# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_General _journal_name_full CrystEngComm _journal_coden_cambridge 1350 #TrackingRef '- ESI-CE-COM-04-2012-025612-revised.cif' _audit_creation_date 2008-01-31 _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 'Masaaki Kojima' _publ_contact_author_address ; Department of Chemistry, Faculty of Science, Okayama University, 3-1-1 Tsushima-naka, Okayama 700-8530, Japan. ; _publ_contact_author_email kojima@cc.okayama-u.ac.jp _publ_contact_author_fax 'ENTER FAX NUMBER' _publ_contact_author_phone 'ENTER PHONE NUMBER' _publ_contact_letter ; Please consider this CIF submission for publication in Chemical Communications ; _publ_requested_category FI _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Conglomerate Crystallization, Chiral Recognition, and Spin-Crossover in a Host-Guest Complex Comprising of Fe^III^ Complexes (Host) and [Cr(ox)~3~]^3-^ (Guest) ; loop_ _publ_author_name _publ_author_address 'Yukinari Sunatsuki' ; Department of Chemistry, Faculty of Science, Okayama University, 3-1-1 Tsushima-naka, Okayama 700-8530, Japan. ; S.Miyahara ; Department of Chemistry, Faculty of Science, Okayama University, 3-1-1 Tsushima-naka, Okayama 700-8530, Japan. ; Y.Sasaki ; Department of Chemistry, Faculty of Science, Okayama University, 3-1-1 Tsushima-naka, Okayama 700-8530, Japan. ; T.Suzuki ; Department of Chemistry, Faculty of Science, Okayama University, 3-1-1 Tsushima-naka, Okayama 700-8530, Japan. ; M.Kojima ; Department of Chemistry, Faculty of Science, Okayama University, 3-1-1 Tsushima-naka, Okayama 700-8530, Japan. ; 'Naohide Matsumoto' ; Department of Chemistry, Faculty of Science, Kumamoto University, Kurokami 2-39-1, Kumamoto 860-8555, Japan ; _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_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. M. C. Burla, R. Caliandro, M. Camalli, B. Carrozzini, G. L. Cascarano, L. De Caro, C. Giacovazzo, G. Polidori, R. Spagna (2005). SIR2004. G. M. Sheldrick (1997). SHELXL97. University of Gottingen, Germany. ; #============================================================================== data_070417 _database_code_depnum_ccdc_archive 'CCDC 859999' #TrackingRef '- ESI-CE-COM-04-2012-025612-revised.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C21 H23.50 Cr0.50 Fe N10 O6.50 ' _chemical_formula_moiety 'C21 H23.50 Cr0.50 Fe N10 O6.50 ' _chemical_formula_weight 601.82 _chemical_melting_point ? _chemical_absolute_configuration ad #============================================================================== # CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 3 2 1' _symmetry_space_group_name_Hall 'P 3 2"' _symmetry_Int_Tables_number 150 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 +Y,+X,-Z 5 +X-Y,-Y,-Z 6 -X,-X+Y,-Z #------------------------------------------------------------------------------ _cell_length_a 12.5886(6) _cell_length_b 12.5886(6) _cell_length_c 9.2180(4) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 120.0000 _cell_volume 1265.09(10) _cell_formula_units_Z 2 _cell_measurement_reflns_used 13587 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 30.0 _cell_measurement_temperature 93.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.580 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 619.00 _exptl_absorpt_coefficient_mu 0.860 _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 0.616 _exptl_absorpt_correction_T_max 0.835 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 93.1 _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 15823 _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 #============================================================================== # 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 1939 _reflns_number_gt 1697 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.1822 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 1939 _refine_ls_number_parameters 151 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1219P)^2^+0.8503P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.48 _refine_diff_density_min -1.21 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 840 Friedel Pairs' _refine_ls_abs_structure_Flack 0.00(4) 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) ; Cr Cr 0.321 0.624 ; 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) ; N N 0.006 0.003 ; 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 Fe(1) Fe 0.3333 0.6667 0.41037(9) 0.0372(2) Uani 1.00 3 d S . . Cr(1) Cr 0.0000 0.0000 1.0000 0.0437(4) Uani 1.00 6 d S . . O(1) O 0.1701(7) 0.0895(19) 1.0597(10) 0.114(4) Uani 0.50 1 d P . . O(2) O 0.0624(17) 0.0967(13) 0.8239(10) 0.112(4) Uani 0.50 1 d P . . O(3) O 0.3291(16) 0.290(2) 0.995(4) 0.25(2) Uani 0.50 1 d P . . O(4) O 0.1857(15) 0.2138(18) 0.675(2) 0.174(11) Uani 0.50 1 d P . . O(5) O 0.059(4) 0.059(4) 0.5000 0.23(3) Uani 0.33 2 d SP . . N(1) N 0.3333 0.6667 0.7490(7) 0.067(2) Uani 1.00 3 d S . . N(2) N 0.4859(4) 0.7845(4) 0.5099(4) 0.0478(9) Uani 1.00 1 d . . . N(3) N 0.4515(3) 0.6485(3) 0.2922(3) 0.0370(7) Uani 1.00 1 d . . . N(4) N 0.5701(3) 0.6289(3) 0.1297(4) 0.0465(9) Uani 1.00 1 d . . . C(1) C 0.4517(8) 0.7729(7) 0.7711(5) 