# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email icsantos@itn.pt _publ_contact_author_name 'Isabel C. Santos' loop_ _publ_author_name 'Elisa Palma' 'Lurdes Gano' 'Bruno L. Oliveira' 'Joao D. G. Correia' 'Isabel C. Santos' 'Isabel Santos' data_bl41 #TrackingRef 'CCDC789827_CifFile.cif' _database_code_depnum_ccdc_archive 'CCDC 789827' #TrackingRef 'bl41.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H24 N4 O5 Re, C2 F3 O2, H2 O' _chemical_formula_sum 'C18 H26 F3 N4 O8 Re' _chemical_formula_weight 669.63 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.7619(2) _cell_length_b 20.2966(5) _cell_length_c 39.1115(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.4290(10) _cell_angle_gamma 90.00 _cell_volume 6924.3(3) _cell_formula_units_Z 12 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.927 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3936 _exptl_absorpt_coefficient_mu 5.341 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3605 _exptl_absorpt_correction_T_max 0.8562 _exptl_absorpt_process_details 'SADABS - Sheldrick 2004' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53647 _diffrn_reflns_av_R_equivalents 0.0823 _diffrn_reflns_av_sigmaI/netI 0.0725 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 25.68 _reflns_number_total 13125 _reflns_number_gt 9654 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL(Keller,1989),Ortep3(Farrugia,1997) _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0252P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13125 _refine_ls_number_parameters 928 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0738 _refine_ls_wR_factor_gt 0.0680 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.003 _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 Re1 Re -0.68415(3) -0.136218(13) 0.944305(7) 0.01859(7) Uani 1 1 d . . . Re2 Re -0.30512(3) 0.106276(13) 0.836598(7) 0.01669(7) Uani 1 1 d . . . Re3 Re 0.18370(3) 0.469976(13) 0.854914(7) 0.02058(7) Uani 1 1 d . . . O1 O -0.7557(5) 0.0041(2) 0.91847(12) 0.0311(11) Uani 1 1 d . . . O2 O -0.8244(5) -0.0909(2) 1.00879(13) 0.0394(13) Uani 1 1 d . . . O3 O -1.0136(5) -0.1811(3) 0.92266(14) 0.0440(14) Uani 1 1 d . . . O4 O -0.7752(4) 0.0017(2) 0.80312(12) 0.0284(11) Uani 1 1 d . . . O5 O -0.9767(5) -0.0414(2) 0.77495(12) 0.0285(11) Uani 1 1 d . . . H5 H -1.0294 -0.0759 0.7755 0.043 Uiso 1 1 calc R . . O6 O -0.0382(5) 0.0106(2) 0.85388(12) 0.0295(11) Uani 1 1 d . . . O7 O -0.3775(6) 0.0815(3) 0.91037(13) 0.0433(14) Uani 1 1 d . . . O8 O -0.0884(5) 0.2160(2) 0.86539(13) 0.0404(13) Uani 1 1 d . . . O9 O 0.3206(5) 0.1767(3) 0.70630(13) 0.0469(15) Uani 1 1 d . . . H9A H 0.3473 0.1769 0.6862 0.070 Uiso 1 1 calc R . . O10 O 0.1096(5) 0.1302(3) 0.68126(13) 0.0388(13) Uani 1 1 d . . . O11 O -0.1025(5) 0.5511(2) 0.83243(13) 0.0377(13) Uani 1 1 d . . . O12 O 0.2471(5) 0.4946(3) 0.78051(12) 0.0387(13) Uani 1 1 d . . . O13 O -0.0113(5) 0.3519(2) 0.82840(13) 0.0392(13) Uani 1 1 d . . . O14 O -0.4352(5) 0.3736(2) 0.98143(14) 0.0383(13) Uani 1 1 d . . . H14 H -0.4991 0.3860 0.9948 0.057 Uiso 1 1 calc R . . O15 O -0.3214(5) 0.4684(2) 0.99674(13) 0.0356(12) Uani 1 1 d . . . O16 O 0.1249(6) 0.3221(3) 1.00289(14) 0.0482(15) Uani 1 1 d . . . O17 O 0.3036(6) 0.2550(3) 0.98372(15) 0.0533(16) Uani 1 1 d . . . O18 O -0.6080(5) 0.1745(2) 0.64090(12) 0.0306(12) Uani 1 1 d . . . O19 O -0.4348(5) 0.1556(3) 0.60323(13) 0.0405(13) Uani 1 1 d . . . O20 O -0.3286(5) 0.3627(2) 0.73128(13) 0.0344(12) Uani 1 1 d . . . O21 O -0.2080(5) 0.4039(2) 0.68753(13) 0.0343(12) Uani 1 1 d . . . O1W O -0.6458(5) 0.4046(2) 1.02396(12) 0.0361(13) Uani 1 1 d . . . H11W H -0.5667 0.3821 1.0206 0.043 Uiso 1 1 d R . . H21W H -0.7036 0.3805 1.0350 0.043 Uiso 1 1 d R . . O2W O -0.6316(5) 0.1760(2) 0.54179(13) 0.0399(13) Uani 1 1 d . . . H12W H -0.5590 0.1782 0.5304 0.048 Uiso 1 1 d R . . H22W H -0.5702 0.1548 0.5627 0.048 Uiso 1 1 d R . . O3W O -0.1594(5) 0.0710(3) 0.59719(13) 0.0496(15) Uani 1 1 d . . . H13W H -0.2418 0.0872 0.5874 0.059 Uiso 1 1 d R . . H23W H -0.1202 0.0995 0.6113 0.059 Uiso 1 1 d R . . F1 F -0.0114(5) 0.2718(3) 0.93820(14) 0.0713(16) Uani 1 1 d . . . F2 F -0.0826(6) 0.2285(3) 0.98227(15) 0.092(2) Uani 1 1 d . . . F3 F 0.0790(7) 0.1790(3) 0.95414(17) 0.094(2) Uani 1 1 d . . . F4 F -0.3609(7) 0.2784(3) 0.64695(15) 0.0868(18) Uani 1 1 d . . . F5 F -0.2180(5) 0.1968(3) 0.64976(16) 0.096(2) Uani 1 1 d . . . F6 F -0.3743(6) 0.2091(3) 0.68578(13) 0.094(2) Uani 1 1 d . . . F7 F 0.0472(5) 0.3684(2) 0.72975(16) 0.0761(18) Uani 1 1 d . . . F8 F -0.0374(6) 0.2865(3) 0.70147(13) 0.0737(16) Uani 1 1 d . . . F9 F -0.0814(4) 0.2955(2) 0.75321(12) 0.0516(13) Uani 1 1 d . . . N1 N -0.4513(5) -0.1054(3) 0.96041(13) 0.0211(12) Uani 1 1 d . . . N2 N -0.3554(5) -0.0801(2) 0.93772(13) 0.0189(12) Uani 1 1 d . . . N3 N -0.5882(5) -0.1797(2) 0.89664(14) 0.0199(12) Uani 1 1 d . . . N4 N -0.6040(5) -0.2339(3) 0.96389(14) 0.0247(13) Uani 1 1 d . . . H4A H -0.5492 -0.2291 0.9850 0.030 Uiso 1 1 calc R . . H4B H -0.6870 -0.2606 0.9665 0.030 Uiso 1 1 calc R . . N5 N -0.5051(5) 0.1708(2) 0.82489(14) 0.0207(12) Uani 1 1 d . . . N6 N -0.4964(5) 0.2251(3) 0.80474(13) 0.0214(12) Uani 1 1 d . . . N7 N -0.2564(5) 0.1198(2) 0.78061(12) 0.0157(11) Uani 1 1 d . . . N8 N -0.4492(5) 0.0287(2) 0.81129(13) 0.0224(12) Uani 1 1 d . . . H8A H -0.4079 -0.0118 0.8172 0.027 Uiso 1 1 calc R . . H8B H -0.5456 0.0306 0.8188 0.027 Uiso 1 1 calc R . . N9 N 0.3950(6) 0.4122(3) 0.86822(14) 0.0259(13) Uani 1 1 d . . . N10 N 0.3924(6) 0.3581(3) 0.88885(14) 0.0238(13) Uani 1 1 d . . . N11 N 0.1317(5) 0.4588(3) 0.91045(13) 0.0213(12) Uani 1 1 d . . . N12 N 0.3116(5) 0.5545(3) 0.87900(13) 0.0226(12) Uani 1 1 d . . . H12D H 0.4120 0.5524 0.8740 0.027 Uiso 1 1 calc R . . H12E H 0.2701 0.5930 0.8699 0.027 Uiso 1 1 calc R . . C1 C -0.7306(6) -0.0499(3) 0.92727(17) 0.0206(15) Uani 1 1 d . . . C2 C -0.7666(7) -0.1081(3) 0.98553(18) 0.0268(16) Uani 1 1 d . . . C3 C -0.8884(8) -0.1657(3) 0.93017(18) 0.0288(17) Uani 1 1 d . . . C4 C -0.5055(7) -0.2647(3) 0.93930(17) 0.0259(16) Uani 1 1 d . . . H4D H -0.4965 -0.3126 0.9437 0.031 Uiso 1 1 calc R . . H4C H -0.4014 -0.2452 0.9422 0.031 Uiso 1 1 calc R . . C5 C -0.5771(7) -0.2526(3) 0.90352(17) 0.0259(16) Uani 1 1 d . . . H5A H -0.6807 -0.2725 0.9007 0.031 Uiso 1 1 calc R . . H5B H -0.5143 -0.2737 0.8868 0.031 Uiso 1 1 calc R . . C6 C -0.4328(6) -0.1553(3) 0.88917(17) 0.0202(15) Uani 1 1 d . . . H6A H -0.4256 -0.1579 