# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_General _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '5748_web_deposit_cif_file_0_NaohideMatsumoto_ #1307326485.FujiCIFall.cif' _audit_creation_date 2010-07-23 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Naohide Matsumoto' _publ_contact_author_email naohide@aster.sci.kumamoto-u.ac.jp _publ_contact_author_fax 81-96-342-3390 _publ_contact_author_phone 81-96-342-3390 _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_category 'CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Ladder- and Layer-Type Spin Crossover Iron(II) Complexes [Fe(HLn-Pr)3]ClY (HLn-Pr = (2-Methylimidazol-4-yl-methylideneamino-n- propyl, Y = AsF6, PF6, ClO4, BF4) ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_footnote _publ_author_address ; Department of Chemistry, Faculty of Science, Kumamoto University ; ; Kurokami 2-39-1, Kumamoto 860-8555 ; _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku Americas and Rigaku Corporation. (2007). CrystalStructure (Version 3.8). Single Crystal Structure Analysis Software. Rigaku Americas, 9009 TX, USA 77381-5209. Rigaku, Tokyo 196-8666, Japan. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M., Polidori, G., and Camalli, M. (1994) J. Appl. Cryst., 27, 435. SIR92 Carruthers, J.R., Rollett,J.S., Betteridge, P.W., Kinna, D., Pearce, L., Larsen, A., and Gabe, E.(1999) CRYSTALS Issue 11, Chemical Crystallography Laboratory, Oxford, UK. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; _publ_author_name T.Fujinami #============================================================================== data__FeHLAsF6 _database_code_depnum_ccdc_archive 'CCDC 828314' #TrackingRef '5748_web_deposit_cif_file_0_NaohideMatsumoto_ #1307326485.FujiCIFall.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H39 As Cl F6 Fe N9 ' _chemical_formula_moiety 'C24 H39 As Cl F6 Fe N9 ' _chemical_formula_weight 733.84 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 10.570(7) _cell_length_b 12.917(8) _cell_length_c 13.155(11) _cell_angle_alpha 86.77(3) _cell_angle_beta 72.56(3) _cell_angle_gamma 79.80(2) _cell_volume 1686(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7430 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 296.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752.00 _exptl_absorpt_coefficient_mu 1.562 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.305 _exptl_absorpt_correction_T_max 0.762 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 16700 _diffrn_reflns_av_R_equivalents 0.093 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_ambient_temperature 296.1 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 1.0 sigma(F^2^). 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 7669 _reflns_number_gt 2957 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0852 _refine_ls_wR_factor_ref 0.2319 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 4435 _refine_ls_number_parameters 418 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0047Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 2.24 _refine_diff_density_min -0.91 _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) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 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) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; As As 0.050 2.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ; 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 As(1) As 0.27001(12) 0.73302(9) 0.58584(9) 0.0866(4) Uani 1.00 1 d . . . Fe(1) Fe 0.89089(12) 0.73940(8) 0.25240(9) 0.0526(3) Uani 1.00 1 d . . . Cl(1) Cl 0.6764(2) 0.86524(16) 0.81899(17) 0.0640(6) Uani 1.00 1 d . . . F(1) F 0.1815(11) 0.6643(9) 0.5355(7) 0.210(5) Uani 1.00 1 d . . . F(2) F 0.3804(9) 0.6259(5) 0.5985(8) 0.160(3) Uani 1.00 1 d . . . F(3) F 0.3711(9) 0.7520(8) 0.4667(6) 0.174(3) Uani 1.00 1 d . . . F(4) F 0.3531(9) 0.8022(6) 0.6409(8) 0.165(3) Uani 1.00 1 d . . . F(5) F 0.1728(11) 0.8428(8) 0.5726(11) 0.233(5) Uani 1.00 1 d . . . F(6) F 0.1721(9) 0.7107(8) 0.7069(6) 0.178(4) Uani 1.00 1 d . . . N(1) N 0.7248(7) 0.7663(6) 0.5968(5) 0.071(2) Uani 1.00 1 d . . . N(2) N 0.8005(7) 0.7549(5) 0.4241(5) 0.059(2) Uani 1.00 1 d . . . N(3) N 0.7484(6) 0.6294(4) 0.2881(5) 0.056(2) Uani 1.00 1 d . . . N(4) N 1.1875(7) 0.9358(6) 0.2390(6) 0.074(2) Uani 1.00 1 d . . . N(5) N 1.0430(7) 0.8317(5) 0.2432(5) 0.059(2) Uani 1.00 1 d . . . N(6) N 1.0543(7) 0.6246(5) 0.2937(5) 0.062(2) Uani 1.00 1 d . . . N(7) N 0.5855(7) 0.9731(5) 0.1723(6) 0.074(2) Uani 1.00 1 d . . . N(8) N 0.7439(7) 0.8586(5) 0.2095(5) 0.060(2) Uani 1.00 1 d . . . N(9) N 0.9480(7) 0.7241(5) 0.0755(5) 0.059(2) Uani 1.00 1 d . . . C(1) C 0.6709(10) 0.6908(8) 0.5679(7) 0.076(3) Uani 1.00 1 d . . . C(2) C 0.8051(9) 0.8030(6) 0.5076(7) 0.065(2) Uani 1.00 1 d . . . C(3) C 0.8831(10) 0.8908(7) 0.5061(7) 0.087(3) Uani 1.00 1 d . . . C(4) C 0.7180(8) 0.6829(6) 0.4614(6) 0.059(2) Uani 1.00 1 d . . . C(5) C 0.6905(9) 0.6200(6) 0.3857(7) 0.063(3) Uani 1.00 1 d . . . C(6) C 0.7112(10) 0.5703(7) 0.2135(8) 0.081(3) Uani 1.00 1 d . . . C(7) C 0.5705(14) 0.6327(10) 0.1976(11) 0.132(5) Uani 1.00 1 d . . . C(8) C 0.5152(14) 0.5800(14) 0.1288(13) 0.166(7) Uani 1.00 1 d . . . C(9) C 1.2367(9) 0.8427(7) 0.2753(8) 0.078(3) Uani 1.00 1 d . . . C(10) C 1.0719(9) 0.9287(6) 0.2195(6) 0.062(2) Uani 1.00 1 d . . . C(11) C 0.9906(11) 1.0158(7) 0.1803(9) 0.091(3) Uani 