0.079(2) Uani 1.00 1 d . . . C(2) C 0.4906(6) 0.8592(5) 0.6382(5) 0.0629(15) Uani 1.00 1 d . . . C(3) C 0.5877(4) 0.8005(5) 0.4529(4) 0.0499(10) Uani 1.00 1 d . . . C(4) C 0.5732(4) 0.7290(4) 0.3265(4) 0.0434(9) Uani 1.00 1 d . . . C(5) C 0.4530(3) 0.5901(3) 0.1727(4) 0.0387(9) Uani 1.00 1 d . . . C(6) C 0.6449(4) 0.7150(4) 0.2269(5) 0.0478(10) Uani 1.00 1 d . . . C(7) C 0.2353(12) 0.2001(14) 0.972(2) 0.096(5) Uani 0.50 1 d P . . C(8) C 0.1616(18) 0.1898(17) 0.800(7) 0.24(2) Uani 0.50 1 d P . . H(1) H 0.5131 0.7469 0.7881 0.095 Uiso 1.00 1 c R . . H(2) H 0.4494 0.8176 0.8582 0.095 Uiso 1.00 1 c R . . H(3) H 0.4339 0.8914 0.6246 0.076 Uiso 1.00 1 c R . . H(4) H 0.5747 0.9292 0.6516 0.076 Uiso 1.00 1 c R . . H(5) H 0.6658 0.8558 0.4927 0.060 Uiso 1.00 1 c R . . H(6) H 0.3819 0.5295 0.1239 0.046 Uiso 1.00 1 c R . . H(7) H 0.5931 0.6031 0.0536 0.056 Uiso 0.50 1 c R . . H(8) H 0.7320 0.7580 0.2255 0.057 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 Fe(1) 0.0418(3) 0.0418(3) 0.0280(4) 0.02090(18) 0.0000 0.0000 Cr(1) 0.0422(5) 0.0422(5) 0.0467(8) 0.0211(2) 0.0000 0.0000 O(1) 0.035(3) 0.185(13) 0.085(5) 0.028(8) -0.028(4) 0.003(9) O(2) 0.183(15) 0.117(8) 0.087(6) 0.114(11) -0.030(8) -0.003(6) O(3) 0.050(6) 0.31(3) 0.168(13) -0.076(14) 0.002(9) -0.05(2) O(4) 0.149(14) 0.23(2) 0.215(16) 0.150(15) 0.130(13) 0.201(17) O(5) 0.25(3) 0.25(3) 0.094(15) 0.05(3) -0.073(18) 0.073(18) N(1) 0.088(3) 0.088(3) 0.024(2) 0.0441(16) 0.0000 0.0000 N(2) 0.057(2) 0.051(2) 0.0362(17) 0.0278(18) -0.0094(16) -0.0128(15) N(3) 0.0384(18) 0.0405(18) 0.0335(16) 0.0207(14) -0.0056(13) -0.0048(14) N(4) 0.047(2) 0.049(2) 0.0458(19) 0.0258(17) 0.0063(16) -0.0042(16) C(1) 0.102(5) 0.097(4) 0.030(2) 0.043(4) -0.010(2) -0.018(2) C(2) 0.077(3) 0.065(3) 0.037(2) 0.028(3) -0.002(2) -0.021(2) C(3) 0.046(2) 0.054(2) 0.0428(19) 0.019(2) -0.0093(16) -0.013(2) C(4) 0.039(2) 0.049(2) 0.041(2) 0.0209(19) -0.0035(16) -0.0080(18) C(5) 0.046(2) 0.039(2) 0.0325(17) 0.022(2) -0.0003(15) -0.0032(14) C(6) 0.039(2) 0.049(2) 0.053(2) 0.021(2) 0.0005(19) -0.008(2) C(7) 0.034(5) 0.073(9) 0.125(15) -0.015(6) 0.030(6) -0.012(9) C(8) 0.052(9) 0.053(9) 0.60(8) 0.015(7) -0.03(2) 0.07(2) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _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 Fe(1) N(2) 1.970(3) yes . . Fe(1) N(2) 1.969(5) yes . 2_665 Fe(1) N(2) 1.970(4) yes . 3_565 Fe(1) N(3) 1.948(4) yes . . Fe(1) N(3) 1.947(4) yes . 2_665 Fe(1) N(3) 1.947(3) yes . 3_565 Cr(1) O(1) 1.935(8) yes . . Cr(1) O(1) 1.94(2) yes . 2_555 Cr(1) O(1) 1.94(2) yes . 3_555 Cr(1) O(1) 1.94(2) yes . 4_557 Cr(1) O(1) 1.94(2) yes . 5_557 Cr(1) O(1) 1.935(8) yes . 6_557 Cr(1) O(2) 1.943(11) yes . . Cr(1) O(2) 1.943(14) yes . 2_555 Cr(1) O(2) 1.943(15) yes . 3_555 Cr(1) O(2) 1.943(12) yes . 4_557 Cr(1) O(2) 1.943(12) yes . 5_557 Cr(1) O(2) 1.943(15) yes . 6_557 O(1) O(2) 1.344(17) yes . 4_557 O(1) C(7) 1.46(2) yes . . O(1) C(7) 1.71(3) yes . 4_557 O(1) C(8) 1.52(5) yes . 4_557 O(2) C(8) 1.23(2) yes . . O(3) O(3) 0.85(4) yes . 4_557 O(3) C(7) 1.18(2) yes . . O(3) C(7) 1.44(2) yes . 4_557 O(4) C(8) 1.19(6) yes . . O(5) O(5) 1.29(6) yes . 2_555 O(5) O(5) 1.29(6) yes . 3_555 N(1) C(1) 1.435(7) yes . . N(1) C(1) 1.434(11) yes . 2_665 N(1) C(1) 1.435(10) yes . 3_565 N(2) C(2) 1.493(7) yes . . N(2) C(3) 1.303(7) yes . . N(3) C(4) 1.386(5) yes . . N(3) C(5) 1.330(5) yes . . N(4) C(5) 1.360(6) yes . . N(4) C(6) 1.358(5) yes . . C(1) C(2) 1.546(8) yes . . C(3) C(4) 1.427(7) yes . . C(4) C(6) 1.359(8) yes . . C(7) C(7) 0.92(2) yes . 4_557 C(7) C(8) 1.81(6) yes . . N(4) H(7) 0.880 no . . C(1) H(1) 0.990 no . . C(1) H(2) 0.990 no . . C(2) H(3) 0.990 no . . C(2) H(4) 0.990 no . . C(3) H(5) 0.950 no . . C(5) H(6) 0.950 no . . C(6) H(8) 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 N(2) Fe(1) N(2) 100.08(19) yes . . 2_665 N(2) Fe(1) N(2) 100.05(19) yes . . 3_565 N(2) Fe(1) N(3) 80.44(18) yes . . . N(2) Fe(1) N(3) 87.51(17) yes . . 2_665 N(2) Fe(1) N(3) 172.12(19) yes . . 3_565 N(2) Fe(1) N(2) 100.1(2) yes 2_665 . 3_565 N(2) Fe(1) N(3) 172.18(18) yes 2_665 . . N(2) Fe(1) N(3) 80.48(19) yes 2_665 . 2_665 N(2) Fe(1) N(3) 87.52(18) yes 2_665 . 3_565 N(2) Fe(1) N(3) 87.48(19) yes 3_565 . . N(2) Fe(1) N(3) 172.16(14) yes 3_565 . 2_665 N(2) Fe(1) N(3) 80.45(16) yes 3_565 . 3_565 N(3) Fe(1) N(3) 91.76(18) yes . . 2_665 N(3) Fe(1) N(3) 91.74(16) yes . . 3_565 N(3) Fe(1) N(3) 91.78(15) yes 2_665 . 3_565 O(1) Cr(1) O(1) 112.2(7) yes . . 2_555 O(1) Cr(1) O(1) 112.2(7) yes . . 3_555 O(1) Cr(1) O(1) 64.8(7) yes . . 4_557 O(1) Cr(1) O(1) 70.7(7) yes . . 5_557 O(1) Cr(1) O(1) 176.7(10) yes . . 6_557 O(1) Cr(1) O(2) 83.7(6) yes . . . O(1) Cr(1) O(2) 139.0(5) yes . . 2_555 O(1) Cr(1) O(2) 93.9(7) yes . . 3_555 O(1) Cr(1) O(2) 40.5(5) yes . . 4_557 O(1) Cr(1) O(2) 87.8(6) yes . . 5_557 O(1) Cr(1) O(2) 94.9(6) yes . . 6_557 O(1) Cr(1) O(1) 112.2(6) yes 2_555 . 3_555 O(1) Cr(1) O(1) 70.7(6) yes 2_555 . 4_557 O(1) Cr(1) O(1) 176.7(5) yes 2_555 . 5_557 O(1) Cr(1) O(1) 64.8(7) yes 2_555 . 6_557 O(1) Cr(1) O(2) 93.9(7) yes 2_555 . . O(1) Cr(1) O(2) 83.7(7) yes 2_555 . 2_555 O(1) Cr(1) O(2) 139.0(6) yes 2_555 . 3_555 O(1) Cr(1) O(2) 87.8(7) yes 2_555 . 4_557 O(1) Cr(1) O(2) 94.9(7) yes 2_555 . 