# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Prof Jie Zhang' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences Fuzhou, Fujian, 350002, CHINA ; _publ_contact_author_email Zhangjie@fjirsm.ac.cn loop_ _publ_author_name _publ_author_address 'Chun-Ding Zhou' ;State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences Fuzhou, Fujian, 350002, CHINA ; 'Chao Chen' ;State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences Fuzhou, Fujian, 350002, CHINA ; 'Li-Xuan Cai' ;State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences Fuzhou, Fujian, 350002, CHINA ; 'Jie Zhang' ;State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences Fuzhou, Fujian, 350002, CHINA ; data_Fe1 _database_code_depnum_ccdc_archive 'CCDC 850154' #TrackingRef '- Fe1-ZCD-R.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H14 Fe3 N4 O16, 2(H2 O)' _chemical_formula_sum 'C12 H18 Fe3 N4 O18' _chemical_formula_weight 673.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.505(9) _cell_length_b 9.049(10) _cell_length_c 9.245(11) _cell_angle_alpha 111.494(7) _cell_angle_beta 107.567(15) _cell_angle_gamma 99.924(2) _cell_volume 527.9(11) _cell_formula_units_Z 1 _cell_measurement_temperature 294 _cell_measurement_reflns_used 606 _cell_measurement_theta_min 2.5523 _cell_measurement_theta_max 27.4487 _exptl_crystal_description Prism _exptl_crystal_colour black _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.120 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 340 _exptl_absorpt_coefficient_mu 2.137 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8010 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku SCXmini diffractometer' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 4170 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2402 _reflns_number_gt 1849 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2402 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0589 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0867 _refine_ls_wR_factor_gt 0.0792 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.11101(7) 0.24631(5) 0.77182(5) 0.02015(15) Uani 1 1 d . . . Fe2 Fe 0.0000 0.0000 0.0000 0.01915(17) Uani 1 2 d S . . O1 O 0.1916(4) 0.5039(3) 0.8464(3) 0.0258(5) Uani 1 1 d . . . O2 O 0.3202(4) 0.7074(3) 0.7921(3) 0.0337(6) Uani 1 1 d . . . O3 O 0.3366(4) 0.5041(3) 0.1949(3) 0.0328(6) Uani 1 1 d . . . O4 O 0.1385(4) 0.2424(3) 0.0107(3) 0.0249(5) Uani 1 1 d . . . O5 O -0.0612(4) 0.0032(3) 0.3380(3) 0.0272(6) Uani 1 1 d . . . N1 N 0.1061(4) 0.2699(3) 0.5402(3) 0.0189(6) Uani 1 1 d . . . N2 N 0.0951(4) 0.1796(3) 0.2601(3) 0.0170(6) Uani 1 1 d . . . C1 C 0.2413(5) 