1.00 1 d . . . C(12) C 1.1476(9) 0.7772(6) 0.2768(7) 0.064(2) Uani 1.00 1 d . . . C(13) C 1.1429(9) 0.6670(6) 0.3084(7) 0.065(2) Uani 1.00 1 d . . . C(14) C 1.0506(10) 0.5147(6) 0.3311(7) 0.073(3) Uani 1.00 1 d . . . C(15) C 1.0769(11) 0.4396(7) 0.2421(9) 0.096(4) Uani 1.00 1 d . . . C(16) C 1.2147(12) 0.4292(7) 0.1658(10) 0.109(4) Uani 1.00 1 d . . . C(17) C 0.6619(10) 0.9305(7) 0.0787(7) 0.074(3) Uani 1.00 1 d . . . C(18) C 0.6342(8) 0.9303(6) 0.2505(7) 0.059(2) Uani 1.00 1 d . . . C(19) C 0.5722(9) 0.9575(6) 0.3642(7) 0.077(3) Uani 1.00 1 d . . . C(20) C 0.7601(8) 0.8585(6) 0.1009(6) 0.062(2) Uani 1.00 1 d . . . C(21) C 0.8704(9) 0.7872(6) 0.0345(6) 0.062(2) Uani 1.00 1 d . . . C(22) C 1.0591(9) 0.6545(7) 0.0050(7) 0.075(3) Uani 1.00 1 d . . . C(23) C 1.1919(10) 0.6823(8) 0.0001(8) 0.093(3) Uani 1.00 1 d . . . C(24) C 1.2174(11) 0.7881(9) -0.0469(9) 0.110(4) Uani 1.00 1 d . . . H(1) H 0.7095 0.7913 0.6667 0.086 Uiso 1.00 1 c R . . H(2) H 1.2276 0.9973 0.2286 0.092 Uiso 1.00 1 c R . . H(3) H 0.5084 1.0266 0.1827 0.090 Uiso 1.00 1 c R . . H(4) H 0.6114 0.6494 0.6140 0.090 Uiso 1.00 1 c R . . H(5) H 0.8294 0.9560 0.4976 0.109 Uiso 1.00 1 c R . . H(6) H 0.9641 0.8812 0.4488 0.109 Uiso 1.00 1 c R . . H(7) H 0.9038 0.8907 0.5716 0.109 Uiso 1.00 1 c R . . H(8) H 0.6304 0.5710 0.4091 0.079 Uiso 1.00 1 c R . . H(9) H 0.7787 0.5632 0.1466 0.101 Uiso 1.00 1 c R . . H(10) H 0.6979 0.5025 0.2421 0.101 Uiso 1.00 1 c R . . H(11) H 0.5048 0.6396 0.2655 0.170 Uiso 1.00 1 c R . . H(12) H 0.5856 0.7005 0.1702 0.170 Uiso 1.00 1 c R . . H(13) H 0.5511 0.6039 0.0580 0.209 Uiso 1.00 1 c R . . H(14) H 0.4198 0.5963 0.1490 0.208 Uiso 1.00 1 c R . . H(15) H 0.5423 0.5061 0.1322 0.209 Uiso 1.00 1 c R . . H(16) H 1.3176 0.8257 0.2948 0.098 Uiso 1.00 1 c R . . H(17) H 0.9281 1.0548 0.2388 0.109 Uiso 1.00 1 c R . . H(18) H 0.9433 0.9888 0.1396 0.109 Uiso 1.00 1 c R . . H(19) H 1.0476 1.0604 0.1368 0.109 Uiso 1.00 1 c R . . H(20) H 1.2076 0.6299 0.3399 0.079 Uiso 1.00 1 c R . . H(21) H 1.1151 0.4942 0.3686 0.086 Uiso 1.00 1 c R . . H(22) H 0.9631 0.5118 0.3777 0.086 Uiso 1.00 1 c R . . H(23) H 1.0629 0.3717 0.2701 0.116 Uiso 1.00 1 c R . . H(24) H 1.0155 0.4643 0.2026 0.116 Uiso 1.00 1 c R . . H(25) H 1.2169 0.4806 0.1110 0.124 Uiso 1.00 1 c R . . H(26) H 1.2411 0.3609 0.1351 0.124 Uiso 1.00 1 c R . . H(27) H 1.2749 0.4398 0.2039 0.124 Uiso 1.00 1 c R . . H(28) H 0.6507 0.9473 0.0103 0.091 Uiso 1.00 1 c R . . H(29) H 0.6109 1.0131 0.3804 0.091 Uiso 1.00 1 c R . . H(30) H 0.5887 0.8979 0.4070 0.091 Uiso 1.00 1 c R . . H(31) H 0.4780 0.9795 0.3782 0.091 Uiso 1.00 1 c R . . H(32) H 0.8854 0.7879 -0.0404 0.075 Uiso 1.00 1 c R . . H(33) H 1.0567 0.5832 0.0266 0.089 Uiso 1.00 1 c R . . H(34) H 1.0499 0.6634 -0.0647 0.089 Uiso 1.00 1 c R . . H(35) H 1.1960 0.6823 0.0713 0.106 Uiso 1.00 1 c R . . H(36) H 1.2621 0.6308 -0.0400 0.106 Uiso 1.00 1 c R . . H(37) H 1.2594 0.7808 -0.1214 0.131 Uiso 1.00 1 c R . . H(38) H 1.2722 0.8188 -0.0157 0.131 Uiso 1.00 1 c R . . H(39) H 1.1321 0.8319 -0.0343 0.131 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 As(1) 0.0954(9) 0.0862(8) 0.0836(8) -0.0240(6) -0.0300(6) 0.0030(6) Fe(1) 0.0610(7) 0.0517(6) 0.0498(7) -0.0119(5) -0.0212(6) -0.0035(5) Cl(1) 0.0772(15) 0.0579(12) 0.0609(14) -0.0107(10) -0.0255(11) -0.0080(10) F(1) 0.225(10) 0.315(13) 0.143(8) -0.156(10) -0.058(7) -0.052(7) F(2) 0.173(7) 0.094(4) 0.223(9) -0.027(4) -0.075(7) 0.029(5) F(3) 0.157(7) 0.242(9) 0.110(6) -0.070(7) -0.010(5) 0.055(6) F(4) 0.179(7) 0.139(6) 0.221(9) -0.075(5) -0.092(7) -0.028(5) F(5) 0.205(10) 0.166(8) 0.328(15) 0.069(7) -0.133(10) -0.002(8) F(6) 0.167(7) 0.288(11) 0.093(5) -0.119(8) -0.014(5) 0.011(6) N(1) 0.082(5) 0.090(5) 0.043(4) -0.017(4) -0.021(4) -0.010(3) N(2) 0.071(4) 0.058(3) 0.053(4) -0.015(3) -0.024(3) -0.004(3) N(3) 0.063(4) 0.063(4) 0.051(4) -0.020(3) -0.022(3) -0.004(3) N(4) 0.074(5) 0.072(5) 0.085(5) -0.030(4) -0.026(4) -0.010(4) N(5) 0.075(4) 0.054(4) 0.051(4) -0.013(3) -0.021(3) -0.002(3) N(6) 0.064(4) 0.056(4) 0.069(5) -0.012(3) -0.022(3) 0.002(3) N(7) 0.078(5) 0.073(4) 0.073(5) 0.003(4) -0.034(4) -0.003(4) N(8) 0.075(4) 0.058(4) 0.051(4) -0.016(3) -0.022(3) -0.001(3) N(9) 0.069(4) 0.058(4) 0.055(4) -0.014(3) -0.020(3) -0.009(3) C(1) 0.077(6) 0.090(6) 0.058(6) -0.014(5) -0.016(5) 0.007(5) C(2) 0.080(6) 0.063(5) 0.050(5) 0.007(4) -0.026(5) -0.014(4) C(3) 0.108(8) 0.093(7) 0.070(7) -0.033(6) -0.028(6) -0.022(5) C(4) 0.059(5) 0.068(5) 0.048(5) -0.007(4) -0.014(4) -0.001(4) C(5) 0.071(6) 0.058(5) 0.069(6) -0.018(4) -0.030(5) 0.000(4) C(6) 0.097(7) 0.079(6) 0.077(7) -0.024(5) -0.034(6) -0.016(5) C(7) 0.146(11) 0.139(10) 0.141(12) 0.000(9) -0.092(10) -0.057(9) C(8) 0.108(11) 0.238(18) 0.175(16) -0.039(11) -0.060(10) -0.056(13) C(9) 0.066(6) 0.070(6) 0.108(8) -0.017(5) -0.035(5) -0.015(5) C(10) 0.075(6) 0.064(5) 0.052(5) -0.019(4) -0.022(4) -0.001(4) C(11) 0.104(8) 0.067(6) 0.102(8) -0.026(5) -0.025(6) 0.010(5) C(12) 0.072(6) 0.067(5) 0.060(5) -0.003(4) -0.032(4) -0.011(4) C(13) 0.061(5) 0.065(5) 0.070(6) -0.004(4) -0.025(4) 0.004(4) C(14) 0.086(7) 0.059(5) 0.071(6) 0.000(4) -0.024(5) 0.002(4) C(15) 0.111(9) 0.063(6) 0.116(9) -0.027(6) -0.033(7) 0.010(6) C(16) 0.126(9) 0.053(5) 0.131(10) -0.007(6) -0.019(8) 0.002(5) C(17) 0.088(6) 0.078(6) 0.061(6) -0.000(5) -0.034(5) -0.006(5) C(18) 0.057(5) 0.060(5) 0.062(5) -0.013(4) -0.016(4) -0.005(4) C(19) 0.083(6) 0.070(5) 