# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Masaaki Ohba' _publ_contact_author_email OHBA@SBCHEM.KYOTO-U.AC.JP _publ_section_title ; Guest-responsive Porous Magnetic Frameworks Using Polycyanometallates ; loop_ _publ_author_name 'Masaaki Ohba' 'Susumu Kitagawa' 'Ko Yoneda' # Attachment 'CIF_1.cif' data___[Ni(dipn)]2[Ni(dipn)(H2O)][Fe(CN)6]2 _database_code_depnum_ccdc_archive 'CCDC 645084' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C30 H63 Fe2 N21 Ni3 O6 ' _chemical_formula_moiety 'C30 H63 Fe2 N21 Ni3 O6 ' _chemical_formula_weight 1101.76 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,1/2-Z 3 -X,-Y,-Z 4 +X,-Y,1/2+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,1/2-Z 7 1/2-X,1/2-Y,-Z 8 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 24.044(8) _cell_length_b 14.343(4) _cell_length_c 16.688(5) _cell_angle_alpha 90.0000 _cell_angle_beta 100.552(4) _cell_angle_gamma 90.0000 _cell_volume 5658(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8303 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 243.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2296.00 _exptl_absorpt_coefficient_mu 1.533 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.755 _exptl_absorpt_correction_T_max 0.832 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 21405 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_ambient_temperature 243.1 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6442 _reflns_number_gt 4745 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.2049 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 6442 _refine_ls_number_parameters 285 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1205P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.82 _refine_diff_density_min -0.65 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Fe Fe 0.346 0.844 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Ni(1) Ni 0.22756(3) 0.18122(4) 0.69343(3) 0.0518(2) Uani 1.00 1 d . . . Ni(2) Ni 0.0000 0.10709(6) 0.2500 0.0602(2) Uani 1.00 2 d S . . Fe(1) Fe 0.19028(2) 0.02940(3) 0.41840(3) 0.03557(17) Uani 1.00 1 d . . . O(1) O 0.0000 0.2545(5) 0.2500 0.148(3) Uani 1.00 2 d S . . O(2) O 0.4127(2) -0.1630(4) 0.5356(6) 0.085(2) Uani 0.50 1 d P . . O(3) O 0.5159(9) -0.1694(13) 0.4129(14) 0.212(7) Uiso 0.50 1 d P . . O(4) O 0.6337(7) -0.1784(10) 0.4971(10) 0.175(5) Uiso 0.50 1 d P . . O(5) O 0.5958(10) -0.0909(16) 0.5651(14) 0.260(10) Uiso 0.50 1 d P . . O(6) O 0.5010(11) -0.0536(19) 0.6444(16) 0.284(11) Uiso 0.50 1 d P . . N(1) N 0.18633(18) 0.1225(2) 0.58330(19) 0.0557(9) Uani 1.00 1 d . . . N(2) N 0.07675(19) 0.1047(3) 0.3280(2) 0.0744(12) Uani 1.00 1 d . . . N(3) N 0.24584(19) 0.2067(2) 0.3668(2) 0.0624(10) Uani 1.00 1 d . . . N(4) N 0.1272(2) -0.1478(3) 0.4568(4) 0.1041(19) Uani 1.00 1 d . . . N(5) N 0.3094(2) -0.0424(4) 0.4903(3) 0.0932(16) Uani 1.00 1 d . . . N(6) N 0.2039(2) -0.0702(2) 0.2602(2) 0.0706(12) Uani 1.00 1 d . . . N(7) N 0.1520(2) 0.2477(3) 0.7020(3) 0.104(2) Uani 1.00 1 d . . . N(8) N 0.2713(3) 0.2392(5) 0.8046(2) 0.122(2) Uani 1.00 1 d . . . N(9) N 0.2963(2) 0.1047(3) 0.6714(3) 0.0935(16) Uani 1.00 1 d . . . N(10) N -0.0405(2) 0.1150(5) 0.3504(3) 0.110(2) Uani 1.00 1 d . . . N(11) N 0.0000 -0.0401(5) 0.2500 0.086(2) Uani 1.00 2 d S . . C(1) C 0.18511(18) 0.0869(2) 0.5218(2) 0.0441(8) Uani 1.00 1 d . . . C(2) C 0.1192(2) 0.0796(3) 0.3646(2) 0.0520(9) Uani 1.00 1 d . . . C(3) C 0.22631(19) 0.1411(2) 0.3875(2) 0.0460(9) Uani 1.00 1 d . . . C(4) C 0.1514(2) -0.0823(3) 0.4448(3) 0.0572(10) Uani 1.00 1 d . . . C(5) C 0.2645(2) -0.0195(3) 0.4650(2) 0.0522(10) Uani 1.00 1 d . . . C(6) C 0.1984(2) -0.0299(2) 0.3176(2) 0.0515(10) Uani 1.00 1 d . . . C(7) C 0.1587(10) 0.3284(10) 0.7677(9) 0.311(13) Uani 1.00 1 d . . . C(8) C 0.1916(9) 0.3271(10) 0.8334(8) 0.221(10) Uani 1.00 1 d . . . C(9) C 0.2507(9) 0.3199(7) 0.8400(6) 0.216(9) Uani 1.00 1 d . . . C(10) C 0.3262(7) 0.2246(10) 0.8237(10) 0.216(9) Uani 1.00 1 d . . . C(11) C 0.3584(4) 0.1605(16) 0.7971(9) 0.237(12) Uani 1.00 1 d . . . C(12) C 0.3531(4) 0.1120(7) 0.7109(11) 0.221(8) Uani 1.00 1 d . . . C(13) C -0.0571(7) 0.0393(11) 0.3870(8) 0.222(8) Uani 1.00 1 d . . . C(14) C -0.0455(4) -0.0473(9) 0.3733(6) 0.148(4) Uani 1.00 1 d . . . C(15) C -0.0222(4) -0.0862(5) 0.3117(6) 0.134(3) Uani 1.00 1 d . . . H(1) H 0.1369 0.2721 0.6525 0.125 Uiso 1.00 1 c R . . H(2) H 0.1273 0.2047 0.7148 0.125 Uiso 1.00 1 c R . . H(3) H 0.1677 0.3849 0.7396 0.373 Uiso 1.00 1 c R . . H(4) H 0.1210 0.3383 0.7805 0.373 Uiso 1.00 1 c R . . H(5) H 0.1799 0.2750 0.8645 0.265 Uiso 1.00 1 c R . . H(6) H 0.1845 0.3841 0.8623 0.265 Uiso 1.00 1 c R . . H(7) H 0.2678 0.3214 0.8980 0.260 Uiso 1.00 1 c R . . H(8) H 0.2640 0.3752 0.8146 0.260 Uiso 1.00 1 c R . . H(9) H 0.2604 0.1957 0.8392 0.147 Uiso 1.00 1 c R . . H(10) H 0.3338 0.2175 0.8831 0.259 Uiso 1.00 1 c R . . H(11) H 0.3433 0.2843 0.8128 0.259 Uiso 1.00 1 c R . . H(12) H 0.3594 0.1087 0.8356 0.284 Uiso 1.00 1 c R . . H(13) H 0.3965 0.1873 0.8075 0.284 Uiso 1.00 1 c R . . H(14) H 0.3742 0.1484 0.6768 0.265 Uiso 1.00 1 c R . . H(15) H 0.3698 