0.5573(4) 0.7523(4) 0.0210(7) Uani 1 1 d . . . C2 C 0.1990(5) 0.4275(4) 0.5744(3) 0.0164(6) Uani 1 1 d . . . C3 C 0.2456(5) 0.4678(4) 0.4578(4) 0.0222(7) Uani 1 1 d . . . H3 H 0.3104 0.5774 0.4841 0.027 Uiso 1 1 calc R . . C4 C 0.1912(5) 0.3374(4) 0.2995(4) 0.0169(6) Uani 1 1 d . . . C5 C 0.2276(5) 0.3660(4) 0.1580(4) 0.0204(7) Uani 1 1 d . . . C6 C 0.0474(5) 0.1466(4) 0.3782(4) 0.0188(7) Uani 1 1 d . . . O1W O 0.4253(3) 0.2664(3) 0.8541(3) 0.0292(6) Uani 1 1 d . . . H1 H 0.5004 0.3408 0.8501 0.044 Uiso 1 1 d R . . H2 H 0.4733 0.2707 0.9484 0.044 Uiso 1 1 d R . . O2W O -0.1977(4) 0.2146(3) 0.7138(3) 0.0386(7) Uani 1 1 d . . . H4 H -0.2195 0.3016 0.7609 0.058 Uiso 1 1 d R . . H5 H -0.2347 0.1834 0.6113 0.058 Uiso 1 1 d R . . O3W O 0.2726(4) -0.0415(3) 0.0451(3) 0.0413(7) Uani 1 1 d . . . H6 H 0.3528 -0.0142 0.1407 0.062 Uiso 1 1 d R . . H7 H 0.2715 -0.1295 -0.0254 0.062 Uiso 1 1 d R . . O4W O 0.4157(4) 0.9165(4) 0.6328(4) 0.0565(9) Uani 1 1 d . . . H8 H 0.3649 0.8505 0.6617 0.085 Uiso 1 1 d R . . H9 H 0.3893 1.0038 0.6672 0.085 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0283(3) 0.0163(3) 0.0151(2) 0.00711(19) 0.0096(2) 0.0032(2) Fe2 0.0272(4) 0.0165(4) 0.0127(3) 0.0054(3) 0.0093(3) 0.0048(3) O1 0.0438(16) 0.0182(12) 0.0148(10) 0.0061(9) 0.0150(11) 0.0050(10) O2 0.0565(18) 0.0165(13) 0.0250(13) 0.0043(10) 0.0234(13) 0.0028(12) O3 0.0471(17) 0.0224(14) 0.0236(12) 0.0082(11) 0.0172(12) -0.0027(12) O4 0.0412(15) 0.0197(12) 0.0138(10) 0.0071(10) 0.0144(11) 0.0040(10) O5 0.0434(16) 0.0126(12) 0.0184(11) 0.0037(9) 0.0136(11) -0.0027(10) N1 0.0276(16) 0.0155(14) 0.0135(12) 0.0060(11) 0.0098(12) 0.0045(11) N2 0.0239(15) 0.0147(13) 0.0118(11) 0.0052(10) 0.0087(11) 0.0035(11) C1 0.0300(19) 0.0144(16) 0.0159(15) 0.0038(13) 0.0101(14) 0.0059(14) C2 0.0225(17) 0.0149(16) 0.0099(13) 0.0030(12) 0.0081(13) 0.0045(13) C3 0.0291(19) 0.0145(16) 0.0228(16) 0.0081(14) 0.0130(15) 0.0025(13) C4 0.0224(17) 0.0159(16) 0.0146(14) 0.0080(12) 0.0100(13) 0.0042(13) C5 0.0284(19) 0.0188(17) 0.0148(15) 0.0081(13) 0.0093(14) 0.0067(14) C6 0.0242(18) 0.0177(17) 0.0140(14) 0.0068(13) 0.0072(13) 0.0069(14) O1W 0.0281(14) 0.0304(14) 0.0279(13) 0.0145(11) 0.0110(11) 0.0036(11) O2W 0.0375(16) 0.0391(16) 0.0416(15) 0.0182(13) 0.0183(13) 0.0126(13) O3W 0.0357(16) 0.0497(17) 0.0236(13) 0.0024(12) 0.0050(12) 0.0229(13) O4W 0.047(2) 0.0446(19) 0.0549(19) 0.0072(16) 0.0088(16) 0.0149(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O5 2.017(3) 2_556 ? Fe1 O1 2.088(3) . ? Fe1 O2W 2.156(4) . ? Fe1 O4 2.169(3) 1_556 ? Fe1 O1W 2.201(4) . ? Fe1 N1 2.219(3) . ? Fe2 O3W 2.089(3) . ? Fe2 O3W 2.089(3) 2 ? Fe2 N2 2.152(3) 