0.8641 0.024 Uiso 1 1 calc R . . H6B H -0.3539 -0.1852 0.9004 0.024 Uiso 1 1 calc R . . C7 C -0.3967(7) -0.0859(3) 0.90089(16) 0.0216(15) Uani 1 1 d . . . H7A H -0.3110 -0.0690 0.8886 0.026 Uiso 1 1 calc R . . H7B H -0.4872 -0.0577 0.8945 0.026 Uiso 1 1 calc R . . C8 C -0.2239(7) -0.0572(3) 0.95421(17) 0.0229(15) Uani 1 1 d . . . C9 C -0.2344(7) -0.0670(3) 0.98850(17) 0.0246(16) Uani 1 1 d . . . H9 H -0.1592 -0.0557 1.0067 0.029 Uiso 1 1 calc R . . C10 C -0.3754(7) -0.0964(3) 0.99184(17) 0.0242(15) Uani 1 1 d . . . C11 C -0.1012(7) -0.0247(3) 0.93654(18) 0.0305(17) Uani 1 1 d . . . H11A H -0.0790 -0.0511 0.9166 0.046 Uiso 1 1 calc R . . H11B H -0.0083 -0.0208 0.9525 0.046 Uiso 1 1 calc R . . H11C H -0.1354 0.0193 0.9289 0.046 Uiso 1 1 calc R . . C12 C -0.4423(8) -0.1118(4) 1.02472(18) 0.0372(19) Uani 1 1 d . . . H12A H -0.5076 -0.0752 1.0307 0.056 Uiso 1 1 calc R . . H12B H -0.3594 -0.1182 1.0431 0.056 Uiso 1 1 calc R . . H12C H -0.5038 -0.1521 1.0219 0.056 Uiso 1 1 calc R . . C13 C -0.6961(7) -0.1738(3) 0.86436(17) 0.0235(15) Uani 1 1 d . . . H13A H -0.7984 -0.1895 0.8696 0.028 Uiso 1 1 calc R . . H13B H -0.6601 -0.2043 0.8470 0.028 Uiso 1 1 calc R . . C14 C -0.7160(7) -0.1052(3) 0.84786(16) 0.0236(15) Uani 1 1 d . . . H14A H -0.7416 -0.0727 0.8653 0.028 Uiso 1 1 calc R . . H14B H -0.6190 -0.0914 0.8389 0.028 Uiso 1 1 calc R . . C15 C -0.8435(7) -0.1073(3) 0.81870(17) 0.0253(16) Uani 1 1 d . . . H15A H -0.8230 -0.1439 0.8030 0.030 Uiso 1 1 calc R . . H15B H -0.9416 -0.1169 0.8283 0.030 Uiso 1 1 calc R . . C16 C -0.8607(6) -0.0448(3) 0.79842(17) 0.0218(15) Uani 1 1 d . . . C17 C -0.1365(7) 0.0465(3) 0.84648(17) 0.0223(15) Uani 1 1 d . . . C18 C -0.3539(7) 0.0910(3) 0.88241(19) 0.0239(16) Uani 1 1 d . . . C19 C -0.1714(7) 0.1747(3) 0.85419(17) 0.0259(16) Uani 1 1 d . . . C20 C -0.4612(7) 0.0365(3) 0.77305(17) 0.0272(16) Uani 1 1 d . . . H20A H -0.5396 0.0700 0.7657 0.033 Uiso 1 1 calc R . . H20B H -0.4921 -0.0058 0.7618 0.033 Uiso 1 1 calc R . . C21 C -0.3066(7) 0.0577(3) 0.76276(17) 0.0250(16) Uani 1 1 d . . . H21A H -0.2303 0.0226 0.7688 0.030 Uiso 1 1 calc R . . H21B H -0.3132 0.0645 0.7376 0.030 Uiso 1 1 calc R . . C22 C -0.3397(7) 0.1761(3) 0.76284(17) 0.0262(16) Uani 1 1 d . . . H22A H -0.4410 0.1602 0.7528 0.031 Uiso 1 1 calc R . . H22B H -0.2816 0.1906 0.7437 0.031 Uiso 1 1 calc R . . C23 C -0.3641(7) 0.2345(3) 0.78523(16) 0.0229(15) Uani 1 1 d . . . H23A H -0.2713 0.2415 0.8013 0.027 Uiso 1 1 calc R . . H23B H -0.3798 0.2743 0.7707 0.027 Uiso 1 1 calc R . . C24 C -0.6270(7) 0.2606(3) 0.80286(16) 0.0208(15) Uani 1 1 d . . . C25 C -0.7222(7) 0.2286(3) 0.82388(16) 0.0230(15) Uani 1 1 d . . . H25 H -0.8222 0.2420 0.8284 0.028 Uiso 1 1 calc R . . C26 C -0.6457(6) 0.1743(3) 0.83686(16) 0.0200(15) Uani 1 1 d . . . C27 C -0.6498(8) 0.3203(3) 0.78121(18) 0.0332(18) Uani 1 1 d . . . H27A H -0.5630 0.3503 0.7863 0.050 Uiso 1 1 calc R . . H27B H -0.7448 0.3423 0.7861 0.050 Uiso 1 1 calc R . . H27C H -0.6567 0.3077 0.7569 0.050 Uiso 1 1 calc R . . C28 C -0.7059(7) 0.1244(3) 0.86066(18) 0.0288(17) Uani 1 1 d . . . H28A H -0.6914 0.0800 0.8517 0.043 Uiso 1 1 calc R . . H28B H -0.8154 0.1322 0.8623 0.043 Uiso 1 1 calc R . . H28C H -0.6502 0.1285 