0.0496 0.7178 0.265 Uiso 1.00 1 c R . . H(16) H 0.2867 0.0440 0.6771 0.112 Uiso 1.00 1 c R . . H(17) H 0.2968 0.1129 0.6175 0.112 Uiso 1.00 1 c R . . H(18) H -0.0171 0.1477 0.3895 0.132 Uiso 1.00 1 c R . . H(19) H -0.0719 0.1508 0.3349 0.132 Uiso 1.00 1 c R . . H(20) H -0.0437 0.0490 0.4455 0.266 Uiso 1.00 1 c R . . H(21) H -0.0984 0.0429 0.3784 0.266 Uiso 1.00 1 c R . . H(22) H -0.0814 -0.0805 0.3713 0.178 Uiso 1.00 1 c R . . H(23) H -0.0209 -0.0681 0.4236 0.178 Uiso 1.00 1 c R . . H(24) H -0.0514 -0.1282 0.2829 0.161 Uiso 1.00 1 c R . . H(25) H 0.0084 -0.1264 0.3391 0.161 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(1) 0.0848(4) 0.0430(3) 0.0282(2) -0.0199(2) 0.0124(2) -0.00070(19) Ni(2) 0.0482(4) 0.0658(5) 0.0606(5) 0.0000 -0.0058(3) 0.0000 Fe(1) 0.0463(3) 0.0341(3) 0.0258(2) -0.0030(2) 0.0051(2) -0.00235(18) O(1) 0.120(6) 0.080(4) 0.213(9) 0.0000 -0.047(6) 0.0000 O(2) 0.053(3) 0.045(3) 0.147(7) -0.011(2) -0.011(4) 0.024(4) N(1) 0.083(2) 0.057(2) 0.0286(17) -0.0144(18) 0.0146(16) -0.0080(14) N(2) 0.056(2) 0.090(3) 0.069(2) 0.017(2) -0.009(2) -0.006(2) N(3) 0.093(3) 0.0484(19) 0.051(2) -0.015(2) 0.026(2) 0.0024(16) N(4) 0.112(4) 0.059(2) 0.151(5) -0.029(2) 0.050(3) -0.002(3) N(5) 0.069(3) 0.119(4) 0.088(3) 0.021(2) 0.006(2) 0.031(3) N(6) 0.101(3) 0.065(2) 0.042(2) 0.028(2) 0.004(2) -0.0196(18) N(7) 0.131(4) 0.057(2) 0.148(5) -0.006(2) 0.088(4) -0.018(2) N(8) 0.158(6) 0.162(6) 0.044(2) -0.105(5) 0.012(3) -0.023(3) N(9) 0.076(3) 0.084(3) 0.119(4) 0.007(2) 0.016(3) 0.025(3) N(10) 0.083(3) 0.161(6) 0.084(3) 0.041(3) 0.009(3) -0.028(3) N(11) 0.105(5) 0.063(3) 0.102(5) 0.0000 0.051(4) 0.0000 C(1) 0.055(2) 0.044(2) 0.0338(19) -0.0121(16) 0.0107(16) 0.0004(15) C(2) 0.056(2) 0.054(2) 0.045(2) 0.0001(19) 0.008(2) -0.0074(18) C(3) 0.064(2) 0.043(2) 0.0336(19) -0.0028(17) 0.0163(18) -0.0006(15) C(4) 0.063(2) 0.044(2) 0.066(2) -0.0090(19) 0.014(2) -0.0012(19) C(5) 0.055(2) 0.056(2) 0.043(2) 0.0046(19) 0.0047(19) 0.0089(18) C(6) 0.067(2) 0.047(2) 0.038(2) 0.0135(19) 0.0026(19) -0.0007(16) C(7) 0.58(3) 0.205(14) 0.181(14) 0.230(19) 0.16(2) 0.003(11) C(8) 0.38(2) 0.184(11) 0.138(10) -0.183(15) 0.154(14) -0.116(9) C(9) 0.42(2) 0.124(8) 0.082(6) -0.122(14) -0.002(11) -0.046(5) C(10) 0.207(15) 0.171(11) 0.207(15) -0.054(11) -0.125(14) -0.008(10) C(11) 0.085(7) 0.45(3) 0.150(12) -0.100(12) -0.050(7) 0.153(17) C(12) 0.105(7) 0.131(8) 0.38(2) 0.010(6) -0.083(11) -0.028(11) C(13) 0.33(2) 0.236(16) 0.149(11) 0.010(15) 0.174(14) -0.001(10) C(14) 0.125(7) 0.221(12) 0.109(7) -0.013(8) 0.051(6) 0.068(7) C(15) 0.167(9) 0.096(5) 0.153(8) -0.012(5) 0.063(7) 0.035(5) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ni(1) N(1) 2.098(3) yes . . Ni(1) N(3) 2.059(4) yes . 7_556 Ni(1) N(6) 2.082(4) yes . 4_555 Ni(1) N(7) 2.079(5) yes . . Ni(1) N(8) 2.127(5) yes . . Ni(1) N(9) 2.071(5) yes . . Ni(2) O(1) 2.114(7) yes . . Ni(2) N(2) 2.055(4) yes . . Ni(2) N(2) 2.055(4) yes . 2_555 Ni(2) N(10) 2.089(6) yes . . Ni(2) N(10) 2.089(6) yes . 2_555 Ni(2) N(11) 2.111(7) yes . . Fe(1) C(1) 1.937(3) yes . . Fe(1) C(2) 1.919(4) yes . . Fe(1) C(3) 1.936(4) yes . . Fe(1) C(4) 1.946(4) yes . . Fe(1) C(5) 1.943(4) yes . . Fe(1) C(6) 1.927(4) yes . . N(1) C(1) 1.142(5) yes . . N(2) C(2) 1.148(6) yes . . N(3) C(3) 1.133(5) yes . . N(4) C(4) 1.142(7) yes . . N(5) C(5) 1.133(6) yes . . N(6) C(6) 1.146(6) yes . . N(7) C(7) 1.581(16) yes . . N(8) C(9) 1.428(15) yes . . N(8) C(10) 1.317(18) yes . . N(9) C(12) 1.407(12) yes . . N(10) C(13) 1.342(18) yes . . N(11) C(15) 1.408(11) yes . . N(11) C(15) 1.408(11) yes . 2_555 C(7) C(8) 1.23(2) yes . . C(8) C(9) 1.41(3) yes . . C(10) C(11) 1.33(2) yes . . C(11) C(12) 1.58(2) yes . . C(13) C(14) 1.30(2) yes . . C(14) C(15) 1.376(16) yes . . N(7) H(1) 0.910 no . . N(7) H(2) 0.910 no . . N(8) H(9) 0.920 no . . N(9) H(16) 0.910 no . . N(9) H(17) 0.910 no . . N(10) H(18) 0.910 no . . N(10) H(19) 0.910 no . . C(7) H(3) 0.980 no . . C(7) H(4) 0.98 no . . C(8) H(5) 0.980 no . . C(8) H(6) 0.980 no . . C(9) H(7) 0.980 no . . C(9) H(8) 0.980 no . . C(10) H(10) 0.980 no . . C(10) H(11) 0.980 no . . C(11) H(12) 0.98 no . . C(11) H(13) 0.980 no . . C(12) H(14) 0.980 no . . C(12) H(15) 0.980 no . . C(13) H(20) 0.980 no . . C(13) H(21) 0.980 no . . C(14) H(22) 0.980 no . . C(14) H(23) 0.980 no . . C(15) H(24) 0.980 no . . C(15) H(25) 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 N(1) Ni(1) N(3) 91.41(14) yes . . 7_556 N(1) Ni(1) N(6) 91.73(14) yes . . 4_555 N(1) Ni(1) N(7) 88.06(19) yes . . . N(1) Ni(1) N(8) 178.6(2) yes . . . N(1) Ni(1) N(9) 84.05(19) yes . . . N(3) Ni(1) N(6) 176.76(15) yes 7_556 . 4_555 N(3) Ni(1) N(7) 91.65(19) yes 7_556 . . N(3) Ni(1) N(8) 88.5(2) yes 7_556 . . N(3) Ni(1) N(9) 89.9(2) yes 7_556 . . N(6) Ni(1) N(7) 89.2(2) yes 4_555 . . N(6) Ni(1) N(8) 88.4(2) yes 4_555 . . N(6) Ni(1) N(9) 89.7(2) yes 4_555 . . N(7) Ni(1) N(8) 93.4(2) yes . . . N(7) Ni(1) N(9) 172.0(2) yes . . . N(8) Ni(1) N(9) 94.5(2) yes . . . O(1) Ni(2) N(2) 90.94(13) yes . . . O(1) Ni(2) N(2) 90.94(13) yes . . 2_555 O(1) Ni(2) N(10) 86.9(2) yes . . . O(1) Ni(2) N(10) 86.9(2) yes . . 