0.073(6) -0.005(5) -0.021(5) -0.011(4) C(20) 0.072(5) 0.064(5) 0.052(5) -0.007(4) -0.025(4) -0.001(4) C(21) 0.079(6) 0.071(5) 0.037(4) -0.023(5) -0.013(4) -0.007(4) C(22) 0.080(6) 0.072(6) 0.072(6) -0.013(5) -0.016(5) -0.018(5) C(23) 0.086(7) 0.108(8) 0.071(7) 0.016(6) -0.019(5) -0.023(6) C(24) 0.109(9) 0.122(9) 0.096(9) -0.043(7) -0.015(7) 0.008(7) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _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 As(1) F(1) 1.684(13) yes . . As(1) F(2) 1.680(8) yes . . As(1) F(3) 1.645(8) yes . . As(1) F(4) 1.681(11) yes . . As(1) F(5) 1.631(10) yes . . As(1) F(6) 1.660(7) yes . . Fe(1) N(2) 2.178(6) yes . . Fe(1) N(3) 2.183(7) yes . . Fe(1) N(5) 2.138(7) yes . . Fe(1) N(6) 2.245(7) yes . . Fe(1) N(8) 2.164(7) yes . . Fe(1) N(9) 2.233(7) yes . . N(1) C(1) 1.337(14) yes . . N(1) C(2) 1.343(11) yes . . N(2) C(2) 1.309(12) yes . . N(2) C(4) 1.359(11) yes . . N(3) C(5) 1.256(11) yes . . N(3) C(6) 1.457(14) yes . . N(4) C(9) 1.344(12) yes . . N(4) C(10) 1.340(14) yes . . N(5) C(10) 1.339(11) yes . . N(5) C(12) 1.377(12) yes . . N(6) C(13) 1.231(13) yes . . N(6) C(14) 1.480(10) yes . . N(7) C(17) 1.341(11) yes . . N(7) C(18) 1.335(13) yes . . N(8) C(18) 1.340(9) yes . . N(8) C(20) 1.388(11) yes . . N(9) C(21) 1.268(11) yes . . N(9) C(22) 1.454(10) yes . . C(1) C(4) 1.342(12) yes . . C(2) C(3) 1.512(15) yes . . C(4) C(5) 1.444(14) yes . . C(6) C(7) 1.628(18) yes . . C(7) C(8) 1.47(2) yes . . C(9) C(12) 1.369(15) yes . . C(10) C(11) 1.459(13) yes . . C(12) C(13) 1.465(12) yes . . C(14) C(15) 1.493(15) yes . . C(15) C(16) 1.489(15) yes . . C(17) C(20) 1.355(13) yes . . C(18) C(19) 1.476(12) yes . . C(20) C(21) 1.439(10) yes . . C(22) C(23) 1.492(16) yes . . C(23) C(24) 1.502(16) yes . . N(1) H(1) 0.950 no . . N(4) H(2) 0.950 no . . N(7) H(3) 0.950 no . . C(1) H(4) 0.950 no . . C(3) H(5) 0.950 no . . C(3) H(6) 0.950 no . . C(3) H(7) 0.950 no . . C(5) H(8) 0.950 no . . C(6) H(9) 0.950 no . . C(6) H(10) 0.950 no . . C(7) H(11) 0.950 no . . C(7) H(12) 0.950 no . . C(8) H(13) 0.950 no . . C(8) H(14) 0.950 no . . C(8) H(15) 0.950 no . . C(9) H(16) 0.950 no . . C(11) H(17) 0.950 no . . C(11) H(18) 0.950 no . . C(11) H(19) 0.950 no . . C(13) H(20) 0.950 no . . C(14) H(21) 0.950 no . . C(14) H(22) 0.950 no . . C(15) H(23) 0.950 no . . C(15) H(24) 0.950 no . . C(16) H(25) 0.950 no . . C(16) H(26) 0.950 no . . C(16) H(27) 0.950 no . . C(17) H(28) 0.950 no . . C(19) H(29) 0.950 no . . C(19) H(30) 0.950 no . . C(19) H(31) 0.950 no . . C(21) H(32) 0.950 no . . C(22) H(33) 0.950 no . . C(22) H(34) 0.950 no . . C(23) H(35) 0.950 no . . C(23) H(36) 0.950 no . . C(24) H(37) 0.950 no . . C(24) H(38) 0.950 no . . C(24) H(39) 0.950 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 F(1) As(1) F(2) 93.3(5) yes . . . F(1) As(1) F(3) 91.9(5) yes . . . F(1) As(1) F(4) 177.6(4) yes . . . F(1) As(1) F(5) 91.0(6) yes . . . F(1) As(1) F(6) 88.6(5) yes . . . F(2) As(1) F(3) 88.7(4) yes . . . F(2) As(1) F(4) 87.4(4) yes . . . F(2) As(1) F(5) 175.2(5) yes . . . F(2) As(1) F(6) 89.4(4) yes . . . F(3) As(1) F(4) 90.4(5) yes . . . F(3) As(1) F(5) 89.0(5) yes . . . F(3) As(1) F(6) 178.0(4) yes . . . F(4) As(1) F(5) 88.4(5) yes . . . F(4) As(1) F(6) 89.1(5) yes . . . F(5) As(1) F(6) 92.9(5) yes . . . N(2) Fe(1) N(3) 77.0(2) yes . . . N(2) Fe(1) N(5) 95.4(2) yes . . . N(2) Fe(1) N(6) 85.0(2) yes . . . N(2) Fe(1) N(8) 96.1(2) yes . . . N(2) Fe(1) N(9) 170.3(3) yes . . . N(3) Fe(1) N(5) 168.5(2) yes . . . N(3) Fe(1) N(6) 94.3(2) yes . . . N(3) Fe(1) N(8) 90.1(2) yes . . . N(3) Fe(1) N(9) 95.9(2) yes . . . N(5) Fe(1) N(6) 76.4(2) yes . . . N(5) Fe(1) N(8) 99.3(2) yes . . . N(5) Fe(1) N(9) 92.5(2) yes . . . N(6) Fe(1) N(8) 175.6(2) yes . . . N(6) Fe(1) N(9) 102.3(2) yes . . . N(8) Fe(1) N(9) 77.2(2) yes . . . C(1) N(1) C(2) 107.4(8) yes . . . Fe(1) N(2) C(2) 142.6(6) yes . . . Fe(1) N(2) C(4) 110.5(5) yes . . . C(2) N(2) C(4) 106.5(7) yes . . . Fe(1) N(3) C(5) 113.9(6) yes . . . Fe(1) N(3) C(6) 128.2(5) yes . . . C(5) N(3) C(6) 117.9(7) yes . . . C(9) N(4) C(10) 109.3(8) yes . . . Fe(1) N(5) C(10) 141.9(6) yes . . . Fe(1) N(5) C(12) 112.4(5) yes . . . C(10) N(5) C(12) 105.6(8) yes . . . Fe(1) N(6) C(13) 113.1(5) yes . . . Fe(1) N(6) C(14) 128.0(6) yes . . . C(13) N(6) C(14) 116.8(8) yes . . . C(17) N(7) C(18) 109.9(7) yes . . . Fe(1) N(8) C(18) 143.0(6) yes . . . Fe(1) N(8) C(20) 111.4(4) yes . . . C(18) N(8) C(20) 105.4(7) yes . . . Fe(1) N(9) C(21) 112.6(5) yes . . . Fe(1) N(9) C(22) 129.1(6) yes . . . C(21) N(9) C(22) 118.2(7) yes . . . N(1) C(1) C(4) 107.3(8) yes . . . N(1) C(2) N(2) 110.2(8) yes . . . N(1) C(2) C(3) 123.8(8) yes . . . N(2) C(2) C(3) 126.0(7) yes . . . N(2) C(4) C(1) 108.7(8) yes . . . N(2) C(4) C(5) 118.7(7) yes . . . C(1) C(4) C(5) 132.5(9) yes . . . N(3) C(5) C(4) 119.4(8) yes . . . N(3) C(6) C(7) 108.3(8) yes . . . C(6) C(7) C(8) 115.1(10) yes . . . N(4) C(9) C(12) 105.9(9) yes . . . N(4) C(10) N(5) 109.9(7) yes . . . N(4) C(10) C(11) 123.9(8) yes . . . N(5) C(10) C(11) 126.2(9) yes . . . N(5) C(12) C(9) 109.4(7) yes . . . N(5) C(12) C(13) 117.7(8) yes . . . C(9) C(12) C(13) 132.9(9) yes . . . N(6) C(13) C(12) 119.0(9) yes . . . N(6) C(14) C(15) 112.6(7) yes . . . C(14) C(15) C(16) 114.5(10) yes . . . N(7) C(17) C(20) 106.0(9) yes . . . N(7) C(18) N(8) 109.4(7) yes . . . N(7) C(18) C(19) 124.1(7) yes . . . N(8) C(18) C(19) 126.5(8) yes . . . N(8) C(20) C(17) 109.3(7) yes . . . N(8) C(20) C(21) 118.5(7) yes . . . C(17) C(20) C(21) 132.3(8) yes . . . N(9) C(21) C(20) 120.3(7) yes . . . N(9) C(22) C(23) 111.9(8) yes . . . C(22) C(23) C(24) 116.1(9) yes . . . 