0.8835 0.043 Uiso 1 1 calc R . . C29 C -0.0858(6) 0.1299(3) 0.77832(16) 0.0199(14) Uani 1 1 d . . . H29A H -0.0290 0.0975 0.7936 0.024 Uiso 1 1 calc R . . H29B H -0.0576 0.1743 0.7872 0.024 Uiso 1 1 calc R . . C30 C -0.0328(7) 0.1231(3) 0.74223(16) 0.0225(15) Uani 1 1 d . . . H30A H -0.0400 0.0764 0.7349 0.027 Uiso 1 1 calc R . . H30B H -0.1007 0.1494 0.7258 0.027 Uiso 1 1 calc R . . C31 C 0.1312(7) 0.1467(3) 0.74178(16) 0.0261(16) Uani 1 1 d . . . H31A H 0.1404 0.1914 0.7519 0.031 Uiso 1 1 calc R . . H31B H 0.1998 0.1171 0.7563 0.031 Uiso 1 1 calc R . . C32 C 0.1828(7) 0.1487(3) 0.70626(19) 0.0268(16) Uani 1 1 d . . . C33 C 0.0056(8) 0.5220(3) 0.84233(17) 0.0263(16) Uani 1 1 d . . . C34 C 0.2296(7) 0.4848(3) 0.80864(18) 0.0248(16) Uani 1 1 d . . . C35 C 0.0646(7) 0.3958(3) 0.83835(18) 0.0272(16) Uani 1 1 d . . . C36 C 0.3070(7) 0.5551(3) 0.91670(16) 0.0270(16) Uani 1 1 d . . . H36A H 0.3165 0.6009 0.9253 0.032 Uiso 1 1 calc R . . H36B H 0.3942 0.5293 0.9277 0.032 Uiso 1 1 calc R . . C37 C 0.1576(7) 0.5256(3) 0.92591(16) 0.0238(15) Uani 1 1 d . . . H37A H 0.1594 0.5224 0.9512 0.029 Uiso 1 1 calc R . . H37B H 0.0718 0.5550 0.9176 0.029 Uiso 1 1 calc R . . C38 C 0.2342(7) 0.4095(3) 0.93030(16) 0.0245(16) Uani 1 1 d . . . H38A H 0.1852 0.3961 0.9510 0.029 Uiso 1 1 calc R . . H38B H 0.3324 0.4313 0.9381 0.029 Uiso 1 1 calc R . . C39 C 0.2678(7) 0.3484(3) 0.91023(17) 0.0269(16) Uani 1 1 d . . . H39A H 0.2945 0.3119 0.9265 0.032 Uiso 1 1 calc R . . H39B H 0.1744 0.3355 0.8955 0.032 Uiso 1 1 calc R . . C40 C 0.5217(7) 0.3210(3) 0.88826(17) 0.0258(16) Uani 1 1 d . . . C41 C 0.6073(7) 0.3522(3) 0.86581(18) 0.0285(17) Uani 1 1 d . . . H41 H 0.7035 0.3379 0.8592 0.034 Uiso 1 1 calc R . . C42 C 0.5283(7) 0.4092(3) 0.85415(17) 0.0268(16) Uani 1 1 d . . . C43 C 0.5518(8) 0.2612(3) 0.90973(19) 0.0372(19) Uani 1 1 d . . . H43A H 0.4718 0.2284 0.9036 0.056 Uiso 1 1 calc R . . H43B H 0.5513 0.2729 0.9340 0.056 Uiso 1 1 calc R . . H43C H 0.6520 0.2428 0.9057 0.056 Uiso 1 1 calc R . . C44 C 0.5804(8) 0.4598(4) 0.83028(19) 0.040(2) Uani 1 1 d . . . H44A H 0.5195 0.4563 0.8080 0.060 Uiso 1 1 calc R . . H44B H 0.6889 0.4527 0.8272 0.060 Uiso 1 1 calc R . . H44C H 0.5672 0.5038 0.8399 0.060 Uiso 1 1 calc R . . C45 C -0.0312(6) 0.4382(3) 0.91305(16) 0.0232(15) Uani 1 1 d . . . H45A H -0.0418 0.3915 0.9059 0.028 Uiso 1 1 calc R . . H45B H -0.0980 0.4646 0.8964 0.028 Uiso 1 1 calc R . . C46 C -0.0907(7) 0.4453(3) 0.94835(17) 0.0279(16) Uani 1 1 d . . . H46A H -0.1019 0.4925 0.9540 0.033 Uiso 1 1 calc R . . H46B H -0.0174 0.4251 0.9661 0.033 Uiso 1 1 calc R . . C47 C -0.2462(8) 0.4107(4) 0.94756(19) 0.038(2) Uani 1 1 d . . . H47A H -0.3108 0.4259 0.9269 0.046 Uiso 1 1 calc R . . H47B H -0.2296 0.3628 0.9450 0.046 Uiso 1 1 calc R . . C48 C -0.3335(7) 0.4212(3) 0.97823(18) 0.0257(16) Uani 1 1 d . . . C49 C 0.1712(9) 0.2740(4) 0.9867(2) 0.040(2) Uani 1 1 d . . . C50 C 0.0435(10) 0.2366(4) 0.9656(2) 0.048(2) Uani 1 1 d . . . C51 C -0.4783(7) 0.1775(3) 0.63057(17) 0.0209(15) Uani 1 1 d . . . C52 C -0.3581(7) 0.2139(4) 0.6536(2) 0.0330(18) Uani 1 1 d . . . C53 C -0.2171(8) 0.3688(3) 0.71366(19) 0.0290(16) Uani 1 1 d . . . C54 C -0.0736(8) 0.3302(4) 0.7252(2) 