5_557 O(1) Cr(1) O(2) 40.5(7) yes 2_555 . 6_557 O(1) Cr(1) O(1) 176.7(6) yes 3_555 . 4_557 O(1) Cr(1) O(1) 64.8(6) yes 3_555 . 5_557 O(1) Cr(1) O(1) 70.7(7) yes 3_555 . 6_557 O(1) Cr(1) O(2) 139.0(5) yes 3_555 . . O(1) Cr(1) O(2) 93.9(4) yes 3_555 . 2_555 O(1) Cr(1) O(2) 83.7(5) yes 3_555 . 3_555 O(1) Cr(1) O(2) 94.9(5) yes 3_555 . 4_557 O(1) Cr(1) O(2) 40.5(4) yes 3_555 . 5_557 O(1) Cr(1) O(2) 87.8(6) yes 3_555 . 6_557 O(1) Cr(1) O(1) 112.2(6) yes 4_557 . 5_557 O(1) Cr(1) O(1) 112.2(7) yes 4_557 . 6_557 O(1) Cr(1) O(2) 40.5(5) yes 4_557 . . O(1) Cr(1) O(2) 87.8(4) yes 4_557 . 2_555 O(1) Cr(1) O(2) 94.9(5) yes 4_557 . 3_555 O(1) Cr(1) O(2) 83.7(4) yes 4_557 . 4_557 O(1) Cr(1) O(2) 139.0(4) yes 4_557 . 5_557 O(1) Cr(1) O(2) 93.9(6) yes 4_557 . 6_557 O(1) Cr(1) O(1) 112.2(7) yes 5_557 . 6_557 O(1) Cr(1) O(2) 87.8(7) yes 5_557 . . O(1) Cr(1) O(2) 94.9(7) yes 5_557 . 2_555 O(1) Cr(1) O(2) 40.5(6) yes 5_557 . 3_555 O(1) Cr(1) O(2) 93.9(7) yes 5_557 . 4_557 O(1) Cr(1) O(2) 83.7(7) yes 5_557 . 5_557 O(1) Cr(1) O(2) 139.0(6) yes 5_557 . 6_557 O(1) Cr(1) O(2) 94.9(6) yes 6_557 . . O(1) Cr(1) O(2) 40.5(5) yes 6_557 . 2_555 O(1) Cr(1) O(2) 87.8(7) yes 6_557 . 3_555 O(1) Cr(1) O(2) 139.0(6) yes 6_557 . 4_557 O(1) Cr(1) O(2) 93.9(7) yes 6_557 . 5_557 O(1) Cr(1) O(2) 83.7(6) yes 6_557 . 6_557 O(2) Cr(1) O(2) 56.9(5) yes . . 2_555 O(2) Cr(1) O(2) 56.9(6) yes . . 3_555 O(2) Cr(1) O(2) 118.0(5) yes . . 4_557 O(2) Cr(1) O(2) 169.6(9) yes . . 5_557 O(2) Cr(1) O(2) 129.8(7) yes . . 6_557 O(2) Cr(1) O(2) 56.9(9) yes 2_555 . 3_555 O(2) Cr(1) O(2) 169.6(8) yes 2_555 . 4_557 O(2) Cr(1) O(2) 129.8(5) yes 2_555 . 5_557 O(2) Cr(1) O(2) 118.0(8) yes 2_555 . 6_557 O(2) Cr(1) O(2) 129.8(8) yes 3_555 . 4_557 O(2) Cr(1) O(2) 118.0(7) yes 3_555 . 5_557 O(2) Cr(1) O(2) 169.6(5) yes 3_555 . 6_557 O(2) Cr(1) O(2) 56.9(5) yes 4_557 . 5_557 O(2) Cr(1) O(2) 56.9(8) yes 4_557 . 6_557 O(2) Cr(1) O(2) 56.9(8) yes 5_557 . 6_557 Cr(1) O(1) O(2) 70.0(7) yes . . 4_557 Cr(1) O(1) C(7) 109.3(10) yes . . . Cr(1) O(1) C(7) 99.3(10) yes . . 4_557 Cr(1) O(1) C(8) 113.0(11) yes . . 4_557 O(2) O(1) C(7) 132(2) yes 4_557 . . O(2) O(1) C(7) 99.5(16) yes 4_557 . 4_557 O(2) O(1) C(8) 50.4(12) yes 4_557 . 4_557 C(7) O(1) C(7) 32.7(11) yes . . 4_557 C(7) O(1) C(8) 93.0(19) yes . . 4_557 C(7) O(1) C(8) 67.8(18) yes 4_557 . 4_557 Cr(1) O(2) O(1) 69.4(8) yes . . 4_557 Cr(1) O(2) C(8) 130(3) yes . . . O(1) O(2) C(8) 72(2) yes 4_557 . . O(3) O(3) C(7) 89(2) yes 4_557 . . O(3) O(3) C(7) 54.7(18) yes 4_557 . 4_557 C(7) O(3) C(7) 39.5(13) yes . . 4_557 O(5) O(5) O(5) 60(3) yes 2_555 . 3_555 C(1) N(1) C(1) 118.1(5) yes . . 2_665 C(1) N(1) C(1) 118.0(5) yes . . 3_565 C(1) N(1) C(1) 118.0(4) yes 2_665 . 3_565 Fe(1) N(2) C(2) 124.0(4) yes . . . Fe(1) N(2) C(3) 116.2(3) yes . . . C(2) N(2) C(3) 119.6(4) yes . . . Fe(1) N(3) C(4) 114.6(3) yes . . . Fe(1) N(3) C(5) 138.7(3) yes . . . C(4) N(3) C(5) 106.1(4) yes . . . C(5) N(4) C(6) 106.8(4) yes . . . N(1) C(1) C(2) 111.0(5) yes . . . N(2) C(2) C(1) 106.6(5) yes . . . N(2) C(3) C(4) 115.2(3) yes . . . N(3) C(4) C(3) 113.2(4) yes . . . N(3) C(4) C(6) 108.3(4) yes . . . C(3) C(4) C(6) 138.6(4) yes . . . N(3) C(5) N(4) 110.8(3) yes . . . N(4) C(6) C(4) 108.1(4) yes . . . O(1) C(7) O(1) 81.6(10) yes . . 4_557 O(1) C(7) O(3) 130(2) yes . . . O(1) C(7) O(3) 133(2) yes . . 4_557 O(1) C(7) C(7) 88.7(18) yes . . 4_557 O(1) C(7) C(8) 113.1(11) yes . . . O(1) C(7) O(3) 134(2) yes 4_557 . . O(1) C(7) O(3) 98.2(17) yes 4_557 . 4_557 O(1) C(7) C(7) 58.6(14) yes 4_557 . 4_557 O(1) C(7) C(8) 51.3(13) yes 4_557 . . O(3) C(7) O(3) 36.2(19) yes . . 4_557 O(3) C(7) C(7) 86(2) yes . . 4_557 O(3) C(7) C(8) 117(2) yes . . . O(3) C(7) C(7) 54.5(16) yes 4_557 . 4_557 O(3) C(7) C(8) 101.7(19) yes 4_557 . . C(7) C(7) C(8) 100(2) yes 4_557 . . O(1) C(8) O(2) 57(2) yes 4_557 . . O(1) C(8) O(4) 156(2) yes 4_557 . . O(1) C(8) C(7) 61(2) yes 4_557 . . O(2) C(8) O(4) 115(4) yes . . . O(2) C(8) C(7) 99(3) yes . . . O(4) C(8) C(7) 140.7(19) yes . . . C(5) N(4) H(7) 126.6 no . . . C(6) N(4) H(7) 126.6 no . . . N(1) C(1) H(1) 109.5 no . . . N(1) C(1) H(2) 109.4 no . . . C(2) C(1) H(1) 109.4 no . . . C(2) C(1) H(2) 109.4 no . . . H(1) C(1) H(2) 108.0 no . . . N(2) C(2) H(3) 110.4 no . . . N(2) C(2) H(4) 110.4 no . . . C(1) C(2) H(3) 110.4 no . . . C(1) C(2) H(4) 110.4 no . . . H(3) C(2) H(4) 108.6 no . . . N(2) C(3) H(5) 122.4 no . . . C(4) C(3) H(5) 122.4 no . . . N(3) C(5) H(6) 124.6 no . . . N(4) C(5) H(6) 124.6 no . . . N(4) C(6) H(8) 126.0 no . . . C(4) C(6) H(8) 126.0 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) C(6) 3.38(2) ? . 2_656 O(2) O(5) 3.020(13) ? . . O(2) O(5) 3.297(18) ? . 2_555 O(2) O(5) 3.44(2) ? . 3_555 O(2) C(6) 3.55(2) ? . 5_566 O(3) C(1) 3.37(3) ? . 6_657 O(3) C(5) 3.26(2) ? . 4_556 O(3) C(6) 3.59(3) ? . 6_656 O(4) O(4) 3.29(2) ? . 4_556 O(4) O(5) 2.42(3) ? . . O(4) O(5) 3.32(3) ? . 2_555 O(4) O(5) 3.44(3) ? . 3_555 O(4) C(2) 3.271(19) ? . 3_565 O(4) C(3) 3.12(2) ? . 3_565 O(4) C(3) 3.09(2) ? . 6_656 O(4) C(4) 3.46(2) ? . 6_656 O(4) C(6) 3.53(2) ? . 6_656 O(5) O(2) 3.020(13) ? . . O(5) O(2) 3.44(2) ? . 2_555 O(5) O(2) 3.30(2) ? . 3_555 O(5) O(2) 3.020(13) ? . 4_556 O(5) O(2) 3.44(2) ? . 