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 Cl(1) N(1) 3.120(8) ? . . Cl(1) N(4) 3.113(8) ? . 2_776 Cl(1) N(7) 3.134(7) ? . 2_676 Cl(1) C(17) 3.517(11) ? . 1_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 #============================================================================== #===END #============================================================================== data__2Me-AsF6-110K _database_code_depnum_ccdc_archive 'CCDC 828315' #TrackingRef '5748_web_deposit_cif_file_0_NaohideMatsumoto_ #1307326485.FujiCIFall.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H39 As Cl F6 Fe N9 ' _chemical_formula_moiety 'C24 H39 As Cl F6 Fe N9 ' _chemical_formula_weight 733.84 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 10.369(2) _cell_length_b 12.897(2) _cell_length_c 12.941(2) _cell_angle_alpha 85.380(14) _cell_angle_beta 69.340(16) _cell_angle_gamma 76.590(16) _cell_volume 1575.1(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 10303 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 110.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.27 _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752.00 _exptl_absorpt_coefficient_mu 1.672 _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 0.548 _exptl_absorpt_correction_T_max 0.639 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 14404 _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.961 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_ambient_temperature 110.1 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 1.0 sigma(F^2^). 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 6949 _reflns_number_gt 4505 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0992 _refine_ls_wR_factor_ref 0.3053 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 5547 _refine_ls_number_parameters 418 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0137Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 5.27 _refine_diff_density_min -1.81 _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) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; As As 0.050 2.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 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) ; #============================================================================== # 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 As(1) As 0.25043(9) 0.73037(6) 0.60744(6) 0.0320(2) Uani 1.00 1 d . . . Fe(1) Fe 0.92600(11) 0.73051(8) 0.24777(8) 0.0241(2) Uani 1.00 1 d . . . Cl(1) Cl 0.66245(19) 0.87217(14) 0.81468(14) 0.0293(4) Uani 1.00 1 d . . . F(1) F 0.1692(5) 0.6485(4) 0.5649(4) 0.0480(15) Uani 1.00 1 d . . . F(2) F 0.3694(5) 0.6201(3) 0.6277(4) 0.0420(13) Uani 1.00 1 d . . . F(3) F 0.3614(5) 0.7380(4) 0.4743(3) 0.0490(15) Uani 1.00 1 d . . . F(4) F 0.3315(5) 0.8128(3) 0.6517(4) 0.0456(14) Uani 1.00 1 d . . . F(5) F 0.1347(5) 0.8386(4) 0.5850(5) 0.0575(17) Uani 1.00 1 d . . . F(6) F 0.1384(5) 0.7231(4) 0.7437(4) 0.0442(14) Uani 1.00 1 d . . . N(1) N 0.7081(7) 0.7733(5) 0.5858(5) 0.0325(17) Uani 1.00 1 d . . . N(2) N 0.8167(6) 0.7522(4) 0.4107(4) 0.0252(15) Uani 1.00 1 d . . . N(3) N 0.8065(6) 0.6240(4) 0.2670(5) 0.0260(15) Uani 1.00 1 d . . . N(4) N 1.1746(7) 0.9438(5) 0.2468(6) 0.0392(19) Uani 1.00 1 d . . . N(5) N 1.0501(6) 0.8270(5) 0.2440(5) 0.0284(16) Uani 1.00 1 d . . . N(6) N 1.0757(6) 0.6242(4) 0.2948(4) 0.0264(15) Uani 1.00 1 d . . . N(7) N 0.6178(6) 0.9581(5) 0.1628(5) 0.0326(17) Uani 1.00 1 d . . . N(8) N 0.7836(6) 0.8392(4) 0.2030(4) 0.0261(15) Uani 1.00 1 d . . . N(9) N 1.0117(6) 0.7161(5) 0.0863(5) 0.0272(15) Uani 1.00 1 d . . . C(1) C 0.6570(8) 0.6955(6) 0.5596(6) 0.0298(19) Uani 1.00 1 d . . . C(2) C 0.8029(8) 0.8063(6) 0.4942(5) 0.0296(19) Uani 1.00 1 d . . . C(3) C 0.8785(10) 0.8920(7) 0.4958(6) 0.039(2) Uani 1.00 1 d . . . C(4) C 0.7273(7) 0.6817(5) 0.4491(5) 0.0264(18) Uani 1.00 1 d . . . C(5) C 0.7252(8) 0.6114(6) 0.3644(6) 0.032(2) Uani 1.00 1 d . . . C(6) C 0.8037(8) 0.5589(5) 0.1826(6) 0.0296(19) Uani 1.00 1 d . . . C(7) C 0.6901(8) 0.6132(6) 0.1319(6) 0.034(2) Uani 1.00 1 d . . . C(8) C 0.5400(10) 0.6202(9) 0.2079(8) 0.058(3) Uani 1.00 1 d . . . C(9) C 1.2347(9) 0.8513(7) 0.2869(8) 0.043(2) Uani 1.00 1 d . . . C(10) C 1.0618(8) 0.9286(6) 0.2257(6) 0.0291(18) Uani 1.00 1 d . . . C(11) C 0.9703(9) 1.0168(6) 0.1829(8) 0.043(2) Uani 1.00 1 d . . . C(12) C 1.1599(7) 0.7781(6) 0.2828(6) 0.0286(19) Uani 1.00 1 d . . . C(13) C 1.1647(7) 0.6670(6) 0.3137(6) 0.0287(18) Uani 1.00 1 d . . . C(14) C 1.0735(8) 0.5120(5) 0.3303(6) 0.0306(19) Uani 1.00 1 d . . . C(15) C 1.1395(9) 0.4337(6) 0.2393(7) 0.041(2) Uani 1.00 1 d . . . C(16) C 1.2986(8) 0.4207(7) 0.1755(7) 0.040(2) Uani 1.00 1 d . . . C(17) C 0.7141(8) 0.9180(6) 0.0652(6) 0.0312(19) Uani 1.00 1 d . . . C(18) C 0.6612(8) 0.9117(6) 0.2486(6) 0.032(2) Uani 1.00 1 d . . . C(19) C 0.5794(8) 0.9392(6) 0.3666(5) 0.0321(19) Uani 1.00 1 d . . . C(20) C 0.8182(8) 0.8454(5) 0.0894(5) 0.0272(18) Uani 1.00 1 d . . . C(21) C 0.9445(8) 0.7746(5) 0.0272(6) 0.0297(19) Uani 1.00 1 d . . . C(22) C 1.1478(7) 0.6409(5) 0.0171(6) 0.0279(18) Uani 1.00 1 d . . . C(23) C 1.2784(9) 0.6811(6) 0.0075(7) 0.038(2) Uani 1.00 1 d . . . C(24) C 1.2866(10) 0.7874(8) -0.0537(8) 