0.0344(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01755(12) 0.01843(14) 0.02020(15) -0.00037(11) 0.00395(10) -0.00257(11) Re2 0.01571(12) 0.01839(14) 0.01643(14) 0.00245(11) 0.00390(10) 0.00147(10) Re3 0.02156(13) 0.02403(15) 0.01616(15) 0.00177(12) 0.00177(11) -0.00213(11) O1 0.035(3) 0.026(3) 0.033(3) 0.004(2) 0.008(2) -0.001(2) O2 0.043(3) 0.041(3) 0.038(3) 0.000(3) 0.023(3) -0.004(2) O3 0.022(3) 0.046(4) 0.064(4) -0.007(3) 0.002(3) -0.008(2) O4 0.020(2) 0.028(3) 0.036(3) 0.004(2) 0.001(2) -0.006(2) O5 0.023(2) 0.031(3) 0.031(3) 0.004(2) -0.001(2) 0.000(2) O6 0.026(2) 0.035(3) 0.028(3) 0.005(2) 0.005(2) 0.014(2) O7 0.052(3) 0.054(4) 0.027(3) 0.010(3) 0.019(3) 0.016(3) O8 0.040(3) 0.037(3) 0.043(4) -0.008(3) 0.000(3) -0.013(3) O9 0.028(3) 0.083(4) 0.032(3) -0.012(3) 0.013(2) -0.025(3) O10 0.026(3) 0.065(4) 0.027(3) -0.011(3) 0.014(2) -0.010(3) O11 0.028(3) 0.041(3) 0.042(3) 0.000(3) -0.010(2) 0.002(2) O12 0.046(3) 0.052(4) 0.018(3) 0.005(3) 0.004(2) -0.002(3) O13 0.040(3) 0.035(3) 0.042(4) -0.008(3) 0.000(3) -0.010(3) O14 0.033(3) 0.042(3) 0.042(4) -0.009(3) 0.017(2) -0.012(2) O15 0.042(3) 0.031(3) 0.034(3) -0.008(3) 0.008(2) -0.003(2) O16 0.049(3) 0.049(4) 0.049(4) -0.011(3) 0.017(3) -0.012(3) O17 0.055(4) 0.045(4) 0.060(4) -0.004(3) 0.003(3) 0.001(3) O18 0.019(2) 0.040(3) 0.032(3) 0.001(2) 0.005(2) -0.001(2) O19 0.041(3) 0.057(4) 0.026(3) -0.013(3) 0.013(2) -0.006(3) O20 0.026(2) 0.039(3) 0.039(3) 0.008(3) 0.004(2) 0.007(2) O21 0.038(3) 0.029(3) 0.035(3) 0.007(2) -0.002(2) -0.001(2) O1W 0.029(3) 0.044(3) 0.037(3) 0.000(3) 0.012(2) 0.000(2) O2W 0.032(3) 0.039(3) 0.049(4) 0.010(3) 0.007(2) 0.009(2) O3W 0.039(3) 0.064(4) 0.044(4) -0.010(3) -0.002(3) 0.012(3) F1 0.065(3) 0.075(4) 0.069(4) 0.015(3) -0.019(3) -0.012(3) F2 0.099(4) 0.098(5) 0.083(5) -0.021(4) 0.034(4) -0.065(4) F3 0.095(4) 0.058(4) 0.120(6) -0.039(4) -0.028(4) 0.007(3) F4 0.109(4) 0.057(4) 0.087(5) 0.002(3) -0.028(4) -0.024(3) F5 0.028(3) 0.132(6) 0.126(6) -0.062(4) -0.003(3) -0.001(3) F6 0.084(4) 0.169(7) 0.028(3) 0.003(3) -0.001(3) -0.074(4) F7 0.025(2) 0.062(4) 0.136(5) 0.041(3) -0.019(3) -0.010(2) F8 0.089(4) 0.078(4) 0.056(4) -0.003(3) 0.011(3) 0.046(3) F9 0.041(2) 0.067(3) 0.048(3) 0.033(3) 0.011(2) 0.019(2) N1 0.022(3) 0.023(3) 0.019(3) 0.001(2) 0.002(2) -0.006(2) N2 0.017(3) 0.023(3) 0.018(3) 0.001(2) 0.002(2) -0.003(2) N3 0.017(3) 0.017(3) 0.025(3) -0.002(2) 0.000(2) -0.001(2) N4 0.023(3) 0.025(3) 0.025(3) 0.001(3) -0.003(2) -0.004(2) N5 0.019(3) 0.019(3) 0.025(3) 0.002(2) 0.006(2) 0.001(2) N6 0.021(3) 0.023(3) 0.021(3) 0.004(3) 0.004(2) 0.006(2) N7 0.015(2) 0.019(3) 0.013(3) 0.002(2) 0.000(2) 0.001(2) N8 0.017(3) 0.020(3) 0.030(3) 0.003(3) 0.002(2) 0.001(2) N9 0.022(3) 0.030(3) 0.026(4) 0.003(3) 0.003(2) -0.005(2) N10 0.026(3) 0.025(3) 0.021(3) -0.001(3) 0.005(2) 0.001(3) N11 0.023(3) 0.022(3) 0.020(3) -0.002(2) 0.003(2) 0.005(2) N12 0.020(3) 0.031(3) 0.017(3) 0.004(3) 0.003(2) -0.005(2) C1 0.015(3) 0.025(4) 0.022(4) -0.003(3) 0.004(3) -0.004(3) C2 0.030(4) 0.025(4) 0.027(4) 0.008(3) 0.010(3) -0.010(3) C3 0.030(4) 0.022(4) 0.036(5) -0.001(3) 0.011(3) -0.004(3) C4 0.026(3) 0.024(4) 0.028(4) 0.000(3) 0.000(3) 0.002(3) C5 0.030(4) 0.019(4) 0.028(4) -0.006(3) 0.000(3) 0.004(3) C6 