3_665 ? N3 K1 C14 72.89(7) . 3_665 ? N3 K1 C14 22.63(6) 3_665 3_665 ? N3 K1 C14 72.38(7) 2_655 3_665 ? C14 K1 C14 53.14(9) . 3_665 ? C15 K1 C14 123.58(7) 3_664 2_655 ? C15 K1 C14 125.93(7) 2_654 2_655 ? C15 K1 C14 176.70(7) 1_554 2_655 ? N3 K1 C14 72.37(7) . 2_655 ? N3 K1 C14 72.89(7) 3_665 2_655 ? N3 K1 C14 22.63(6) 2_655 2_655 ? C14 K1 C14 53.14(9) . 2_655 ? C14 K1 C14 53.14(9) 3_665 2_655 ? C15 K1 N4 21.52(6) 3_664 3_664 ? C15 K1 N4 75.21(7) 2_654 3_664 ? C15 K1 N4 76.05(7) 1_554 3_664 ? N3 K1 N4 175.21(6) . 3_664 ? N3 K1 N4 93.72(6) 3_665 3_664 ? N3 K1 N4 87.29(6) 2_655 3_664 ? C14 K1 N4 155.72(7) . 3_664 ? C14 K1 N4 108.04(6) 3_665 3_664 ? C14 K1 N4 104.27(6) 2_655 3_664 ? C15 K1 N4 76.05(7) 3_664 2_654 ? C15 K1 N4 21.52(6) 2_654 2_654 ? C15 K1 N4 75.21(7) 1_554 2_654 ? N3 K1 N4 87.29(6) . 2_654 ? N3 K1 N4 175.21(6) 3_665 2_654 ? N3 K1 N4 93.72(6) 2_655 2_654 ? C14 K1 N4 104.27(6) . 2_654 ? C14 K1 N4 155.72(7) 3_665 2_654 ? C14 K1 N4 108.04(6) 2_655 2_654 ? N4 K1 N4 90.60(6) 3_664 2_654 ? C15 K1 N4 75.21(7) 3_664 1_554 ? C15 K1 N4 76.05(7) 2_654 1_554 ? C15 K1 N4 21.52(6) 1_554 1_554 ? N3 K1 N4 93.72(6) . 1_554 ? N3 K1 N4 87.29(6) 3_665 1_554 ? N3 K1 N4 175.21(6) 2_655 1_554 ? C14 K1 N4 108.03(6) . 1_554 ? C14 K1 N4 104.27(6) 3_665 1_554 ? C14 K1 N4 155.72(7) 2_655 1_554 ? N4 K1 N4 90.60(6) 3_664 1_554 ? N4 K1 N4 90.60(6) 2_654 1_554 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.29 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.409 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.072 # Attachment 'K223-[Ru(CN)6]2(632).cif' data_e632a _database_code_depnum_ccdc_archive 'CCDC 748255' #TrackingRef 'K223-[Ru(CN)6]2(632).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C26 H44 N4), 2(C6 K N6 Ru)' _chemical_formula_sum 'C90 H132 K2 N24 Ru2' _chemical_formula_weight 1830.54 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 _symmetry_space_group_name_Hall '-P 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 19.2156(9) _cell_length_b 19.2156(9) _cell_length_c 7.1461(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2285.1(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1197 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 23.63 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 966 _exptl_absorpt_coefficient_mu 0.480 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9101 _exptl_absorpt_correction_T_max 0.9857 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10016 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.0945 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.57 _reflns_number_total 3526 _reflns_number_gt 2593 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0819P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3526 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1525 _refine_ls_wR_factor_gt 0.1392 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 C1 C 0.9592(2) 0.5573(2) 0.6699(5) 0.0151(7) Uani 1 1 d . . . N1 N 0.88369(17) 0.53659(17) 0.6478(4) 0.0151(6) Uani 1 1 d . . . H1 H 0.8490 0.5097 0.7371 0.018 Uiso 1 1 calc R . . C2 C 0.8559(2) 0.5572(2) 0.4785(5) 0.0173(7) Uani 1 1 d . . . H2A H 0.8039 0.5545 0.5033 0.021 Uiso 1 1 calc R . . H2B H 0.8474 0.5179 0.3788 0.021 Uiso 1 1 calc R . . C3 C 0.9177(2) 0.6419(2) 0.4133(5) 0.0143(7) Uani 1 1 d . . . C4 C 0.9975(2) 0.6422(2) 0.3898(5) 0.0169(7) Uani 1 1 d . . . H4A H 0.9954 0.6135 0.2730 0.020 Uiso 1 1 calc R . . H4B H 1.0418 0.6984 0.3775 0.020 Uiso 1 1 calc R . . N2 N 1.01459(18) 0.60403(18) 0.5482(4) 0.0169(6) Uani 1 1 d . . . H2 H 1.0638 0.6127 0.5621 0.020 Uiso 1 1 calc R . . C5 C 0.8928(2) 0.6570(2) 0.2205(5) 0.0173(7) Uani 1 1 d . . . H5A H 0.9347 0.7107 0.1765 0.021 Uiso 1 1 calc R . . H5B H 0.8915 0.6168 0.1319 0.021 Uiso 1 1 calc R . . C6 C 0.8119(2) 0.6535(2) 0.2125(5) 0.0207(8) Uani 1 1 d . . . H6A H 0.7691 0.5993 0.2509 0.025 Uiso 1 1 calc R . . H6B H 0.8120 0.6928 0.3023 0.025 Uiso 1 1 calc R . . C7 C 0.7931(3) 0.6717(3) 0.0177(5) 0.0294(9) Uani 1 1 d . . . H7A H 0.8366 0.7242 -0.0235 0.044 Uiso 1 1 calc R . . H7B H 0.7425 0.6725 0.0209 0.044 Uiso 1 1 calc R . . H7C H 0.7881 0.6301 -0.0696 0.044 Uiso 1 1 calc R . . C8 C 0.9245(2) 0.7018(2) 0.5637(5) 0.0169(7) Uani 1 1 d . . . H8A H 0.8695 0.6888 0.5987 0.020 Uiso 1 1 calc R . . H8B H 0.9493 0.6931 0.6760 0.020 Uiso 1 1 calc R . . C9 C 0.9722(2) 0.7906(2) 0.5136(5) 0.0224(8) Uani 1 1 d . . . H9A H 0.9462 0.8012 0.4063 0.027 Uiso 1 1 calc R . . H9B H 1.0271 0.8045 0.4750 0.027 Uiso 1 1 calc R . . C10 C 0.9775(2) 0.8439(2) 0.6779(6) 0.0315(10) Uani 1 1 d . . . H10A H 0.9232 0.8297 0.7179 0.047 Uiso 1 1 calc R . . H10B H 1.0069 0.9003 0.6392 0.047 Uiso 1 1 calc R . . H10C H 1.0058 0.8357 0.7821 0.047 Uiso 1 1 calc R . . C11 C 0.9815(2) 0.5276(2) 0.8391(5) 0.0135(7) Uani 1 1 d . . . C12 C 0.9260(2) 0.4534(2) 0.9147(5) 0.0166(7) Uani 1 1 d . . . H12 H 0.8754 0.4216 0.8556 0.020 Uiso 1 1 calc R . . C13 C 0.9443(2) 0.4259(2) 1.0755(5) 0.0155(7) Uani 1 1 d . . . H13 H 0.9064 0.3755 1.1274 0.019 Uiso 1 1 calc R . . Ru1 Ru 0.6667 0.3333 0.22152(6) 0.01195(17) Uani 1 3 d S . . C14 C 0.7368(2) 0.4281(2) 0.0528(5) 0.0153(7) Uani 1 1 d . . . N3 N 0.77137(19) 0.47703(19) -0.0588(5) 0.0243(7) Uani 1 1 d . . . C15 C 0.7650(2) 0.3532(2) 0.3763(5) 0.0142(7) Uani 1 1 d . . . N4 N 0.82047(18) 0.36104(19) 0.4590(4) 0.0205(7) Uani 1 1 d . . . K1 K 0.6667 0.3333 -0.29223(18) 0.0205(3) Uani 1 3 d S . . 