2 ? Fe2 N2 2.152(3) . ? Fe2 O4 2.212(3) . ? Fe2 O4 2.212(3) 2 ? O1 C1 1.253(4) . ? O2 C1 1.248(4) . ? O3 C5 1.230(4) . ? O4 C5 1.277(4) . ? O4 Fe1 2.169(3) 1_554 ? O5 C6 1.259(4) . ? O5 Fe1 2.017(3) 2_556 ? N1 C2 1.347(4) . ? N1 C6 1.375(4) . ? N2 C4 1.341(4) . ? N2 C6 1.360(4) . ? C1 C2 1.525(4) . ? C2 C3 1.374(4) . ? C3 C4 1.382(4) . ? C3 H3 0.9300 . ? C4 C5 1.514(4) . ? O1W H1 0.8199 . ? O1W H2 0.8202 . ? O2W H4 0.8200 . ? O2W H5 0.8200 . ? O3W H6 0.8201 . ? O3W H7 0.8200 . ? O4W H8 0.8200 . ? O4W H9 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Fe1 O1 166.96(9) 2_556 . ? O5 Fe1 O2W 92.41(10) 2_556 . ? O1 Fe1 O2W 94.70(10) . . ? O5 Fe1 O4 90.46(10) 2_556 1_556 ? O1 Fe1 O4 100.67(9) . 1_556 ? O2W Fe1 O4 88.22(10) . 1_556 ? O5 Fe1 O1W 85.22(9) 2_556 . ? O1 Fe1 O1W 88.95(9) . . ? O2W Fe1 O1W 172.85(9) . . ? O4 Fe1 O1W 85.06(9) 1_556 . ? O5 Fe1 N1 93.06(10) 2_556 . ? O1 Fe1 N1 75.43(9) . . ? O2W Fe1 N1 95.16(10) . . ? O4 Fe1 N1 175.01(9) 1_556 . ? O1W Fe1 N1 91.71(10) . . ? O3W Fe2 O3W 180.00(13) . 2 ? O3W Fe2 N2 87.88(10) . 2 ? O3W Fe2 N2 92.12(10) 2 2 ? O3W Fe2 N2 92.12(10) . . ? O3W Fe2 N2 87.88(10) 2 . ? N2 Fe2 N2 180.00(10) 2 . ? O3W Fe2 O4 88.43(12) . . ? O3W Fe2 O4 91.57(12) 2 . ? N2 Fe2 O4 104.79(11) 2 . ? N2 Fe2 O4 75.21(11) . . ? O3W Fe2 O4 91.57(12) . 2 ? O3W Fe2 O4 88.43(12) 2 2 ? N2 Fe2 O4 75.21(11) 2 2 ? N2 Fe2 O4 104.79(11) . 2 ? O4 Fe2 O4 180.00(18) . 2 ? C1 O1 Fe1 118.63(19) . . ? C5 O4 Fe1 126.6(2) . 1_554 ? C5 O4 Fe2 116.2(2) . . ? Fe1 O4 Fe2 117.15(9) 1_554 . ? C6 O5 Fe1 147.0(2) . 2_556 ? C2 N1 C6 117.7(3) . . ? C2 N1 Fe1 112.28(19) . . ? C6 N1 Fe1 129.3(2) . . ? C4 N2 C6 119.3(2) . . ? C4 N2 Fe2 115.9(2) . . ? C6 N2 Fe2 124.5(2) . . ? O2 C1 O1 125.2(3) . . ? O2 C1 C2 117.8(3) . . ? O1 C1 C2 116.9(3) . . ? N1 C2 C3 123.0(3) . . ? N1 C2 C1 113.7(3) . . ? C3 C2 C1 123.3(3) . . ? C2 C3 C4 116.7(3) . . ? C2 C3 H3 121.7 . . ? C4 C3 H3 121.7 . . ? N2 C4 C3 121.9(3) . . ? N2 C4 C5 116.1(3) . . ? C3 C4 C5 121.8(3) . . ? O3 C5 O4 126.7(3) . . ? O3 C5 C4 117.8(3) . . ? O4 C5 C4 115.5(3) . . ? O5 C6 N2 120.1(3) . . ? O5 C6 N1 118.6(3) . . ? N2 C6 N1 121.2(3) . . ? Fe1 O1W H1 117.9 . . ? Fe1 O1W H2 113.5 . . ? H1 O1W H2 108.0 . . ? Fe1 O2W H4 113.5 . . ? Fe1 O2W H5 97.9 . . ? H4 O2W H5 112.0 . . ? Fe2 O3W H6 122.6 . . ? Fe2 O3W H7 115.1 . . ? H6 O3W H7 112.4 . . ? H8 O4W H9 110.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Fe1 O1 C1 14.0(6) 2_556 . . . ? O2W Fe1 O1 C1 -108.8(3) . . . . ? O4 Fe1 O1 C1 162.1(2) 1_556 . . . ? O1W Fe1 O1 C1 77.3(3) . . . . ? N1 Fe1 O1 C1 -14.7(2) . . . . ? O3W Fe2 O4 C5 -84.7(2) . . . . ? O3W Fe2 O4 C5 95.3(2) 2 . . . ? N2 Fe2 O4 C5 -172.0(2) 2 . . . ? N2 Fe2 O4 C5 8.0(2) . . . . ? O4 Fe2 O4 C5 83(71) 2 . . . ? O3W Fe2 O4 Fe1 95.10(12) . . . 