# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_f:\disser~1\chapte~4\cpds\ms135la\ms135r~1\work\135f _audit_creation_method SHELXL-97 __chemical_name_systematic (Et4N)2[(triphosRe(CN)3)2(La(NO3)3)3].4CH3CN _chemical_name_common 1 _chemical_formula_moiety C88H78N15O27P6Re2La3,2C8H20N),4(C2H3N) _chemical_formula_sum 'C108 H124 La3 N19 O27 P6 Re2' _chemical_properties_physical air-sensitive _exptl_crystal_recrystallization_method CH3CN _chemical_melting_point 300 _chemical_formula_weight 3095.21 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 '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 'C 2/c' _symmetry_int_tables_number 15 _chemical_absolute_configuration ? _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 36.170(7) _cell_length_b 13.788(3) _cell_length_c 26.153(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.07(3) _cell_angle_gamma 90.00 _cell_volume 12705(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6128 _exptl_absorpt_coefficient_mu 3.036 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3142 _exptl_absorpt_correction_T_max 0.4305 _exptl_absorpt_process_details 'Bruker AXS Scale, SADABS (Bruker 2008)' _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 69706 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 27.46 _reflns_number_total 14378 _reflns_number_gt 12095 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEXII (Bruker 2008)' _computing_cell_refinement 'SAINT v7.60A (Bruker 2008)' _computing_data_reduction 'SAINT v7.60A, XPREP v2008/2 (Bruker 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond (Pennington, 2013)' _computing_publication_material 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0480P)^2^+42.2327P] 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 14378 _refine_ls_number_parameters 742 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0947 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.002 _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 0.129647(4) 0.788188(12) 0.325844(6) 0.03087(5) Uani 1 1 d . . . La2 La 0.0000 1.01490(2) 0.2500 0.03083(8) Uani 1 2 d S . . La1 La 0.015760(6) 0.680283(19) 0.149822(9) 0.03562(7) Uani 1 1 d . . . P1 P 0.16406(3) 0.88165(8) 0.40006(4) 0.0361(2) Uani 1 1 d . . . P2 P 0.18000(3) 0.83803(8) 0.28458(4) 0.0372(2) Uani 1 1 d . . . P3 P 0.17042(3) 0.65270(8) 0.36102(5) 0.0379(2) Uani 1 1 d . . . N1 N 0.07716(11) 0.6960(3) 0.22121(16) 0.0498(10) Uani 1 1 d . . . C1 C 0.09843(11) 0.7240(3) 0.25817(17) 0.0380(9) Uani 1 1 d . . . C32 C 0.13805(15) 0.9717(4) 0.21611(19) 0.0538(12) Uani 1 1 d . . . H32 H 0.1184 0.9249 0.2129 0.065 Uiso 1 1 calc R . . C2 C 0.09143(11) 0.8982(3) 0.30039(16) 0.0361(9) Uani 1 1 d . . . C3 C 0.08431(11) 0.7341(3) 0.35361(16) 0.0348(8) Uani 1 1 d . . . C11 C 0.10413(14) 0.8865(4) 0.45005(18) 0.0484(11) Uani 1 1 d . . . H11 H 0.0888 0.8866 0.4153 0.058 Uiso 1 1 calc R . . O11 O 0.04200(10) 1.1651(2) 0.28258(16) 0.0570(9) Uani 1 1 d . . . O5 O -0.01043(9) 0.6750(2) 0.05007(12) 0.0456(7) Uani 1 1 d . . . O3 O 0.06787(12) 0.7548(3) 0.10768(16) 0.0679(10) Uani 1 1 d . . . C16 C 0.21229(12) 0.8304(3) 0.42450(18) 0.0458(11) Uani 1 1 d . . . H16A H 0.2286 0.8815 0.4446 0.055 Uiso 1 1 calc R . . H16B H 0.2105 0.7773 0.4493 0.055 Uiso 1 1 calc R . . O10 O 0.04142(9) 1.1164(3) 0.20352(14) 0.0530(8) Uani 1 1 d . . . O4 O 0.06852(10) 0.5980(3) 0.11377(15) 0.0626(10) Uani 1 1 d . . . C19 C 0.22144(12) 0.6829(3) 0.3687(2) 0.0456(11) Uani 1 1 d . . . H19A H 0.2365 0.6413 0.3967 0.055 Uiso 1 1 calc R . . H19B H 0.2289 0.6665 0.3357 0.055 Uiso 1 1 calc R . . C17 C 0.23224(12) 0.7905(3) 0.3825(2) 0.0466(11) Uani 1 1 d . . . O6 O -0.01480(10) 0.5405(2) 0.09105(13) 0.0502(8) Uani 1 1 d . . . C20 C 0.22527(12) 0.8553(4) 0.33327(19) 0.0462(11) Uani 1 1 d . . . H20A H 0.2463 0.8445 0.3154 0.055 Uiso 1 1 calc R . . H20B H 0.2267 0.9238 0.3449 0.055 Uiso 1 1 calc R . . C5 C 0.15260(12) 1.0666(3) 0.35168(16) 0.0391(9) Uani 1 1 d . . . H5 H 0.1342 1.0350 0.3253 0.047 Uiso 1 1 calc R . . N2 N 0.06698(9) 0.9531(3) 0.28554(15) 0.0441(9) Uani 1 1 d . . . O13 O -0.03992(13) 0.5516(3) 0.00722(14) 0.0752(12) Uani 1 1 d . . . C4 C 0.17376(11) 1.0124(3) 0.39281(16) 0.0375(9) Uani 1 1 d . . . C8 C 