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 0.0138(17) 0.0090(16) 0.0230(18) -0.0019(13) -0.0028(14) 0.0061(14) N1 0.0087(14) 0.0121(15) 0.0214(14) 0.0063(12) 0.0029(11) 0.0029(12) C2 0.0119(17) 0.0162(18) 0.0217(17) 0.0040(14) -0.0017(14) 0.0054(15) C3 0.0081(16) 0.0124(17) 0.0212(16) 0.0011(14) -0.0004(13) 0.0042(14) C4 0.0130(17) 0.0191(18) 0.0230(18) 0.0074(14) 0.0039(14) 0.0112(15) N2 0.0128(15) 0.0181(16) 0.0228(15) 0.0069(13) 0.0026(12) 0.0098(13) C5 0.0142(17) 0.0149(18) 0.0230(18) 0.0036(14) -0.0011(14) 0.0074(15) C6 0.0172(19) 0.0212(19) 0.0249(18) 0.0031(15) -0.0023(15) 0.0104(16) C7 0.028(2) 0.032(2) 0.032(2) 0.0053(18) -0.0042(18) 0.019(2) C8 0.0120(17) 0.0136(18) 0.0239(18) 0.0011(14) -0.0003(14) 0.0054(14) C9 0.0135(18) 0.0157(19) 0.037(2) -0.0010(16) -0.0023(16) 0.0063(15) C10 0.019(2) 0.021(2) 0.053(3) -0.0105(19) -0.0050(19) 0.0093(18) C11 0.0127(17) 0.0096(16) 0.0198(16) 0.0026(13) 0.0014(13) 0.0067(14) C12 0.0122(17) 0.0142(17) 0.0246(18) 0.0006(14) -0.0019(14) 0.0073(14) C13 0.0108(16) 0.0121(17) 0.0242(17) 0.0032(14) 0.0009(14) 0.0061(14) Ru1 0.00742(18) 0.00742(18) 0.0210(3) 0.000 0.000 0.00371(9) C14 0.0098(16) 0.0117(17) 0.0256(19) -0.0035(14) -0.0011(14) 0.0062(14) N3 0.0205(17) 0.0171(17) 0.0312(17) 0.0043(14) 0.0052(14) 0.0065(14) C15 0.0119(17) 0.0077(16) 0.0226(17) -0.0016(13) 0.0043(14) 0.0047(13) N4 0.0125(15) 0.0178(16) 0.0320(17) -0.0006(13) -0.0025(13) 0.0082(13) K1 0.0211(4) 0.0211(4) 0.0193(7) 0.000 0.000 0.0106(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.309(4) . ? C1 N2 1.319(4) . ? C1 C11 1.489(5) . ? N1 C2 1.455(4) . ? N1 H1 0.8800 . ? C2 C3 1.531(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.532(5) . ? C3 C5 1.533(5) . ? C3 C4 1.539(5) . ? C4 N2 1.473(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C6 1.523(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.522(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.522(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.527(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.388(5) 4_767 ? C11 C12 1.394(5) . ? C12 C13 1.381(5) . ? C12 H12 0.9500 . ? C13 C11 1.388(5) 4_767 ? C13 H13 0.9500 . ? Ru1 C14 2.033(4) 2_655 ? Ru1 C14 2.033(4) 3_665 ? Ru1 C14 2.033(4) . ? Ru1 C15 2.055(3) 3_665 ? Ru1 C15 2.055(4) . ? Ru1 C15 2.055(3) 2_655 ? Ru1 K1 3.4748(14) 1_556 ? Ru1 K1 3.6713(14) . ? C14 N3 1.156(5) . ? C14 K1 2.959(3) . ? N3 K1 2.983(3) . ? C15 N4 1.160(4) . ? C15 K1 2.934(3) 1_556 ? N4 K1 3.257(3) 1_556 ? K1 C15 2.934(3) 1_554 ? K1 C15 2.934(3) 3_664 ? K1 C15 2.934(3) 2_654 ? K1 C14 2.959(3) 3_665 ? K1 C14 2.959(3) 2_655 ? K1 N3 2.983(3) 2_655 ? K1 N3 2.983(3) 3_665 ? K1 N4 3.257(3) 3_664 ? K1 N4 3.257(3) 1_554 ? K1 N4 3.257(3) 2_654 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 121.5(3) . . ? N1 C1 C11 118.0(3) . . ? N2 C1 C11 120.5(3) . . ? C1 N1 C2 121.3(3) . . ? C1 N1 H1 119.3 . . ? C2 N1 H1 119.3 . . ? N1 C2 C3 110.3(3) . . ? N1 C2 H2A 109.6 . . ? C3 C2 H2A 109.6 . . ? N1 C2 H2B 109.6 . . ? C3 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? C2 C3 C8 108.4(3) . . ? C2 C3 C5 109.0(3) . . ? C8 C3 C5 113.9(3) . . ? C2 C3 C4 106.2(3) . . ? C8 C3 C4 111.3(3) . . ? C5 C3 C4 107.8(3) . . ? N2 C4 C3 112.6(3) . . ? N2 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? N2 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? C1 N2 C4 122.8(3) . . ? C1 N2 H2 118.6 . . ? C4 N2 H2 118.6 . . ? C6 C5 C3 115.7(3) . . ? C6 C5 H5A 108.3 . . ? C3 C5 H5A 108.3 . . ? C6 C5 H5B 108.3 . . ? C3 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? C7 C6 C5 112.2(3) . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C3 117.1(3) . . ? C9 C8 H8A 108.0 . . ? C3 C8 H8A 108.0 . . ? C9 C8 H8B 108.0 . . ? C3 C8 H8B 108.0 . . ? H8A C8 H8B 107.3 . . ? C8 C9 C10 111.8(3) . . ? C8 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? C8 C9 H9B 109.2 . . ? C10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C12 120.2(3) 4_767 . ? C13 C11 C1 120.6(3) 4_767 . ? C12 C11 C1 119.2(3) . . ? C13 C12 C11 120.1(3) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C11 119.7(3) . 4_767 ? C12 C13 H13 120.1 . . ? C11 C13 H13 120.1 4_767 . ? C14 Ru1 C14 88.41(13) 2_655 3_665 ? C14 Ru1 C14 88.41(13) 2_655 . ? C14 Ru1 C14 88.41(13) 3_665 . ? C14 Ru1 C15 86.80(13) 2_655 3_665 ? C14 Ru1 C15 90.99(13) 3_665 3_665 ? C14 Ru1 C15 175.19(13) . 3_665 ? C14 Ru1 C15 175.19(13) 2_655 . ? C14 Ru1 C15 86.81(13) 3_665 . ? C14 Ru1 C15 90.99(13) . . ? C15 Ru1 C15 93.74(12) 3_665 . ? C14 Ru1 C15 90.99(13) 2_655 2_655 ? C14 Ru1 C15 175.19(13) 3_665 2_655 ? C14 Ru1 C15 86.81(13) . 2_655 ? C15 Ru1 C15 93.74(12) 3_665 2_655 ? C15 Ru1 C15 93.74(12) . 2_655 ? C14 Ru1 K1 126.38(9) 2_655 1_556 ? C14 Ru1 K1 126.38(9) 3_665 1_556 ? C14 Ru1 K1 126.38(9) . 1_556 ? C15 Ru1 K1 57.43(9) 3_665 1_556 ? C15 Ru1 K1 57.43(9) . 1_556 ? C15 Ru1 K1 57.43(9) 2_655 1_556 ? C14 Ru1 K1 53.62(9) 2_655 . ? C14 Ru1 K1 53.62(9) 3_665 . ? C14 Ru1 K1 53.62(9) . . ? C15 Ru1 K1 122.57(9) 3_665 . ? C15 Ru1 K1 122.57(9) . . ? C15 Ru1 K1 122.57(9) 2_655 . ? K1 Ru1 K1 180.0 1_556 . ? N3 C14 Ru1 172.6(3) . . ? N3 C14 K1 79.9(2) . . ? Ru1 C14 K1 92.80(12) . . ? C14 N3 K1 77.6(2) . . ? N4 C15 Ru1 176.5(3) . . ? N4 C15 K1 95.5(2) . 1_556 ? Ru1 C15 K1 86.41(11) . 1_556 ? C15 N4 K1 63.7(2) . 1_556 ? C15 K1 C15 61.47(11) 1_554 3_664 ? C15 K1 C15 61.47(11) 1_554 2_654 ? C15 K1 C15 61.47(11) 3_664 2_654 ? C15 K1 C14 119.48(10) 1_554 3_665 ? C15 K1 C14 121.82(9) 3_664 3_665 ? C15 K1 C14 176.71(10) 2_654 3_665 ? C15 K1 C14 176.71(10) 1_554 2_655 ? C15 K1 C14 119.48(10) 3_664 2_655 ? C15 K1 C14 121.82(9) 2_654 2_655 ? C14 K1 C14 57.24(11) 3_665 2_655 ? C15 K1 C14 121.82(9) 1_554 . ? C15 K1 C14 176.71(10) 3_664 . ? C15 K1 C14 119.48(10) 2_654 . ? C14 K1 C14 57.24(11) 3_665 . ? C14 K1 C14 57.24(11) 2_655 . ? C15 K1 N3 159.94(10) 1_554 2_655 ? C15 K1 N3 100.15(9) 3_664 2_655 ? C15 K1 N3 103.81(9) 2_654 2_655 ? C14 K1 N3 76.04(10) 3_665 2_655 ? C14 K1 N3 22.43(9) 2_655 2_655 ? C14 K1 N3 76.59(10) . 2_655 ? C15 K1 N3 103.81(9) 1_554 . ? C15 K1 N3 159.94(10) 3_664 . ? C15 K1 N3 100.15(9) 2_654 . ? C14 K1 N3 76.59(10) 3_665 . ? C14 K1 N3 76.05(10) 2_655 . ? C14 K1 N3 22.43(9) . . ? N3 K1 N3 91.78(9) 2_655 . ? C15 K1 N3 100.15(9) 1_554 3_665 ? C15 K1 N3 103.81(9) 3_664 3_665 ? C15 K1 N3 159.94(10) 2_654 3_665 ? C14 K1 N3 22.43(9) 3_665 3_665 ? C14 K1 N3 76.59(10) 2_655 3_665 ? C14 K1 N3 76.05(10) . 3_665 ? N3 K1 N3 91.78(9) 2_655 3_665 ? N3 K1 N3 91.78(9) . 