5_556 O(5) O(2) 3.30(2) ? . 6_556 O(5) O(4) 2.42(3) ? . . O(5) O(4) 3.44(4) ? . 2_555 O(5) O(4) 3.32(5) ? . 3_555 O(5) O(4) 2.42(3) ? . 4_556 O(5) O(4) 3.44(4) ? . 5_556 O(5) O(4) 3.32(5) ? . 6_556 O(5) C(8) 3.15(6) ? . . O(5) C(8) 3.15(6) ? . 4_556 N(4) N(4) 2.713(6) ? . 4_555 C(1) O(3) 3.37(2) ? . 6_667 C(2) O(4) 3.271(19) ? . 2_665 C(3) O(4) 3.116(17) ? . 2_665 C(3) O(4) 3.093(16) ? . 6_666 C(4) O(4) 3.458(17) ? . 6_666 C(5) O(3) 3.26(3) ? . 4_556 C(6) O(1) 3.378(10) ? . 3_664 C(6) O(2) 3.547(18) ? . 5_666 C(6) O(3) 3.59(3) ? . 6_666 C(6) O(4) 3.53(2) ? . 6_666 C(6) C(7) 3.286(18) ? . 6_666 C(6) C(8) 3.454(18) ? . 6_666 C(7) C(6) 3.29(2) ? . 6_656 C(8) O(5) 3.15(6) ? . . C(8) C(6) 3.45(2) ? . 6_656 O(1) H(8) 2.566 ? . 2_656 O(1) H(8) 3.171 ? . 6_656 O(2) H(8) 2.613 ? . 5_566 O(2) H(8) 3.163 ? . 6_656 O(3) H(1) 3.140 ? . 6_657 O(3) H(2) 3.311 ? . 3_565 O(3) H(2) 2.798 ? . 6_657 O(3) H(4) 3.531 ? . 3_565 O(3) H(4) 3.428 ? . 6_657 O(3) H(6) 2.987 ? . 1_556 O(3) H(6) 2.447 ? . 4_556 O(4) H(1) 3.346 ? . 3_565 O(4) H(4) 2.449 ? . 3_565 O(4) H(5) 2.247 ? . 3_565 O(4) H(5) 2.557 ? . 6_656 O(4) H(8) 3.003 ? . 5_566 O(4) H(8) 3.154 ? . 6_656 O(5) H(5) 3.002 ? . 3_565 O(5) H(5) 3.002 ? . 6_656 N(2) H(4) 3.464 ? . 5_676 N(3) H(3) 3.452 ? . 6_656 N(3) H(4) 3.585 ? . 6_656 N(4) H(1) 3.301 ? . 4_556 N(4) H(2) 3.345 ? . 3_564 N(4) H(2) 3.168 ? . 6_656 N(4) H(3) 3.111 ? . 6_656 N(4) H(7) 1.849 ? . 4_555 C(1) H(6) 3.376 ? . 2_666 C(2) H(4) 3.583 ? . 5_676 C(3) H(4) 3.249 ? . 5_676 C(4) H(3) 3.404 ? . 6_656 C(5) H(2) 3.042 ? . 3_564 C(5) H(2) 3.581 ? . 6_656 C(5) H(3) 3.268 ? . 6_656 C(5) H(4) 3.241 ? . 6_656 C(5) H(7) 2.802 ? . 4_555 C(6) H(1) 3.376 ? . 4_556 C(6) H(3) 3.186 ? . 6_656 C(6) H(7) 2.917 ? . 4_555 C(7) H(6) 3.357 ? . 4_556 C(7) H(8) 3.034 ? . 6_656 C(8) H(1) 3.382 ? . 3_565 C(8) H(4) 3.061 ? . 3_565 C(8) H(5) 3.291 ? . 3_565 C(8) H(5) 3.466 ? . 6_656 C(8) H(8) 2.761 ? . 5_566 C(8) H(8) 2.977 ? . 6_656 H(1) O(3) 3.140 ? . 6_667 H(1) O(4) 3.346 ? . 2_665 H(1) N(4) 3.301 ? . 4_556 H(1) C(6) 3.376 ? . 4_556 H(1) C(8) 3.382 ? . 2_665 H(1) H(6) 3.513 ? . 2_666 H(1) H(7) 3.478 ? . 1_556 H(1) H(7) 3.060 ? . 4_556 H(1) H(8) 3.184 ? . 4_556 H(2) O(3) 3.311 ? . 2_665 H(2) O(3) 2.798 ? . 6_667 H(2) N(4) 3.345 ? . 2_666 H(2) N(4) 3.168 ? . 6_666 H(2) C(5) 3.042 ? . 2_666 H(2) C(5) 3.581 ? . 6_666 H(2) H(6) 2.478 ? . 2_666 H(2) H(7) 3.133 ? . 2_666 H(2) H(7) 2.848 ? . 6_666 H(3) N(3) 3.452 ? . 6_666 H(3) N(4) 3.111 ? . 6_666 H(3) C(4) 3.404 ? . 6_666 H(3) C(5) 3.268 ? . 6_666 H(3) C(6) 3.186 ? . 6_666 H(3) H(3) 3.298 ? . 5_676 H(3) H(4) 3.558 ? . 5_676 H(3) H(7) 3.414 ? . 6_666 H(3) H(8) 3.561 ? . 6_666 H(4) O(3) 3.531 ? . 2_665 H(4) O(3) 3.428 ? . 6_667 H(4) O(4) 2.449 ? . 2_665 H(4) N(2) 3.464 ? . 5_676 H(4) N(3) 3.585 ? . 6_666 H(4) C(2) 3.583 ? . 5_676 H(4) C(3) 3.249 ? . 5_676 H(4) C(5) 3.241 ? . 6_666 H(4) C(8) 3.061 ? . 2_665 H(4) H(3) 3.558 ? . 5_676 H(4) H(4) 3.192 ? . 5_676 H(4) H(5) 3.139 ? . 5_676 H(4) H(6) 3.262 ? . 6_666 H(5) O(4) 2.247 ? . 2_665 H(5) O(4) 2.557 ? . 6_666 H(5) O(5) 3.002 ? . 2_665 H(5) C(8) 3.291 ? . 2_665 H(5) C(8) 3.466 ? . 6_666 H(5) H(4) 3.139 ? . 5_676 H(5) H(5) 3.147 ? . 5_676 H(5) H(8) 3.511 ? . 4_556 H(6) O(3) 2.987 ? . 1_554 H(6) O(3) 2.447 ? . 4_556 H(6) C(1) 3.376 ? . 3_564 H(6) C(7) 3.357 ? . 4_556 H(6) H(1) 3.513 ? . 3_564 H(6) H(2) 2.478 ? . 3_564 H(6) H(4) 3.262 ? . 6_656 H(6) H(7) 2.974 ? . 4_555 H(7) N(4) 1.849 ? . 4_555 H(7) C(5) 2.802 ? . 4_555 H(7) C(6) 2.917 ? . 4_555 H(7) H(1) 3.478 ? . 1_554 H(7) H(1) 3.060 ? . 4_556 H(7) H(2) 3.133 ? . 3_564 H(7) H(2) 2.848 ? . 6_656 H(7) H(3) 3.414 ? . 6_656 H(7) H(6) 2.974 ? . 4_555 H(7) H(7) 1.012 ? . 4_555 H(7) H(8) 3.192 ? . 4_555 H(8) O(1) 2.566 ? . 3_664 H(8) O(1) 3.171 ? . 6_666 H(8) O(2) 2.613 ? . 5_666 H(8) O(2) 3.163 ? . 6_666 H(8) O(4) 3.003 ? . 5_666 H(8) O(4) 3.154 ? . 6_666 H(8) C(7) 3.034 ? . 6_666 H(8) C(8) 2.761 ? . 5_666 H(8) C(8) 2.977 ? . 6_666 H(8) H(1) 3.184 ? . 4_556 H(8) H(3) 3.561 ? . 6_656 H(8) H(5) 3.511 ? . 4_556 H(8) H(7) 3.192 ? . 4_555 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 N(4) H(7) N(4) . . 4_555 2.713(6) 0.880 1.849 166.7 no #============================================================================== # End of CIF #============================================================================== #============================================================================== data_070418 _database_code_depnum_ccdc_archive 'CCDC 860000' #TrackingRef '- ESI-CE-COM-04-2012-025612-revised.