0.20563(15) 1.1614(4) 0.4276(2) 0.0554(13) Uani 1 1 d . . . H8 H 0.2240 1.1935 0.4539 0.066 Uiso 1 1 calc R . . N8 N 0.05467(12) 1.1739(3) 0.2411(2) 0.0547(11) Uani 1 1 d . . . C7 C 0.18427(14) 1.2137(4) 0.3864(2) 0.0490(11) Uani 1 1 d . . . H7 H 0.1877 1.2818 0.3841 0.059 Uiso 1 1 calc R . . O14 O 0.07936(13) 1.2324(3) 0.2383(2) 0.0882(15) Uani 1 1 d . . . N6 N -0.02224(11) 0.5880(3) 0.04821(15) 0.0480(9) Uani 1 1 d . . . O12 O 0.11031(13) 0.6718(5) 0.0793(2) 0.1060(19) Uani 1 1 d . . . N5 N 0.08243(14) 0.6730(5) 0.10030(18) 0.0656(13) Uani 1 1 d . . . C6 C 0.15773(13) 1.1658(3) 0.34836(18) 0.0431(10) Uani 1 1 d . . . H6 H 0.1429 1.2012 0.3198 0.052 Uiso 1 1 calc R . . C9 C 0.20037(14) 1.0621(4) 0.4308(2) 0.0512(12) Uani 1 1 d . . . H9 H 0.2152 1.0271 0.4595 0.061 Uiso 1 1 calc R . . O1 O 0.00901(8) 0.8607(2) 0.18992(12) 0.0403(7) Uani 1 1 d . . . O7 O 0.0000 0.6673(3) 0.2500 0.0429(10) Uani 1 2 d S . . O2 O -0.00474(11) 0.8571(3) 0.10456(13) 0.0579(9) Uani 1 1 d . . . N3 N 0.05645(10) 0.7049(3) 0.36230(15) 0.0416(8) Uani 1 1 d . . . N4 N -0.00286(11) 0.9034(3) 0.14553(15) 0.0452(9) Uani 1 1 d . . . C44 C 0.16317(12) 0.5428(3) 0.32129(17) 0.0396(9) Uani 1 1 d . . . C21 C 0.19397(12) 0.7583(4) 0.23535(19) 0.0462(11) Uani 1 1 d . . . C26 C 0.17411(13) 0.6744(4) 0.21652(19) 0.0463(10) Uani 1 1 d . . . H26 H 0.1530 0.6553 0.2301 0.056 Uiso 1 1 calc R . . C33 C 0.16830(13) 0.5997(4) 0.42518(18) 0.0467(11) Uani 1 1 d . . . O8 O 0.0065(2) 0.5365(3) 0.21041(17) 0.136(3) Uani 1 1 d . . . C39 C 0.12534(13) 0.5112(3) 0.3041(2) 0.0491(11) Uani 1 1 d . . . H39 H 0.1056 0.5461 0.3144 0.059 Uiso 1 1 calc R . . O9 O -0.01288(11) 0.9905(2) 0.14545(13) 0.0536(8) Uani 1 1 d . . . C10 C 0.14330(13) 0.8865(3) 0.45774(17) 0.0425(10) Uani 1 1 d . . . C27 C 0.17388(13) 0.9526(4) 0.24807(18) 0.0442(10) Uani 1 1 d . . . C28 C 0.20237(18) 1.0222(4) 0.2506(2) 0.0628(14) Uani 1 1 d . . . H28 H 0.2270 1.0109 0.2719 0.075 Uiso 1 1 calc R . . C35 C 0.13844(15) 0.5825(4) 0.4987(2) 0.0581(13) Uani 1 1 d . . . H35 H 0.1205 0.6044 0.5175 0.070 Uiso 1 1 calc R . . C18 C 0.27553(14) 0.7927(4) 0.4066(3) 0.0644(15) Uani 1 1 d . . . H18A H 0.2890 0.7631 0.3820 0.097 Uiso 1 1 calc R . . H18B H 0.2810 0.7562 0.4396 0.097 Uiso 1 1 calc R . . H18C H 0.2839 0.8600 0.4134 0.097 Uiso 1 1 calc R . . C34 C 0.14199(14) 0.6303(4) 0.45294(18) 0.0489(11) Uani 1 1 d . . . H34 H 0.1262 0.6843 0.4407 0.059 Uiso 1 1 calc R . . C38 C 0.19181(15) 0.5196(4) 0.4440(2) 0.0577(13) Uani 1 1 d . . . H38 H 0.2100 0.4977 0.4256 0.069 Uiso 1 1 calc R . . C43 C 0.19139(13) 0.4901(4) 0.3052(2) 0.0528(12) Uani 1 1 d . . . H43 H 0.2172 0.5090 0.3164 0.063 Uiso 1 1 calc R . . C24 C 0.21545(16) 0.6440(5) 0.1581(2) 0.0662(15) Uani 1 1 d . . . H24 H 0.2230 0.6039 0.1327 0.079 Uiso 1 1 calc R . . C42 C 0.18170(15) 0.4098(4) 0.2729(2) 0.0608(14) Uani 1 1 d . . . H42 H 0.2011 0.3745 0.2619 0.073 Uiso 1 1 calc R . . C15 C 0.16530(16) 0.8898(4) 0.50884(18) 0.0562(13) Uani 1 1 d . . . H15 H 0.1922 0.8917 0.5148 0.067 Uiso 1 1 calc R . . C25 C 0.18458(15) 0.6182(4) 0.1784(2) 0.0561(13) Uani 1 1 d . . . H25 H 0.1705 0.5615 0.1660 0.067 Uiso 1 1 calc R . . C37 C 0.18811(18) 0.4732(5) 0.4895(2) 0.0707(17) Uani 1 1 d . . . H37 H 0.2042 0.4201 0.5024 0.085 Uiso 1 1 calc R . . C31 C 0.13108(19) 1.0592(5) 0.1889(2) 0.0702(18) Uani 1 1 d . . . H31 H 0.1065 1.0721 0.1680 0.084 Uiso 1 1 calc R . . N7 N 0.0000 0.5787(5) 0.2500 0.084(3) Uani 1 2 d S . . C41 C 0.14471(15) 0.3805(4) 0.2567(2) 0.0585(13) Uani 1 1 d . . . H41 H 0.1385 0.3256 0.2345 0.070 Uiso 1 1 calc R . . C12 C 0.08706(17) 0.8862(4) 0.4921(2) 0.0622(14) Uani 1 1 d . . . H12 H 0.0602 0.8862 0.4864 0.075 Uiso 1 1 calc R . . C22 C 0.22414(15) 0.7849(5) 0.2134(3) 0.0743(19) Uani 1 1 d . . . H22 H 0.2376 0.8430 0.2249 0.089 Uiso 1 1 calc R . . C36 C 0.16133(18) 0.5029(4) 0.5164(2) 0.0665(16) Uani 1 1 d . . . H36 H 0.1586 0.4690 0.5470 0.080 Uiso 1 1 calc R . . C40 C 0.11660(14) 0.4316(4) 0.2729(2) 0.0585(14) Uani 1 1 d . . . H40 H 0.0909 0.4110 0.2622 0.070 Uiso 1 1 calc R . . C14 C 0.14794(19) 0.8903(5) 0.5508(2) 0.0695(17) Uani 1 1 d . . . H14 H 0.1630 0.8935 0.5856 0.083 Uiso 1 1 calc R . . C13 C 0.1090(2) 0.8861(5) 0.5425(2) 0.0707(17) Uani 1 1 