0.014(3) 0.024(4) 0.024(4) -0.003(3) 0.004(3) -0.001(3) C7 0.014(3) 0.028(4) 0.022(4) 0.003(3) -0.001(3) -0.001(3) C8 0.018(3) 0.022(4) 0.029(4) 0.001(3) 0.008(3) -0.007(3) C9 0.024(3) 0.029(4) 0.020(4) -0.005(3) -0.004(3) -0.009(3) C10 0.028(3) 0.022(4) 0.023(4) -0.005(3) 0.005(3) 0.004(3) C11 0.018(3) 0.038(4) 0.035(5) -0.006(4) -0.002(3) -0.009(3) C12 0.041(4) 0.048(5) 0.024(4) -0.001(4) 0.008(3) -0.009(4) C13 0.015(3) 0.023(4) 0.031(4) -0.003(3) 0.000(3) 0.002(3) C14 0.025(3) 0.028(4) 0.018(4) 0.004(3) 0.001(3) -0.003(3) C15 0.022(3) 0.026(4) 0.029(4) 0.004(3) 0.008(3) 0.001(3) C16 0.009(3) 0.033(4) 0.023(4) -0.001(3) 0.000(3) 0.000(3) C17 0.026(4) 0.022(4) 0.020(4) 0.002(3) 0.010(3) -0.003(3) C18 0.022(3) 0.018(4) 0.033(5) 0.003(3) 0.005(3) 0.006(3) C19 0.027(4) 0.030(4) 0.022(4) 0.000(3) 0.008(3) 0.005(3) C20 0.020(3) 0.035(4) 0.024(4) -0.001(3) -0.008(3) -0.005(3) C21 0.021(3) 0.031(4) 0.022(4) -0.004(3) -0.001(3) 0.005(3) C22 0.025(3) 0.031(4) 0.024(4) 0.007(3) 0.005(3) 0.010(3) C23 0.024(3) 0.022(4) 0.023(4) 0.009(3) 0.009(3) 0.004(3) C24 0.024(3) 0.023(4) 0.014(4) -0.008(3) -0.004(3) 0.006(3) C25 0.017(3) 0.029(4) 0.023(4) -0.004(3) 0.003(3) 0.009(3) C26 0.013(3) 0.031(4) 0.016(4) -0.003(3) 0.001(3) 0.000(3) C27 0.040(4) 0.028(4) 0.031(5) 0.004(3) 0.001(3) 0.012(3) C28 0.017(3) 0.033(4) 0.037(5) 0.005(3) 0.006(3) 0.003(3) C29 0.017(3) 0.025(4) 0.020(4) 0.005(3) 0.009(3) -0.008(3) C30 0.025(3) 0.025(4) 0.018(4) -0.010(3) 0.007(3) -0.003(3) C31 0.025(3) 0.038(4) 0.016(4) 0.002(3) 0.004(3) 0.003(3) C32 0.016(3) 0.035(4) 0.029(4) -0.004(3) 0.000(3) 0.001(3) C33 0.032(4) 0.028(4) 0.018(4) -0.002(3) -0.002(3) -0.013(3) C34 0.025(3) 0.026(4) 0.023(4) -0.003(3) -0.001(3) -0.007(3) C35 0.028(4) 0.023(4) 0.031(4) 0.004(3) 0.004(3) 0.009(3) C36 0.027(3) 0.036(4) 0.018(4) 0.001(3) 0.002(3) -0.009(3) C37 0.026(3) 0.032(4) 0.013(4) -0.007(3) 0.002(3) -0.007(3) C38 0.025(3) 0.034(4) 0.014(4) 0.008(3) 0.003(3) 0.006(3) C39 0.022(3) 0.031(4) 0.027(4) 0.011(3) 0.002(3) 0.003(3) C40 0.026(4) 0.025(4) 0.025(4) -0.010(3) 0.000(3) 0.000(3) C41 0.022(3) 0.033(4) 0.031(4) -0.015(3) -0.001(3) 0.003(3) C42 0.023(3) 0.035(4) 0.023(4) -0.010(3) 0.004(3) -0.004(3) C43 0.047(4) 0.025(4) 0.040(5) -0.002(4) 0.000(4) 0.011(3) C44 0.032(4) 0.056(6) 0.034(5) -0.001(4) 0.010(3) -0.010(4) C45 0.018(3) 0.036(4) 0.015(4) -0.002(3) -0.001(3) -0.008(3) C46 0.021(3) 0.037(4) 0.026(4) -0.002(3) 0.004(3) -0.004(3) C47 0.037(4) 0.045(5) 0.035(5) -0.012(4) 0.019(4) -0.010(4) C48 0.024(3) 0.027(4) 0.026(4) 0.004(3) 0.002(3) 0.000(3) C49 0.046(5) 0.041(5) 0.034(5) 0.014(4) 0.006(4) -0.008(4) C50 0.063(6) 0.035(5) 0.048(6) 0.001(4) 0.008(5) -0.006(4) C51 0.019(3) 0.020(4) 0.024(4) 0.008(3) 0.003(3) -0.002(3) C52 0.023(4) 0.039(5) 0.037(5) 0.002(4) 0.005(3) -0.002(3) C53 0.035(4) 0.023(4) 0.029(4) -0.004(3) 0.001(3) -0.003(3) C54 0.034(4) 0.034(5) 0.036(5) 0.008(4) 0.007(4) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C1 1.905(7) . ? Re1 C2 1.915(7) . ? Re1 C3 1.918(7) . ? Re1 N1 2.170(5) . ? Re1 N4 2.215(5) . ? Re1 N3 2.293(5) . ? Re2 C19 1.903(7) . ? Re2 C18 1.907(7) . ? Re2 C17 1.922(7) . ? Re2 N8 2.194(5) . ? Re2 N5 2.201(5) . ? Re2 N7 2.287(5) . ? Re3 C35 1.909(7) . ? Re3 