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C21 H23.50 Cr0.50 Fe N10 O6.50' _chemical_formula_moiety 'C21 H23.50 Cr0.50 Fe N10 O6.50' _chemical_formula_weight 601.82 _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 'P 3 2 1' _symmetry_space_group_name_Hall 'P 3 2"' _symmetry_Int_Tables_number 150 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 +Y,+X,-Z 5 +X-Y,-Y,-Z 6 -X,-X+Y,-Z #------------------------------------------------------------------------------ _cell_length_a 12.6333(5) _cell_length_b 12.6333(5) _cell_length_c 9.2580(4) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 120.0000 _cell_volume 1279.63(9) _cell_formula_units_Z 2 _cell_measurement_reflns_used 13448 _cell_measurement_theta_min 3.23 _cell_measurement_theta_max 29.93 _cell_measurement_temperature 293 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour dark _exptl_crystal_size_max 0.370 _exptl_crystal_size_mid 0.310 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 619.00 _exptl_absorpt_coefficient_mu 0.850 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'NUMABS (Rigaku, 1999)' _exptl_absorpt_correction_T_min 0.902 _exptl_absorpt_correction_T_max 0.958 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 293 _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 17873 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_max 1.062 _diffrn_measured_fraction_theta_full 1.062 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _reflns_number_total 1976 _reflns_number_gt 1526 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1905 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 1976 _refine_ls_number_parameters 150 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1215P)^2^+0.3110P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.003 _refine_diff_density_max 0.390 _refine_diff_density_min -1.080 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 857 Friedel Pairs' _refine_ls_abs_structure_Flack 0.05(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 ; 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' ; H H 0.0000 0.0000 ; 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' ; Cr Cr 0.3209 0.6236 ; 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' ; Fe Fe 0.3463 0.8444 ; 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' ; N N 0.0061 0.0033 ; 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' ; O O 0.0106 0.0060 ; 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' ; #============================================================================== # 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 Fe(1) Fe 0.3333 0.6667 0.09022(9) 0.0513(4) Uani 1.0 2 d . . . Cr(1) Cr 0.0000 0.0000 0.5000 0.0642(5) Uani 1.0 1 d . . . O(1) O -0.087(2) 0.085(3) 0.4416(14) 0.134(6) Uani 0.5000 6 d . . . O(2) O 0.0389(15) 0.0982(17) 0.6715(16) 0.151(6) Uani 0.5000 6 d . . . O(3) O -0.036(5) 0.289(4) 0.493(5) 0.35(3) Uani 0.5000 6 d . . . O(4) O 0.0382(17) 0.225(3) 0.809(4) 0.32(3) Uani 0.5000 6 d . . . O(5) O 0.094(4) 0.094(4) 1.0000 0.77(19) Uani 0.3300 3 d . . . N(1) N 0.3333 0.6667 -0.2438(7) 0.081(2) Uani 1.0 2 d . . . N(2) N 0.2160(5) 0.5122(5) -0.0081(4) 0.0620(11) Uani 1.0 6 d . . . N(3) N 0.3521(4) 0.5491(4) 0.2092(4) 0.0531(9) Uani 1.0 6 d . . . N(4) N 0.3728(5) 0.4322(5) 0.3708(5) 0.0715(12) Uani 1.0 6 d . . . C(1) C 0.2298(8) 0.5478(8) -0.2688(6) 0.094(3) Uani 1.0 6 d . . . C(2) C 0.1421(7) 0.5075(7) -0.1360(6) 0.0826(18) Uani 1.0 6 d . . . C(3) C 0.2012(7) 0.4134(5) 0.0488(5) 0.0677(12) Uani 1.0 6 d . . . C(4) C 0.2728(5) 0.4278(5) 0.1742(5) 0.0601(12) Uani 1.0 6 d . . . C(5) C 0.4093(5) 0.5464(5) 0.3285(5) 0.0562(12) Uani 1.0 6 d . . . C(6) C 0.2879(6) 0.3587(6) 0.2753(6) 0.0721(14) Uani 1.0 6 d . . . C(8) C 0.026(2) 0.182(3) 0.652(7) 0.23(3) Uani 0.5000 6 d . . . C(7) C -0.033(3) 0.2014(16) 0.526(4) 0.131(8) Uani 0.5000 6 d . . . H(1) H 0.2571 0.4893 -0.2849 0.1128 Uiso 1.0 6 calc R . . H(2) H 0.1866 0.5496 -0.3545 0.1128 Uiso 1.0 6 calc R . . H(3) H 0.1100 0.5623 -0.1228 0.0991 Uiso 1.0 6 calc R . . H(4) H 0.0742 0.4252 -0.1498 0.0991 Uiso 1.0 6 calc R . . H(5) H 0.1470 0.3369 0.0108 0.0812 Uiso 1.0 6 calc R . . H(6) H 0.4678 0.6157 0.3766 0.0674 Uiso 1.0 6 calc R . . H(7) H 0.3986 0.4102 0.4445 0.0858 Uiso 0.5000 6 calc R . . H(8) H 0.2461 0.2737 0.2779 0.0865 Uiso 1.0 6 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 Fe(1) 0.0542(4) 0.0542(4) 0.0454(5) 0.0271(2) 0.0000 0.0000 Cr(1) 0.0619(7) 0.0619(7) 0.0689(10) 0.0309(3) 0.0000 0.0000 O(1) 0.155(13) 0.22(2) 0.104(7) 0.153(14) -0.027(10) -0.008(11) O(2) 0.104(11) 0.155(13) 0.159(12) 0.038(11) -0.053(11) -0.009(10) O(3) 0.72(8) 0.44(5) 0.216(19) 0.54(6) 0.08(4) 0.09(3) O(4) 0.134(14) 0.41(4) 0.42(4) 0.15(2) -0.14(2) -0.38(4) O(5) 0.40(8) 0.40(8) 1.0(3) -0.21(10) 0.51(15) -0.51(15) N(1) 0.098(4) 0.098(4) 0.046(3) 0.0492(17) 0.0000 0.0000 N(2) 0.068(3) 0.070(3) 0.0485(18) 0.035(2) -0.0140(17) -0.0019(18) N(3) 0.062(3) 0.055(2) 0.0416(17) 0.0283(17) -0.0071(16) -0.0034(15) N(4) 0.078(3) 0.078(3) 0.064(3) 0.043(3) -0.007(3) 0.015(3) C(1) 0.113(6) 0.108(5) 0.053(3) 0.049(5) -0.023(3) -0.013(3) C(2) 0.085(4) 0.093(5) 0.053(3) 0.032(4) -0.028(3) 0.002(3) C(3) 0.071(4) 0.063(3) 0.056(3) 0.024(4) -0.016(3) -0.0067(19) C(4) 0.071(3) 0.055(3) 0.052(3) 0.030(3) -0.010(2) 0.0006(19) C(5) 0.060(3) 0.069(3) 0.0432(18) 0.035(3) -0.0089(18) 0.0016(18) C(6) 0.076(4) 0.058(3) 0.078(4) 0.031(3) -0.008(3) 0.015(3) C(8) 0.076(13) 0.099(16) 0.49(8) 0.036(11) -0.09(3) 0.04(3) C(7) 0.15(3) 0.085(12) 0.20(3) 0.091(16) 0.065(16) 0.019(14) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SIR2004 (Burla, et al., 2005)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Fe(1) N(2) 1.985(4) yes . . Fe(1) N(2) 1.986(4) yes . 2_665 Fe(1) N(2) 1.985(4) yes . 3_565 Fe(1) N(3) 1.958(5) yes . . Fe(1) N(3) 1.957(5) yes . 2_665 Fe(1) N(3) 1.957(5) yes . 