2_555 O(1) Ni(2) N(11) 180 yes . . . N(2) Ni(2) N(2) 178.11(19) yes . . 2_555 N(2) Ni(2) N(10) 89.4(2) yes . . . N(2) Ni(2) N(10) 90.7(2) yes . . 2_555 N(2) Ni(2) N(11) 89.06(13) yes . . . N(2) Ni(2) N(10) 90.7(2) yes 2_555 . . N(2) Ni(2) N(10) 89.4(2) yes 2_555 . 2_555 N(2) Ni(2) N(11) 89.06(13) yes 2_555 . . N(10) Ni(2) N(10) 173.7(3) yes . . 2_555 N(10) Ni(2) N(11) 93.1(2) yes . . . N(10) Ni(2) N(11) 93.1(2) yes 2_555 . . C(1) Fe(1) C(2) 93.44(18) yes . . . C(1) Fe(1) C(3) 89.44(16) yes . . . C(1) Fe(1) C(4) 92.10(19) yes . . . C(1) Fe(1) C(5) 90.06(18) yes . . . C(1) Fe(1) C(6) 177.64(17) yes . . . C(2) Fe(1) C(3) 88.21(18) yes . . . C(2) Fe(1) C(4) 89.46(19) yes . . . C(2) Fe(1) C(5) 175.5(2) yes . . . C(2) Fe(1) C(6) 88.93(18) yes . . . C(3) Fe(1) C(4) 177.28(17) yes . . . C(3) Fe(1) C(5) 88.99(18) yes . . . C(3) Fe(1) C(6) 90.61(17) yes . . . C(4) Fe(1) C(5) 93.24(19) yes . . . C(4) Fe(1) C(6) 87.9(2) yes . . . C(5) Fe(1) C(6) 87.58(18) yes . . . Ni(1) N(1) C(1) 153.8(3) yes . . . Ni(2) N(2) C(2) 161.9(4) yes . . . Ni(1) N(3) C(3) 168.5(3) yes 7_556 . . Ni(1) N(6) C(6) 156.5(3) yes 4_554 . . Ni(1) N(7) C(7) 113.9(8) yes . . . Ni(1) N(8) C(9) 121.6(7) yes . . . Ni(1) N(8) C(10) 117.5(8) yes . . . C(9) N(8) C(10) 115.9(11) yes . . . Ni(1) N(9) C(12) 127.9(7) yes . . . Ni(2) N(10) C(13) 122.8(8) yes . . . Ni(2) N(11) C(15) 118.0(4) yes . . . Ni(2) N(11) C(15) 118.0(4) yes . . 2_555 C(15) N(11) C(15) 124.0(7) yes . . 2_555 Fe(1) C(1) N(1) 174.8(4) yes . . . Fe(1) C(2) N(2) 174.9(4) yes . . . Fe(1) C(3) N(3) 177.4(3) yes . . . Fe(1) C(4) N(4) 176.9(4) yes . . . Fe(1) C(5) N(5) 175.0(4) yes . . . Fe(1) C(6) N(6) 175.8(3) yes . . . N(7) C(7) C(8) 125.0(15) yes . . . C(7) C(8) C(9) 123.1(18) yes . . . N(8) C(9) C(8) 116.6(12) yes . . . N(8) C(10) C(11) 130.4(13) yes . . . C(10) C(11) C(12) 130.8(11) yes . . . N(9) C(12) C(11) 111.6(10) yes . . . N(10) C(13) C(14) 126.9(14) yes . . . C(13) C(14) C(15) 130.3(12) yes . . . N(11) C(15) C(14) 128.1(8) yes . . . Ni(1) N(7) H(1) 108.8 no . . . Ni(1) N(7) H(2) 108.8 no . . . C(7) N(7) H(1) 108.8 no . . . C(7) N(7) H(2) 108.8 no . . . H(1) N(7) H(2) 107.7 no . . . Ni(1) N(8) H(9) 97.5 no . . . C(9) N(8) H(9) 97.5 no . . . C(10) N(8) H(9) 97.5 no . . . Ni(1) N(9) H(16) 105.3 no . . . Ni(1) N(9) H(17) 105.3 no . . . C(12) N(9) H(16) 105.3 no . . . C(12) N(9) H(17) 105.3 no . . . H(16) N(9) H(17) 106.0 no . . . Ni(2) N(10) H(18) 106.6 no . . . Ni(2) N(10) H(19) 106.6 no . . . C(13) N(10) H(18) 106.6 no . . . C(13) N(10) H(19) 106.6 no . . . H(18) N(10) H(19) 106.6 no . . . N(7) C(7) H(3) 106.1 no . . . N(7) C(7) H(4) 106.1 no . . . C(8) C(7) H(3) 106.1 no . . . C(8) C(7) H(4) 106.1 no . . . H(3) C(7) H(4) 106.3 no . . . C(7) C(8) H(5) 106.5 no . . . C(7) C(8) H(6) 106.5 no . . . C(9) C(8) H(5) 106.6 no . . . C(9) C(8) H(6) 106.6 no . . . H(5) C(8) H(6) 106.5 no . . . N(8) C(9) H(7) 108.2 no . . . N(8) C(9) H(8) 108.2 no . . . C(8) C(9) H(7) 108.1 no . . . C(8) C(9) H(8) 108.1 no . . . H(7) C(9) H(8) 107.3 no . . . N(8) C(10) H(10) 104.7 no . . . N(8) C(10) H(11) 104.7 no . . . C(11) C(10) H(10) 104.7 no . . . C(11) C(10) H(11) 104.7 no . . . H(10) C(10) H(11) 105.7 no . . . C(10) C(11) H(12) 104.6 no . . . C(10) C(11) H(13) 104.6 no . . . C(12) C(11) H(12) 104.6 no . . . C(12) C(11) H(13) 104.6 no . . . H(12) C(11) H(13) 105.7 no . . . N(9) C(12) H(14) 109.3 no . . . N(9) C(12) H(15) 109.3 no . . . C(11) C(12) H(14) 109.3 no . . . C(11) C(12) H(15) 109.3 no . . . H(14) C(12) H(15) 108.0 no . . . N(10) C(13) H(20) 105.6 no . . . N(10) C(13) H(21) 105.6 no . . . C(14) C(13) H(20) 105.6 no . . . C(14) C(13) H(21) 105.6 no . . . H(20) C(13) H(21) 106.1 no . . . C(13) C(14) H(22) 104.7 no . . . C(13) C(14) H(23) 104.7 no . . . C(15) C(14) H(22) 104.7 no . . . C(15) C(14) H(23) 104.7 no . . . H(22) C(14) H(23) 105.7 no . . . N(11) C(15) H(24) 105.3 no . . . N(11) C(15) H(25) 105.3 no . . . C(14) C(15) H(24) 105.3 no . . . C(14) C(15) H(25) 105.3 no . . . H(24) C(15) H(25) 106.0 no . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O(1) O(3) 2.89(2) ? . 5_455 O(1) O(3) 2.89(2) ? . 6_555 O(2) O(3) 3.50(2) ? . . O(2) O(6) 2.98(2) ? . . O(2) N(4) 2.888(8) ? . 7_546 O(2) N(5) 3.008(8) ? . . O(3) O(1) 2.89(2) ? . 5_545 O(3) O(2) 3.50(2) ? . . O(3) O(4) 2.93(2) ? . . O(3) O(5) 3.10(3) ? . . O(3) O(6) 3.34(3) ? . 3_656 O(3) N(10) 3.46(2) ? . 5_545 O(4) O(3) 2.93(2) ? . . O(4) O(5) 2.02(3) ? . . O(4) N(1) 3.340(15) ? . 5_545 O(4) N(3) 3.361(16) ? . 3_656 O(4) N(5) 3.441(16) ? . 3_656 O(4) N(7) 3.530(18) ? . 5_545 O(4) C(1) 3.583(15) ? . 5_545 O(4) C(3) 3.598(17) ? . 3_656 O(5) O(3) 3.10(3) ? . . O(5) O(4) 2.02(3) ? . . O(5) O(6) 2.89(4) ? . . O(5) N(5) 3.24(2) ? . 3_656 O(5) N(7) 3.36(2) ? . 5_545 O(6) O(2) 2.98(2) ? . . O(6) O(3) 3.34(3) ? . 3_656 O(6) O(5) 2.89(4) ? . . O(6) O(6) 3.53(4) ? . 2_656 N(1) O(4) 3.340(15) ? . 5_455 N(3) O(4) 3.361(16) ? . 3_656 N(4) O(2) 2.888(8) ? . 7_546 N(5) O(2) 3.008(8) ? . . N(5) O(4) 3.441(16) ? . 3_656 N(5) O(5) 3.24(2) ? . 3_656 N(5) C(8) 3.492(16) ? . 6_546 N(7) O(4) 3.530(18) ? . 5_455 N(7) O(5) 3.36(2) ? . 