d . . . H13 H 0.0974 0.8831 0.5716 0.085 Uiso 1 1 calc R . . C23 C 0.23529(18) 0.7285(6) 0.1750(3) 0.085(2) Uani 1 1 d . . . H23 H 0.2561 0.7478 0.1607 0.102 Uiso 1 1 calc R . . C30 C 0.1590(2) 1.1264(5) 0.1918(2) 0.079(2) Uani 1 1 d . . . H30 H 0.1540 1.1859 0.1731 0.095 Uiso 1 1 calc R . . N9 N 0.04870(13) 1.2432(3) 0.43160(17) 0.0538(10) Uani 1 1 d . . . C46 C 0.07643(16) 1.1708(4) 0.4184(2) 0.0578(13) Uani 1 1 d . . . H46A H 0.0836 1.1915 0.3857 0.069 Uiso 1 1 calc R . . H46B H 0.0637 1.1070 0.4117 0.069 Uiso 1 1 calc R . . C45 C 0.11227(19) 1.1592(5) 0.4613(3) 0.0741(17) Uani 1 1 d . . . H45A H 0.1254 1.2217 0.4678 0.111 Uiso 1 1 calc R . . H45B H 0.1290 1.1116 0.4503 0.111 Uiso 1 1 calc R . . H45C H 0.1056 1.1368 0.4936 0.111 Uiso 1 1 calc R . . C48 C 0.01410(17) 1.2427(5) 0.3855(2) 0.0668(15) Uani 1 1 d . . . H48A H 0.0224 1.2634 0.3536 0.080 Uiso 1 1 calc R . . H48B H 0.0048 1.1751 0.3797 0.080 Uiso 1 1 calc R . . C50 C 0.06559(17) 1.3434(4) 0.4411(2) 0.0633(14) Uani 1 1 d . . . H50A H 0.0856 1.3420 0.4740 0.076 Uiso 1 1 calc R . . H50B H 0.0455 1.3883 0.4468 0.076 Uiso 1 1 calc R . . C52 C 0.0369(2) 1.2131(5) 0.4814(2) 0.0730(18) Uani 1 1 d . . . H52A H 0.0596 1.2140 0.5108 0.088 Uiso 1 1 calc R . . H52B H 0.0189 1.2621 0.4893 0.088 Uiso 1 1 calc R . . C47 C -0.0185(2) 1.3060(5) 0.3915(3) 0.091(2) Uani 1 1 d . . . H47A H -0.0260 1.2895 0.4242 0.137 Uiso 1 1 calc R . . H47B H -0.0401 1.2955 0.3617 0.137 Uiso 1 1 calc R . . H47C H -0.0108 1.3742 0.3924 0.137 Uiso 1 1 calc R . . C49 C 0.0827(2) 1.3844(5) 0.3975(3) 0.088(2) Uani 1 1 d . . . H49A H 0.1043 1.3442 0.3937 0.132 Uiso 1 1 calc R . . H49B H 0.0914 1.4509 0.4063 0.132 Uiso 1 1 calc R . . H49C H 0.0635 1.3845 0.3644 0.132 Uiso 1 1 calc R . . C51 C 0.0185(2) 1.1144(5) 0.4797(3) 0.093(2) Uani 1 1 d . . . H51A H -0.0055 1.1145 0.4534 0.139 Uiso 1 1 calc R . . H51B H 0.0137 1.0992 0.5142 0.139 Uiso 1 1 calc R . . H51C H 0.0355 1.0653 0.4704 0.139 Uiso 1 1 calc R . . C29 C 0.19489(14) 1.1068(3) 0.22240(15) 0.081(2) Uani 1 1 d . . . H29 H 0.2147 1.1529 0.2239 0.097 Uiso 1 1 calc R . . C54 C 0.16543(14) 1.1300(3) 0.59991(15) 0.103(3) Uani 1 1 d R . . H54A H 0.1576 1.1976 0.5926 0.154 Uiso 1 1 calc R . . H54B H 0.1690 1.1173 0.6376 0.154 Uiso 1 1 calc R . . H54C H 0.1458 1.0867 0.5803 0.154 Uiso 1 1 calc R . . C53 C 0.20192(14) 1.1126(3) 0.58351(15) 0.119(3) Uani 1 1 d R . . N10 N 0.22751(14) 1.1017(3) 0.56980(15) 0.243(8) Uani 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 Re1 0.01963(8) 0.03596(9) 0.03401(9) 0.00177(6) -0.00021(6) 0.00178(6) La2 0.02126(14) 0.02619(15) 0.04088(17) 0.000 -0.00169(12) 0.000 La1 0.02522(11) 0.04602(14) 0.03462(12) -0.00727(10) 0.00470(9) -0.00032(9) P1 0.0290(5) 0.0394(6) 0.0346(5) 0.0026(4) -0.0035(4) 0.0023(4) P2 0.0208(5) 0.0453(6) 0.0439(6) -0.0006(5) 0.0042(4) 0.0011(4) P3 0.0269(5) 0.0384(6) 0.0447(6) 0.0051(5) 0.0005(4) 0.0050(4) N1 0.034(2) 0.064(3) 0.048(2) -0.0130(19) 0.0029(17) 0.0029(18) C1 0.0251(19) 0.043(2) 0.044(2) -0.0022(18) 0.0044(17) 0.0030(16) C32 0.050(3) 0.066(3) 0.049(3) 0.015(2) 0.018(2) 0.015(2) C2 0.0248(18) 0.039(2) 0.041(2) 0.0011(17) 0.0003(16) -0.0031(16) C3 0.027(2) 0.040(2) 0.035(2) 0.0008(17) 0.0015(16) 0.0049(16) C11 0.054(3) 0.052(3) 0.039(2) -0.002(2) 0.010(2) -0.001(2) O11 0.0443(19) 0.0431(19) 0.080(3) -0.0147(18) 0.0060(18) -0.0092(15) O5 0.0485(19) 0.0491(18) 0.0385(16) 0.0003(14) 0.0087(14) -0.0103(15) O3 0.060(2) 0.078(3) 0.065(2) 0.013(2) 0.0129(19) -0.011(2) C16 0.035(2) 0.045(2) 0.046(2) 0.003(2) -0.0140(19) 0.0032(19) O10 0.0395(17) 0.056(2) 0.059(2) 0.0131(17) 0.0005(15) -0.0093(15) O4 0.049(2) 0.076(3) 0.064(2) -0.023(2) 0.0154(18) -0.0035(19) C19 0.027(2) 0.049(3) 0.056(3) 0.005(2) -0.0001(19) 0.0073(18) C17 0.023(2) 0.051(3) 0.058(3) -0.002(2) -0.0072(19) 0.0037(18) O6 0.059(2) 0.0409(17) 0.0469(18) -0.0007(14) 0.0039(15) -0.0067(15) C20 0.024(2) 0.052(3) 0.058(3) -0.004(2) -0.0005(19) -0.0034(18) C5 0.034(2) 0.045(2) 0.037(2) 0.0011(18) 0.0049(17) 0.0011(18) N2 0.0244(17) 0.046(2) 0.057(2) 0.0053(18) -0.0015(15) 0.0008(15) O13 0.087(3) 0.083(3) 0.046(2) -0.019(2) -0.005(2) -0.022(2) C4 0.029(2) 0.042(2) 0.039(2) -0.0014(18) 0.0015(16) -0.0026(17) C8 0.045(3) 0.055(3) 