0.054(3) Uani 1.00 1 d . . . H(1) H 0.6811 0.8012 0.6579 0.041 Uiso 1.00 1 c R . . H(2) H 1.2060 1.0087 0.2371 0.050 Uiso 1.00 1 c R . . H(3) H 0.5326 1.0096 0.1717 0.040 Uiso 1.00 1 c R . . H(4) H 0.5887 0.6591 0.6073 0.036 Uiso 1.00 1 c R . . H(5) H 0.8238 0.9585 0.4830 0.051 Uiso 1.00 1 c R . . H(6) H 0.9691 0.8794 0.4397 0.051 Uiso 1.00 1 c R . . H(7) H 0.8886 0.8933 0.5658 0.051 Uiso 1.00 1 c R . . H(8) H 0.6676 0.5605 0.3819 0.040 Uiso 1.00 1 c R . . H(9) H 0.8933 0.5460 0.1253 0.034 Uiso 1.00 1 c R . . H(10) H 0.7833 0.4931 0.2148 0.034 Uiso 1.00 1 c R . . H(11) H 0.7031 0.6832 0.1098 0.043 Uiso 1.00 1 c R . . H(12) H 0.7040 0.5732 0.0689 0.043 Uiso 1.00 1 c R . . H(13) H 0.5089 0.5584 0.2003 0.070 Uiso 1.00 1 c R . . H(14) H 0.4815 0.6815 0.1893 0.070 Uiso 1.00 1 c R . . H(15) H 0.5347 0.6259 0.2821 0.070 Uiso 1.00 1 c R . . H(16) H 1.3135 0.8395 0.3109 0.054 Uiso 1.00 1 c R . . H(17) H 0.8957 1.0543 0.2432 0.054 Uiso 1.00 1 c R . . H(18) H 0.9320 0.9878 0.1380 0.054 Uiso 1.00 1 c R . . H(19) H 1.0263 1.0644 0.1403 0.054 Uiso 1.00 1 c R . . H(20) H 1.2303 0.6279 0.3462 0.035 Uiso 1.00 1 c R . . H(21) H 1.1242 0.4945 0.3801 0.036 Uiso 1.00 1 c R . . H(22) H 0.9781 0.5069 0.3673 0.036 Uiso 1.00 1 c R . . H(23) H 1.1245 0.3663 0.2703 0.053 Uiso 1.00 1 c R . . H(24) H 1.0913 0.4536 0.1880 0.053 Uiso 1.00 1 c R . . H(25) H 1.3121 0.4685 0.1148 0.052 Uiso 1.00 1 c R . . H(26) H 1.3378 0.3496 0.1492 0.052 Uiso 1.00 1 c R . . H(27) H 1.3440 0.4362 0.2228 0.052 Uiso 1.00 1 c R . . H(28) H 0.7108 0.9378 -0.0063 0.037 Uiso 1.00 1 c R . . H(29) H 0.6096 0.9963 0.3866 0.037 Uiso 1.00 1 c R . . H(30) H 0.5952 0.8790 0.4115 0.037 Uiso 1.00 1 c R . . H(31) H 0.4816 0.9602 0.3771 0.037 Uiso 1.00 1 c R . . H(32) H 0.9770 0.7704 -0.0511 0.039 Uiso 1.00 1 c R . . H(33) H 1.1527 0.5729 0.0516 0.032 Uiso 1.00 1 c R . . H(34) H 1.1448 0.6348 -0.0546 0.032 Uiso 1.00 1 c R . . H(35) H 1.2772 0.6915 0.0796 0.047 Uiso 1.00 1 c R . . H(36) H 1.3592 0.6281 -0.0297 0.047 Uiso 1.00 1 c R . . H(37) H 1.3361 0.7725 -0.1300 0.072 Uiso 1.00 1 c R . . H(38) H 1.3358 0.8260 -0.0268 0.072 Uiso 1.00 1 c R . . H(39) H 1.1944 0.8286 -0.0439 0.072 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 As(1) 0.0324(5) 0.0323(4) 0.0334(4) -0.0124(3) -0.0110(3) 0.0010(3) Fe(1) 0.0246(6) 0.0247(5) 0.0250(5) -0.0105(4) -0.0075(4) 0.0001(4) Cl(1) 0.0304(10) 0.0289(9) 0.0302(9) -0.0104(7) -0.0092(7) -0.0032(7) F(1) 0.052(3) 0.058(3) 0.046(2) -0.028(2) -0.017(2) -0.017(2) F(2) 0.038(2) 0.032(2) 0.053(2) -0.011(2) -0.009(2) 0.000(2) F(3) 0.050(3) 0.057(3) 0.034(2) -0.024(2) 0.001(2) 0.000(2) F(4) 0.043(3) 0.040(2) 0.063(3) -0.023(2) -0.024(2) 0.014(2) F(5) 0.046(3) 0.054(3) 0.078(4) -0.013(2) -0.032(3) 0.023(3) F(6) 0.037(2) 0.051(2) 0.043(2) -0.022(2) -0.007(2) 0.009(2) N(1) 0.028(3) 0.042(3) 0.031(3) -0.018(2) -0.009(2) 0.004(3) N(2) 0.025(3) 0.024(2) 0.026(2) -0.009(2) -0.004(2) -0.007(2) N(3) 0.021(3) 0.024(2) 0.033(3) -0.009(2) -0.005(2) -0.004(2) N(4) 0.041(4) 0.030(3) 0.053(4) -0.019(3) -0.020(3) 0.007(3) N(5) 0.024(3) 0.029(3) 0.033(3) -0.009(2) -0.007(2) -0.003(2) N(6) 0.026(3) 0.027(3) 0.025(2) -0.009(2) -0.004(2) -0.004(2) N(7) 0.028(3) 0.035(3) 0.037(3) -0.011(2) -0.011(2) -0.003(3) N(8) 0.028(3) 0.028(3) 0.024(2) -0.011(2) -0.006(2) -0.007(2) N(9) 0.023(3) 0.028(3) 0.031(3) -0.013(2) -0.005(2) -0.002(2) C(1) 0.023(3) 0.040(4) 0.026(3) -0.015(3) -0.002(3) -0.005(3) C(2) 0.034(4) 0.029(3) 0.024(3) -0.004(3) -0.006(3) -0.013(3) C(3) 0.059(6) 0.045(4) 0.024(3) -0.025(4) -0.016(3) -0.013(3) C(4) 0.021(3) 0.033(3) 0.027(3) -0.016(2) -0.005(2) 0.007(3) C(5) 0.027(4) 0.031(3) 0.041(4) -0.016(3) -0.014(3) 0.011(3) C(6) 0.029(4) 0.025(3) 0.031(3) -0.003(2) -0.007(3) -0.004(3) C(7) 0.034(4) 0.040(4) 0.035(3) -0.015(3) -0.014(3) 0.001(3) C(8) 0.038(5) 0.082(7) 0.055(5) 0.003(5) -0.021(4) -0.033(5) C(9) 0.029(4) 0.043(4) 0.063(5) -0.021(3) -0.018(4) 0.020(4) C(10) 0.028(4) 0.025(3) 0.034(3) -0.006(2) -0.009(3) -0.007(3) C(11) 0.040(5) 0.032(4) 0.064(5) -0.019(3) -0.021(4) 0.012(4) C(12) 0.021(3) 0.037(4) 0.034(3) -0.020(3) -0.008(3) 0.005(3) C(13) 0.018(3) 0.033(3) 0.036(3) -0.012(2) -0.008(3) 0.007(3) C(14) 0.028(4) 0.026(3) 0.037(3) -0.010(3) -0.009(3) 0.007(3) C(15) 0.056(5) 0.029(4) 0.048(4) -0.012(3) -0.029(4) 0.014(3) C(16) 0.037(4) 0.040(4) 0.053(5) -0.018(3) -0.023(4) 0.011(4) C(17) 0.040(4) 0.030(3) 0.022(3) -0.002(3) -0.009(3) -0.011(3) C(18) 0.032(4) 0.030(3) 0.038(4) -0.012(3) -0.016(3) 0.005(3) C(19) 0.036(4) 0.031(3) 0.025(3) -0.003(3) -0.007(3) -0.011(3) C(20) 0.041(4) 0.026(3) 0.017(3) -0.014(3) -0.007(3) -0.005(2) C(21) 0.038(4) 0.025(3) 0.033(3) -0.015(3) -0.018(3) 0.008(3) C(22) 0.025(3) 0.026(3) 0.029(3) -0.003(2) -0.006(3) -0.007(3) C(23) 0.034(4) 0.037(4) 0.046(4) -0.015(3) -0.014(3) 0.010(4) C(24) 0.048(5) 0.061(6) 0.069(6) -0.039(4) -0.030(5) 0.036(5) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _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 As(1) F(1) 1.720(6) yes . . As(1) F(2) 1.723(4) yes . . As(1) F(3) 1.711(4) yes . . As(1) F(4) 1.737(6) yes . . As(1) F(5) 1.696(5) yes . . As(1) F(6) 1.745(4) yes . . Fe(1) N(2) 2.018(5) yes . . Fe(1) N(3) 2.000(7) yes . . Fe(1) N(5) 1.975(7) yes . . Fe(1) N(6) 2.050(6) yes . . Fe(1) N(8) 1.998(6) yes . . Fe(1) N(9) 1.966(5) yes . . N(1) C(1) 1.353(12) yes . . N(1) C(2) 1.357(9) yes . . N(2) C(2) 1.281(10) yes . . N(2) C(4) 1.388(10) yes . . N(3) C(5) 