3_665 ? C15 K1 N4 79.38(9) 1_554 3_664 ? C15 K1 N4 20.76(8) 3_664 3_664 ? C15 K1 N4 78.29(9) 2_654 3_664 ? C14 K1 N4 104.93(8) 3_665 3_664 ? C14 K1 N4 100.97(8) 2_655 3_664 ? C14 K1 N4 156.44(9) . 3_664 ? N3 K1 N4 84.38(8) 2_655 3_664 ? N3 K1 N4 175.34(8) . 3_664 ? N3 K1 N4 90.97(8) 3_665 3_664 ? C15 K1 N4 20.76(8) 1_554 1_554 ? C15 K1 N4 78.29(9) 3_664 1_554 ? C15 K1 N4 79.38(9) 2_654 1_554 ? C14 K1 N4 100.97(8) 3_665 1_554 ? C14 K1 N4 156.44(9) 2_655 1_554 ? C14 K1 N4 104.93(8) . 1_554 ? N3 K1 N4 175.34(8) 2_655 1_554 ? N3 K1 N4 90.98(8) . 1_554 ? N3 K1 N4 84.38(8) 3_665 1_554 ? N4 K1 N4 93.03(8) 3_664 1_554 ? C15 K1 N4 78.29(9) 1_554 2_654 ? C15 K1 N4 79.38(9) 3_664 2_654 ? C15 K1 N4 20.76(8) 2_654 2_654 ? C14 K1 N4 156.44(9) 3_665 2_654 ? C14 K1 N4 104.93(8) 2_655 2_654 ? C14 K1 N4 100.97(8) . 2_654 ? N3 K1 N4 90.98(8) 2_655 2_654 ? N3 K1 N4 84.38(8) . 2_654 ? N3 K1 N4 175.34(8) 3_665 2_654 ? N4 K1 N4 93.03(8) 3_664 2_654 ? N4 K1 N4 93.03(8) 1_554 2_654 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.957 _refine_diff_density_min -1.301 _refine_diff_density_rms 0.129 # Attachment 'Na223-[Fe(CN)6]2(712).cif' data_e712a _database_code_depnum_ccdc_archive 'CCDC 748256' #TrackingRef 'Na223-[Fe(CN)6]2(712).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C26 H44 N4), 2(C6 Fe N6), 2(Na)' _chemical_formula_sum 'C90 H132 Fe2 N24 Na2' _chemical_formula_weight 1707.88 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 _symmetry_space_group_name_Hall '-P 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 19.1776(8) _cell_length_b 19.1776(8) _cell_length_c 6.9473(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2212.8(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1602 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 25.76 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 914 _exptl_absorpt_coefficient_mu 0.398 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9613 _exptl_absorpt_correction_T_max 0.9882 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10800 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0626 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3379 _reflns_number_gt 2402 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0626P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3379 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0780 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1207 _refine_ls_wR_factor_gt 0.1066 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 C1 C 0.95876(13) 0.55626(12) 0.6604(3) 0.0123(4) Uani 1 1 d . . . N1 N 0.88282(10) 0.53490(10) 0.6375(2) 0.0137(4) Uani 1 1 d . . . H1 H 0.8481 0.5070 0.7287 0.016 Uiso 1 1 calc R . . C2 C 0.85444(13) 0.55611(13) 0.4650(3) 0.0153(5) Uani 1 1 d . . . H2A H 0.8023 0.5531 0.4917 0.018 Uiso 1 1 calc R . . H2B H 0.8461 0.5175 0.3607 0.018 Uiso 1 1 calc R . . C3 C 0.91641(12) 0.64159(12) 0.4012(3) 0.0118(4) Uani 1 1 d . . . C4 C 0.99642(13) 0.64265(14) 0.3745(3) 0.0140(5) Uani 1 1 d . . . H4A H 0.9943 0.6144 0.2534 0.017 Uiso 1 1 calc R . . H4B H 1.0406 0.6991 0.3627 0.017 Uiso 1 1 calc R . . N2 N 1.01411(11) 0.60405(10) 0.5351(2) 0.0140(4) Uani 1 1 d . . . H2 H 1.0636 0.6131 0.5485 0.017 Uiso 1 1 calc R . . C5 C 0.89015(13) 0.65765(14) 0.2047(3) 0.0155(5) Uani 1 1 d . . . H5A H 0.9310 0.7121 0.1610 0.019 Uiso 1 1 calc R . . H5B H 0.8893 0.6185 0.1105 0.019 Uiso 1 1 calc R . . C6 C 0.80774(14) 0.65201(14) 0.2031(3) 0.0188(5) Uani 1 1 d . . . H6A H 0.7663 0.5975 0.2457 0.023 Uiso 1 1 calc R . . H6B H 0.8081 0.6914 0.2960 0.023 Uiso 1 1 calc R . . C7 C 0.78528(15) 0.66835(16) 0.0051(3) 0.0261(6) Uani 1 1 d . . . H7A H 0.8275 0.7211 -0.0407 0.039 Uiso 1 1 calc R . . H7B H 0.7341 0.6681 0.0132 0.039 Uiso 1 1 calc R . . H7C H 0.7797 0.6265 -0.0847 0.039 Uiso 1 1 calc R . . C8 C 0.92295(13) 0.70101(13) 0.5593(3) 0.0158(5) Uani 1 1 d . . . H8A H 0.8678 0.6882 0.5942 0.019 Uiso 1 1 calc R . . H8B H 0.9470 0.6912 0.6748 0.019 Uiso 1 1 calc R . . C9 C 0.97159(14) 0.79033(13) 0.5115(3) 0.0214(5) Uani 1 1 d . . . H9A H 1.0267 0.8040 0.4730 0.026 Uiso 1 1 calc R . . H9B H 0.9464 0.8019 0.4009 0.026 Uiso 1 1 calc R . . C10 C 0.97660(16) 0.84286(15) 0.6810(4) 0.0310(6) Uani 1 1 d . . . H10A H 0.9221 0.8279 0.7233 0.047 Uiso 1 1 calc R . . H10B H 1.0053 0.8995 0.6416 0.047 Uiso 1 1 calc R . . H10C H 1.0056 0.8350 0.7871 0.047 Uiso 1 1 calc R . . C11 C 0.98118(13) 0.52687(13) 0.8333(3) 0.0128(4) Uani 1 1 d . . . C12 C 0.92480(13) 0.45359(13) 0.9143(3) 0.0138(4) Uani 1 1 d . . . H12 H 0.8737 0.4220 0.8551 0.017 Uiso 1 1 calc R . . C13 C 0.94337(13) 0.42685(13) 1.0817(3) 0.0140(5) Uani 1 1 d . . . H13 H 0.9049 0.3772 1.1381 0.017 Uiso 1 1 calc R . . Fe1 Fe 0.6667 0.3333 0.22362(7) 0.01133(16) Uani 1 3 d S . . C14 C 0.73137(13) 0.42050(13) 0.0513(3) 0.0144(5) Uani 1 1 d . . . N3 N 0.76394(12) 0.46614(12) -0.0724(3) 0.0223(5) Uani 1 1 d . . . C15 C 0.75945(13) 0.35147(12) 0.3763(3) 0.0134(5) Uani 1 1 d . . . N4 N 0.81513(11) 0.35965(11) 0.4634(3) 0.0185(4) Uani 1 1 d . . . Na1 Na 0.6667 0.3333 -0.2949(2) 0.0243(4) Uani 1 3 d S . . 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 0.0148(11) 0.0097(10) 0.0135(10) -0.0012(8) -0.0005(8) 0.0070(9) N1 0.0112(9) 0.0150(10) 0.0128(9) 0.0062(7) 0.0014(7) 0.0051(8) C2 0.0141(11) 0.0158(12) 0.0149(11) 0.0036(9) -0.0027(9) 0.0066(10) C3 0.0105(11) 0.0121(11) 0.0122(10) 0.0035(8) 0.0005(8) 0.0053(9) C4 0.0125(11) 0.0177(12) 0.0134(10) 0.0056(9) 0.0030(8) 0.0087(9) N2 0.0111(9) 0.0172(10) 0.0161(9) 0.0044(7) 0.0009(7) 0.0090(8) C5 0.0158(11) 0.0181(12) 0.0132(11) 0.0037(9) 0.0010(9) 0.0089(10) C6 0.0174(12) 0.0238(13) 0.0175(11) 0.0034(9) -0.0022(9) 0.0120(11) C7 0.0251(14) 0.0309(15) 0.0239(13) 0.0070(11) -0.0057(10) 0.0153(12) C8 0.0133(11) 0.0181(12) 0.0153(11) 0.0003(9) -0.0007(9) 0.0073(10) C9 0.0172(12) 0.0155(12) 0.0301(13) -0.0004(10) -0.0012(10) 0.0071(10) C10 0.0230(14) 0.0236(14) 0.0458(17) -0.0103(12) -0.0054(12) 0.0111(12) C11 0.0170(11) 0.0154(11) 0.0106(10) 0.0020(8) 0.0023(8) 0.0115(10) C12 0.0118(11) 0.0153(11) 0.0151(10) 0.0013(9) 0.0014(8) 0.0072(9) C13 