0.059(3) -0.006(2) -0.002(2) -0.012(2) N8 0.039(2) 0.039(2) 0.082(3) 0.008(2) 0.004(2) -0.0057(17) C7 0.045(3) 0.045(3) 0.059(3) 0.001(2) 0.018(2) -0.009(2) O14 0.062(3) 0.059(3) 0.143(5) 0.006(3) 0.022(3) -0.032(2) N6 0.050(2) 0.050(2) 0.043(2) -0.0080(18) 0.0064(17) -0.0082(18) O12 0.050(3) 0.197(6) 0.080(3) 0.003(4) 0.034(2) 0.001(3) N5 0.048(3) 0.101(4) 0.047(2) -0.006(3) 0.006(2) 0.002(3) C6 0.043(2) 0.048(3) 0.040(2) 0.0063(19) 0.0115(19) 0.000(2) C9 0.043(3) 0.053(3) 0.049(3) 0.001(2) -0.007(2) -0.005(2) O1 0.0341(15) 0.0371(15) 0.0444(16) -0.0044(13) -0.0018(12) 0.0049(12) O7 0.035(2) 0.049(3) 0.043(2) 0.000 0.0036(18) 0.000 O2 0.080(3) 0.049(2) 0.0439(18) -0.0064(15) 0.0137(18) 0.0021(18) N3 0.0294(18) 0.051(2) 0.043(2) 0.0028(16) 0.0049(15) 0.0008(16) N4 0.046(2) 0.042(2) 0.048(2) -0.0025(17) 0.0122(17) -0.0062(17) C44 0.032(2) 0.037(2) 0.048(2) 0.0081(18) 0.0056(18) 0.0070(17) C21 0.024(2) 0.059(3) 0.055(3) -0.005(2) 0.0070(18) 0.0050(19) C26 0.038(2) 0.051(3) 0.048(3) 0.003(2) 0.008(2) 0.007(2) C33 0.042(2) 0.048(3) 0.044(2) 0.008(2) -0.0059(19) -0.001(2) O8 0.320(9) 0.040(2) 0.047(2) -0.0022(19) 0.038(4) 0.003(4) C39 0.034(2) 0.044(3) 0.073(3) -0.004(2) 0.019(2) -0.0012(19) O9 0.075(2) 0.0300(16) 0.056(2) 0.0009(14) 0.0148(18) -0.0013(15) C10 0.050(3) 0.040(2) 0.035(2) 0.0031(18) 0.0034(19) 0.0020(19) C27 0.041(2) 0.053(3) 0.042(2) 0.000(2) 0.0165(19) 0.001(2) C28 0.070(4) 0.070(4) 0.054(3) 0.001(3) 0.026(3) -0.014(3) C35 0.054(3) 0.071(4) 0.044(3) 0.012(2) -0.001(2) -0.006(3) C18 0.027(2) 0.072(4) 0.082(4) -0.002(3) -0.013(2) 0.003(2) C34 0.045(3) 0.053(3) 0.044(2) 0.008(2) 0.000(2) -0.001(2) C38 0.051(3) 0.058(3) 0.056(3) 0.014(2) -0.005(2) 0.013(2) C43 0.033(2) 0.048(3) 0.075(3) 0.002(2) 0.007(2) 0.006(2) C24 0.052(3) 0.085(4) 0.061(3) -0.017(3) 0.013(3) 0.017(3) C42 0.043(3) 0.047(3) 0.095(4) -0.006(3) 0.022(3) 0.011(2) C15 0.061(3) 0.064(3) 0.037(2) 0.003(2) -0.003(2) 0.008(3) C25 0.054(3) 0.057(3) 0.057(3) -0.003(2) 0.013(2) 0.011(2) C37 0.072(4) 0.067(4) 0.062(3) 0.026(3) -0.006(3) 0.012(3) C31 0.081(4) 0.091(5) 0.047(3) 0.020(3) 0.032(3) 0.039(4) N7 0.172(9) 0.039(4) 0.038(3) 0.000 0.016(4) 0.000 C41 0.056(3) 0.036(2) 0.086(4) -0.012(2) 0.021(3) -0.004(2) C12 0.062(3) 0.073(4) 0.056(3) -0.006(3) 0.022(3) -0.005(3) C22 0.036(3) 0.104(5) 0.090(4) -0.037(4) 0.028(3) -0.018(3) C36 0.072(4) 0.072(4) 0.045(3) 0.020(3) -0.008(3) -0.012(3) C40 0.039(3) 0.043(3) 0.094(4) -0.011(3) 0.019(3) -0.008(2) C14 0.086(4) 0.082(4) 0.037(3) 0.009(3) 0.007(3) 0.020(3) C13 0.092(5) 0.083(4) 0.044(3) 0.003(3) 0.030(3) 0.007(4) C23 0.046(3) 0.128(6) 0.092(5) -0.031(4) 0.037(3) -0.003(4) C30 0.137(7) 0.061(4) 0.053(3) 0.014(3) 0.052(4) 0.017(4) N9 0.069(3) 0.048(2) 0.054(2) -0.0083(19) 0.032(2) -0.001(2) C46 0.064(3) 0.056(3) 0.058(3) -0.010(2) 0.025(3) -0.001(3) C45 0.077(4) 0.078(4) 0.072(4) -0.003(3) 0.025(3) 0.016(3) C48 0.065(4) 0.069(4) 0.065(4) -0.013(3) 0.010(3) -0.009(3) C50 0.066(4) 0.051(3) 0.069(4) -0.016(3) 0.008(3) -0.002(3) C52 0.088(5) 0.084(4) 0.060(3) -0.004(3) 0.041(3) 0.009(3) C47 0.071(4) 0.080(5) 0.111(6) -0.029(4) -0.004(4) 0.008(4) C49 0.112(6) 0.055(4) 0.108(6) 0.004(4) 0.049(5) -0.016(4) C51 0.111(6) 0.073(4) 0.119(6) 0.016(4) 0.078(5) 0.001(4) C29 0.123(6) 0.069(4) 0.061(4) 0.002(3) 0.043(4) -0.027(4) C54 0.116(7) 0.113(6) 0.083(5) 0.001(5) 0.031(5) -0.010(5) C53 0.104(7) 0.140(8) 0.096(6) -0.048(6) -0.015(5) 0.036(6) N10 0.099(7) 0.382(19) 0.215(11) -0.203(13) -0.030(7) 0.077(9) _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 C2 2.058(4) . ? Re1 C1 2.070(4) . ? Re1 C3 2.076(4) . ? Re1 P2 2.4173(12) . ? Re1 P1 2.4259(12) . ? Re1 P3 2.4284(11) . ? La2 N2 2.538(3) 2 ? La2 N2 2.538(3) . ? La2 O10 2.550(3) . ? La2 O10 2.550(3) 2 ? La2 O11 2.595(3) 2 ? La2 O11 2.595(3) . ? La2 O9 2.689(3) . ? La2 O9 2.689(3) 2 ? La2 O1 2.706(3) 2 ? La2 O1 2.707(3) . ? La2 N8 2.996(4) 2 ? La2 N8 2.996(4) . ? La1 O6 2.555(3) . ? La1 N1 2.567(4) . ? La1 O5 2.567(3) . ? La1 O4 2.575(4) . ? La1 N3 2.581(4) 2 ? La1 O3 2.601(4) . ? La1 O8 2.607(5) . ? La1 O1 2.732(3) . ? La1 O2 2.739(4) . ? La1 O7 2.8101(7) . ? La1 N6 2.986(4) . ? La1 N5 2.986(5) . ? P1 C10 1.832(5) . ? P1 C4 1.855(4) . ? P1 C16 1.857(4) . ? P2 C27 