1_554 ? O3W Fe2 O4 Fe1 -84.90(12) 2 . . 1_554 ? N2 Fe2 O4 Fe1 7.71(14) 2 . . 1_554 ? N2 Fe2 O4 Fe1 -172.29(14) . . . 1_554 ? O4 Fe2 O4 Fe1 -97(71) 2 . . 1_554 ? O5 Fe1 N1 C2 -158.9(2) 2_556 . . . ? O1 Fe1 N1 C2 14.8(2) . . . . ? O2W Fe1 N1 C2 108.4(2) . . . . ? O4 Fe1 N1 C2 -24.1(11) 1_556 . . . ? O1W Fe1 N1 C2 -73.6(2) . . . . ? O5 Fe1 N1 C6 11.5(3) 2_556 . . . ? O1 Fe1 N1 C6 -174.7(3) . . . . ? O2W Fe1 N1 C6 -81.2(3) . . . . ? O4 Fe1 N1 C6 146.3(9) 1_556 . . . ? O1W Fe1 N1 C6 96.8(3) . . . . ? O3W Fe2 N2 C4 85.5(2) . . . . ? O3W Fe2 N2 C4 -94.5(2) 2 . . . ? N2 Fe2 N2 C4 -118(5) 2 . . . ? O4 Fe2 N2 C4 -2.3(2) . . . . ? O4 Fe2 N2 C4 177.7(2) 2 . . . ? O3W Fe2 N2 C6 -101.3(3) . . . . ? O3W Fe2 N2 C6 78.7(3) 2 . . . ? N2 Fe2 N2 C6 55(5) 2 . . . ? O4 Fe2 N2 C6 170.9(3) . . . . ? O4 Fe2 N2 C6 -9.1(3) 2 . . . ? Fe1 O1 C1 O2 -168.7(3) . . . . ? Fe1 O1 C1 C2 12.1(4) . . . . ? C6 N1 C2 C3 -3.4(5) . . . . ? Fe1 N1 C2 C3 168.3(3) . . . . ? C6 N1 C2 C1 174.7(3) . . . . ? Fe1 N1 C2 C1 -13.6(3) . . . . ? O2 C1 C2 N1 -177.3(3) . . . . ? O1 C1 C2 N1 2.0(4) . . . . ? O2 C1 C2 C3 0.8(5) . . . . ? O1 C1 C2 C3 -179.9(3) . . . . ? N1 C2 C3 C4 0.3(5) . . . . ? C1 C2 C3 C4 -177.5(3) . . . . ? C6 N2 C4 C3 0.8(5) . . . . ? Fe2 N2 C4 C3 174.3(2) . . . . ? C6 N2 C4 C5 -176.2(3) . . . . ? Fe2 N2 C4 C5 -2.7(3) . . . . ? C2 C3 C4 N2 1.0(5) . . . . ? C2 C3 C4 C5 177.9(3) . . . . ? Fe1 O4 C5 O3 -10.6(5) 1_554 . . . ? Fe2 O4 C5 O3 169.1(3) . . . . ? Fe1 O4 C5 C4 168.6(2) 1_554 . . . ? Fe2 O4 C5 C4 -11.7(3) . . . . ? N2 C4 C5 O3 -171.0(3) . . . . ? C3 C4 C5 O3 12.0(5) . . . . ? N2 C4 C5 O4 9.7(4) . . . . ? C3 C4 C5 O4 -167.3(3) . . . . ? Fe1 O5 C6 N2 51.4(5) 2_556 . . . ? Fe1 O5 C6 N1 -132.3(3) 2_556 . . . ? C4 N2 C6 O5 172.2(3) . . . . ? Fe2 N2 C6 O5 -0.7(4) . . . . ? C4 N2 C6 N1 -4.0(4) . . . . ? Fe2 N2 C6 N1 -176.9(2) . . . . ? C2 N1 C6 O5 -171.1(3) . . . . ? Fe1 N1 C6 O5 18.9(4) . . . . ? C2 N1 C6 N2 5.2(4) . . . . ? Fe1 N1 C6 N2 -164.8(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1 O3 0.82 1.94 2.758(4) 171.6 2_666 O1W H2 O2 0.82 2.34 3.148(5) 166.4 2_667 O1W H2 O1 0.82 2.57 3.028(4) 116.8 2_667 O2W H4 O3 0.82 2.06 2.854(4) 162.4 2_566 O2W H5 O4W 0.82 2.00 2.781(5) 159.8 2_566 O3W H6 O4W 0.82 2.03 2.835(4) 168.9 2_666 O3W H7 O2 0.82 1.97 2.766(4) 162.4 1_544 O4W H8 O2 0.82 2.12 2.911(5) 162.9 . O4W H9 O1W 0.82 2.28 3.050(5) 156.9 1_565 O4W H9 O5 0.82 2.44 2.938(5) 120.3 2_566 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.475 _refine_diff_density_min -0.584 _refine_diff_density_rms 0.099