1.267(8) yes . . N(3) C(6) 1.442(11) yes . . N(4) C(9) 1.366(11) yes . . N(4) C(10) 1.349(13) yes . . N(5) C(10) 1.337(10) yes . . N(5) C(12) 1.402(11) yes . . N(6) C(13) 1.279(12) yes . . N(6) C(14) 1.485(9) yes . . N(7) C(17) 1.355(8) yes . . N(7) C(18) 1.384(11) yes . . N(8) C(18) 1.358(8) yes . . N(8) C(20) 1.386(9) yes . . N(9) C(21) 1.296(10) yes . . N(9) C(22) 1.531(8) yes . . C(1) C(4) 1.361(9) yes . . C(2) C(3) 1.501(14) yes . . C(4) C(5) 1.486(12) yes . . C(6) C(7) 1.548(12) yes . . C(7) C(8) 1.505(11) yes . . C(9) C(12) 1.368(14) yes . . C(10) C(11) 1.507(12) yes . . C(12) C(13) 1.450(11) yes . . C(14) C(15) 1.476(11) yes . . C(15) C(16) 1.538(11) yes . . C(17) C(20) 1.364(11) yes . . C(18) C(19) 1.486(10) yes . . C(20) C(21) 1.421(9) yes . . C(22) C(23) 1.521(13) yes . . C(23) C(24) 1.532(13) yes . . N(1) H(1) 0.950 no . . N(4) H(2) 0.950 no . . N(7) H(3) 0.950 no . . C(1) H(4) 0.950 no . . C(3) H(5) 0.950 no . . C(3) H(6) 0.950 no . . C(3) H(7) 0.950 no . . C(5) H(8) 0.950 no . . C(6) H(9) 0.950 no . . C(6) H(10) 0.950 no . . C(7) H(11) 0.950 no . . C(7) H(12) 0.950 no . . C(8) H(13) 0.950 no . . C(8) H(14) 0.950 no . . C(8) H(15) 0.950 no . . C(9) H(16) 0.950 no . . C(11) H(17) 0.950 no . . C(11) H(18) 0.950 no . . C(11) H(19) 0.950 no . . C(13) H(20) 0.950 no . . C(14) H(21) 0.950 no . . C(14) H(22) 0.950 no . . C(15) H(23) 0.950 no . . C(15) H(24) 0.950 no . . C(16) H(25) 0.950 no . . C(16) H(26) 0.950 no . . C(16) H(27) 0.950 no . . C(17) H(28) 0.950 no . . C(19) H(29) 0.950 no . . C(19) H(30) 0.950 no . . C(19) H(31) 0.950 no . . C(21) H(32) 0.950 no . . C(22) H(33) 0.950 no . . C(22) H(34) 0.950 no . . C(23) H(35) 0.950 no . . C(23) H(36) 0.950 no . . C(24) H(37) 0.950 no . . C(24) H(38) 0.950 no . . C(24) H(39) 0.950 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 F(1) As(1) F(2) 89.7(2) yes . . . F(1) As(1) F(3) 89.9(2) yes . . . F(1) As(1) F(4) 179.5(2) yes . . . F(1) As(1) F(5) 90.0(3) yes . . . F(1) As(1) F(6) 90.7(2) yes . . . F(2) As(1) F(3) 89.4(2) yes . . . F(2) As(1) F(4) 90.3(2) yes . . . F(2) As(1) F(5) 179.0(2) yes . . . F(2) As(1) F(6) 90.5(2) yes . . . F(3) As(1) F(4) 90.7(2) yes . . . F(3) As(1) F(5) 89.7(2) yes . . . F(3) As(1) F(6) 179.4(3) yes . . . F(4) As(1) F(5) 90.1(3) yes . . . F(4) As(1) F(6) 88.8(2) yes . . . F(5) As(1) F(6) 90.5(2) yes . . . N(2) Fe(1) N(3) 81.8(2) yes . . . N(2) Fe(1) N(5) 93.9(2) yes . . . N(2) Fe(1) N(6) 85.9(2) yes . . . N(2) Fe(1) N(8) 93.7(2) yes . . . N(2) Fe(1) N(9) 173.4(2) yes . . . N(3) Fe(1) N(5) 173.0(2) yes . . . N(3) Fe(1) N(6) 93.0(2) yes . . . N(3) Fe(1) N(8) 89.4(2) yes . . . N(3) Fe(1) N(9) 95.5(2) yes . . . N(5) Fe(1) N(6) 81.2(2) yes . . . N(5) Fe(1) N(8) 96.4(2) yes . . . N(5) Fe(1) N(9) 89.4(2) yes . . . N(6) Fe(1) N(8) 177.5(3) yes . . . N(6) Fe(1) N(9) 100.3(2) yes . . . N(8) Fe(1) N(9) 80.2(2) yes . . . C(1) N(1) C(2) 110.4(6) yes . . . Fe(1) N(2) C(2) 142.4(5) yes . . . Fe(1) N(2) C(4) 110.7(5) yes . . . C(2) N(2) C(4) 106.8(5) yes . . . Fe(1) N(3) C(5) 116.5(6) yes . . . Fe(1) N(3) C(6) 127.3(4) yes . . . C(5) N(3) C(6) 116.3(7) yes . . . C(9) N(4) C(10) 108.9(7) yes . . . Fe(1) N(5) C(10) 142.1(6) yes . . . Fe(1) N(5) C(12) 112.4(5) yes . . . C(10) N(5) C(12) 105.1(7) yes . . . Fe(1) N(6) C(13) 113.9(5) yes . . . Fe(1) N(6) C(14) 127.2(5) yes . . . C(13) N(6) C(14) 117.6(6) yes . . . C(17) N(7) C(18) 109.7(6) yes . . . Fe(1) N(8) C(18) 140.2(5) yes . . . Fe(1) N(8) C(20) 112.2(4) yes . . . C(18) N(8) C(20) 107.6(6) yes . . . Fe(1) N(9) C(21) 117.6(4) yes . . . Fe(1) N(9) C(22) 129.1(5) yes . . . C(21) N(9) C(22) 113.2(5) yes . . . N(1) C(1) C(4) 103.5(6) yes . . . N(1) C(2) N(2) 109.3(7) yes . . . N(1) C(2) C(3) 123.3(7) yes . . . N(2) C(2) C(3) 127.3(6) yes . . . N(2) C(4) C(1) 110.0(7) yes . . . N(2) C(4) C(5) 115.8(5) yes . . . C(1) C(4) C(5) 134.2(7) yes . . . N(3) C(5) C(4) 115.1(7) yes . . . N(3) C(6) C(7) 111.9(5) yes . . . C(6) C(7) C(8) 114.7(7) yes . . . N(4) C(9) C(12) 105.7(8) yes . . . N(4) C(10) N(5) 110.6(7) yes . . . N(4) C(10) C(11) 121.9(7) yes . . . N(5) C(10) C(11) 127.5(8) yes . . . N(5) C(12) C(9) 109.5(7) yes . . . N(5) C(12) C(13) 115.3(7) yes . . . C(9) C(12) C(13) 135.1(8) yes . . . N(6) C(13) C(12) 116.4(7) yes . . . N(6) C(14) C(15) 114.3(6) yes . . . C(14) C(15) C(16) 117.7(8) yes . . . N(7) C(17) C(20) 106.7(6) yes . . . N(7) C(18) N(8) 107.0(6) yes . . . N(7) C(18) C(19) 123.2(6) yes . . . N(8) C(18) C(19) 129.8(7) yes . . . N(8) C(20) C(17) 109.0(5) yes . . . N(8) C(20) C(21) 115.6(6) yes . . . C(17) C(20) C(21) 135.4(7) yes . . . N(9) C(21) C(20) 114.3(6) yes . . . N(9) C(22) C(23) 111.9(6) yes . . . C(22) C(23) C(24) 113.7(8) yes . . . 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 Cl(1) N(1) 3.156(7) ? . . Cl(1) N(4) 3.119(8) ? . 2_776 Cl(1) N(7) 3.143(6) ? . 2_676 Cl(1) C(17) 3.582(9) ? . 1_556 F(1) C(5) 3.433(9) ? . 2_666 F(1) C(13) 3.256(10) ? . 1_455 F(1) C(14) 3.467(10) ? . 2_666 F(2) C(1) 3.158(10) ? . . F(2) C(5) 3.335(10) ? . 2_666 F(2) C(6) 3.533(8) ? . 2_666 F(3) C(1) 3.526(11) ? . . F(3) C(4) 3.594(9) ? . . F(3) C(5) 3.558(8) ? . . F(3) C(8) 3.558(11) ? . . F(3) C(9) 3.245(12) ? . 1_455 F(4) C(1) 3.191(8) ? . . F(4) C(11) 3.471(8) ? . 2_676 F(4) C(19) 3.498(10) ? . 2_676 F(5) C(3) 3.171(12) ? . 1_455 F(5) C(3) 3.533(10) ? . 2_676 F(5) C(11) 3.367(11) ? . 2_676 F(6) C(11) 3.380(9) ? . 2_676 F(6) C(21) 3.537(8) ? . 