1.833(5) . ? P2 C21 1.848(5) . ? P2 C20 1.848(4) . ? P3 C44 1.823(5) . ? P3 C33 1.848(5) . ? P3 C19 1.858(4) . ? N1 C1 1.157(6) . ? C32 C31 1.394(8) . ? C32 C27 1.399(7) . ? C2 N2 1.162(5) . ? C3 N3 1.154(5) . ? C11 C12 1.378(7) . ? C11 C10 1.385(7) . ? O11 N8 1.275(6) . ? O5 N6 1.270(5) . ? O3 N5 1.277(7) . ? C16 C17 1.546(7) . ? O10 N8 1.269(6) . ? O4 N5 1.236(6) . ? C19 C17 1.555(7) . ? C17 C20 1.539(7) . ? C17 C18 1.550(6) . ? O6 N6 1.273(5) . ? C5 C6 1.386(6) . ? C5 C4 1.389(6) . ? O13 N6 1.225(5) . ? C4 C9 1.397(6) . ? C8 C7 1.379(8) . ? C8 C9 1.388(7) . ? N8 O14 1.218(5) . ? C7 C6 1.384(7) . ? O12 N5 1.252(6) . ? O1 N4 1.286(5) . ? O7 N7 1.221(8) . ? O7 La1 2.8101(7) 2 ? O2 N4 1.236(5) . ? N3 La1 2.581(4) 2 ? N4 O9 1.255(5) . ? C44 C43 1.393(6) . ? C44 C39 1.409(6) . ? C21 C26 1.392(7) . ? C21 C22 1.391(7) . ? C26 C25 1.381(7) . ? C33 C34 1.387(7) . ? C33 C38 1.413(7) . ? O8 N7 1.256(5) . ? C39 C40 1.362(7) . ? C10 C15 1.393(6) . ? C27 C28 1.399(7) . ? C28 C29 1.374(7) . ? C35 C36 1.391(8) . ? C35 C34 1.396(7) . ? C38 C37 1.382(8) . ? C43 C42 1.389(7) . ? C24 C23 1.388(9) . ? C24 C25 1.387(8) . ? C42 C41 1.369(7) . ? C15 C14 1.382(8) . ? C37 C36 1.383(9) . ? C31 C30 1.361(10) . ? N7 O8 1.256(5) 2 ? C41 C40 1.380(7) . ? C12 C13 1.377(8) . ? C22 C23 1.401(8) . ? C14 C13 1.376(9) . ? C30 C29 1.388(9) . ? N9 C50 1.508(7) . ? N9 C46 1.509(7) . ? N9 C52 1.519(7) . ? N9 C48 1.530(7) . ? C46 C45 1.519(8) . ? C48 C47 1.504(9) . ? C50 C49 1.525(9) . ? C52 C51 1.511(9) . ? C54 C53 1.4966 . ? C53 N10 1.0761 . ? 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 C2 Re1 C1 80.89(16) . . ? C2 Re1 C3 81.48(16) . . ? C1 Re1 C3 79.89(16) . . ? C2 Re1 P2 99.49(12) . . ? C1 Re1 P2 93.45(12) . . ? C3 Re1 P2 173.06(12) . . ? C2 Re1 P1 93.04(12) . . ? C1 Re1 P1 173.20(12) . . ? C3 Re1 P1 102.34(12) . . ? P2 Re1 P1 84.50(4) . . ? C2 Re1 P3 174.30(12) . . ? C1 Re1 P3 99.34(12) . . ? C3 Re1 P3 92.94(11) . . ? P2 Re1 P3 86.19(4) . . ? P1 Re1 P3 87.01(4) . . ? N2 La2 N2 140.76(17) 2 . ? N2 La2 O10 128.66(12) 2 . ? N2 La2 O10 75.15(12) . . ? N2 La2 O10 75.15(12) 2 2 ? N2 La2 O10 128.66(12) . 2 ? O10 La2 O10 113.46(17) . 2 ? N2 La2 O11 73.03(12) 2 2 ? N2 La2 O11 145.85(12) . 2 ? O10 La2 O11 76.66(12) . 2 ? O10 La2 O11 49.87(12) 2 2 ? N2 La2 O11 145.85(12) 2 . ? N2 La2 O11 73.03(12) . . ? O10 La2 O11 49.87(12) . . ? O10 La2 O11 76.66(12) 2 . ? O11 La2 O11 74.16(16) 2 . ? N2 La2 O9 69.77(12) 2 . ? N2 La2 O9 105.19(13) . . ? O10 La2 O9 64.48(11) . . ? O10 La2 O9 124.60(11) 2 . ? O11 La2 O9 79.15(12) 2 . ? O11 La2 O9 112.80(12) . . ? N2 La2 O9 105.19(13) 2 2 ? N2 La2 O9 69.76(12) . 2 ? O10 La2 O9 124.60(11) . 2 ? O10 La2 O9 64.48(11) 2 2 ? O11 La2 O9 112.80(12) 2 2 ? O11 La2 O9 79.15(12) . 2 ? O9 La2 O9 165.65(13) . 2 ? N2 La2 O1 73.65(11) 2 2 ? N2 La2 O1 75.76(11) . 2 ? O10 La2 O1 150.28(10) . 2 ? O10 La2 O1 89.62(11) 2 2 ? O11 La2 O1 132.75(11) 2 2 ? O11 La2 O1 125.06(11) . 2 ? O9 La2 O1 118.44(9) . 2 ? O9 La2 O1 47.74(9) 2 2 ? N2 La2 O1 75.76(11) 2 . ? N2 La2 O1 73.66(11) . . ? O10 La2 O1 89.62(11) . . ? O10 La2 O1 150.28(10) 2 . ? O11 La2 O1 125.05(11) 2 . ? O11 La2 O1 132.75(11) . . ? O9 La2 O1 47.74(9) . . ? O9 La2 O1 118.44(9) 2 . ? O1 La2 O1 76.48(13) 2 . ? N2 La2 N8 71.45(12) 2 2 ? N2 La2 N8 144.03(12) . 2 ? O10 La2 N8 96.02(13) . 2 ? O10 La2 N8 24.83(12) 2 2 ? O11 La2 N8 25.08(12) 2 2 ? O11 La2 N8 74.84(11) . 2 ? O9 La2 N8 101.81(12) . 2 ? O9 La2 N8 88.74(13) 2 2 ? O1 La2 N8 111.18(12) 2 2 ? O1 La2 N8 141.99(11) . 2 ? N2 La2 N8 144.04(12) 2 . ? N2 La2 N8 71.45(12) . . ? O10 La2 N8 24.83(12) . . ? O10 La2 N8 96.02(13) 2 . ? O11 La2 N8 74.84(11) 2 . ? O11 La2 N8 25.07(12) . . ? O9 La2 N8 88.74(13) . . ? O9 La2 N8 101.81(13) 2 . ? O1 La2 N8 141.98(11) 2 . ? O1 La2 N8 111.18(12) . . ? N8 La2 N8 85.97(17) 2 . ? O6 La1 N1 133.35(12) . . ? O6 La1 O5 50.00(10) . . ? N1 La1 O5 143.25(12) . . ? O6 La1 O4 72.73(12) . . ? N1 La1 O4 73.30(12) . . ? O5 La1 O4 75.47(12) . . ? O6 La1 N3 74.78(12) . 2 ? N1 La1 N3 139.74(12) . 2 ? O5 La1 N3 75.43(12) . 2 ? O4 La1 N3 145.70(12) . 