0.0163(11) 0.0127(11) 0.0146(11) 0.0037(8) 0.0027(9) 0.0085(9) Fe1 0.0109(2) 0.0109(2) 0.0122(3) 0.000 0.000 0.00545(10) C14 0.0116(11) 0.0157(11) 0.0172(11) -0.0027(9) -0.0013(9) 0.0078(10) N3 0.0203(11) 0.0229(11) 0.0239(11) 0.0061(9) 0.0061(9) 0.0110(9) C15 0.0158(11) 0.0079(10) 0.0139(10) 0.0004(8) 0.0035(9) 0.0040(9) N4 0.0150(10) 0.0166(10) 0.0224(10) -0.0002(8) -0.0027(8) 0.0067(8) Na1 0.0285(6) 0.0285(6) 0.0160(8) 0.000 0.000 0.0143(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.310(3) . ? C1 N2 1.324(3) . ? C1 C11 1.479(3) . ? N1 C2 1.456(3) . ? N1 H1 0.8800 . ? C2 C3 1.532(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.536(3) . ? C3 C5 1.538(3) . ? C3 C8 1.542(3) . ? C4 N2 1.470(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C6 1.529(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.520(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.522(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.521(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.393(3) . ? C11 C13 1.395(3) 4_767 ? C12 C13 1.387(3) . ? C12 H12 0.9500 . ? C13 C11 1.395(3) 4_767 ? C13 H13 0.9500 . ? Fe1 C14 1.922(2) 2_655 ? Fe1 C14 1.922(2) 3_665 ? Fe1 C14 1.922(2) . ? Fe1 C15 1.948(2) . ? Fe1 C15 1.948(2) 2_655 ? Fe1 C15 1.948(2) 3_665 ? Fe1 Na1 3.3447(16) 1_556 ? C14 N3 1.161(3) . ? C14 Na1 2.837(2) . ? N3 Na1 2.758(2) . ? C15 N4 1.168(3) . ? C15 Na1 2.808(2) 1_556 ? Na1 N3 2.758(2) 2_655 ? Na1 N3 2.758(2) 3_665 ? Na1 C15 2.808(2) 3_664 ? Na1 C15 2.808(2) 2_654 ? Na1 C15 2.808(2) 1_554 ? Na1 C14 2.837(2) 3_665 ? Na1 C14 2.837(2) 2_655 ? Na1 Fe1 3.3447(16) 1_554 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 121.18(19) . . ? N1 C1 C11 117.96(19) . . ? N2 C1 C11 120.84(19) . . ? C1 N1 C2 121.66(18) . . ? C1 N1 H1 119.2 . . ? C2 N1 H1 119.2 . . ? N1 C2 C3 109.80(17) . . ? N1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? N1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C2 C3 C4 106.53(17) . . ? C2 C3 C5 108.32(17) . . ? C4 C3 C5 108.38(17) . . ? C2 C3 C8 108.51(17) . . ? C4 C3 C8 111.39(17) . . ? C5 C3 C8 113.44(18) . . ? N2 C4 C3 112.49(17) . . ? N2 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? N2 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? C1 N2 C4 122.75(18) . . ? C1 N2 H2 118.6 . . ? C4 N2 H2 118.6 . . ? C6 C5 C3 115.00(18) . . ? C6 C5 H5A 108.5 . . ? C3 C5 H5A 108.5 . . ? C6 C5 H5B 108.5 . . ? C3 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? C7 C6 C5 112.41(19) . . ? C7 C6 H6A 109.1 . . ? C5 C6 H6A 109.1 . . ? C7 C6 H6B 109.1 . . ? C5 C6 H6B 109.1 . . ? H6A C6 H6B 107.9 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C3 116.99(18) . . ? C9 C8 H8A 108.0 . . ? C3 C8 H8A 108.0 . . ? C9 C8 H8B 108.0 . . ? C3 C8 H8B 108.0 . . ? H8A C8 H8B 107.3 . . ? C10 C9 C8 112.1(2) . . ? C10 C9 H9A 109.2 . . ? C8 C9 H9A 109.2 . . ? C10 C9 H9B 109.2 . . ? C8 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C13 120.36(19) . 4_767 ? C12 C11 C1 119.06(19) . . ? C13 C11 C1 120.54(19) 4_767 . ? C13 C12 C11 119.9(2) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C11 119.7(2) . 4_767 ? C12 C13 H13 120.1 . . ? C11 C13 H13 120.1 4_767 . ? C14 Fe1 C14 85.30(9) 2_655 3_665 ? C14 Fe1 C14 85.30(9) 2_655 . ? C14 Fe1 C14 85.30(9) 3_665 . ? C14 Fe1 C15 173.70(9) 2_655 . ? C14 Fe1 C15 88.56(9) 3_665 . ? C14 Fe1 C15 92.81(9) . . ? C14 Fe1 C15 92.81(9) 2_655 2_655 ? C14 Fe1 C15 173.70(9) 3_665 2_655 ? C14 Fe1 C15 88.56(9) . 2_655 ? C15 Fe1 C15 93.15(9) . 2_655 ? C14 Fe1 C15 88.56(9) 2_655 3_665 ? C14 Fe1 C15 92.81(9) 3_665 3_665 ? C14 Fe1 C15 173.70(9) . 3_665 ? C15 Fe1 C15 93.15(9) . 3_665 ? C15 Fe1 C15 93.15(9) 2_655 3_665 ? C14 Fe1 Na1 128.53(6) 2_655 1_556 ? C14 Fe1 Na1 128.53(6) 3_665 1_556 ? C14 Fe1 Na1 128.53(6) . 1_556 ? C15 Fe1 Na1 57.00(6) . 1_556 ? C15 Fe1 Na1 57.00(6) 2_655 1_556 ? C15 Fe1 Na1 57.00(6) 3_665 1_556 ? N3 C14 Fe1 170.7(2) . . ? N3 C14 Na1 74.25(15) . . ? Fe1 C14 Na1 96.53(8) . . ? C14 N3 Na1 81.85(15) . . ? N4 C15 Fe1 177.02(19) . . ? N4 C15 Na1 94.32(15) . 1_556 ? Fe1 C15 Na1 87.43(8) . 1_556 ? N3 Na1 N3 91.63(7) . 2_655 ? N3 Na1 N3 91.63(7) . 3_665 ? N3 Na1 N3 91.63(7) 2_655 3_665 ? N3 Na1 C15 159.44(8) . 3_664 ? N3 Na1 C15 100.62(6) 2_655 3_664 ? N3 Na1 C15 104.33(6) 3_665 3_664 ? N3 Na1 C15 100.62(6) . 2_654 ? N3 Na1 C15 104.33(6) 2_655 2_654 ? N3 Na1 C15 159.44(8) 3_665 2_654 ? C15 Na1 C15 60.50(8) 3_664 2_654 ? N3 Na1 C15 104.33(6) . 1_554 ? N3 Na1 C15 159.44(8) 2_655 1_554 ? N3 Na1 C15 100.62(6) 3_665 1_554 ? C15 Na1 C15 60.50(8) 3_664 1_554 ? C15 Na1 C15 60.50(8) 2_654 1_554 ? N3 Na1 C14 23.90(6) . . ? N3 Na1 C14 75.40(7) 2_655 . ? N3 Na1 C14 74.92(7) 3_665 . ? C15 Na1 C14 175.87(7) 3_664 . ? C15 Na1 C14 121.24(6) 2_654 . ? C15 Na1 C14 123.60(6) 1_554 . ? N3 Na1 C14 75.40(7) . 3_665 ? N3 Na1 C14 74.93(7) 2_655 3_665 ? N3 Na1 C14 23.90(6) 3_665 3_665 ? C15 Na1 C14 123.60(6) 3_664 3_665 ? C15 Na1 C14 175.87(7) 2_654 3_665 ? C15 Na1 C14 121.24(6) 1_554 3_665 ? C14 Na1 C14 54.64(8) . 3_665 ? N3 Na1 C14 74.92(7) . 2_655 ? N3 Na1 C14 23.90(6) 2_655 2_655 ? N3 Na1 C14 75.40(7) 3_665 2_655 ? C15 Na1 C14 121.24(6) 3_664 2_655 ? C15 Na1 C14 123.60(6) 2_654 2_655 ? C15 Na1 C14 175.87(7) 1_554 2_655 ? C14 Na1 C14 54.64(8) . 2_655 ? C14 Na1 C14 54.64(8) 3_665 2_655 ? N3 Na1 Fe1 124.10(5) . 1_554 ? N3 Na1 Fe1 124.10(5) 2_655 1_554 ? N3 Na1 Fe1 124.10(5) 3_665 1_554 ? C15 Na1 Fe1 35.57(5) 3_664 1_554 ? C15 Na1 Fe1 35.57(5) 2_654 1_554 ? C15 Na1 Fe1 35.57(5) 1_554 1_554 ? C14 Na1 Fe1 148.00(5) . 1_554 ? C14 Na1 Fe1 148.00(5) 3_665 1_554 ? C14 Na1 Fe1 148.00(5) 2_655 1_554 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.450 _refine_diff_density_min -0.529 _refine_diff_density_rms 0.072 # Attachment 'Rb223-[Fe(CN)6]2(1133).cif' data_e1133a _database_code_depnum_ccdc_archive 'CCDC 748257' #TrackingRef 'Rb223-[Fe(CN)6]2(1133).