3_565 Cr(1) O(1) 1.96(4) yes . . Cr(1) O(1) 1.96(4) yes . 2_555 Cr(1) O(1) 1.96(4) yes . 3_555 Cr(1) O(1) 1.96(4) yes . 4_556 Cr(1) O(1) 1.96(4) yes . 5_556 Cr(1) O(1) 1.96(4) yes . 6_556 Cr(1) O(2) 1.922(16) yes . . Cr(1) O(2) 1.922(16) yes . 2_555 Cr(1) O(2) 1.922(16) yes . 3_555 Cr(1) O(2) 1.922(16) yes . 4_556 Cr(1) O(2) 1.922(16) yes . 5_556 Cr(1) O(2) 1.922(16) yes . 6_556 O(1) O(2) 1.33(3) yes . 6_556 O(1) C(8) 1.21(6) yes . 6_556 O(1) C(7) 1.49(4) yes . . O(1) C(7) 1.76(4) yes . 6_556 O(2) O(2) 1.87(3) yes . 2_555 O(2) O(2) 1.87(3) yes . 3_555 O(2) C(8) 1.16(5) yes . . O(3) O(3) 0.80(8) yes . 6_556 O(3) C(7) 1.17(6) yes . . O(3) C(7) 1.37(7) yes . 6_556 O(4) C(8) 1.53(7) yes . . N(1) C(1) 1.434(7) yes . . N(1) C(1) 1.434(7) yes . 2_665 N(1) C(1) 1.433(7) yes . 3_565 N(2) C(2) 1.490(8) yes . . N(2) C(3) 1.280(8) yes . . N(3) C(4) 1.386(6) yes . . N(3) C(5) 1.329(7) yes . . N(4) C(5) 1.335(8) yes . . N(4) C(6) 1.341(7) yes . . C(1) C(2) 1.560(9) yes . . C(3) C(4) 1.426(8) yes . . C(4) C(6) 1.358(10) yes . . C(8) C(7) 1.48(6) yes . . C(8) C(7) 1.76(7) yes . 6_556 C(7) C(7) 0.87(4) yes . 6_556 N(4) H(7) 0.860 no . . C(1) H(1) 0.970 no . . C(1) H(2) 0.970 no . . C(2) H(3) 0.970 no . . C(2) H(4) 0.970 no . . C(3) H(5) 0.930 no . . C(5) H(6) 0.930 no . . C(6) H(8) 0.930 no . . H(7) H(7) 1.058 no . 4_556 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(2) Fe(1) N(2) 100.6(3) yes . . 2_665 N(2) Fe(1) N(2) 100.6(3) yes . . 3_565 N(2) Fe(1) N(3) 79.97(19) yes . . . N(2) Fe(1) N(3) 171.3(2) yes . . 2_665 N(2) Fe(1) N(3) 87.7(2) yes . . 3_565 N(2) Fe(1) N(2) 100.6(3) yes 2_665 . 3_565 N(2) Fe(1) N(3) 87.7(2) yes 2_665 . . N(2) Fe(1) N(3) 79.98(19) yes 2_665 . 2_665 N(2) Fe(1) N(3) 171.3(2) yes 2_665 . 3_565 N(2) Fe(1) N(3) 171.4(2) yes 3_565 . . N(2) Fe(1) N(3) 87.7(2) yes 3_565 . 2_665 N(2) Fe(1) N(3) 80.02(19) yes 3_565 . 3_565 N(3) Fe(1) N(3) 91.40(17) yes . . 2_665 N(3) Fe(1) N(3) 91.41(17) yes . . 3_565 N(3) Fe(1) N(3) 91.43(17) yes 2_665 . 3_565 O(1) Cr(1) O(1) 112.7(8) yes . . 2_555 O(1) Cr(1) O(1) 112.7(8) yes . . 3_555 O(1) Cr(1) O(1) 179.1(8) yes . . 4_556 O(1) Cr(1) O(1) 66.5(8) yes . . 5_556 O(1) Cr(1) O(1) 68.1(9) yes . . 6_556 O(1) Cr(1) O(2) 84.6(9) yes . . . O(1) Cr(1) O(2) 90.6(7) yes . . 2_555 O(1) Cr(1) O(2) 140.0(7) yes . . 3_555 O(1) Cr(1) O(2) 95.8(9) yes . . 4_556 O(1) Cr(1) O(2) 88.9(7) yes . . 5_556 O(1) Cr(1) O(2) 40.1(7) yes . . 6_556 O(1) Cr(1) O(1) 112.7(8) yes 2_555 . 3_555 O(1) Cr(1) O(1) 66.5(8) yes 2_555 . 4_556 O(1) Cr(1) O(1) 68.1(9) yes 2_555 . 5_556 O(1) Cr(1) O(1) 179.1(8) yes 2_555 . 6_556 O(1) Cr(1) O(2) 140.0(7) yes 2_555 . . O(1) Cr(1) O(2) 84.6(9) yes 2_555 . 2_555 O(1) Cr(1) O(2) 90.6(7) yes 2_555 . 3_555 O(1) Cr(1) O(2) 88.9(7) yes 2_555 . 4_556 O(1) Cr(1) O(2) 40.1(7) yes 2_555 . 5_556 O(1) Cr(1) O(2) 95.8(9) yes 2_555 . 6_556 O(1) Cr(1) O(1) 68.1(9) yes 3_555 . 4_556 O(1) Cr(1) O(1) 179.1(8) yes 3_555 . 5_556 O(1) Cr(1) O(1) 66.5(8) yes 3_555 . 6_556 O(1) Cr(1) O(2) 90.6(7) yes 3_555 . . O(1) Cr(1) O(2) 140.0(7) yes 3_555 . 2_555 O(1) Cr(1) O(2) 84.6(9) yes 3_555 . 3_555 O(1) Cr(1) O(2) 40.1(7) yes 3_555 . 4_556 O(1) Cr(1) O(2) 95.8(9) yes 3_555 . 5_556 O(1) Cr(1) O(2) 88.9(7) yes 3_555 . 6_556 O(1) Cr(1) O(1) 112.7(8) yes 4_556 . 5_556 O(1) Cr(1) O(1) 112.7(8) yes 4_556 . 6_556 O(1) Cr(1) O(2) 95.8(9) yes 4_556 . . O(1) Cr(1) O(2) 88.9(7) yes 4_556 . 2_555 O(1) Cr(1) O(2) 40.1(7) yes 4_556 . 3_555 O(1) Cr(1) O(2) 84.6(9) yes 4_556 . 4_556 O(1) Cr(1) O(2) 90.6(7) yes 4_556 . 5_556 O(1) Cr(1) O(2) 140.0(7) yes 4_556 . 6_556 O(1) Cr(1) O(1) 112.7(8) yes 5_556 . 6_556 O(1) Cr(1) O(2) 88.9(7) yes 5_556 . . O(1) Cr(1) O(2) 40.1(7) yes 5_556 . 2_555 O(1) Cr(1) O(2) 95.8(9) yes 5_556 . 3_555 O(1) Cr(1) O(2) 140.0(7) yes 5_556 . 4_556 O(1) Cr(1) O(2) 84.6(9) yes 5_556 . 5_556 O(1) Cr(1) O(2) 90.6(7) yes 5_556 . 6_556 O(1) Cr(1) O(2) 40.1(7) yes 6_556 . . O(1) Cr(1) O(2) 95.8(9) yes 6_556 . 2_555 O(1) Cr(1) O(2) 88.9(7) yes 6_556 . 3_555 O(1) Cr(1) O(2) 90.6(7) yes 6_556 . 4_556 O(1) Cr(1) O(2) 140.0(7) yes 6_556 . 5_556 O(1) Cr(1) O(2) 84.6(9) yes 6_556 . 6_556 O(2) Cr(1) O(2) 58.4(8) yes . . 2_555 O(2) Cr(1) O(2) 58.4(8) yes . . 3_555 O(2) Cr(1) O(2) 126.4(6) yes . . 4_556 O(2) Cr(1) O(2) 172.3(9) yes . . 5_556 O(2) Cr(1) O(2) 117.6(10) yes . . 6_556 O(2) Cr(1) O(2) 58.4(8) yes 2_555 . 3_555 O(2) Cr(1) O(2) 172.3(9) yes 2_555 . 4_556 O(2) Cr(1) O(2) 117.6(10) yes 2_555 . 5_556 O(2) Cr(1) O(2) 126.4(6) yes 2_555 . 6_556 O(2) Cr(1) O(2) 117.6(10) yes 3_555 . 4_556 O(2) Cr(1) O(2) 126.4(6) yes 3_555 . 5_556 O(2) Cr(1) O(2) 172.3(9) yes 3_555 . 6_556 O(2) Cr(1) O(2) 58.4(8) yes 4_556 . 5_556 O(2) Cr(1) O(2) 58.4(8) yes 4_556 . 6_556 O(2) Cr(1) O(2) 58.4(8) yes 5_556 . 6_556 Cr(1) O(1) O(2) 68.3(16) yes . . 6_556 Cr(1) O(1) C(8) 106(2) yes . . 6_556 Cr(1) O(1) C(7) 106.8(16) yes . . . Cr(1) O(1) C(7) 96.8(12) yes . . 6_556 O(2) O(1) C(8) 54(3) yes 6_556 . 6_556 O(2) O(1) C(7) 128(2) yes 6_556 . . O(2) O(1) C(7) 98.0(17) yes 6_556 . 6_556 C(8) O(1) C(7) 81(3) yes 6_556 . . C(8) O(1) C(7) 56(3) yes 6_556 . 6_556 C(7) O(1) C(7) 29.5(14) yes . . 6_556 Cr(1) O(2) O(1) 71.6(14) yes . . 6_556 Cr(1) O(2) O(2) 60.8(7) yes . . 