2 ? O6 La1 O3 107.42(13) . . ? N1 La1 O3 71.59(13) . . ? O5 La1 O3 73.55(12) . . ? O4 La1 O3 49.51(14) . . ? N3 La1 O3 134.92(13) 2 . ? O6 La1 O8 72.21(13) . . ? N1 La1 O8 80.27(19) . . ? O5 La1 O8 121.83(14) . . ? O4 La1 O8 95.48(19) . . ? N3 La1 O8 84.8(2) 2 . ? O3 La1 O8 139.8(2) . . ? O6 La1 O1 148.60(10) . . ? N1 La1 O1 77.40(11) . . ? O5 La1 O1 111.81(10) . . ? O4 La1 O1 132.81(11) . . ? N3 La1 O1 75.61(10) 2 . ? O3 La1 O1 86.51(13) . . ? O8 La1 O1 115.11(12) . . ? O6 La1 O2 111.93(11) . . ? N1 La1 O2 110.15(13) . . ? O5 La1 O2 65.45(10) . . ? O4 La1 O2 112.61(13) . . ? N3 La1 O2 70.26(12) 2 . ? O3 La1 O2 67.43(13) . . ? O8 La1 O2 151.71(18) . . ? O1 La1 O2 46.86(9) . . ? O6 La1 O7 111.19(11) . . ? N1 La1 O7 69.62(10) . . ? O5 La1 O7 147.10(7) . . ? O4 La1 O7 129.55(11) . . ? N3 La1 O7 73.14(9) 2 . ? O3 La1 O7 137.69(11) . . ? O8 La1 O7 45.87(14) . . ? O1 La1 O7 69.24(11) . . ? O2 La1 O7 111.56(11) . . ? O6 La1 N6 25.04(10) . . ? N1 La1 N6 146.26(12) . . ? O5 La1 N6 25.01(10) . . ? O4 La1 N6 73.54(12) . . ? N3 La1 N6 72.39(12) 2 . ? O3 La1 N6 91.32(12) . . ? O8 La1 N6 96.91(14) . . ? O1 La1 N6 131.79(10) . . ? O2 La1 N6 88.26(11) . . ? O7 La1 N6 130.76(10) . . ? O6 La1 N5 89.76(13) . . ? N1 La1 N5 70.58(13) . . ? O5 La1 N5 72.95(12) . . ? O4 La1 N5 24.26(14) . . ? N3 La1 N5 147.69(12) 2 . ? O3 La1 N5 25.25(14) . . ? O8 La1 N5 117.8(2) . . ? O1 La1 N5 110.36(14) . . ? O2 La1 N5 90.49(14) . . ? O7 La1 N5 139.14(9) . . ? N6 La1 N5 81.61(12) . . ? C10 P1 C4 99.8(2) . . ? C10 P1 C16 105.0(2) . . ? C4 P1 C16 102.7(2) . . ? C10 P1 Re1 116.54(15) . . ? C4 P1 Re1 120.62(14) . . ? C16 P1 Re1 110.20(16) . . ? C27 P2 C21 99.8(2) . . ? C27 P2 C20 103.4(2) . . ? C21 P2 C20 102.6(2) . . ? C27 P2 Re1 117.59(14) . . ? C21 P2 Re1 119.62(16) . . ? C20 P2 Re1 111.62(16) . . ? C44 P3 C33 99.1(2) . . ? C44 P3 C19 105.1(2) . . ? C33 P3 C19 103.5(2) . . ? C44 P3 Re1 115.27(14) . . ? C33 P3 Re1 120.13(16) . . ? C19 P3 Re1 111.82(15) . . ? C1 N1 La1 159.7(4) . . ? N1 C1 Re1 171.1(4) . . ? C31 C32 C27 120.2(6) . . ? N2 C2 Re1 173.0(4) . . ? N3 C3 Re1 171.0(4) . . ? C12 C11 C10 120.8(5) . . ? N8 O11 La2 95.3(3) . . ? N6 O5 La1 96.3(2) . . ? N5 O3 La1 94.5(3) . . ? C17 C16 P1 116.3(3) . . ? N8 O10 La2 97.7(3) . . ? N5 O4 La1 96.8(3) . . ? C17 C19 P3 115.5(3) . . ? C20 C17 C16 112.0(4) . . ? C20 C17 C18 106.8(4) . . ? C16 C17 C18 107.2(4) . . ? C20 C17 C19 112.0(4) . . ? C16 C17 C19 111.7(4) . . ? C18 C17 C19 106.8(4) . . ? N6 O6 La1 96.8(2) . . ? C17 C20 P2 117.0(3) . . ? C6 C5 C4 121.4(4) . . ? C2 N2 La2 158.8(3) . . ? C5 C4 C9 117.2(4) . . ? C5 C4 P1 121.2(3) . . ? C9 C4 P1 121.3(3) . . ? C7 C8 C9 120.2(5) . . ? O14 N8 O10 121.4(5) . . ? O14 N8 O11 121.6(5) . . ? O10 N8 O11 117.0(4) . . ? O14 N8 La2 174.3(4) . . ? O10 N8 La2 57.5(2) . . ? O11 N8 La2 59.6(2) . . ? C8 C7 C6 119.1(5) . . ? O13 N6 O5 121.6(4) . . ? O13 N6 O6 121.6(4) . . ? O5 N6 O6 116.7(4) . . ? O13 N6 La1 176.1(4) . . ? O5 N6 La1 58.7(2) . . ? O6 N6 La1 58.2(2) . . ? O4 N5 O12 122.3(6) . . ? O4 N5 O3 119.2(5) . . ? O12 N5 O3 118.6(6) . . ? O4 N5 La1 58.9(3) . . ? O12 N5 La1 178.8(5) . . ? O3 N5 La1 60.3(3) . . ? C7 C6 C5 120.5(4) . . ? C8 C9 C4 121.6(5) . . ? N4 O1 La2 96.0(2) . . ? N4 O1 La1 96.4(2) . . ? La2 O1 La1 166.16(13) . . ? N7 O7 La1 93.65(9) . . ? N7 O7 La1 93.65(9) . 2 ? La1 O7 La1 172.70(19) . 2 ? N4 O2 La1 97.4(3) . . ? C3 N3 La1 157.8(3) . 2 ? O2 N4 O9 122.2(4) . . ? O2 N4 O1 119.2(4) . . ? O9 N4 O1 118.5(4) . . ? C43 C44 C39 117.9(4) . . ? C43 C44 P3 125.8(4) . . ? C39 C44 P3 116.3(3) . . ? C26 C21 C22 117.6(5) . . ? C26 C21 P2 122.7(4) . . ? C22 C21 P2 119.6(4) . . ? C25 C26 C21 121.2(5) . . ? C34 C33 C38 119.0(5) . . ? C34 C33 P3 122.0(3) . . ? C38 C33 P3 118.7(4) . . ? N7 O8 La1 102.8(4) . . ? C40 C39 C44 121.2(4) . . ? N4 O9 La2 97.7(3) . . ? C11 C10 C15 118.9(5) . . ? C11 C10 P1 118.5(3) . . ? C15 C10 P1 122.7(4) . . ? C32 C27 C28 118.2(5) . . ? C32 C27 P2 117.4(4) . . ? C28 C27 P2 124.5(4) . . ? C29 C28 C27 120.3(5) . . ? C36 C35 C34 119.7(6) . . ? C33 C34 C35 120.8(5) . . ? C37 C38 C33 119.6(6) . . ? C42 C43 C44 119.9(5) . . ? C23 C24 C25 119.7(5) . . ? C41 C42 C43 121.2(5) . . ? C14 C15 C10 119.9(5) . . ? C26 C25 C24 120.6(5) . . ? C38 C37 C36 121.1(5) . . ? C30 C31 C32 121.0(6) . . ? O7 N7 O8 117.6(3) . 