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C26 H44 N4), 2(C6 Fe N6 Rb)' _chemical_formula_sum 'C90 H132 Fe2 N24 Rb2' _chemical_formula_weight 1832.84 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 _symmetry_space_group_name_Hall '-P 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 18.9482(8) _cell_length_b 18.9482(8) _cell_length_c 7.3664(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2290.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 989 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 27.38 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 966 _exptl_absorpt_coefficient_mu 1.431 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9191 _exptl_absorpt_correction_T_max 0.9450 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10885 _diffrn_reflns_av_R_equivalents 0.0858 _diffrn_reflns_av_sigmaI/netI 0.1197 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 27.51 _reflns_number_total 3508 _reflns_number_gt 1598 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1491P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.019(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3508 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1768 _refine_ls_R_factor_gt 0.0864 _refine_ls_wR_factor_ref 0.2851 _refine_ls_wR_factor_gt 0.2178 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 C1 C 0.4036(4) 0.9602(4) 1.1764(9) 0.0347(14) Uani 1 1 d . . . N1 N 0.4130(3) 1.0180(3) 1.0600(8) 0.0376(13) Uani 1 1 d . . . H1 H 0.4538 1.0679 1.0759 0.045 Uiso 1 1 calc R . . C2 C 0.3578(4) 1.0016(4) 0.9061(9) 0.0387(15) Uani 1 1 d . . . H2A H 0.3859 1.0016 0.7927 0.046 Uiso 1 1 calc R . . H2B H 0.3447 1.0459 0.8971 0.046 Uiso 1 1 calc R . . C3 C 0.2786(4) 0.9203(4) 0.9226(9) 0.0344(14) Uani 1 1 d . . . C4 C 0.3021(4) 0.8573(4) 0.9818(9) 0.0404(16) Uani 1 1 d . . . H4A H 0.2523 0.8038 1.0005 0.049 Uiso 1 1 calc R . . H4B H 0.3351 0.8510 0.8856 0.049 Uiso 1 1 calc R . . N2 N 0.3485(3) 0.8834(3) 1.1487(8) 0.0383(13) Uani 1 1 d . . . H2 H 0.3396 0.8472 1.2334 0.046 Uiso 1 1 calc R . . C5 C 0.2218(4) 0.9247(4) 1.0670(9) 0.0401(16) Uani 1 1 d . . . H5A H 0.1790 0.8683 1.0958 0.048 Uiso 1 1 calc R . . H5B H 0.2541 0.9482 1.1789 0.048 Uiso 1 1 calc R . . C6 C 0.1806(4) 0.9727(4) 1.0210(10) 0.0452(17) Uani 1 1 d . . . H6A H 0.1442 0.9473 0.9153 0.054 Uiso 1 1 calc R . . H6B H 0.2223 1.0288 0.9865 0.054 Uiso 1 1 calc R . . C7 C 0.1306(5) 0.9762(5) 1.1809(11) 0.055(2) Uani 1 1 d . . . H7A H 0.0907 0.9207 1.2186 0.082 Uiso 1 1 calc R . . H7B H 0.1021 1.0051 1.1436 0.082 Uiso 1 1 calc R . . H7C H 0.1671 1.0051 1.2826 0.082 Uiso 1 1 calc R . . C8 C 0.2400(4) 0.8978(4) 0.7325(10) 0.0412(16) Uani 1 1 d . . . H8A H 0.2283 0.9408 0.6927 0.049 Uiso 1 1 calc R . . H8B H 0.2807 0.8983 0.6475 0.049 Uiso 1 1 calc R . . C9 C 0.1620(4) 0.8158(4) 0.7158(10) 0.0448(17) Uani 1 1 d . . . H9A H 0.1736 0.7719 0.7477 0.054 Uiso 1 1 calc R . . H9B H 0.1213 0.8136 0.8034 0.054 Uiso 1 1 calc R . . C10 C 0.1266(5) 0.8010(5) 0.5271(11) 0.053(2) Uani 1 1 d . . . H10A H 0.1128 0.8431 0.4968 0.079 Uiso 1 1 calc R . . H10B H 0.0773 0.7473 0.5219 0.079 Uiso 1 1 calc R . . H10C H 0.1666 0.8031 0.4398 0.079 Uiso 1 1 calc R . . C11 C 0.4539(4) 0.9828(4) 1.3411(9) 0.0338(14) Uani 1 1 d . . . C12 C 0.4795(4) 1.0554(4) 1.4304(9) 0.0393(15) Uani 1 1 d . . . H12 H 0.4659 1.0937 1.3828 0.047 Uiso 1 1 calc R . . C13 C 0.4753(4) 0.9264(4) 1.4116(9) 0.0382(15) Uani 1 1 d . . . H13 H 0.4585 0.8763 1.3507 0.046 Uiso 1 1 calc R . . Fe2 Fe 0.6667 0.3333 1.3050(2) 0.0327(4) Uani 1 3 d S . . C14 C 0.5916(4) 0.2403(4) 1.1619(9) 0.0385(15) Uani 1 1 d . . . N3 N 0.8149(3) 0.3593(3) 1.0779(8) 0.0403(14) Uani 1 1 d . . . C15 C 0.5753(5) 0.3095(4) 0.4566(10) 0.0410(16) Uani 1 1 d . . . N4 N 0.7045(4) 0.2283(4) 0.5617(8) 0.0427(14) Uani 1 1 d . . . Rb1 Rb 0.6667 0.3333 0.81647(17) 0.0469(4) Uani 1 3 d S . . 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 0.036(3) 0.039(3) 0.030(4) 0.000(3) 0.000(3) 0.019(3) N1 0.038(3) 0.038(3) 0.036(3) 0.005(2) -0.002(2) 0.019(2) C2 0.037(3) 0.042(4) 0.035(4) 0.001(3) 0.001(3) 0.018(3) C3 0.036(3) 0.032(3) 0.031(4) 0.004(3) 0.001(3) 0.014(3) C4 0.043(4) 0.040(4) 0.035(4) -0.001(3) -0.003(3) 0.019(3) N2 0.041(3) 0.035(3) 0.036(3) 0.001(2) -0.008(2) 0.017(2) C5 0.042(4) 0.041(4) 0.035(4) 0.002(3) 0.000(3) 0.019(3) C6 0.046(4) 0.043(4) 0.047(5) -0.005(3) -0.005(3) 0.023(3) C7 0.043(4) 0.049(4) 0.067(6) -0.002(4) 0.006(4) 0.019(4) C8 0.043(4) 0.046(4) 0.035(4) 0.000(3) -0.003(3) 0.023(3) C9 0.042(4) 0.041(4) 0.051(5) -0.005(3) -0.008(3) 0.020(3) C10 0.053(4) 0.054(5) 0.047(5) -0.006(4) -0.009(4) 0.023(4) C11 0.039(3) 0.036(3) 0.026(4) 0.002(3) -0.001(3) 0.018(3) C12 0.040(4) 0.040(4) 0.037(4) 0.004(3) -0.005(3) 0.019(3) C13 0.039(3) 0.040(3) 0.037(4) 0.007(3) 0.000(3) 0.020(3) Fe2 0.0344(6) 0.0344(6) 0.0292(9) 0.000 0.000 0.0172(3) C14 0.046(4) 0.046(4) 0.035(4) 0.009(3) 0.007(3) 0.031(3) N3 0.032(3) 0.049(3) 0.036(3) -0.005(3) 0.001(2) 0.018(3) C15 0.050(4) 0.031(3) 0.040(4) -0.005(3) -0.012(3) 0.018(3) N4 0.052(4) 0.045(3) 0.036(4) 0.006(3) 0.004(3) 0.028(3) Rb1 0.0532(5) 0.0532(5) 0.0341(8) 0.000 0.000 0.0266(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.315(8) . ? C1 N1 1.331(8) . ? C1 C11 1.469(9) . ? N1 C2 1.466(8) . ? N1 H1 0.8800 . ? C2 C3 1.525(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.531(9) . ? C3 C8 1.538(9) . ? C3 C5 1.544(9) . ? C4 N2 1.447(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C6 1.504(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.534(10) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.523(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.508(10) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.376(9) . ? C11 C13 1.416(8) . ? C12 C13 1.383(9) 4_678 ? C12 H12 0.9500 . ? C13 C12 1.383(9) 4_678 ? C13 H13 0.9500 . ? Fe2 C15 1.914(8) 1_556 ? Fe2 C15 1.914(8) 2_656 ? Fe2 C15 1.914(8) 3_666 ? Fe2 C14 1.932(8) 2_655 ? Fe2 C14 1.932(8) . ? Fe2 C14 1.932(8) 3_665 ? Fe2 Rb1 3.598(2) . ? Fe2 Rb1 3.768(2) 1_556 ? C14 N3 1.159(8) 3_665 ? C14 Rb1 3.016(7) . ? N3 C14 1.159(8) 2_655 ? N3 Rb1 3.234(6) . ? C15 N4 1.169(9) 3_665 ? C15 Fe2 1.914(8) 1_554 ? C15 Rb1 3.073(7) . ? N4 C15 1.169(9) 2_655 ? N4 Rb1 3.071(6) . ? Rb1 C14 3.016(7) 2_655 ? Rb1 C14 3.016(7) 3_665 ? Rb1 N4 3.071(6) 3_665 ? Rb1 N4 3.071(6) 2_655 ? Rb1 C15 3.073(7) 2_655 ? Rb1 C15 3.073(7) 3_665 ? Rb1 N3 3.234(6) 3_665 ? Rb1 N3 3.234(6) 2_655 ? 