C33 1.910(7) . ? Re3 C34 1.915(7) . ? Re3 N12 2.210(5) . ? Re3 N9 2.212(5) . ? Re3 N11 2.272(5) . ? O1 C1 1.164(7) . ? O2 C2 1.138(7) . ? O3 C3 1.152(7) . ? O4 C16 1.207(7) . ? O5 C16 1.306(7) . ? O6 C17 1.145(7) . ? O7 C18 1.148(7) . ? O8 C19 1.168(8) . ? O9 C32 1.334(7) . ? O10 C32 1.179(8) . ? O11 C33 1.152(8) . ? O12 C34 1.143(7) . ? O13 C35 1.157(8) . ? O14 C48 1.328(8) . ? O15 C48 1.199(8) . ? O16 C49 1.251(9) . ? O17 C49 1.239(9) . ? O18 C51 1.243(7) . ? O19 C51 1.250(7) . ? O20 C53 1.253(7) . ? O21 C53 1.255(8) . ? F1 C50 1.340(9) . ? F2 C50 1.344(9) . ? F3 C50 1.300(9) . ? F4 C52 1.335(8) . ? F5 C52 1.298(7) . ? F6 C52 1.285(8) . ? F7 C54 1.311(8) . ? F8 C54 1.342(8) . ? F9 C54 1.310(8) . ? N1 C10 1.353(8) . ? N1 N2 1.377(6) . ? N2 C8 1.349(8) . ? N2 C7 1.456(8) . ? N3 C6 1.504(7) . ? N3 C5 1.505(8) . ? N3 C13 1.509(8) . ? N4 C4 1.490(7) . ? N5 C26 1.361(7) . ? N5 N6 1.362(7) . ? N6 C24 1.347(7) . ? N6 C23 1.460(7) . ? N7 C21 1.487(8) . ? N7 C22 1.492(7) . ? N7 C29 1.519(7) . ? N8 C20 1.498(8) . ? N9 C42 1.339(7) . ? N9 N10 1.364(7) . ? N10 C40 1.363(8) . ? N10 C39 1.450(7) . ? N11 C37 1.494(8) . ? N11 C45 1.500(7) . ? N11 C38 1.509(8) . ? N12 C36 1.479(8) . ? C4 C5 1.499(9) . ? C6 C7 1.507(8) . ? C8 C9 1.368(9) . ? C8 C11 1.486(8) . ? C9 C10 1.390(8) . ? C10 C12 1.496(9) . ? C13 C14 1.538(8) . ? C14 C15 1.519(9) . ? C15 C16 1.497(9) . ? C20 C21 1.512(8) . ? C22 C23 1.501(9) . ? C24 C25 1.387(8) . ? C24 C27 1.481(9) . ? C25 C26 1.363(9) . ? C26 C28 1.504(8) . ? C29 C30 1.533(8) . ? C30 C31 1.516(8) . ? C31 C32 1.502(9) . ? C36 C37 1.513(8) . ? C38 C39 1.512(9) . ? C40 C41 1.363(9) . ? C40 C43 1.485(9) . ? C41 C42 1.401(9) . ? C42 C44 1.488(9) . ? C45 C46 1.528(8) . ? C46 C47 1.530(8) . ? C47 C48 1.498(9) . ? C49 C50 1.528(11) . ? C51 C52 1.511(9) . ? C53 C54 1.513(10) . ? 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 C1 Re1 C2 86.3(3) . . ? C1 Re1 C3 91.3(3) . . ? C2 Re1 C3 85.4(3) . . ? C1 Re1 N1 90.0(2) . . ? C2 Re1 N1 95.1(2) . . ? C3 Re1 N1 178.6(2) . . ? C1 Re1 N4 173.9(2) . . ? C2 Re1 N4 96.2(2) . . ? C3 Re1 N4 94.4(2) . . ? N1 Re1 N4 84.22(19) . . ? C1 Re1 N3 98.8(2) . . ? C2 Re1 N3 174.7(2) . . ? C3 Re1 N3 92.8(2) . . ? N1 Re1 N3 86.57(18) . . ? N4 Re1 N3 78.92(18) . . ? C19 Re2 C18 87.9(3) . . ? C19 Re2 C17 87.3(3) . . ? C18 Re2 C17 86.8(3) . . ? C19 Re2 N8 174.1(2) . . ? C18 Re2 N8 97.8(2) . . ? C17 Re2 N8 92.1(2) . . ? C19 Re2 N5 95.3(2) . . ? C18 Re2 N5 92.7(2) . . ? C17 Re2 N5 177.4(2) . . ? N8 Re2 N5 85.42(19) . . ? C19 Re2 N7 95.4(2) . . ? C18 Re2 N7 176.6(2) . . ? C17 Re2 N7 93.4(2) . . ? N8 Re2 N7 78.79(18) . . ? N5 Re2 N7 86.94(17) . . ? C35 Re3 C33 86.6(3) . . ? C35 Re3 C34 87.7(3) . . ? C33 Re3 C34 84.8(3) . . ? C35 Re3 N12 174.3(2) . . ? C33 Re3 N12 92.8(2) . . ? C34 Re3 N12 97.9(2) . . ? C35 Re3 N9 94.6(2) . . ? C33 Re3 N9 177.8(2) . . ? C34 Re3 N9 93.4(2) . . ? N12 Re3 N9 86.09(19) . . ? C35 Re3 N11 95.3(2) . . ? C33 Re3 N11 93.9(2) . . ? C34 Re3 N11 176.6(2) . . ? N12 Re3 N11 79.03(18) . . ? N9 Re3 N11 87.77(18) . . ? C10 N1 N2 105.0(5) . . ? C10 N1 Re1 132.1(4) . . ? N2 N1 Re1 122.3(4) . . ? C8 N2 N1 111.5(5) . . ? C8 N2 C7 128.4(5) . . ? N1 N2 C7 119.9(5) . . ? C6 N3 C5 108.3(4) . . ? C6 N3 C13 