1_456 N(1) Cl(1) 3.156(7) ? . . N(4) Cl(1) 3.119(8) ? . 2_776 N(7) Cl(1) 3.143(6) ? . 2_676 C(1) F(2) 3.158(10) ? . . C(1) F(3) 3.526(11) ? . . C(1) F(4) 3.191(8) ? . . C(3) F(5) 3.171(12) ? . 1_655 C(3) F(5) 3.533(10) ? . 2_676 C(4) F(3) 3.594(9) ? . . C(5) F(1) 3.433(9) ? . 2_666 C(5) F(2) 3.335(10) ? . 2_666 C(5) F(3) 3.558(8) ? . . C(6) F(2) 3.533(8) ? . 2_666 C(8) F(3) 3.558(11) ? . . C(8) C(13) 3.559(11) ? . 1_455 C(9) F(3) 3.245(12) ? . 1_655 C(11) F(4) 3.471(8) ? . 2_676 C(11) F(5) 3.367(11) ? . 2_676 C(11) F(6) 3.380(9) ? . 2_676 C(13) F(1) 3.256(10) ? . 1_655 C(13) C(8) 3.559(11) ? . 1_655 C(14) F(1) 3.467(10) ? . 2_666 C(17) Cl(1) 3.582(9) ? . 1_554 C(19) F(4) 3.498(10) ? . 2_676 C(19) C(19) 3.572(10) ? . 2_676 C(21) F(6) 3.537(8) ? . 1_654 As(1) H(4) 3.413 ? . . As(1) H(10) 3.543 ? . 2_666 As(1) H(17) 3.255 ? . 2_676 Cl(1) H(1) 2.220 ? . . Cl(1) H(2) 2.198 ? . 2_776 Cl(1) H(3) 2.193 ? . 2_676 Cl(1) H(7) 3.282 ? . . Cl(1) H(23) 3.351 ? . 2_766 Cl(1) H(26) 2.861 ? . 2_766 Cl(1) H(28) 2.769 ? . 1_556 Cl(1) H(38) 3.445 ? . 1_456 #============================================================================== # 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 #============================================================================== #============================================================================== data_Fe(HL2Me(Pr))3ClBF4 _database_code_depnum_ccdc_archive 'CCDC 828316' #TrackingRef '5748_web_deposit_cif_file_0_NaohideMatsumoto_ #1307326485.FujiCIFall.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H39 B Cl F4 Fe N9' _chemical_formula_moiety 'C24 H39 B Cl F4 Fe N9' _chemical_formula_weight 631.74 _chemical_melting_point ? _chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 3 c:H' _symmetry_space_group_name_Hall 'R 3 -2"c' _symmetry_Int_Tables_number 161 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -Y,+X-Y,+Z 3 -X+Y,-X,+Z 4 -X+Y,+Y,1/2+Z 5 +X,+X-Y,1/2+Z 6 -Y,-X,1/2+Z 7 2/3+X,1/3+Y,1/3+Z 8 2/3-Y,1/3+X-Y,1/3+Z 9 2/3-X+Y,1/3-X,1/3+Z 10 2/3-X+Y,1/3+Y,5/6+Z 11 2/3+X,1/3+X-Y,5/6+Z 12 2/3-Y,1/3-X,5/6+Z 13 1/3+X,2/3+Y,2/3+Z 14 1/3-Y,2/3+X-Y,2/3+Z 15 1/3-X+Y,2/3-X,2/3+Z 16 1/3-X+Y,2/3+Y,1/6+Z 17 1/3+X,2/3+X-Y,1/6+Z 18 1/3-Y,2/3-X,1/6+Z #------------------------------------------------------------------------------ _cell_length_a 10.699(4) _cell_length_b 10.699(4) _cell_length_c 47.49(2) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 120.0000 _cell_volume 4707(3) _cell_formula_units_Z 6 _cell_measurement_reflns_used 10414 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 27.46 _cell_measurement_temperature 296 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.688 _exptl_crystal_size_mid 0.449 _exptl_crystal_size_min 0.394 _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1980.00 _exptl_absorpt_coefficient_mu 0.619 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.551 _exptl_absorpt_correction_T_max 0.784 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 296 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 14211 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_max 1.064 _diffrn_measured_fraction_theta_full 1.064 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 60 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 2.0 sigma(F^2^). 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 2251 _reflns_number_gt 1910 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.1024 _refine_ls_number_restraints ? _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 1910 _refine_ls_number_parameters 161 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0018Fo^2^ + 1.0700\s(Fo^2^)]/(4Fo^2^)' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.363 _refine_diff_density_min -0.482 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 1052 Friedel Pairs' _refine_ls_abs_structure_Flack 0.01(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.1484 0.1585 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; B B 0.0013 0.0007 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.0171 0.0103 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Fe Fe 0.3463 0.8444 ; 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 Fe1 Fe 0.6667 0.3333 0.39981(11) 0.04681(13) Uani 1.0 6 d . . . Cl1 Cl 0.3333 0.6667 0.47847(11) 0.0626(3) Uani 1.0 6 d . . . F1 F 0.3333 0.6667 0.3389(3) 0.262(8) Uani 0.6000 6 d . . . F2 F 0.3333 0.6667 0.3900(7) 0.287(18) Uani 0.4000 6 d . . . F3 F 0.437(7) 0.753(7) 0.3361(12) 0.102(14) Uiso 0.0500 18 d . . . F4 F 0.420(4) 0.653(3) 0.3465(7) 0.090(7) Uiso 0.1000 18 d . . . F5 F 0.441(3) 0.637(3) 0.3678(8) 0.055(6) Uiso 0.1000 18 d . . . F6 F 0.4605(17) 0.6698(18) 0.3593(5) 0.078(4) Uiso 0.2000 18 d . . . F7 F 0.426(3) 0.652(4) 0.3839(7) 0.058(7) Uiso 0.1000 18 d . . . F8 F 0.454(3) 0.686(3) 0.3840(5) 0.078(6) Uiso 0.2000 18 d . . . F9 F 0.349(6) 0.820(6) 0.3786(11) 0.055(12) Uiso 0.0500 18 d . . . F10 F 0.2140(18) 0.5345(15) 0.3732(5) 0.056(4) Uiso 0.2000 18 d . . . N1 N 0.2702(3) 0.1946(3) 0.35110(12) 0.0684(7) Uani 1.0 18 d . . . N2 N 0.4684(3) 0.2655(3) 0.37591(11) 0.0510(6) Uani 1.0 18 d . . . N3 N 0.5601(3) 0.4355(3) 0.42337(12) 0.0567(7) Uani 1.0 18 d . . . C1 C 0.4247(4) 0.0931(4) 0.33636(12) 0.0851(11) Uani 1.0 18 d . . . C2 C 0.3901(3) 0.1834(3) 0.35443(12) 0.0568(7) Uani 1.0 18 d . . . C3 C 0.2712(3) 0.2867(4) 0.37109(12) 0.0710(9) Uani 1.0 18 d . . . C4 C 0.3939(3) 0.3302(3) 0.38629(12) 0.0571(7) Uani 