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 N2 C1 N1 121.0(6) . . ? N2 C1 C11 119.5(6) . . ? N1 C1 C11 119.5(6) . . ? C1 N1 C2 122.4(6) . . ? C1 N1 H1 118.8 . . ? C2 N1 H1 118.8 . . ? N1 C2 C3 112.9(5) . . ? N1 C2 H2A 109.0 . . ? C3 C2 H2A 109.0 . . ? N1 C2 H2B 109.0 . . ? C3 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C2 C3 C4 106.7(5) . . ? C2 C3 C8 107.3(5) . . ? C4 C3 C8 109.1(5) . . ? C2 C3 C5 111.1(5) . . ? C4 C3 C5 109.2(5) . . ? C8 C3 C5 113.2(6) . . ? N2 C4 C3 109.8(5) . . ? N2 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? N2 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C1 N2 C4 121.4(6) . . ? C1 N2 H2 119.3 . . ? C4 N2 H2 119.3 . . ? C6 C5 C3 117.7(6) . . ? C6 C5 H5A 107.9 . . ? C3 C5 H5A 107.9 . . ? C6 C5 H5B 107.9 . . ? C3 C5 H5B 107.9 . . ? H5A C5 H5B 107.2 . . ? C5 C6 C7 111.9(6) . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C3 116.1(6) . . ? C9 C8 H8A 108.3 . . ? C3 C8 H8A 108.3 . . ? C9 C8 H8B 108.3 . . ? C3 C8 H8B 108.3 . . ? H8A C8 H8B 107.4 . . ? C10 C9 C8 112.3(6) . . ? C10 C9 H9A 109.2 . . ? C8 C9 H9A 109.2 . . ? C10 C9 H9B 109.2 . . ? C8 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C13 119.2(6) . . ? C12 C11 C1 122.6(6) . . ? C13 C11 C1 118.1(6) . . ? C11 C12 C13 121.1(6) . 4_678 ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 4_678 . ? C12 C13 C11 119.7(6) 4_678 . ? C12 C13 H13 120.1 4_678 . ? C11 C13 H13 120.1 . . ? C15 Fe2 C15 89.4(3) 1_556 2_656 ? C15 Fe2 C15 89.4(3) 1_556 3_666 ? C15 Fe2 C15 89.4(3) 2_656 3_666 ? C15 Fe2 C14 175.7(3) 1_556 2_655 ? C15 Fe2 C14 86.4(3) 2_656 2_655 ? C15 Fe2 C14 91.2(3) 3_666 2_655 ? C15 Fe2 C14 86.4(3) 1_556 . ? C15 Fe2 C14 91.2(3) 2_656 . ? C15 Fe2 C14 175.7(3) 3_666 . ? C14 Fe2 C14 93.1(3) 2_655 . ? C15 Fe2 C14 91.2(3) 1_556 3_665 ? C15 Fe2 C14 175.7(3) 2_656 3_665 ? C15 Fe2 C14 86.4(3) 3_666 3_665 ? C14 Fe2 C14 93.1(3) 2_655 3_665 ? C14 Fe2 C14 93.1(3) . 3_665 ? C15 Fe2 Rb1 125.7(2) 1_556 . ? C15 Fe2 Rb1 125.7(2) 2_656 . ? C15 Fe2 Rb1 125.7(2) 3_666 . ? C14 Fe2 Rb1 56.9(2) 2_655 . ? C14 Fe2 Rb1 56.9(2) . . ? C14 Fe2 Rb1 56.9(2) 3_665 . ? C15 Fe2 Rb1 54.3(2) 1_556 1_556 ? C15 Fe2 Rb1 54.3(2) 2_656 1_556 ? C15 Fe2 Rb1 54.3(2) 3_666 1_556 ? C14 Fe2 Rb1 123.1(2) 2_655 1_556 ? C14 Fe2 Rb1 123.1(2) . 1_556 ? C14 Fe2 Rb1 123.1(2) 3_665 1_556 ? Rb1 Fe2 Rb1 180.0 . 1_556 ? N3 C14 Fe2 177.5(6) 3_665 . ? N3 C14 Rb1 90.2(5) 3_665 . ? Fe2 C14 Rb1 90.6(2) . . ? C14 N3 Rb1 68.8(4) 2_655 . ? N4 C15 Fe2 174.2(6) 3_665 1_554 ? N4 C15 Rb1 78.9(5) 3_665 . ? Fe2 C15 Rb1 95.3(3) 1_554 . ? C15 N4 Rb1 79.1(4) 2_655 . ? C14 Rb1 C14 55.4(2) 2_655 . ? C14 Rb1 C14 55.4(2) 2_655 3_665 ? C14 Rb1 C14 55.4(2) . 3_665 ? C14 Rb1 N4 159.95(19) 2_655 3_665 ? C14 Rb1 N4 106.02(17) . 3_665 ? C14 Rb1 N4 109.36(17) 3_665 3_665 ? C14 Rb1 N4 106.02(17) 2_655 . ? C14 Rb1 N4 109.36(17) . . ? C14 Rb1 N4 159.95(19) 3_665 . ? N4 Rb1 N4 86.54(16) 3_665 . ? C14 Rb1 N4 109.36(17) 2_655 2_655 ? C14 Rb1 N4 159.95(19) . 2_655 ? C14 Rb1 N4 106.02(17) 3_665 2_655 ? N4 Rb1 N4 86.54(16) 3_665 2_655 ? N4 Rb1 N4 86.54(16) . 2_655 ? C14 Rb1 C15 177.02(18) 2_655 . ? C14 Rb1 C15 125.1(2) . . ? C14 Rb1 C15 127.51(19) 3_665 . ? N4 Rb1 C15 21.93(16) 3_665 . ? N4 Rb1 C15 71.00(19) . . ? N4 Rb1 C15 70.82(19) 2_655 . ? C14 Rb1 C15 125.1(2) 2_655 2_655 ? C14 Rb1 C15 127.52(19) . 2_655 ? C14 Rb1 C15 177.02(19) 3_665 2_655 ? N4 Rb1 C15 70.82(19) 3_665 2_655 ? N4 Rb1 C15 21.93(16) . 2_655 ? N4 Rb1 C15 71.00(19) 2_655 2_655 ? C15 Rb1 C15 52.0(2) . 2_655 ? C14 Rb1 C15 127.51(19) 2_655 3_665 ? C14 Rb1 C15 177.02(18) . 3_665 ? C14 Rb1 C15 125.1(2) 3_665 3_665 ? N4 Rb1 C15 71.00(19) 3_665 3_665 ? N4 Rb1 C15 70.82(19) . 3_665 ? N4 Rb1 C15 21.93(16) 2_655 3_665 ? C15 Rb1 C15 52.0(2) . 3_665 ? C15 Rb1 C15 52.0(2) 2_655 3_665 ? C14 Rb1 N3 73.75(17) 2_655 3_665 ? C14 Rb1 N3 20.99(16) . 3_665 ? C14 Rb1 N3 72.94(18) 3_665 3_665 ? N4 Rb1 N3 89.77(15) 3_665 3_665 ? N4 Rb1 N3 95.68(15) . 3_665 ? N4 Rb1 N3 175.57(15) 2_655 3_665 ? C15 Rb1 N3 106.25(17) . 3_665 ? C15 Rb1 N3 110.04(16) 2_655 3_665 ? C15 Rb1 N3 156.70(18) 3_665 3_665 ? C14 Rb1 N3 20.99(16) 2_655 . ? C14 Rb1 N3 72.94(18) . . ? C14 Rb1 N3 73.75(17) 3_665 . ? N4 Rb1 N3 175.58(15) 3_665 . ? N4 Rb1 N3 89.77(15) . . ? N4 Rb1 N3 95.67(15) 2_655 . ? C15 Rb1 N3 156.70(18) . . ? C15 Rb1 N3 106.25(17) 2_655 . ? C15 Rb1 N3 110.04(16) 3_665 . ? N3 Rb1 N3 88.18(15) 3_665 . ? C14 Rb1 N3 72.94(18) 2_655 2_655 ? C14 Rb1 N3 73.75(17) . 2_655 ? C14 Rb1 N3 20.99(16) 3_665 2_655 ? N4 Rb1 N3 95.67(15) 3_665 2_655 ? N4 Rb1 N3 175.57(15) . 2_655 ? N4 Rb1 N3 89.77(15) 2_655 2_655 ? C15 Rb1 N3 110.04(16) . 2_655 ? C15 Rb1 N3 156.70(18) 2_655 2_655 ? C15 Rb1 N3 106.25(17) 3_665 2_655 ? N3 Rb1 N3 88.18(15) 3_665 2_655 ? N3 Rb1 N3 88.18(15) . 2_655 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.597 _refine_diff_density_min -1.378 _refine_diff_density_rms 0.130 # Attachment '(Cs223- [FeII(CN)6]2)0.83(23-[FeIII(CN)6]2)0.17.cif' data_e1138a _database_code_depnum_ccdc_archive 'CCDC 748258' #TrackingRef '(Cs223- [FeII(CN)6]2)0.83(23-[FeIII(CN)6]2)0.17.