5_455 N(10) O(3) 3.46(2) ? . 5_455 C(1) O(4) 3.583(15) ? . 5_455 C(3) O(4) 3.598(17) ? . 3_656 C(8) N(5) 3.492(16) ? . 6_556 O(1) H(13) 2.947 ? . 8_454 O(1) H(14) 3.351 ? . 8_454 O(2) H(4) 3.313 ? . 6_546 O(2) H(5) 3.144 ? . 6_546 O(2) H(6) 3.207 ? . 6_546 O(2) H(10) 2.987 ? . 4_554 O(2) H(12) 3.440 ? . 4_554 O(3) H(13) 3.09 ? . 4_554 O(3) H(14) 3.28 ? . 3_656 O(3) H(18) 2.746 ? . 5_545 O(3) H(19) 3.433 ? . 5_545 O(4) H(1) 2.676 ? . 5_545 O(4) H(14) 2.905 ? . 3_656 O(4) H(17) 2.915 ? . 3_656 O(5) H(1) 2.54 ? . 5_545 O(5) H(3) 3.12 ? . 5_545 O(5) H(12) 3.38 ? . 2_656 N(1) H(21) 3.316 ? . 3_556 N(1) H(22) 2.830 ? . 3_556 N(4) H(7) 3.192 ? . 6_546 N(4) H(10) 3.291 ? . 6_546 N(4) H(20) 3.145 ? . 3_556 N(4) H(21) 3.316 ? . 3_556 N(5) H(5) 3.547 ? . 6_546 N(5) H(6) 2.656 ? . 6_546 N(5) H(7) 3.466 ? . 6_546 N(7) H(22) 3.063 ? . 3_556 N(7) H(24) 3.015 ? . 3_556 N(9) H(3) 3.525 ? . 6_546 N(9) H(6) 3.261 ? . 6_546 N(10) H(11) 3.105 ? . 8_454 N(10) H(13) 3.233 ? . 8_454 C(1) H(21) 3.442 ? . 3_556 C(1) H(22) 3.323 ? . 3_556 C(4) H(7) 3.270 ? . 6_546 C(4) H(20) 3.466 ? . 3_556 C(4) H(21) 3.466 ? . 3_556 C(5) H(6) 3.229 ? . 6_546 C(5) H(7) 3.419 ? . 6_546 C(7) H(15) 3.264 ? . 6_556 C(7) H(16) 3.419 ? . 6_556 C(8) H(15) 3.555 ? . 6_556 C(8) H(16) 3.165 ? . 6_556 C(9) H(16) 3.336 ? . 6_556 C(10) H(19) 3.010 ? . 8_555 C(11) H(19) 3.19 ? . 8_555 C(12) H(3) 3.420 ? . 6_546 C(12) H(6) 3.548 ? . 6_546 C(13) H(11) 3.547 ? . 8_454 C(13) H(20) 3.578 ? . 3_556 C(13) H(23) 3.392 ? . 3_556 C(14) H(2) 3.172 ? . 3_556 C(14) H(20) 3.372 ? . 3_556 C(15) H(2) 3.009 ? . 3_556 H(1) O(4) 2.676 ? . 5_455 H(1) O(5) 2.54 ? . 5_455 H(1) H(22) 3.049 ? . 3_556 H(1) H(24) 3.235 ? . 3_556 H(2) C(14) 3.172 ? . 3_556 H(2) C(15) 3.009 ? . 3_556 H(2) H(22) 2.424 ? . 3_556 H(2) H(24) 2.136 ? . 3_556 H(2) H(25) 3.411 ? . 3_556 H(3) O(5) 3.12 ? . 5_455 H(3) N(9) 3.525 ? . 6_556 H(3) C(12) 3.420 ? . 6_556 H(3) H(12) 3.464 ? . 6_556 H(3) H(15) 2.672 ? . 6_556 H(3) H(16) 2.790 ? . 6_556 H(4) O(2) 3.313 ? . 6_556 H(4) H(15) 3.039 ? . 6_556 H(4) H(24) 3.514 ? . 3_556 H(5) O(2) 3.144 ? . 6_556 H(5) N(5) 3.547 ? . 6_556 H(6) O(2) 3.207 ? . 6_556 H(6) N(5) 2.656 ? . 6_556 H(6) N(9) 3.261 ? . 6_556 H(6) C(5) 3.229 ? . 6_556 H(6) C(12) 3.548 ? . 6_556 H(6) H(15) 2.913 ? . 6_556 H(6) H(16) 2.517 ? . 6_556 H(6) H(17) 3.320 ? . 6_556 H(7) N(4) 3.192 ? . 6_556 H(7) N(5) 3.466 ? . 6_556 H(7) C(4) 3.270 ? . 6_556 H(7) C(5) 3.419 ? . 6_556 H(7) H(16) 3.589 ? . 6_556 H(8) H(16) 2.727 ? . 6_556 H(8) H(21) 3.487 ? . 8_555 H(10) O(2) 2.987 ? . 4_555 H(10) N(4) 3.291 ? . 6_556 H(10) H(19) 3.166 ? . 8_555 H(11) N(10) 3.105 ? . 8_555 H(11) C(13) 3.547 ? . 8_555 H(11) H(18) 3.504 ? . 8_555 H(11) H(19) 2.210 ? . 8_555 H(11) H(21) 2.956 ? . 8_555 H(12) O(2) 3.440 ? . 4_555 H(12) O(5) 3.38 ? . 2_656 H(12) H(3) 3.464 ? . 6_546 H(13) O(3) 3.09 ? . 4_555 H(13) N(10) 3.233 ? . 8_555 H(13) H(18) 3.278 ? . 8_555 H(13) H(19) 2.460 ? . 8_555 H(14) O(3) 3.28 ? . 3_656 H(14) O(4) 2.905 ? . 3_656 H(15) C(7) 3.264 ? . 6_546 H(15) C(8) 3.555 ? . 6_546 H(15) H(3) 2.672 ? . 6_546 H(15) H(4) 3.039 ? . 6_546 H(15) H(6) 2.913 ? . 6_546 H(16) C(7) 3.419 ? . 6_546 H(16) C(8) 3.165 ? . 6_546 H(16) C(9) 3.336 ? . 6_546 H(16) H(3) 2.790 ? . 6_546 H(16) H(6) 2.517 ? . 6_546 H(16) H(7) 3.589 ? . 6_546 H(16) H(8) 2.727 ? . 6_546 H(17) O(4) 2.915 ? . 3_656 H(17) H(6) 3.320 ? . 6_546 H(18) O(3) 2.746 ? . 5_455 H(18) H(11) 3.504 ? . 8_454 H(18) H(13) 3.278 ? . 8_454 H(18) H(23) 3.290 ? . 3_556 H(19) O(3) 3.433 ? . 5_455 H(19) C(10) 3.010 ? . 8_454 H(19) C(11) 3.19 ? . 8_454 H(19) H(10) 3.166 ? . 8_454 H(19) H(11) 2.210 ? . 8_454 H(19) H(13) 2.460 ? . 8_454 H(20) N(4) 3.145 ? . 3_556 H(20) C(4) 3.466 ? . 3_556 H(20) C(13) 3.578 ? . 3_556 H(20) C(14) 3.372 ? . 3_556 H(20) H(20) 2.881 ? . 3_556 H(20) H(23) 2.453 ? . 3_556 H(21) N(1) 3.316 ? . 3_556 H(21) N(4) 3.316 ? . 3_556 H(21) C(1) 3.442 ? . 3_556 H(21) C(4) 3.466 ? . 3_556 H(21) H(8) 3.487 ? . 8_454 H(21) H(11) 2.956 ? . 8_454 H(22) N(1) 2.830 ? . 3_556 H(22) N(7) 3.063 ? . 3_556 H(22) C(1) 3.323 ? . 3_556 H(22) H(1) 3.049 ? . 3_556 H(22) H(2) 2.424 ? . 3_556 H(23) C(13) 3.392 ? . 3_556 H(23) H(18) 3.290 ? . 3_556 H(23) H(20) 2.453 ? . 3_556 H(23) H(23) 3.223 ? . 3_556 H(24) N(7) 3.015 ? . 3_556 H(24) H(1) 3.235 ? . 3_556 H(24) H(2) 2.136 ? . 3_556 H(24) H(4) 3.514 ? . 3_556 H(25) H(2) 3.411 ? . 3_556 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment 'CIF_2a.cif' data_3D_[Mn(NNdmenH)][Cr(CN)6](2a) _database_code_depnum_ccdc_archive 'CCDC 746508' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C10 H13 Cr Mn N8 ' _chemical_formula_moiety 'C10 H13 Cr Mn N8 ' _chemical_formula_weight 352.20 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 7.844(18) _cell_length_b 14.31(3) _cell_length_c 12.96(3) _cell_angle_alpha 90.0000 _cell_angle_beta 90.07(3) _cell_angle_gamma 90.0000 _cell_volume 1456(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2686 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 343.