1.0 18 d . . . C5 C 0.4473(3) 0.4189(3) 0.41092(12) 0.0599(8) Uani 1.0 18 d . . . C6 C 0.6037(5) 0.5185(5) 0.44959(13) 0.0823(11) Uani 1.0 18 d . . . C7 C 0.7343(5) 0.6622(5) 0.44709(13) 0.0960(13) Uani 1.0 18 d . . . C8 C 0.7188(7) 0.7586(5) 0.42828(15) 0.136(2) Uani 1.0 18 d . . . B1 B 0.3333 0.6667 0.3652(2) 0.0736(16) Uani 1.0 6 d . . . H1 H 0.1988 0.1469 0.3370 0.0810 Uiso 1.0 18 calc R . . H2 H 0.1999 0.3132 0.3744 0.0901 Uiso 1.0 18 calc R . . H3 H 0.3979 0.4652 0.4181 0.0754 Uiso 1.0 18 calc R . . H4 H 0.5266 0.5315 0.4558 0.1029 Uiso 1.0 18 calc R . . H5 H 0.6211 0.4636 0.4631 0.1031 Uiso 1.0 18 calc R . . H6 H 0.7593 0.7035 0.4654 0.1197 Uiso 1.0 18 calc R . . H7 H 0.8103 0.6502 0.4398 0.1194 Uiso 1.0 18 calc R . . H8 H 0.4825 0.1470 0.3208 0.1061 Uiso 1.0 18 calc R . . H9 H 0.3367 0.0146 0.3297 0.1059 Uiso 1.0 18 calc R . . H10 H 0.4751 0.0573 0.3471 0.1059 Uiso 1.0 18 calc R . . H11 H 0.7442 0.7492 0.4096 0.1562 Uiso 1.0 18 calc R . . H12 H 0.7791 0.8549 0.4346 0.1560 Uiso 1.0 18 calc R . . H13 H 0.6209 0.7359 0.4288 0.1563 Uiso 1.0 18 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe1 0.04150(19) 0.04150(19) 0.0574(4) 0.02076(10) 0.0000 0.0000 Cl1 0.0605(4) 0.0605(4) 0.0669(10) 0.03025(18) 0.0000 0.0000 F1 0.36(2) 0.36(2) 0.061(7) 0.181(11) 0.0000 0.0000 F2 0.35(4) 0.35(4) 0.15(3) 0.177(19) 0.0000 0.0000 N1 0.0563(13) 0.0688(14) 0.0780(16) 0.0297(11) -0.0123(11) 0.0003(12) N2 0.0452(10) 0.0479(10) 0.0612(12) 0.0242(9) -0.0035(9) -0.0037(9) N3 0.0555(12) 0.0511(11) 0.0664(15) 0.0288(10) 0.0015(9) -0.0053(9) C1 0.091(2) 0.090(3) 0.084(2) 0.0518(19) -0.0218(17) -0.0311(18) C2 0.0499(13) 0.0532(13) 0.0634(16) 0.0229(11) -0.0069(12) -0.0005(11) C3 0.0578(16) 0.0810(19) 0.0864(19) 0.0437(15) -0.0068(12) -0.0034(16) C4 0.0502(12) 0.0554(13) 0.0707(14) 0.0300(11) 0.0021(11) 0.0038(11) C5 0.0561(14) 0.0591(14) 0.0732(15) 0.0352(12) 0.0033(12) -0.0046(12) C6 0.096(3) 0.087(2) 0.0743(19) 0.053(2) -0.0151(17) -0.0247(16) C7 0.096(3) 0.106(3) 0.097(3) 0.059(2) -0.021(2) -0.039(2) C8 0.186(6) 0.083(3) 0.121(4) 0.053(4) -0.031(4) -0.001(3) B1 0.070(3) 0.070(3) 0.081(5) 0.0348(13) 0.0000 0.0000 #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'CRYSTALS (Carruthers, et al., 1999)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # 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 Fe1 N2 2.185(5) yes . . Fe1 N2 2.185(5) yes . 2_655 Fe1 N2 2.185(5) yes . 3_665 Fe1 N3 2.234(5) yes . . Fe1 N3 2.234(5) yes . 2_655 Fe1 N3 2.234(5) yes . 3_665 F1 F3 1.04(5) yes . . F1 F3 1.04(5) yes . 2_665 F1 F3 1.04(5) yes . 3_565 F1 F4 1.08(4) yes . . F1 F4 1.08(4) yes . 2_665 F1 F4 1.08(4) yes . 3_565 F1 F6 1.66(3) yes . . F1 F6 1.66(3) yes . 2_665 F1 F6 1.66(3) yes . 3_565 F1 B1 1.249(18) yes . . F2 F5 1.70(4) yes . . F2 F5 1.70(4) yes . 2_665 F2 F5 1.70(4) yes . 3_565 F2 F7 1.12(4) yes . . F2 F7 1.12(4) yes . 2_665 F2 F7 1.12(4) yes . 3_565 F2 F8 1.23(3) yes . . F2 F8 1.23(3) yes . 2_665 F2 F8 1.23(3) yes . 3_565 F2 F9 1.66(7) yes . . F2 F9 1.66(7) yes . 2_665 F2 F9 1.66(7) yes . 3_565 F2 F10 1.57(3) yes . . F2 F10 1.57(3) yes . 2_665 F2 F10 1.57(3) yes . 3_565 F2 B1 1.18(4) yes . . F3 F3 1.79(9) yes . 2_665 F3 F3 1.79(9) yes . 3_565 F3 F4 1.11(8) yes . . F3 F4 1.16(8) yes . 2_665 F3 F6 1.51(7) yes . . F3 F6 1.78(8) yes . 2_665 F3 B1 1.72(6) yes . . F4 F4 1.75(6) yes . 2_665 F4 F4 1.75(6) yes . 3_565 F4 F5 1.07(5) yes . . F4 F6 0.71(4) yes . . F4 F7 1.78(5) yes . . F4 F9 1.62(7) yes . 3_565 F4 F10 1.34(4) yes . 2_665 F4 B1 1.35(4) yes . . F5 F6 0.51(4) yes . . F5 F7 0.81(5) yes . . F5 F8 0.90(4) yes . . F5 F9 0.59(7) yes . 3_565 F5 F10 0.47(4) yes . 2_665 F5 B1 1.34(4) yes . . F6 F7 1.21(4) yes . . F6 F8 1.19(4) yes . . F6 F9 0.96(6) yes . 3_565 F6 F10 0.67(3) yes . 2_665 F6 B1 1.37(2) yes . . F7 F8 0.34(3) yes . . F7 F8 1.79(4) yes . 3_565 F7 F9 0.55(7) yes . 3_565 F7 F10 0.63(4) yes . 2_665 F7 B1 1.40(4) yes . . F8 F9 0.56(6) yes . 3_565 F8 F10 0.54(4) yes . 2_665 F8 B1 1.49(3) yes . . F9 F10 0.43(5) yes . 3_565 F9 B1 1.69(6) yes . . F10 B1 1.403(14) yes . . N1 C2 1.356(5) yes . . N1 C3 1.365(7) yes . . N2 C2 1.334(7) yes . . N2 C4 1.382(6) yes . . N3 C5 1.274(6) yes . . N3 C6 1.463(8) yes . . C1 C2 1.471(7) yes . . C3 C4 1.360(6) yes . . C4 C5 1.433(7) yes . . C6 C7 1.477(5) yes . . C7 C8 1.435(9) yes . . 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 N2 Fe1 N2 95.5(2) yes . . 2_655 N2 Fe1 N2 95.5(2) yes . . 3_665 N2 Fe1 N3 76.98(16) yes . . . N2 Fe1 N3 91.11(13) yes . . 2_655 N2 Fe1 N3 170.45(10) yes . . 3_665 N2 Fe1 N2 95.5(2) yes 2_655 . 3_665 N2 Fe1 N3 170.45(10) yes 2_655 . . N2 Fe1 N3 76.98(16) yes 2_655 . 2_655 N2 Fe1 N3 91.11(13) yes 2_655 . 3_665 N2 Fe1 N3 91.12(13) yes 3_665 . . N2 Fe1 N3 170.45(10) yes 3_665 . 2_655 N2 Fe1 N3 76.98(16) yes 3_665 . 3_665 N3 Fe1 N3 97.1(2) yes . . 2_655 N3 Fe1 N3 97.1(2) yes . . 3_665 N3 Fe1 N3 97.1(2) yes 2_655 . 3_665 #============================================================================== loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_publ_flag N2 H1 Cl1 . . 10_444 3.187(5) 0.950 2.254 166.8 no N2 H1 Cl1 . . 11_454 3.187(5) 0.950 2.255 166.8 no N2 H1 Cl1 . . 12_554 3.187(5) 0.950 2.254 166.8 no #============================================================================== # 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 #==============================================================================