2_555 Cr(1) O(2) O(2) 60.8(8) yes . . 3_555 Cr(1) O(2) C(8) 111(3) yes . . . O(1) O(2) O(2) 127.1(15) yes 6_556 . 2_555 O(1) O(2) O(2) 115.0(18) yes 6_556 . 3_555 O(1) O(2) C(8) 57(3) yes 6_556 . . O(2) O(2) O(2) 60.0(11) yes 2_555 . 3_555 O(2) O(2) C(8) 119.4(18) yes 2_555 . . O(2) O(2) C(8) 171(4) yes 3_555 . . O(3) O(3) C(7) 86(7) yes 6_556 . . O(3) O(3) C(7) 58(6) yes 6_556 . 6_556 C(7) O(3) C(7) 39(3) yes . . 6_556 C(1) N(1) C(1) 117.4(7) yes . . 2_665 C(1) N(1) C(1) 117.5(7) yes . . 3_565 C(1) N(1) C(1) 117.4(7) yes 2_665 . 3_565 Fe(1) N(2) C(2) 123.3(5) yes . . . Fe(1) N(2) C(3) 116.3(4) yes . . . C(2) N(2) C(3) 120.3(5) yes . . . Fe(1) N(3) C(4) 114.3(4) yes . . . Fe(1) N(3) C(5) 139.5(4) yes . . . C(4) N(3) C(5) 105.5(5) yes . . . C(5) N(4) C(6) 106.2(6) yes . . . N(1) C(1) C(2) 109.9(6) yes . . . N(2) C(2) C(1) 106.6(6) yes . . . N(2) C(3) C(4) 115.9(5) yes . . . N(3) C(4) C(3) 113.2(5) yes . . . N(3) C(4) C(6) 107.1(5) yes . . . C(3) C(4) C(6) 139.7(5) yes . . . N(3) C(5) N(4) 111.9(4) yes . . . N(4) C(6) C(4) 109.2(5) yes . . . O(1) C(8) O(2) 69(3) yes 6_556 . . O(1) C(8) O(4) 140(3) yes 6_556 . . O(1) C(8) C(7) 82(4) yes 6_556 . . O(1) C(8) C(7) 57(3) yes 6_556 . 6_556 O(2) C(8) O(4) 98(4) yes . . . O(2) C(8) C(7) 126(4) yes . . . O(2) C(8) C(7) 119(4) yes . . 6_556 O(4) C(8) C(7) 131(3) yes . . . O(4) C(8) C(7) 141(3) yes . . 6_556 C(7) C(8) C(7) 29.6(17) yes . . 6_556 O(1) C(7) O(1) 84(2) yes . . 6_556 O(1) C(7) O(3) 126(4) yes . . . O(1) C(7) O(3) 141(3) yes . . 6_556 O(1) C(7) C(8) 106(3) yes . . . O(1) C(7) C(8) 42.5(16) yes . . 6_556 O(1) C(7) C(7) 93(3) yes . . 6_556 O(1) C(7) O(3) 133(3) yes 6_556 . . O(1) C(7) O(3) 98(3) yes 6_556 . 6_556 O(1) C(7) C(8) 43(2) yes 6_556 . . O(1) C(7) C(8) 84.3(17) yes 6_556 . 6_556 O(1) C(7) C(7) 58(3) yes 6_556 . 6_556 O(3) C(7) O(3) 36(3) yes . . 6_556 O(3) C(7) C(8) 129(3) yes . . . O(3) C(7) C(8) 96(3) yes . . 6_556 O(3) C(7) C(7) 83(4) yes . . 6_556 O(3) C(7) C(8) 102(3) yes 6_556 . . O(3) C(7) C(8) 99(3) yes 6_556 . 6_556 O(3) C(7) C(7) 58(3) yes 6_556 . 6_556 C(8) C(7) C(8) 125(3) yes . . 6_556 C(8) C(7) C(7) 94(4) yes . . 6_556 C(8) C(7) C(7) 57(3) yes 6_556 . 6_556 C(5) N(4) H(7) 126.884 no . . . C(6) N(4) H(7) 126.880 no . . . N(1) C(1) H(1) 109.696 no . . . N(1) C(1) H(2) 109.658 no . . . C(2) C(1) H(1) 109.667 no . . . C(2) C(1) H(2) 109.676 no . . . H(1) C(1) H(2) 108.169 no . . . N(2) C(2) H(3) 110.413 no . . . N(2) C(2) H(4) 110.427 no . . . C(1) C(2) H(3) 110.410 no . . . C(1) C(2) H(4) 110.415 no . . . H(3) C(2) H(4) 108.621 no . . . N(2) C(3) H(5) 122.065 no . . . C(4) C(3) H(5) 122.071 no . . . N(3) C(5) H(6) 124.044 no . . . N(4) C(5) H(6) 124.048 no . . . N(4) C(6) H(8) 125.379 no . . . C(4) C(6) H(8) 125.373 no . . . N(4) H(7) H(7) 156.418 no . . 4_556 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 Fe(1) N(1) 3.092(7) no . . Fe(1) C(2) 3.068(6) no . 2_665 Fe(1) C(2) 3.067(6) no . 3_565 Fe(1) C(3) 2.799(5) no . 2_665 Fe(1) C(3) 2.798(5) no . 3_565 Fe(1) C(4) 2.826(6) no . 2_665 Fe(1) C(4) 2.825(6) no . 3_565 Fe(1) C(5) 3.091(6) no . 2_665 Fe(1) C(5) 3.091(6) no . 3_565 Cr(1) C(8) 2.57(5) no . 2_555 Cr(1) C(8) 2.57(5) no . 3_555 Cr(1) C(8) 2.57(5) no . 4_556 Cr(1) C(8) 2.57(5) no . 5_556 Cr(1) C(7) 2.79(3) no . 2_555 Cr(1) C(7) 2.79(3) no . 3_555 Cr(1) C(7) 2.79(3) no . 4_556 Cr(1) C(7) 2.79(3) no . 5_556 O(1) C(8) 3.29(6) no . 2_555 O(1) C(8) 3.15(4) no . 5_556 O(1) C(7) 3.15(4) no . 5_556 O(2) O(3) 3.43(6) no . . O(2) O(3) 3.26(6) no . 6_556 O(2) O(4) 3.36(4) no . 3_555 O(2) C(8) 3.28(6) no . 6_556 O(2) C(7) 3.26(4) no . 3_555 O(3) O(4) 3.29(6) no . . O(3) O(4) 3.08(6) no . 6_556 N(1) N(2) 2.806(7) no . . N(1) N(2) 2.806(7) no . 2_665 N(1) N(2) 2.805(7) no . 3_565 N(1) C(2) 2.454(7) no . 2_665 N(1) C(2) 2.453(7) no . 3_565 N(2) C(1) 3.596(9) no . 2_665 N(2) C(2) 3.255(8) no . 2_665 N(2) C(4) 3.594(8) no . 3_565 N(2) C(5) 3.561(7) no . 3_565 N(3) C(2) 3.551(7) no . 2_665 N(3) C(3) 3.338(8) no . 2_665 N(3) C(4) 3.379(8) no . 2_665 N(3) C(5) 3.210(8) no . 3_565 N(4) N(4) 2.722(8) no . 4_556 C(1) C(2) 3.177(11) no . 2_665 C(1) C(3) 3.324(8) no . . C(3) C(5) 3.467(7) no . . C(4) C(5) 3.569(9) no . 3_565 O(1) C(6) 3.35(2) no . 2_555 O(1) C(6) 3.59(3) no . 6_556 O(2) O(5) 3.13(2) no . . O(2) O(5) 3.39(3) no . 2_555 O(2) C(6) 3.553(16) no . 4_556 O(3) C(1) 3.36(6) no . 6_555 O(3) C(5) 3.36(6) no . 5_566 O(4) O(5) 2.74(6) no . . O(4) O(5) 3.04(6) no . 2_555 O(4) N(2) 3.60(3) no . 1_556 O(4) C(2) 3.17(4) no . 1_556 O(4) C(3) 3.15(3) no . 1_556 O(4) C(3) 3.23(3) no . 6_556 O(4) C(4) 3.57(3) no . 6_556 O(5) O(2) 3.13(2) no . . O(5) O(2) 3.39(3) no . 3_555 O(5) O(2) 3.13(2) no . 4_557 O(5) O(2) 3.39(3) no . 6_557 O(5) O(4) 2.74(6) no . . O(5) O(4) 3.04(6) no . 3_555 O(5) O(4) 2.74(6) no . 4_557 O(5) O(4) 3.04(6) no . 6_557 O(5) O(5) 2.06(7) no . 2_555 O(5) O(5) 2.06(7) no . 3_555 O(5) C(3) 3.59(5) no . 1_556 O(5) C(3) 3.59(5) no . 4_556 N(2) O(4) 3.60(3) no . 1_554 C(1) O(3) 3.36(6) no . 6_555 C(2) O(4) 3.17(4) no . 1_554 C(3) O(4) 3.15(3) no . 1_554 C(3) O(4) 3.23(3) no . 6_556 C(3) O(5) 3.59(5) no . 1_554 C(4) O(4) 3.57(3) no . 6_556 C(5) O(3) 3.36(6) no . 5_666 C(6) O(1) 3.35(2) no . 3_555 C(6) O(1) 3.59(3) no . 