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712.00 _exptl_absorpt_coefficient_mu 1.616 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.303 _exptl_absorpt_correction_T_max 0.748 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.71 _diffrn_reflns_number 3173 _diffrn_reflns_av_R_equivalents 0.116 _diffrn_reflns_theta_max 27.47 _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.913 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_ambient_temperature 343.1 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 0.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3046 _reflns_number_gt 1020 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0984 _refine_ls_wR_factor_ref 0.1368 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2935 _refine_ls_number_parameters 209 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00076|Fo|^2^]' _refine_ls_shift/su_max 0.0033 _refine_diff_density_max 1.48 _refine_diff_density_min -1.18 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.011(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cr Cr 0.321 0.624 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Mn Mn 0.337 0.728 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn(1) Mn 0.7499(2) 0.66207(10) 0.1468(1) 0.0407(5) Uani 1.00 d . . . Cr(1) Cr 0.2500(2) 0.8087(1) 0.3855(1) 0.0392(5) Uani 1.00 d . . . N(1) N 0.551(1) 0.7204(6) 0.2504(7) 0.054(3) Uani 1.00 d . . . N(2) N 0.544(1) 0.8726(6) 0.5380(6) 0.053(3) Uani 1.00 d . . . N(3) N 0.249(1) 1.0182(6) 0.2980(6) 0.055(3) Uani 1.00 d . . . N(4) N 0.255(2) 0.6184(8) 0.5068(9) 0.137(6) Uani 1.00 d . . . N(5) N -0.051(1) 0.7206(6) 0.2507(7) 0.055(3) Uani 1.00 d . . . N(6) N -0.045(1) 0.8726(7) 0.5379(6) 0.059(3) Uani 1.00 d . . . N(7) N 0.750(2) 0.8012(7) 0.0469(7) 0.083(4) Uani 1.00 d . . . N(8) N 0.752(2) 0.9946(10) 0.1818(10) 0.090(5) Uani 1.00 d . . . C(1) C 0.442(1) 0.7539(6) 0.2924(8) 0.044(3) Uani 1.00 d . . . C(2) C 0.436(1) 0.8554(6) 0.4839(7) 0.043(3) Uani 1.00 d . . . C(3) C 0.251(1) 0.9373(7) 0.3197(7) 0.044(3) Uani 1.00 d . . . C(4) C 0.252(2) 0.6860(8) 0.4630(9) 0.066(4) Uani 1.00 d . . . C(5) C 0.058(1) 0.7535(6) 0.2926(8) 0.046(3) Uani 1.00 d . . . C(6) C 0.062(1) 0.8554(6) 0.4844(7) 0.042(3) Uani 1.00 d . . . C(7') C 0.832(3) 0.882(2) 0.048(2) 0.080(9) Uani 0.50 d P . . C(7) C 0.663(3) 0.885(2) 0.053(2) 0.10(1) Uani 0.50 d P . . C(8') C 0.839(5) 0.911(2) 0.172(3) 0.11(1) Uani 0.50 d P . . C(8) C 0.688(5) 0.914(2) 0.178(3) 0.11(1) Uani 0.50 d P . . C(9) C 0.757(3) 1.016(1) 0.294(1) 0.147(9) Uani 1.00 d . . . C(10') C 0.592(4) 0.968(3) 0.152(3) 0.12(1) Uani 0.50 d P . . C(10) C 0.910(4) 0.975(3) 0.158(2) 0.10(1) Uani 0.50 d P . . H(1) H 0.7316 0.7797 -0.0204 0.0956 Uiso 1.00 calc . . . H(2') H 0.6396 0.8222 0.0522 0.0956 Uiso 0.50 calc P . . H(2) H 0.8694 0.8210 0.0524 0.0956 Uiso 0.50 calc P . . H(3') H 0.7834 0.9227 0.0073 0.1260 Uiso 0.50 calc P . . H(3) H 0.7215 0.9282 0.0143 0.1366 Uiso 0.50 calc P . . H(4') H 0.9504 0.8663 0.0223 0.1260 Uiso 0.50 calc P . . H(4) H 0.5540 0.8721 0.0281 0.1366 Uiso 0.50 calc P . . H(5') H 0.9789 0.9308 0.1652 0.1088 Uiso 1.00 calc . . . H(5) H 0.5275 0.9264 0.1847 0.0936 Uiso 1.00 calc . . . H(6') H 0.8332 0.8629 0.2016 0.1433 Uiso 0.50 calc P . . H(6) H 0.7204 0.8601 0.2113 0.1456 Uiso 0.50 calc P . . H(7') H 0.7885 1.0428 0.1455 0.1244 Uiso 0.50 calc P . . H(7) H 0.6968 1.0381 0.1426 0.1244 Uiso 0.50 calc P . . H(8) H 0.6853 1.0725 0.3000 0.2027 Uiso 1.00 calc . . . H(9) H 0.6975 0.9692 0.3355 0.2027 Uiso 1.00 calc . . . H(10) H 0.8623 1.0261 0.3152 0.2027 Uiso 1.00 calc . . . H(11') H 0.5199 1.0347 0.1807 0.0936 Uiso 0.50 calc P . . H(11) H 0.9838 1.0324 0.2070 0.1088 Uiso 0.50 calc P . . H(12') H 0.5704 0.9785 0.0831 0.0936 Uiso 0.50 calc P . . H(12) H 0.9422 1.0141 0.0918 0.1088 Uiso 0.50 calc P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn(1) 0.0291(9) 0.0465(10) 0.0464(9) -0.0006(6) -0.0010(6) -0.0032(6) Cr(1) 0.0254(9) 0.0460(10) 0.0461(10) 0.0002(6) -0.0009(6) -0.0028(6) N(1) 0.041(5) 0.057(5) 0.064(6) -0.003(4) -0.001(4) -0.015(4) N(2) 0.041(5) 0.071(6) 0.046(5) 0.003(4) -0.009(4) -0.001(4) N(3) 0.058(6) 0.066(6) 0.042(5) -0.010(5) -0.003(4) 0.002(4) N(4) 0.25(2) 0.061(8) 0.10(1) -0.014(10) -0.01(1) 0.016(7) N(5) 0.036(5) 0.064(6) 0.065(6) 0.000(4) -0.005(4) -0.011(4) N(6) 0.057(6) 0.075(6) 0.046(5) 0.003(5) 0.014(4) 0.001(4) N(7) 0.14(1) 0.065(6) 0.042(6) -0.007(7) -0.018(6) -0.005(5) N(8) 0.065(9) 0.12(1) 0.088(9) 0.008(7) 0.004(7) -0.029(8) C(1) 0.033(5) 0.046(6) 0.055(6) -0.003(4) 0.004(4) -0.005(4) C(2) 0.033(5) 0.053(6) 0.043(5) 0.002(4) 0.002(4) 0.004(4) C(3) 0.036(5) 0.047(6) 0.051(6) -0.003(4) -0.006(4) -0.009(4) C(4) 0.085(10) 0.059(7) 0.053(7) 0.004(6) -0.003(6) -0.002(5) C(5) 0.034(5) 0.048(6) 0.055(6) 0.002(4) -0.001(4) -0.001(4) C(6) 0.032(5) 0.049(5) 0.043(5) 0.001(4) -0.002(4) -0.002(4) C(7') 0.06(2) 0.10(2) 0.08(2) -0.01(2) 0.04(1) -0.03(2) C(7) 0.03(1) 0.11(2) 0.16(3) 0.04(1) -0.04(2) -0.07(2) C(8') 0.09(3) 0.03(1) 0.19(4) 0.03(2) -0.09(3) -0.04(2) C(8) 0.14(3) 0.05(2) 0.15(3) 0.04(2) 0.11(3) 0.01(2) C(9) 0.17(2) 0.18(2) 0.09(1) -0.02(1) 0.01(1) -0.06(1) C(10') 0.09(2) 0.13(3) 0.14(3) -0.07(2) -0.06(2) 0.05(2) C(10) 0.10(3) 0.12(3) 0.09(2) 0.06(2) 0.00(2) -0.01(2) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution DirectMethod _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn(1) N(1) 2.221(9) . . yes Mn(1) N(2) 2.197(8) . 