108.6(5) . . ? C5 N3 C13 104.6(5) . . ? C6 N3 Re1 116.1(4) . . ? C5 N3 Re1 104.8(4) . . ? C13 N3 Re1 113.6(3) . . ? C4 N4 Re1 109.7(4) . . ? C26 N5 N6 105.0(5) . . ? C26 N5 Re2 133.5(4) . . ? N6 N5 Re2 121.0(3) . . ? C24 N6 N5 111.7(5) . . ? C24 N6 C23 127.9(5) . . ? N5 N6 C23 119.9(5) . . ? C21 N7 C22 108.7(5) . . ? C21 N7 C29 109.6(4) . . ? C22 N7 C29 108.1(5) . . ? C21 N7 Re2 105.9(4) . . ? C22 N7 Re2 114.2(3) . . ? C29 N7 Re2 110.3(3) . . ? C20 N8 Re2 111.0(4) . . ? C42 N9 N10 105.7(5) . . ? C42 N9 Re3 132.1(5) . . ? N10 N9 Re3 120.4(4) . . ? C40 N10 N9 112.0(5) . . ? C40 N10 C39 127.4(6) . . ? N9 N10 C39 120.4(5) . . ? C37 N11 C45 109.5(5) . . ? C37 N11 C38 109.4(5) . . ? C45 N11 C38 107.7(5) . . ? C37 N11 Re3 105.0(4) . . ? C45 N11 Re3 111.8(4) . . ? C38 N11 Re3 113.3(3) . . ? C36 N12 Re3 111.8(4) . . ? O1 C1 Re1 176.5(6) . . ? O2 C2 Re1 175.6(6) . . ? O3 C3 Re1 176.8(6) . . ? N4 C4 C5 108.5(5) . . ? C4 C5 N3 110.0(5) . . ? N3 C6 C7 114.6(5) . . ? N2 C7 C6 113.7(5) . . ? N2 C8 C9 106.5(5) . . ? N2 C8 C11 123.6(6) . . ? C9 C8 C11 129.8(6) . . ? C8 C9 C10 107.3(6) . . ? N1 C10 C9 109.7(6) . . ? N1 C10 C12 123.6(6) . . ? C9 C10 C12 126.5(6) . . ? N3 C13 C14 117.4(5) . . ? C15 C14 C13 109.6(5) . . ? C16 C15 C14 113.8(5) . . ? O4 C16 O5 119.8(6) . . ? O4 C16 C15 123.5(6) . . ? O5 C16 C15 116.7(6) . . ? O6 C17 Re2 176.8(5) . . ? O7 C18 Re2 177.4(6) . . ? O8 C19 Re2 178.9(7) . . ? N8 C20 C21 108.4(5) . . ? N7 C21 C20 110.4(5) . . ? N7 C22 C23 115.1(6) . . ? N6 C23 C22 111.5(5) . . ? N6 C24 C25 105.9(6) . . ? N6 C24 C27 122.4(6) . . ? C25 C24 C27 131.7(6) . . ? C26 C25 C24 107.3(5) . . ? N5 C26 C25 110.0(6) . . ? N5 C26 C28 124.1(6) . . ? C25 C26 C28 125.9(5) . . ? N7 C29 C30 115.3(5) . . ? C31 C30 C29 110.7(5) . . ? C32 C31 C30 112.8(5) . . ? O10 C32 O9 123.9(6) . . ? O10 C32 C31 124.8(6) . . ? O9 C32 C31 111.2(6) . . ? O11 C33 Re3 175.0(6) . . ? O12 C34 Re3 175.5(6) . . ? O13 C35 Re3 178.1(6) . . ? N12 C36 C37 109.9(5) . . ? N11 C37 C36 111.4(5) . . ? N11 C38 C39 114.3(5) . . ? N10 C39 C38 112.5(5) . . ? N10 C40 C41 105.2(6) . . ? N10 C40 C43 123.0(6) . . ? C41 C40 C43 131.7(6) . . ? C40 C41 C42 108.0(6) . . ? N9 C42 C41 109.1(6) . . ? N9 C42 C44 123.9(6) . . ? C41 C42 C44 127.0(6) . . ? N11 C45 C46 116.3(5) . . ? C45 C46 C47 108.5(5) . . ? C48 C47 C46 116.1(6) . . ? O15 C48 O14 123.1(6) . . ? O15 C48 C47 125.1(6) . . ? O14 C48 C47 111.7(6) . . ? O17 C49 O16 129.9(8) . . ? O17 C49 C50 116.0(8) . . ? O16 C49 C50 113.9(7) . . ? F3 C50 F1 106.4(8) . . ? F3 C50 F2 107.0(7) . . ? F1 C50 F2 101.7(7) . . ? F3 C50 C49 116.5(8) . . ? F1 C50 C49 110.9(7) . . ? F2 C50 C49 113.2(7) . . ? O18 C51 O19 128.5(6) . . ? O18 C51 C52 116.0(6) . . ? O19 C51 C52 115.6(5) . . ? F6 C52 F5 106.6(7) . . ? F6 C52 F4 105.3(7) . . ? F5 C52 F4 104.0(6) . . ? F6 C52 C51 114.3(6) . . ? F5 C52 C51 114.5(6) . . ? F4 C52 C51 111.4(6) . . ? O20 C53 O21 128.0(7) . . ? O20 C53 C54 117.0(6) . . ? O21 C53 C54 114.9(6) . . ? F9 C54 F7 107.9(7) . . ? F9 C54 F8 105.0(6) . . ? F7 C54 F8 104.2(6) . . ? F9 C54 C53 114.8(6) . . ? F7 C54 C53 111.8(6) . . ? F8 C54 C53 112.4(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.885 _refine_diff_density_min -0.853 _refine_diff_density_rms 0.161