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C26 H44 N4), 2(C6 Cs0.83 Fe N6)' _chemical_formula_sum 'C90 H132 Cs1.66 Fe2 N24' _chemical_formula_weight 1880.40 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' Cs Cs -0.3680 2.1192 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 _symmetry_space_group_name_Hall '-P 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 18.0505(4) _cell_length_b 18.0505(4) _cell_length_c 8.4055(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2371.77(14) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3790 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 25.53 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 980 _exptl_absorpt_coefficient_mu 0.984 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8869 _exptl_absorpt_correction_T_max 0.8964 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17497 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 30.01 _reflns_number_total 4538 _reflns_number_gt 3420 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0888P)^2^+8.4272P] 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 4538 _refine_ls_number_parameters 201 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0686 _refine_ls_wR_factor_ref 0.2329 _refine_ls_wR_factor_gt 0.2132 _refine_ls_goodness_of_fit_ref 1.234 _refine_ls_restrained_S_all 1.233 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 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 0.3979(3) 0.9451(3) 0.7178(6) 0.0279(10) Uani 1 1 d . . . N1 N 0.3289(3) 0.8676(3) 0.7195(5) 0.0287(9) Uani 1 1 d . . . H1 H 0.3177 0.8359 0.8054 0.034 Uiso 1 1 calc R . . C2 C 0.2710(4) 0.8332(3) 0.5836(6) 0.0300(11) Uani 1 1 d . . . H2A H 0.2121 0.7943 0.6220 0.036 Uiso 1 1 calc R . . H2B H 0.2883 0.7997 0.5156 0.036 Uiso 1 1 calc R . . C3 C 0.2722(4) 0.9050(4) 0.4857(6) 0.0309(11) Uani 1 1 d . B . C4 C 0.3658(4) 0.9696(4) 0.4476(6) 0.0330(12) Uani 1 1 d . . . H4A H 0.3886 0.9436 0.3728 0.040 Uiso 1 1 calc R . . H4B H 0.3693 1.0204 0.3953 0.040 Uiso 1 1 calc R . . N2 N 0.4178(3) 0.9962(3) 0.5926(5) 0.0289(9) Uani 1 1 d . . . H2 H 0.4636 1.0475 0.5967 0.035 Uiso 1 1 calc R . . C5 C 0.2361(4) 0.9533(4) 0.5800(7) 0.0330(11) Uani 1 1 d . . . H5A H 0.2705 0.9762 0.6782 0.040 Uiso 1 1 calc R . . H5B H 0.2446 1.0029 0.5155 0.040 Uiso 1 1 calc R . . C6 C 0.1413(4) 0.9019(5) 0.6276(10) 0.0506(17) Uani 1 1 d . . . H6A H 0.1066 0.8725 0.5326 0.061 Uiso 1 1 calc R . . H6B H 0.1334 0.8576 0.7061 0.061 Uiso 1 1 calc R . . C7 C 0.1101(6) 0.9579(6) 0.6981(11) 0.059(2) Uani 1 1 d . . . H7A H 0.1429 0.9856 0.7944 0.089 Uiso 1 1 calc R . . H7B H 0.0493 0.9229 0.7253 0.089 Uiso 1 1 calc R . . H7C H 0.1175 1.0016 0.6207 0.089 Uiso 1 1 calc R . . C8 C 0.2229(4) 0.8630(4) 0.3309(7) 0.0390(13) Uani 1 1 d D . . H8A H 0.2499 0.8345 0.2745 0.047 Uiso 1 1 calc R A 1 H8B H 0.1629 0.8196 0.3556 0.047 Uiso 1 1 calc R A 1 C9 C 0.226(10) 0.935(5) 0.226(10) 0.07(2) Uani 0.26(15) 1 d PD B 1 H9A H 0.1917 0.9578 0.2763 0.082 Uiso 0.26(15) 1 calc PR B 1 H9B H 0.2852 0.9818 0.2140 0.082 Uiso 0.26(15) 1 calc PR B 1 C10 C 0.188(6) 0.896(4) 0.063(9) 0.043(12) Uani 0.26(15) 1 d PD B 1 H10A H 0.2275 0.8837 0.0059 0.065 Uiso 0.26(15) 1 calc PR B 1 H10B H 0.1783 0.9367 0.0021 0.065 Uiso 0.26(15) 1 calc PR B 1 H10C H 0.1331 0.8429 0.0782 0.065 Uiso 0.26(15) 1 calc PR B 1 C9A C 0.214(3) 0.921(2) 0.206(4) 0.055(6) Uani 0.74(15) 1 d PD B 2 H9A1 H 0.1854 0.9502 0.2556 0.067 Uiso 0.74(15) 1 calc PR B 2 H9A2 H 0.2710 0.9653 0.1695 0.067 Uiso 0.74(15) 1 calc PR B 2 C10A C 0.161(4) 0.870(5) 0.063(4) 0.071(10) Uani 0.74(15) 1 d PD B 2 H10D H 0.1867 0.8373 0.0187 0.107 Uiso 0.74(15) 1 calc PR B 2 H10E H 0.1610 0.9086 -0.0173 0.107 Uiso 0.74(15) 1 calc PR B 2 H10F H 0.1025 0.8299 0.0973 0.107 Uiso 0.74(15) 1 calc PR B 2 C11 C 0.4514(3) 0.9744(3) 0.8630(6) 0.0282(10) Uani 1 1 d . . . C12 C 0.4742(4) 0.9189(3) 0.9362(6) 0.0304(11) Uani 1 1 d . . . H12 H 0.4569 0.8642 0.8918 0.037 Uiso 1 1 calc R . . C13 C 0.5230(3) 0.9453(3) 1.0761(7) 0.0301(11) Uani 1 1 d . . . H13 H 0.5383 0.9083 1.1286 0.036 Uiso 1 1 calc R . . Fe1 Fe 0.3333 0.6667 0.21544(14) 0.0224(3) Uani 1 3 d S . . C14 C 0.4001(3) 0.7670(3) 0.3434(6) 0.0242(9) Uani 1 1 d . . . N3 N 0.4436(3) 0.8283(3) 0.4206(5) 0.0320(10) Uani 1 1 d . . . C15 C 0.4297(3) 0.7033(3) 0.0764(6) 0.0247(9) Uani 1 1 d . . . N4 N 0.2738(3) 0.7568(3) 0.9797(6) 0.0331(10) Uani 1 1 d . . . Cs1 Cs 0.3333 0.6667 0.69670(7) 0.0282(2) Uani 0.822(5) 3 d SP . . 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 0.024(2) 0.021(2) 0.035(2) 0.0008(19) -0.0022(19) 0.008(2) N1 0.030(2) 0.020(2) 0.032(2) 0.0002(16) -0.0037(17) 0.0089(18) C2 0.027(3) 0.026(3) 0.035(3) 0.000(2) -0.003(2) 0.011(2) C3 0.026(3) 0.032(3) 0.034(2) 0.001(2) -0.001(2) 0.013(2) C4 0.031(3) 0.033(3) 0.031(2) 0.007(2) -0.001(2) 0.013(2) N2 0.025(2) 0.020(2) 0.034(2) 0.0030(16) -0.0026(17) 0.0064(17) C5 0.030(3) 0.026(3) 0.043(3) -0.003(2) -0.003(2) 0.014(2) C6 0.035(3) 0.048(4) 0.066(4) -0.015(3) 0.000(3) 0.019(3) C7 0.052(5) 0.063(5) 0.074(5) 0.004(4) 0.010(4) 0.038(4) C8 0.040(3) 0.043(3) 0.039(3) -0.007(2) -0.009(2) 0.024(3) C9 0.10(5) 0.08(4) 0.04(2) -0.01(2) -0.04(3) 0.05(4) C10 0.05(3) 0.03(2) 0.05(2) -0.008(17) -0.017(19) 0.02(2) C9A 0.071(14) 0.060(10) 0.045(10) 0.001(7) -0.019(10) 0.040(10) C10A 0.09(2) 0.10(3) 0.059(9) -0.033(13) -0.043(12) 0.07(2) C11 0.026(3) 0.024(2) 0.033(2) 0.0025(19) -0.0029(19) 0.012(2) C12 0.030(3) 0.024(3) 0.036(3) -0.001(2) -0.003(2) 0.013(2) C13 0.026(3) 0.026(3) 0.037(3) 0.002(2) -0.004(2) 0.012(2) Fe1 0.0193(4) 0.0193(4) 0.0286(6) 0.000 0.000 0.0097(2) C14 0.023(2) 0.022(2) 0.029(2) 0.0014(17) 0.0025(18) 0.0127(19) N3 0.034(3) 0.028(2) 0.032(2) 0.0007(17) -0.0016(18) 0.014(2) C15 0.023(2) 0.023(2) 0.030(2) -0.0028(17) -0.0034(18) 0.012(2) N4 0.034(3) 0.029(2) 0.040(2) 0.0076(19) 0.0030(19) 0.019(2) Cs1 0.0295(3) 0.0295(3) 0.0256(3) 0.000 0.000 0.01474(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 C1 N2 1.325(7) . ? C1 N1 1.329(7) . ? C1 C11 1.480(7) . ? N1 C2 1.460(7) . ? N1 H1 0.8800 . ? C2 C3 1.526(8) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.532(8) . ? C3 C5 1.543(8) . ? C3 C8 1.545(8) . ? C4 N2 1.465(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C6 1.536(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.503(10) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.54(2) . ? C8 C9A 1.550(13) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.53(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C9A C10A 1.518(16) . ? C9A H9A1 0.9900 . ? C9A H9A2 0.9900 . ? C10A H10D 0.9800 . ? C10A H10E 0.9800 . ? C10A H10F 0.9800 . ? C11 C13 1.380(8) 4_677 ? C11 C12 1.402(7) . ? C12 C13 1.402(7) . ? C12 H12 0.9500 . ? C13 C11 1.380(8) 4_677 ? C13 H13 0.9500 . ? Fe1 C15 1.918(5) 3_565 ? Fe1 C15 1.918(5) . ? Fe1 C15 1.918(5) 2_665 ? Fe1 C14 1.925(5) 2_665 ? Fe1 C14 1.925(5) . ? Fe1 C14 1.925(5) 3_565 ? Fe1 Cs1 4.0452(13) . ? Fe1 Cs1 4.3603(13) 1_554 ? C14 N3 1.181(7) . ? C14 Cs1 3.372(5) . ? N3 Cs1 3.472(5) . ? C15 N4 1.166(7) 3_564 ? C15 Cs1 3.536(5) 1_554 ? N4 C15 1.166(7) 2_666 ? N4 Cs1 3.347(5) . ? Cs1 N4 3.347(5) 2_665 ? Cs1 N4 3.347(5) 3_565 ? Cs1 C14 3.372(5) 2_665 ? Cs1 C14 3.372(5) 3_565 ? Cs1 N3 3.472(5) 2_665 ? Cs1 N3 3.472(5) 3_565 ? Cs1 C15 3.536(5) 3_566 ? Cs1 C15 3.536(5) 1_556 ? Cs1 C15 3.536(5) 2_666 ? 