4_564 yes Mn(1) N(3) 2.181(8) . 2_645 yes Mn(1) N(5) 2.223(9) . 1_655 yes Mn(1) N(6) 2.197(9) . 4_664 yes Mn(1) N(7) 2.375(10) . . yes Cr(1) C(1) 2.086(10) . . yes Cr(1) C(2) 2.049(10) . . yes Cr(1) C(3) 2.03(1) . . yes Cr(1) C(4) 2.02(1) . . yes Cr(1) C(5) 2.081(10) . . yes Cr(1) C(6) 2.066(10) . . yes N(1) C(1) 1.12(1) . . yes N(2) C(2) 1.13(1) . . yes N(3) C(3) 1.19(1) . . yes N(4) C(4) 1.12(1) . . yes N(5) C(5) 1.12(1) . . yes N(6) C(6) 1.12(1) . . yes N(7) C(7') 1.33(3) . . yes N(7) C(7) 1.38(2) . . yes N(8) C(8') 1.39(3) . . yes N(8) C(8) 1.26(3) . . yes N(8) C(9) 1.49(2) . . yes N(8) C(10') 1.37(3) . . yes N(8) C(10) 1.30(3) . . yes C(7') C(7) 1.33(3) . . yes C(7') C(8') 1.66(4) . . yes C(7) C(8) 1.68(5) . . yes C(7) C(10') 1.84(5) . . yes C(8') C(8) 1.19(5) . . yes C(8') C(10) 1.09(4) . . yes C(8) C(10') 1.13(4) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Mn(1) N(2) 87.6(3) . . 4_564 yes N(1) Mn(1) N(3) 99.2(3) . . 2_645 yes N(1) Mn(1) N(5) 89.1(3) . . 1_655 yes N(1) Mn(1) N(6) 171.0(3) . . 4_664 yes N(1) Mn(1) N(7) 90.8(4) . . . yes N(2) Mn(1) N(3) 90.0(3) 4_564 . 2_645 yes N(2) Mn(1) N(5) 170.9(3) 4_564 . 1_655 yes N(2) Mn(1) N(6) 94.2(3) 4_564 . 4_664 yes N(2) Mn(1) N(7) 80.8(4) 4_564 . . yes N(3) Mn(1) N(5) 98.8(3) 2_645 . 1_655 yes N(3) Mn(1) N(6) 89.7(3) 2_645 . 4_664 yes N(3) Mn(1) N(7) 166.1(3) 2_645 . . yes N(5) Mn(1) N(6) 87.8(3) 1_655 . 4_664 yes N(5) Mn(1) N(7) 90.9(3) 1_655 . . yes N(6) Mn(1) N(7) 80.7(4) 4_664 . . yes C(1) Cr(1) C(2) 88.2(4) . . . yes C(1) Cr(1) C(3) 95.5(4) . . . yes C(1) Cr(1) C(4) 87.4(5) . . . yes C(1) Cr(1) C(5) 92.6(4) . . . yes C(1) Cr(1) C(6) 176.1(4) . . . yes C(2) Cr(1) C(3) 87.9(4) . . . yes C(2) Cr(1) C(4) 88.2(4) . . . yes C(2) Cr(1) C(5) 176.0(4) . . . yes C(2) Cr(1) C(6) 90.9(4) . . . yes C(3) Cr(1) C(4) 175.0(4) . . . yes C(3) Cr(1) C(5) 96.0(4) . . . yes C(3) Cr(1) C(6) 88.3(4) . . . yes C(4) Cr(1) C(5) 87.9(4) . . . yes C(4) Cr(1) C(6) 88.7(4) . . . yes C(5) Cr(1) C(6) 88.0(4) . . . yes Mn(1) N(1) C(1) 171.8(9) . . . yes Mn(1) N(2) C(2) 154.3(8) 4_565 . . yes Mn(1) N(3) C(3) 147.1(7) 2_655 . . yes Mn(1) N(5) C(5) 171.7(9) 1_455 . . yes Mn(1) N(6) C(6) 154.2(9) 4_465 . . yes Mn(1) N(7) C(7') 136(1) . . . yes Mn(1) N(7) C(7) 134(1) . . . yes C(7') N(7) C(7) 58(1) . . . yes C(8') N(8) C(8) 53(2) . . . yes C(8') N(8) C(9) 104(2) . . . yes C(8') N(8) C(10') 100(2) . . . yes C(8') N(8) C(10) 47(1) . . . yes C(8) N(8) C(9) 103(2) . . . yes C(8) N(8) C(10') 50(2) . . . yes C(8) N(8) C(10) 99(2) . . . yes C(9) N(8) C(10') 111(2) . . . yes C(9) N(8) C(10) 104(1) . . . yes C(10') N(8) C(10) 138(2) . . . yes Cr(1) C(1) N(1) 173.5(10) . . . yes Cr(1) C(2) N(2) 173.4(9) . . . yes Cr(1) C(3) N(3) 168.8(8) . . . yes Cr(1) C(4) N(4) 179(1) . . . yes Cr(1) C(5) N(5) 173.6(10) . . . yes Cr(1) C(6) N(6) 173.7(9) . . . yes N(7) C(7') C(7) 62(1) . . . yes N(7) C(7') C(8') 104(2) . . . yes C(7) C(7') C(8') 89(2) . . . yes N(7) C(7) C(7') 58(1) . . . yes N(7) C(7) C(8) 102(2) . . . yes N(7) C(7) C(10') 138(2) . . . yes C(7') C(7) C(8) 86(2) . . . yes C(7') C(7) C(10') 110(2) . . . yes C(8) C(7) C(10') 37(1) . . . yes N(8) C(8') C(7') 106(2) . . . yes N(8) C(8') C(8) 57(1) . . . yes N(8) C(8') C(10) 62(1) . . . yes C(7') C(8') C(8) 92(2) . . . yes C(7') C(8') C(10) 93(4) . . . yes C(8) C(8') C(10) 118(3) . . . yes N(8) C(8) C(7) 108(2) . . . yes N(8) C(8) C(8') 69(2) . . . yes N(8) C(8) C(10') 69(2) . . . yes C(7) C(8) C(8') 92(2) . . . yes C(7) C(8) C(10') 78(3) . . . yes C(8') C(8) C(10') 132(4) . . . yes N(8) C(10') C(7) 95(2) . . . yes N(8) C(10') C(8) 59(2) . . . yes C(7) C(10') C(8) 64(3) . . . yes N(8) C(10) C(8') 70(2) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag N(2) N(7) 2.96(1) . 4_565 ? N(2) N(3) 3.10(1) . 3_676 ? N(2) C(9) 3.59(2) . 3_676 ? N(3) N(6) 3.09(1) . 3_576 ? N(3) C(10) 3.28(4) . 1_455 ? N(3) N(5) 3.34(1) . 2_555 ? N(4) C(7) 3.26(3) . 4_565 ? N(4) C(7') 3.36(3) . 4_465 ? N(4) C(10') 3.47(3) . 4_565 ? N(5) C(8') 3.03(3) . 1_455 ? N(5) N(7) 3.28(1) . 1_455 ? N(5) C(8) 3.57(4) . 1_455 ? N(6) N(7) 2.96(1) . 4_465 ? N(6) C(9) 3.52(2) . 3_676 ? N(8) C(4) 3.32(2) . 2_655 ? C(3) C(10) 3.44(3) . 1_455 ? C(4) C(7) 3.58(3) . 4_565 ? C(5) C(8') 3.23(3) . 1_455 ? #------------------------------------------------------------------------------ #============================================================================== # End of CIF #============================================================================== # Attachment 'CIF_2.cif' data_2D_[Mn(NNdmenH)(H2O)][Cr(CN)6](2) _database_code_depnum_ccdc_archive 'CCDC 746507' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C10 H17 Cr Mn N8 O2 ' _chemical_formula_moiety 'C10 H17 Cr Mn N8 O2 ' _chemical_formula_weight 388.23 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 7.680(3) _cell_length_b 14.499(5) _cell_length_c 16.596(5) _cell_angle_alpha 90.0000 _cell_angle_beta 97.323(5) _cell_angle_gamma 90.0000 _cell_volume 1833.0(10) _cell_formula_units_Z 4 _cell_measurement_reflns_used 5057 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 243.