2 ? O7 N7 O8 117.6(3) . . ? O8 N7 O8 124.7(7) 2 . ? C42 C41 C40 119.4(5) . . ? C13 C12 C11 119.9(6) . . ? C21 C22 C23 122.0(6) . . ? C37 C36 C35 119.7(5) . . ? C39 C40 C41 120.5(5) . . ? C13 C14 C15 120.5(5) . . ? C12 C13 C14 119.9(5) . . ? C24 C23 C22 118.9(6) . . ? C31 C30 C29 119.0(5) . . ? C50 N9 C46 112.3(4) . . ? C50 N9 C52 106.9(4) . . ? C46 N9 C52 110.2(4) . . ? C50 N9 C48 111.3(4) . . ? C46 N9 C48 106.5(4) . . ? C52 N9 C48 109.7(5) . . ? N9 C46 C45 113.7(4) . . ? C47 C48 N9 115.9(5) . . ? N9 C50 C49 115.7(5) . . ? C51 C52 N9 115.3(5) . . ? C28 C29 C30 121.3(5) . . ? N10 C53 C54 177.1 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.044 _refine_diff_density_min -1.510 _refine_diff_density_rms 0.181 _database_code_depnum_ccdc_archive 'CCDC 972572' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_f:\ms057tb\struct\2\57sc _audit_creation_method SHELXL-97 __chemical_name_systematic (Et4N)2[(triphosRe(CN)3)2(Tb(NO3)3)3]?4CH3CN _chemical_name_common 2 _chemical_formula_moiety C88H78N15O27P6Re2Tb3,2C8H20N),4(C2H3N) _chemical_formula_sum 'C112 H130 N21 O27 P6 Re2 Tb3' _chemical_properties_physical air-sensitive _exptl_crystal_recrystallization_method CH3CN _chemical_melting_point 300 _chemical_formula_weight 3237.35 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 '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 'C 2/c' _symmetry_int_tables_number 15 _chemical_absolute_configuration ? _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 36.149(7) _cell_length_b 13.737(3) _cell_length_c 26.215(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.85(3) _cell_angle_gamma 90.00 _cell_volume 12640(4) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6400 _exptl_absorpt_coefficient_mu 3.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4566 _exptl_absorpt_correction_T_max 0.6639 _exptl_absorpt_process_details 'Bruker AXS Scale, SADABS (Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 67419 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 26.73 _reflns_number_total 13403 _reflns_number_gt 10760 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEXII (Bruker 2008)' _computing_cell_refinement 'SAINT v7.60A (Bruker 2008)' _computing_data_reduction 'SAINT v7.60A, XPREP v2008/2 (Bruker 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond (Pennington, 2013)' _computing_publication_material 'SHELXS-97 (Sheldrick, 2008)' _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 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+212.6166*P+(0.0634P)^2^+0.0400sin\q/\l] where P = 0.33330Fo^2^ + 0.66670Fc^2^ ; _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 13403 _refine_ls_number_parameters 778 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1473 _refine_ls_wR_factor_gt 0.1301 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.001 _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 0.127157(7) 0.79413(2) 0.323920(11) 0.03532(9) Uani 1 1 d . . . Tb1 Tb -0.014557(10) 0.70106(3) 0.348688(14) 0.04040(11) Uani 1 1 d . . . Tb2 Tb 0.0000 1.01842(3) 0.2500 0.03554(12) Uani 1 2 d S . . P1 P 0.16146(6) 0.88454(15) 0.39992(8) 0.0447(5) Uani 1 1 d . . . P2 P 0.16728(6) 0.65702(15) 0.35924(8) 0.0436(5) Uani 1 1 d . . . P3 P 0.17850(5) 0.84378(15) 0.28526(9) 0.0442(5) Uani 1 1 d . . . C2 C 0.08895(19) 0.9052(5) 0.2979(3) 0.0369(15) Uani 1 1 d . . . C1 C 0.0816(2) 0.7435(5) 0.3506(3) 0.0391(16) Uani 1 1 d . . . N6 N 0.0206(2) 0.6016(5) 0.4443(3) 0.0540(17) Uani 1 1 d . . . O13 O 0.03922(16) 1.1596(4) 0.2846(2) 0.0515(14) Uani 1 1 d . . . C3 C 0.0953(2) 0.7313(6) 0.2556(3) 0.0407(16) Uani 1 1 d . . . O12 O 0.03968(16) 1.1149(4) 0.2055(2) 0.0515(14) Uani 1 1 d . . . N1 N 0.05309(19) 0.7177(5) 0.3584(2) 0.0425(14) Uani 1 1 d . . . O6 O 0.01108(18) 0.6906(4) 0.4441(2) 0.0546(15) Uani 1 1 d . . . C20 C 0.2185(2) 0.6859(7) 0.3682(4) 0.060(2) Uani 1 1 d . . . H20A H 0.2334 0.6423 0.3955 0.072 Uiso 1 1 calc R . . H20B H 0.2259 0.6715 0.3349 0.072 Uiso 1 1 calc R . . N8 N 0.05263(19) 1.1713(5) 0.2438(3) 0.0511(17) Uani 1 1 d . . . C10 C 0.1719(2) 1.0158(6) 0.3940(3) 0.0446(18) Uani 1 1 d . . . C17 C 0.2237(2) 0.8597(7) 0.3357(4) 0.058(2) Uani 1 1 d . . . H17A H 0.2451 0.8490 0.3187 0.070 Uiso 1 1 calc R . . H17B H 0.2252 0.9281 0.3479 0.070 Uiso 1 1 calc R . . C13 C 0.1852(2) 1.2157(7) 0.3883(4) 