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 N2 C1 N1 121.8(5) . . ? N2 C1 C11 120.3(5) . . ? N1 C1 C11 117.9(5) . . ? C1 N1 C2 122.3(5) . . ? C1 N1 H1 118.9 . . ? C2 N1 H1 118.9 . . ? N1 C2 C3 110.9(4) . . ? N1 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108.0 . . ? C2 C3 C4 107.6(5) . . ? C2 C3 C5 111.8(5) . . ? C4 C3 C5 107.1(5) . . ? C2 C3 C8 106.1(5) . . ? C4 C3 C8 110.1(5) . . ? C5 C3 C8 114.0(5) . . ? N2 C4 C3 111.0(4) . . ? N2 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? N2 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C1 N2 C4 121.7(4) . . ? C1 N2 H2 119.1 . . ? C4 N2 H2 119.1 . . ? C6 C5 C3 116.7(5) . . ? C6 C5 H5A 108.1 . . ? C3 C5 H5A 108.1 . . ? C6 C5 H5B 108.1 . . ? C3 C5 H5B 108.1 . . ? H5A C5 H5B 107.3 . . ? C7 C6 C5 112.1(6) . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C3 107(4) . . ? C9 C8 C9A 11(4) . . ? C3 C8 C9A 118.1(18) . . ? C9 C8 H8A 110.2 . . ? C3 C8 H8A 110.2 . . ? C9A C8 H8A 105.9 . . ? C9 C8 H8B 110.2 . . ? C3 C8 H8B 110.2 . . ? C9A C8 H8B 103.4 . . ? H8A C8 H8B 108.5 . . ? C10 C9 C8 108(5) . . ? C10 C9 H9A 110.1 . . ? C8 C9 H9A 110.1 . . ? C10 C9 H9B 110.2 . . ? C8 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? C10A C9A C8 112(2) . . ? C10A C9A H9A1 109.3 . . ? C8 C9A H9A1 109.3 . . ? C10A C9A H9A2 109.3 . . ? C8 C9A H9A2 109.3 . . ? H9A1 C9A H9A2 108.0 . . ? C9A C10A H10D 109.5 . . ? C9A C10A H10E 109.5 . . ? H10D C10A H10E 109.5 . . ? C9A C10A H10F 109.5 . . ? H10D C10A H10F 109.5 . . ? H10E C10A H10F 109.5 . . ? C13 C11 C12 121.5(5) 4_677 . ? C13 C11 C1 119.8(5) 4_677 . ? C12 C11 C1 118.6(5) . . ? C13 C12 C11 119.0(5) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C11 C13 C12 119.5(5) 4_677 . ? C11 C13 H13 120.2 4_677 . ? C12 C13 H13 120.2 . . ? C15 Fe1 C15 86.7(2) 3_565 . ? C15 Fe1 C15 86.7(2) 3_565 2_665 ? C15 Fe1 C15 86.7(2) . 2_665 ? C15 Fe1 C14 92.4(2) 3_565 2_665 ? C15 Fe1 C14 175.7(2) . 2_665 ? C15 Fe1 C14 89.0(2) 2_665 2_665 ? C15 Fe1 C14 175.7(2) 3_565 . ? C15 Fe1 C14 89.0(2) . . ? C15 Fe1 C14 92.3(2) 2_665 . ? C14 Fe1 C14 91.8(2) 2_665 . ? C15 Fe1 C14 89.0(2) 3_565 3_565 ? C15 Fe1 C14 92.4(2) . 3_565 ? C15 Fe1 C14 175.7(2) 2_665 3_565 ? C14 Fe1 C14 91.8(2) 2_665 3_565 ? C14 Fe1 C14 91.8(2) . 3_565 ? C15 Fe1 Cs1 127.54(15) 3_565 . ? C15 Fe1 Cs1 127.54(15) . . ? C15 Fe1 Cs1 127.53(15) 2_665 . ? C14 Fe1 Cs1 56.05(15) 2_665 . ? C14 Fe1 Cs1 56.05(15) . . ? C14 Fe1 Cs1 56.05(15) 3_565 . ? C15 Fe1 Cs1 52.46(15) 3_565 1_554 ? C15 Fe1 Cs1 52.46(15) . 1_554 ? C15 Fe1 Cs1 52.47(15) 2_665 1_554 ? C14 Fe1 Cs1 123.95(15) 2_665 1_554 ? C14 Fe1 Cs1 123.95(15) . 1_554 ? C14 Fe1 Cs1 123.95(15) 3_565 1_554 ? Cs1 Fe1 Cs1 180.0 . 1_554 ? N3 C14 Fe1 177.6(5) . . ? N3 C14 Cs1 84.9(3) . . ? Fe1 C14 Cs1 95.69(18) . . ? C14 N3 Cs1 75.3(3) . . ? N4 C15 Fe1 172.9(5) 3_564 . ? N4 C15 Cs1 71.2(3) 3_564 1_554 ? Fe1 C15 Cs1 102.06(18) . 1_554 ? C15 N4 Cs1 89.5(4) 2_666 . ? N4 Cs1 N4 75.08(12) 2_665 3_565 ? N4 Cs1 N4 75.08(12) 2_665 . ? N4 Cs1 N4 75.08(12) 3_565 . ? N4 Cs1 C14 163.38(12) 2_665 . ? N4 Cs1 C14 116.05(12) 3_565 . ? N4 Cs1 C14 118.70(11) . . ? N4 Cs1 C14 118.70(11) 2_665 2_665 ? N4 Cs1 C14 163.38(12) 3_565 2_665 ? N4 Cs1 C14 116.05(12) . 2_665 ? C14 Cs1 C14 48.42(14) . 2_665 ? N4 Cs1 C14 116.05(12) 2_665 3_565 ? N4 Cs1 C14 118.70(11) 3_565 3_565 ? N4 Cs1 C14 163.38(12) . 3_565 ? C14 Cs1 C14 48.42(14) . 3_565 ? C14 Cs1 C14 48.42(14) 2_665 3_565 ? N4 Cs1 N3 104.77(11) 2_665 2_665 ? N4 Cs1 N3 175.01(11) 3_565 2_665 ? N4 Cs1 N3 100.01(12) . 2_665 ? C14 Cs1 N3 65.27(12) . 2_665 ? C14 Cs1 N3 19.80(11) 2_665 2_665 ? C14 Cs1 N3 65.98(11) 3_565 2_665 ? N4 Cs1 N3 100.01(12) 2_665 3_565 ? N4 Cs1 N3 104.77(11) 3_565 3_565 ? N4 Cs1 N3 175.01(11) . 3_565 ? C14 Cs1 N3 65.98(11) . 3_565 ? C14 Cs1 N3 65.27(12) 2_665 3_565 ? C14 Cs1 N3 19.80(11) 3_565 3_565 ? N3 Cs1 N3 80.19(12) 2_665 3_565 ? N4 Cs1 N3 175.01(11) 2_665 . ? N4 Cs1 N3 100.01(12) 3_565 . ? N4 Cs1 N3 104.77(11) . . ? C14 Cs1 N3 19.80(11) . . ? C14 Cs1 N3 65.98(11) 2_665 . ? C14 Cs1 N3 65.27(12) 3_565 . ? N3 Cs1 N3 80.20(12) 2_665 . ? N3 Cs1 N3 80.19(12) 3_565 . ? N4 Cs1 C15 19.25(11) 2_665 3_566 ? N4 Cs1 C15 60.99(12) 3_565 3_566 ? N4 Cs1 C15 60.30(12) . 3_566 ? C14 Cs1 C15 176.91(12) . 3_566 ? C14 Cs1 C15 134.62(12) 2_665 3_566 ? C14 Cs1 C15 133.19(12) 3_565 3_566 ? N3 Cs1 C15 117.60(11) 2_665 3_566 ? N3 Cs1 C15 115.13(11) 3_565 3_566 ? N3 Cs1 C15 157.31(12) . 3_566 ? N4 Cs1 C15 60.31(12) 2_665 1_556 ? N4 Cs1 C15 19.25(11) 3_565 1_556 ? N4 Cs1 C15 60.99(12) . 1_556 ? C14 Cs1 C15 133.19(12) . 1_556 ? C14 Cs1 C15 176.92(12) 2_665 1_556 ? C14 Cs1 C15 134.62(12) 3_565 1_556 ? N3 Cs1 C15 157.31(11) 2_665 1_556 ? N3 Cs1 C15 117.59(11) 3_565 1_556 ? N3 Cs1 C15 115.12(11) . 1_556 ? C15 Cs1 C15 43.74(14) 3_566 1_556 ? N4 Cs1 C15 60.99(12) 2_665 2_666 ? N4 Cs1 C15 60.31(12) 3_565 2_666 ? N4 Cs1 C15 19.25(11) . 2_666 ? C14 Cs1 C15 134.62(12) . 2_666 ? C14 Cs1 C15 133.18(12) 2_665 2_666 ? C14 Cs1 C15 176.92(12) 3_565 2_666 ? N3 Cs1 C15 115.12(11) 2_665 2_666 ? N3 Cs1 C15 157.31(11) 3_565 2_666 ? N3 Cs1 C15 117.59(11) . 2_666 ? C15 Cs1 C15 43.74(14) 3_566 2_666 ? C15 Cs1 C15 43.75(14) 1_556 2_666 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.550 _refine_diff_density_min -1.757 _refine_diff_density_rms 0.186