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792.00 _exptl_absorpt_coefficient_mu 1.298 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.549 _exptl_absorpt_correction_T_max 0.878 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 4294 _diffrn_reflns_av_R_equivalents 0.078 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9843 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9843 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_ambient_temperature 243.1 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 0.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4134 _reflns_number_gt 2333 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.0955 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3932 _refine_ls_number_parameters 217 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00078|Fo|^2^]' _refine_ls_shift/su_max 0.0033 _refine_diff_density_max 0.94 _refine_diff_density_min -0.90 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cr Cr 0.321 0.624 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Mn Mn 0.337 0.728 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn(1) Mn 0.2575(1) 0.31890(5) 0.29180(5) 0.0226(2) Uani 1.00 d . . . Cr(1) Cr 0.7379(1) 0.06886(5) 0.22404(5) 0.0213(2) Uani 1.00 d . . . O(1) O 0.3127(6) 0.2599(3) 0.4151(2) 0.037(1) Uani 1.00 d . . . O(2) O 0.310(1) 0.5795(5) 0.0677(4) 0.109(3) Uani 1.00 d . . . N(1) N 0.4462(6) 0.2183(3) 0.2565(3) 0.035(1) Uani 1.00 d . . . N(2) N 0.4313(6) -0.0782(3) 0.1726(3) 0.033(1) Uani 1.00 d . . . N(3) N 0.6898(9) 0.1481(5) 0.0432(3) 0.061(2) Uani 1.00 d . . . N(4) N 0.765(1) -0.0015(5) 0.4091(4) 0.075(3) Uani 1.00 d . . . N(5) N 1.0420(6) 0.2189(3) 0.2677(3) 0.036(1) Uani 1.00 d . . . N(6) N 1.0315(7) -0.0767(3) 0.1879(3) 0.038(1) Uani 1.00 d . . . N(7) N 0.1926(9) 0.3807(4) 0.1617(3) 0.050(2) Uani 1.00 d . . . N(8) N 0.290(1) 0.1908(5) 0.0189(5) 0.039(2) Uani 0.70 d P . . N(8') N 0.181(3) 0.202(2) -0.0046(10) 0.050(6) Uani 0.30 d P . . C(1) C 0.5503(7) 0.1647(4) 0.2472(3) 0.026(1) Uani 1.00 d . . . C(2) C 0.5435(7) -0.0259(3) 0.1905(3) 0.026(1) Uani 1.00 d . . . C(3) C 0.7120(7) 0.1184(4) 0.1067(4) 0.028(1) Uani 1.00 d . . . C(4) C 0.7577(9) 0.0226(4) 0.3437(4) 0.038(2) Uani 1.00 d . . . C(5) C 0.9327(7) 0.1655(4) 0.2535(3) 0.028(1) Uani 1.00 d . . . C(6) C 0.9259(7) -0.0256(4) 0.1989(3) 0.025(1) Uani 1.00 d . . . C(7) C 0.273(2) 0.3385(7) 0.0943(6) 0.049(3) Uani 0.70 d P . . C(7') C 0.114(7) 0.329(2) 0.086(2) 0.12(2) Uani 0.30 d P . . C(8) C 0.203(1) 0.2446(5) 0.0762(5) 0.054(2) Uani 1.00 d . . . C(9) C 0.285(1) 0.2301(6) -0.0646(4) 0.060(2) Uani 1.00 d . . . C(10) C 0.216(1) 0.0970(6) 0.0128(5) 0.073(3) Uani 1.00 d . . . H(1) H 0.3411 0.2938 0.4619 0.0396 Uiso 1.00 calc . . . H(2) H 0.3683 0.2019 0.4249 0.0396 Uiso 1.00 calc . . . H(3) H 0.2344 0.4421 0.1648 0.0581 Uiso 0.70 calc P . . H(3') H 0.1255 0.4331 0.1680 0.0581 Uiso 0.30 calc P . . H(4) H 0.0709 0.3788 0.1489 0.0581 Uiso 0.70 calc P . . H(4') H 0.3055 0.3984 0.1471 0.0581 Uiso 0.30 calc P . . H(5) H 0.2360 0.3767 0.0464 0.0639 Uiso 0.70 calc P . . H(5') H 0.0968 0.3655 0.0351 0.0742 Uiso 0.30 calc P . . H(6) H 0.3903 0.3356 0.1048 0.0639 Uiso 0.70 calc P . . H(6') H -0.0200 0.3126 0.0893 0.0742 Uiso 0.30 calc P . . H(7) H 0.1715 0.2035 0.1146 0.0635 Uiso 1.00 calc . . . H(8) H 0.0783 0.2526 0.0531 0.0635 Uiso 0.70 calc P . . H(8') H 0.3192 0.2623 0.0847 0.0635 Uiso 0.30 calc P . . H(9) H 0.4050 0.1866 0.0409 0.0549 Uiso 0.70 calc P . . H(9') H 0.0426 0.2108 -0.0280 0.0528 Uiso 0.30 calc P . . H(10) H 0.4055 0.2337 -0.0759 0.0646 Uiso 0.70 calc P . . H(10') H 0.3510 0.1769 -0.0770 0.0646 Uiso 0.30 calc P . . H(11) H 0.2215 0.1917 -0.1031 0.0646 Uiso 0.70 calc P . . H(11') H 0.2241 0.2542 -0.1124 0.0646 Uiso 0.30 calc P . . H(12) H 0.2379 0.2902 -0.0663 0.0646 Uiso 0.70 calc P . . H(12') H 0.3677 0.2754 -0.0403 0.0646 Uiso 0.30 calc P . . H(13) H 0.1238 0.0938 0.0480 0.0938 Uiso 0.70 calc P . . H(13') H 0.1179 0.0587 0.0021 0.0938 Uiso 0.30 calc P . . H(14) H 0.1748 0.0812 -0.0389 0.0938 Uiso 0.70 calc P . . H(14') H 0.3078 0.0795 -0.0151 0.0938 Uiso 0.30 calc P . . H(15) H 0.3079 0.0560 0.0362 0.0938 Uiso 0.70 calc P . . H(15') H 0.2576 0.0918 0.0719 0.0938 Uiso 0.30 calc P . . H(16) H 0.1563 0.5802 0.0516 0.0331 Uiso 1.00 calc . . . H(17) H 0.3355 0.6240 0.0158 0.0331 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn(1) 0.0217(4) 0.0154(4) 0.0314(5) -0.0005(3) 0.0069(3) -0.0025(3) Cr(1) 0.0205(4) 0.0142(4) 0.0303(5) -0.0007(3) 0.0071(3) -0.0003(3) O(1) 0.050(3) 0.034(2) 0.029(2) 0.006(2) 0.008(2) 0.002(2) O(2) 0.169(8) 0.087(5) 0.068(5) 0.009(5) 0.000(5) -0.011(4) N(1) 0.030(3) 0.032(3) 0.044(3) 0.003(2) 0.014(2) -0.010(2) N(2) 0.030(3) 0.023(2) 0.048(3) -0.003(2) 0.010(2) 0.002(2) N(3) 0.081(5) 0.068(4) 0.035(3) -0.010(4) 0.006(3) 0.008(3) N(4) 0.122(7) 0.067(5) 0.036(4) 