6_556 C(6) O(2) 3.553(16) no . 4_556 C(6) C(8) 3.55(3) no . 6_556 C(6) C(7) 3.34(3) no . 6_556 C(8) C(6) 3.55(3) no . 6_556 C(7) C(6) 3.34(3) no . 6_556 Fe(1) H(3) 3.1412 no . . Fe(1) H(3) 3.1421 no . 2_665 Fe(1) H(3) 3.1413 no . 3_565 Fe(1) H(6) 3.3801 no . . Fe(1) H(6) 3.3794 no . 2_665 Fe(1) H(6) 3.3796 no . 3_565 N(1) H(1) 1.9836 no . 2_665 N(1) H(1) 1.9826 no . 3_565 N(1) H(2) 1.9839 no . 2_665 N(1) H(2) 1.9828 no . 3_565 N(1) H(3) 2.6897 no . . N(1) H(3) 2.6908 no . 2_665 N(1) H(3) 2.6898 no . 3_565 N(1) H(4) 3.2851 no . . N(1) H(4) 3.2858 no . 2_665 N(1) H(4) 3.2846 no . 3_565 N(2) H(1) 2.6583 no . . N(2) H(2) 3.2900 no . . N(2) H(3) 2.8135 no . 2_665 N(3) H(3) 3.2613 no . 2_665 N(3) H(5) 3.2137 no . . N(3) H(6) 2.9243 no . 3_565 N(3) H(7) 3.0326 no . . N(3) H(8) 3.1050 no . . C(1) H(1) 3.2367 no . 2_665 C(1) H(1) 2.4542 no . 3_565 C(1) H(2) 2.5545 no . 2_665 C(1) H(2) 3.0127 no . 3_565 C(1) H(3) 2.9552 no . 2_665 C(1) H(5) 3.4800 no . . C(2) H(1) 2.9422 no . 3_565 C(2) H(3) 3.5101 no . 2_665 C(2) H(5) 2.5749 no . . C(3) H(1) 3.2072 no . . C(3) H(3) 3.0918 no . . C(3) H(3) 3.0435 no . 2_665 C(3) H(4) 2.4939 no . . C(3) H(6) 3.5950 no . 3_565 C(3) H(8) 2.9891 no . . C(4) H(3) 3.3229 no . 2_665 C(4) H(6) 3.0604 no . . C(4) H(6) 3.1331 no . 3_565 C(4) H(7) 3.0317 no . . C(5) H(6) 3.2474 no . 3_565 C(5) H(7) 2.8148 no . 4_556 C(5) H(8) 3.0389 no . . C(6) H(5) 2.9582 no . . C(6) H(6) 3.0348 no . . C(6) H(6) 3.5630 no . 3_565 C(6) H(7) 2.9306 no . 4_556 H(1) H(1) 3.3715 no . 2_665 H(1) H(1) 3.3715 no . 3_565 H(1) H(2) 2.3028 no . 2_665 H(1) H(3) 2.8756 no . . H(1) H(3) 2.5141 no . 2_665 H(1) H(4) 2.3845 no . . H(1) H(5) 3.2339 no . . H(2) H(2) 2.9405 no . 2_665 H(2) H(2) 2.9405 no . 3_565 H(2) H(3) 2.3920 no . . H(2) H(4) 2.4179 no . . H(3) H(5) 3.3456 no . . H(3) H(5) 3.5111 no . 3_565 H(4) H(5) 2.3091 no . . H(5) H(8) 3.0522 no . . H(6) H(7) 2.3729 no . . H(6) H(7) 2.9665 no . 4_556 H(7) H(8) 2.3966 no . . H(7) H(8) 3.1813 no . 4_556 O(1) H(8) 2.5513 no . 2_555 O(1) H(8) 3.1361 no . 6_556 O(2) H(8) 2.6393 no . 4_556 O(2) H(8) 3.2810 no . 6_556 O(3) H(1) 3.1657 no . 6_555 O(3) H(2) 3.3869 no . 1_556 O(3) H(2) 2.8116 no . 6_555 O(3) H(4) 3.3643 no . 6_555 O(3) H(6) 2.9759 no . 3_565 O(3) H(6) 2.5674 no . 5_566 O(4) H(1) 3.2134 no . 1_556 O(4) H(4) 2.3682 no . 1_556 O(4) H(5) 2.3323 no . 1_556 O(4) H(5) 2.7240 no . 6_556 O(4) H(8) 2.9617 no . 4_556 O(4) H(8) 3.2870 no . 6_556 O(5) H(5) 2.7958 no . 1_556 O(5) H(5) 2.7958 no . 4_556 O(5) H(8) 3.3321 no . 1_556 O(5) H(8) 3.3321 no . 4_556 N(2) H(4) 3.5019 no . 6_555 N(3) H(3) 3.4925 no . 5_665 N(4) H(1) 3.3088 no . 4_555 N(4) H(2) 3.4033 no . 2_666 N(4) H(2) 3.2314 no . 5_665 N(4) H(3) 3.1626 no . 5_665 C(1) H(6) 3.4175 no . 3_564 C(3) H(4) 3.2951 no . 6_555 C(4) H(3) 3.4453 no . 5_665 C(5) H(2) 3.0981 no . 2_666 C(5) H(3) 3.3111 no . 5_665 C(5) H(4) 3.3079 no . 5_665 C(6) H(1) 3.3750 no . 4_555 C(6) H(3) 3.2375 no . 5_665 C(8) H(1) 3.5519 no . 1_556 C(8) H(4) 3.3656 no . 1_556 C(8) H(8) 2.8840 no . 4_556 C(8) H(8) 3.0568 no . 6_556 C(7) H(6) 3.4052 no . 5_566 C(7) H(8) 3.0742 no . 6_556 H(1) O(3) 3.1657 no . 6_555 H(1) O(4) 3.2134 no . 1_554 H(1) N(4) 3.3088 no . 4_555 H(1) C(6) 3.3750 no . 4_555 H(1) C(8) 3.5519 no . 1_554 H(1) H(6) 3.5729 no . 3_564 H(1) H(7) 3.5012 no . 1_554 H(1) H(7) 3.0754 no . 4_555 H(1) H(8) 3.1837 no . 4_555 H(2) O(3) 3.3869 no . 1_554 H(2) O(3) 2.8116 no . 6_555 H(2) N(4) 3.4033 no . 3_564 H(2) N(4) 3.2314 no . 5_565 H(2) C(5) 3.0981 no . 3_564 H(2) H(6) 2.5248 no . 3_564 H(2) H(7) 3.1968 no . 3_564 H(2) H(7) 2.9139 no . 5_565 H(3) N(3) 3.4925 no . 5_565 H(3) N(4) 3.1626 no . 5_565 H(3) C(4) 3.4453 no . 5_565 H(3) C(5) 3.3111 no . 5_565 H(3) C(6) 3.2375 no . 5_565 H(3) H(3) 3.3101 no . 6_555 H(3) H(4) 3.5632 no . 6_555 H(3) H(7) 3.4477 no . 5_565 H(4) O(3) 3.3643 no . 6_555 H(4) O(4) 2.3682 no . 1_554 H(4) N(2) 3.5019 no . 6_555 H(4) C(3) 3.2951 no . 6_555 H(4) C(5) 3.3079 no . 5_565 H(4) C(8) 3.3656 no . 1_554 H(4) H(3) 3.5632 no . 6_555 H(4) H(4) 3.2146 no . 6_555 H(4) H(5) 3.1624 no . 6_555 H(4) H(6) 3.3314 no . 5_565 H(5) O(4) 2.3323 no . 1_554 H(5) O(4) 2.7240 no . 6_556 H(5) O(5) 2.7958 no . 1_554 H(5) H(4) 3.1624 no . 6_555 H(5) H(5) 3.2237 no . 6_555 H(5) H(8) 3.5853 no . 4_555 H(6) O(3) 2.9759 no . 2_665 H(6) O(3) 2.5674 no . 5_666 H(6) C(1) 3.4175 no . 2_666 H(6) C(7) 3.4052 no . 5_666 H(6) H(1) 3.5729 no . 2_666 H(6) H(2) 2.5248 no . 2_666 H(6) H(4) 3.3314 no . 5_665 H(7) H(1) 3.5012 no . 1_556 H(7) H(1) 3.0754 no . 4_555 H(7) H(2) 3.1968 no . 2_666 H(7) H(2) 2.9139 no . 5_665 H(7) H(3) 3.4477 no . 5_665 H(8) O(1) 2.5513 no . 3_555 H(8) O(1) 3.1361 no . 6_556 H(8) O(2) 2.6393 no . 4_556 H(8) O(2) 3.2810 no . 6_556 H(8) O(4) 2.9617 no . 4_556 H(8) O(4) 3.2870 no . 6_556 H(8) O(5) 3.3321 no . 1_554 H(8) C(8) 2.8840 no . 4_556 H(8) C(8) 3.0568 no . 6_556 H(8) C(7) 3.0742 no . 6_556 H(8) H(1) 3.1837 no . 4_555 H(8) H(5) 3.5853 no . 4_555 #============================================================================== 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 N(4) H(7) N(4) . . 4_556 2.722(8) 0.860 1.878 166.8 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