0.000(5) 0.013(4) 0.012(3) N(5) 0.028(3) 0.030(3) 0.052(3) -0.012(2) 0.009(2) -0.007(2) N(6) 0.032(3) 0.028(3) 0.056(3) 0.008(2) 0.008(2) 0.003(2) N(7) 0.080(5) 0.034(3) 0.036(3) 0.003(3) 0.009(3) 0.001(2) N(8) 0.038(5) 0.034(4) 0.044(5) 0.003(4) 0.004(4) -0.009(3) N(8') 0.04(1) 0.10(2) 0.010(8) 0.02(1) 0.006(7) -0.020(9) C(1) 0.027(3) 0.025(3) 0.027(3) -0.002(2) 0.007(2) -0.001(2) C(2) 0.029(3) 0.015(2) 0.036(3) -0.002(2) 0.010(2) 0.003(2) C(3) 0.031(3) 0.022(3) 0.034(3) -0.004(2) 0.010(2) -0.002(2) C(4) 0.049(4) 0.038(3) 0.027(3) -0.005(3) 0.004(3) 0.001(3) C(5) 0.032(3) 0.023(3) 0.028(3) 0.002(2) 0.005(2) -0.002(2) C(6) 0.023(3) 0.018(2) 0.036(3) 0.005(2) 0.007(2) -0.002(2) C(7) 0.093(9) 0.033(5) 0.020(4) -0.011(6) 0.010(5) 0.002(4) C(7') 0.24(6) 0.04(2) 0.07(2) 0.03(3) -0.06(3) -0.03(1) C(8) 0.061(5) 0.049(4) 0.053(4) -0.001(4) 0.004(4) -0.008(4) C(9) 0.080(6) 0.060(5) 0.040(4) -0.006(4) 0.008(4) 0.002(4) C(10) 0.104(8) 0.048(5) 0.065(6) -0.009(5) 0.010(5) 0.002(4) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution DirectMethod _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn(1) O(1) 2.209(4) . . yes Mn(1) N(1) 2.188(5) . . yes Mn(1) N(2) 2.213(5) . 2_555 yes Mn(1) N(5) 2.199(5) . 1_455 yes Mn(1) N(6) 2.212(5) . 2_655 yes Mn(1) N(7) 2.332(6) . . yes Cr(1) C(1) 2.072(5) . . yes Cr(1) C(2) 2.053(5) . . yes Cr(1) C(3) 2.061(6) . . yes Cr(1) C(4) 2.083(6) . . yes Cr(1) C(5) 2.062(6) . . yes Cr(1) C(6) 2.071(5) . . yes N(1) C(1) 1.139(7) . . yes N(2) C(2) 1.158(7) . . yes N(3) C(3) 1.131(8) . . yes N(4) C(4) 1.135(8) . . yes N(5) C(5) 1.145(7) . . yes N(6) C(6) 1.130(7) . . yes N(7) C(7) 1.48(1) . . yes N(7) C(7') 1.52(3) . . yes N(8) N(8') 0.89(2) . . yes N(8) C(8) 1.46(1) . . yes N(8) C(9) 1.49(1) . . yes N(8) C(10) 1.47(1) . . yes N(8') C(8) 1.47(2) . . yes N(8') C(9) 1.41(2) . . yes N(8') C(10) 1.56(2) . . yes C(7) C(7') 1.22(5) . . yes C(7) C(8) 1.48(1) . . yes C(7') C(8) 1.42(3) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Mn(1) N(1) 86.3(2) . . . yes O(1) Mn(1) N(2) 93.9(2) . . 2_555 yes O(1) Mn(1) N(5) 87.9(2) . . 1_455 yes O(1) Mn(1) N(6) 94.2(2) . . 2_655 yes O(1) Mn(1) N(7) 178.7(2) . . . yes N(1) Mn(1) N(2) 179.4(2) . . 2_555 yes N(1) Mn(1) N(5) 91.2(2) . . 1_455 yes N(1) Mn(1) N(6) 90.0(2) . . 2_655 yes N(1) Mn(1) N(7) 94.5(2) . . . yes N(2) Mn(1) N(5) 89.4(2) 2_555 . 1_455 yes N(2) Mn(1) N(6) 89.4(2) 2_555 . 2_655 yes N(2) Mn(1) N(7) 85.3(2) 2_555 . . yes N(5) Mn(1) N(6) 177.6(2) 1_455 . 2_655 yes N(5) Mn(1) N(7) 91.0(2) 1_455 . . yes N(6) Mn(1) N(7) 86.8(2) 2_655 . . yes C(1) Cr(1) C(2) 90.0(2) . . . yes C(1) Cr(1) C(3) 87.5(2) . . . yes C(1) Cr(1) C(4) 90.4(2) . . . yes C(1) Cr(1) C(5) 90.1(2) . . . yes C(1) Cr(1) C(6) 178.9(2) . . . yes C(2) Cr(1) C(3) 89.9(2) . . . yes C(2) Cr(1) C(4) 90.3(2) . . . yes C(2) Cr(1) C(5) 178.0(2) . . . yes C(2) Cr(1) C(6) 90.3(2) . . . yes C(3) Cr(1) C(4) 177.9(2) . . . yes C(3) Cr(1) C(5) 88.1(2) . . . yes C(3) Cr(1) C(6) 91.5(2) . . . yes C(4) Cr(1) C(5) 91.7(2) . . . yes C(4) Cr(1) C(6) 90.7(2) . . . yes C(5) Cr(1) C(6) 89.6(2) . . . yes Mn(1) N(1) C(1) 172.3(5) . . . yes Mn(1) N(2) C(2) 149.8(5) 2_545 . . yes Mn(1) N(5) C(5) 177.9(5) 1_655 . . yes Mn(1) N(6) C(6) 162.1(5) 2_645 . . yes Mn(1) N(7) C(7) 118.7(5) . . . yes Mn(1) N(7) C(7') 126(1) . . . yes C(7) N(7) C(7') 47(1) . . . yes N(8') N(8) C(8) 73(1) . . . yes N(8') N(8) C(9) 67(1) . . . yes N(8') N(8) C(10) 78(1) . . . yes C(8) N(8) C(9) 116.2(7) . . . yes C(8) N(8) C(10) 109.6(7) . . . yes C(9) N(8) C(10) 108.9(7) . . . yes N(8) N(8') C(8) 71(1) . . . yes N(8) N(8') C(9) 77(1) . . . yes N(8) N(8') C(10) 67(1) . . . yes C(8) N(8') C(9) 120(1) . . . yes C(8) N(8') C(10) 104(1) . . . yes C(9) N(8') C(10) 108(1) . . . yes Cr(1) C(1) N(1) 177.1(5) . . . yes Cr(1) C(2) N(2) 178.4(5) . . . yes Cr(1) C(3) N(3) 176.3(6) . . . yes Cr(1) C(4) N(4) 178.3(7) . . . yes Cr(1) C(5) N(5) 178.1(5) . . . yes Cr(1) C(6) N(6) 177.5(5) . . . yes N(7) C(7) C(7') 67(1) . . . yes N(7) C(7) C(8) 110.9(8) . . . yes C(7') C(7) C(8) 62(1) . . . yes N(7) C(7') C(7) 64(1) . . . yes N(7) C(7') C(8) 111(2) . . . yes C(7) C(7') C(8) 67(2) . . . yes N(8) C(8) N(8') 35.3(7) . . . yes N(8) C(8) C(7) 116.1(7) . . . yes N(8) C(8) C(7') 143(1) . . . yes N(8') C(8) C(7) 124(1) . . . yes N(8') C(8) C(7') 118(1) . . . yes C(7) C(8) C(7') 49(1) . . . yes N(8) C(9) N(8') 35.4(8) . . . yes N(8) C(10) N(8') 33.9(7) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) N(3) 2.775(7) . 4_455 ? O(1) O(2) 2.806(8) . 2_545 ? O(1) N(8') 3.02(2) . 4_555 ? O(2) N(4) 2.845(9) . 4_454 ? O(2) N(4) 3.45(1) . 2_655 ? O(2) N(7) 3.452(9) . . ? O(2) N(5) 3.471(9) . 2_655 ? O(2) C(7) 3.54(1) . . ? O(2) C(4) 3.55(1) . 2_655 ? O(2) C(5) 3.574(9) . 2_655 ? N(2) N(7) 3.080(7) . 2_545 ? N(2) N(5) 3.103(7) . 2_645 ? N(5) N(7) 3.234(7) . 1_655 ? N(5) C(7') 3.52(4) . 1_655 ? N(5) C(8) 3.574(9) . 1_655 ? N(6) N(7) 3.122(8) . 2_645 ? #============================================================================== # End of CIF #==============================================================================