0.054(2) Uani 1 1 d . . . H13 H 0.1898 1.2834 0.3860 0.065 Uiso 1 1 calc R . . C40 C 0.2240(3) 0.7901(8) 0.2166(5) 0.080(4) Uani 1 1 d . . . H40 H 0.2374 0.8485 0.2284 0.096 Uiso 1 1 calc R . . O14 O 0.0766(2) 1.2339(5) 0.2428(3) 0.077(2) Uani 1 1 d . . . O10 O 0.0370(2) 0.5613(6) 0.4855(3) 0.078(2) Uani 1 1 d . . . C22 C 0.1890(3) 0.5246(7) 0.4426(4) 0.063(3) Uani 1 1 d . . . H22 H 0.2072 0.5027 0.4244 0.076 Uiso 1 1 calc R . . C16 C 0.2093(3) 0.8314(7) 0.4255(4) 0.064(3) Uani 1 1 d . . . H16A H 0.2257 0.8814 0.4469 0.077 Uiso 1 1 calc R . . H16B H 0.2069 0.7769 0.4493 0.077 Uiso 1 1 calc R . . C26 C 0.1386(3) 0.6331(6) 0.4499(3) 0.053(2) Uani 1 1 d . . . H26 H 0.1222 0.6862 0.4368 0.063 Uiso 1 1 calc R . . C29 C 0.1131(2) 0.4339(6) 0.2706(4) 0.0490(19) Uani 1 1 d . . . H29 H 0.0873 0.4139 0.2583 0.059 Uiso 1 1 calc R . . C11 C 0.1990(3) 1.0631(7) 0.4332(4) 0.062(3) Uani 1 1 d . . . H11 H 0.2132 1.0272 0.4623 0.075 Uiso 1 1 calc R . . O5 O 0.0133(2) 0.5592(4) 0.4004(2) 0.0633(17) Uani 1 1 d . . . C31 C 0.1797(3) 0.4090(7) 0.2765(4) 0.057(2) Uani 1 1 d . . . H31 H 0.1995 0.3723 0.2675 0.068 Uiso 1 1 calc R . . C12 C 0.2051(3) 1.1627(7) 0.4298(4) 0.064(3) Uani 1 1 d . . . H12 H 0.2234 1.1942 0.4568 0.077 Uiso 1 1 calc R . . C4 C 0.1405(3) 0.8878(6) 0.4565(3) 0.050(2) Uani 1 1 d . . . C34 C 0.1375(3) 0.9790(8) 0.2173(4) 0.062(2) Uani 1 1 d . . . H34 H 0.1173 0.9335 0.2146 0.075 Uiso 1 1 calc R . . C28 C 0.1217(2) 0.5171(6) 0.3007(3) 0.0450(17) Uani 1 1 d . . . H28 H 0.1017 0.5547 0.3085 0.054 Uiso 1 1 calc R . . C15 C 0.1519(2) 1.0708(6) 0.3523(3) 0.0428(17) Uani 1 1 d . . . H15 H 0.1334 1.0400 0.3252 0.051 Uiso 1 1 calc R . . C21 C 0.1649(2) 0.6039(6) 0.4230(3) 0.0488(19) Uani 1 1 d . . . C43 C 0.1838(3) 0.6231(7) 0.1795(3) 0.053(2) Uani 1 1 d . . . H43 H 0.1694 0.5668 0.1662 0.063 Uiso 1 1 calc R . . C9 C 0.1016(3) 0.8951(7) 0.4484(3) 0.059(2) Uani 1 1 d . . . H9 H 0.0865 0.9010 0.4135 0.070 Uiso 1 1 calc R . . C27 C 0.1598(2) 0.5467(6) 0.3197(3) 0.0425(17) Uani 1 1 d . . . C39 C 0.1930(2) 0.7625(7) 0.2366(4) 0.055(2) Uani 1 1 d . . . C42 C 0.2153(3) 0.6483(8) 0.1616(4) 0.064(3) Uani 1 1 d . . . H42 H 0.2233 0.6078 0.1369 0.077 Uiso 1 1 calc R . . C5 C 0.1621(4) 0.8815(8) 0.5083(4) 0.076(3) Uani 1 1 d . . . H5 H 0.1891 0.8776 0.5152 0.091 Uiso 1 1 calc R . . C6 C 0.1443(5) 0.8810(9) 0.5495(4) 0.090(4) Uani 1 1 d . . . H6 H 0.1593 0.8767 0.5846 0.108 Uiso 1 1 calc R . . C32 C 0.1885(2) 0.4913(6) 0.3076(4) 0.053(2) Uani 1 1 d . . . H32 H 0.2143 0.5099 0.3205 0.063 Uiso 1 1 calc R . . C8 C 0.0839(4) 0.8939(8) 0.4897(4) 0.071(3) Uani 1 1 d . . . H8 H 0.0569 0.8982 0.4831 0.085 Uiso 1 1 calc R . . C14 C 0.1581(2) 1.1695(6) 0.3493(3) 0.0472(18) Uani 1 1 d . . . H14 H 0.1439 1.2060 0.3204 0.057 Uiso 1 1 calc R . . C41 C 0.2352(3) 0.7323(10) 0.1793(6) 0.089(4) Uani 1 1 d . . . H41 H 0.2565 0.7505 0.1661 0.107 Uiso 1 1 calc R . . C7 C 0.1057(4) 0.8863(9) 0.5409(4) 0.083(4) Uani 1 1 d . . . H7 H 0.0939 0.8850 0.5696 0.100 Uiso 1 1 calc R . . C44 C 0.1729(2) 0.6806(6) 0.2175(3) 0.0489(19) Uani 1 1 d . . . H44 H 0.1514 0.6625 0.2302 0.059 Uiso 1 1 calc R . . C30 C 0.1421(3) 0.3798(6) 0.2586(4) 0.055(2) Uani 1 1 d . . . H30 H 0.1363 0.3224 0.2380 0.066 Uiso 1 1 calc R . . C18 C 0.2296(2) 0.7931(7) 0.3840(4) 0.064(3) Uani 1 1 d . . . O8 O 0.0000 0.7007(5) 0.2500 0.0413(16) Uani 1 2 d S . . O9 O 0.01459(18) 1.0012(4) 0.3518(2) 0.0541(14) Uani 1 1 d . . . O7 O -0.00562(18) 0.5641(4) 0.2896(2) 0.0517(14) Uani 1 1 d . . . N2 N 0.06359(17) 0.9581(5) 0.2826(3) 0.0426(15) Uani 1 1 d . . . O2 O 0.0051(2) 0.8673(5) 0.3926(2) 0.071(2) Uani 1 1 d . . . N3 N 0.07282(19) 0.7055(5) 0.2185(3) 0.0454(15) Uani 1 1 d . . . O3 O -0.0665(2) 0.7650(7) 0.3890(3) 0.0724(19) Uani 1 1 d . . . N7 N 0.0000 0.6087(8) 0.2500 0.049(2) Uani 1 2 d S . . O4 O -0.0624(2) 0.6053(6) 0.3802(3) 0.081(2) Uani 1 1 d . . . N4 N 0.0038(2) 0.9140(5) 0.3518(3) 0.0550(18) Uani 1 1 d . . . N5 N -0.0765(3) 0.6816(9) 0.3950(3) 0.081(3) Uani 1 1 d . . . C23 C 0.1858(4) 0.4790(8) 0.4885(4) 0.080(3) Uani 1 1 d . . . H23 H 0.2026 0.4271 0.5023 0.096 Uiso 1 1 calc R . . O1 O -0.00880(15) 0.8710(4) 0.3071(2) 0.0445(12) Uani 1 1 d . . . N9 N 0.0497(3) 1.2556(6) 0.4300(3) 0.061(2) Uani 1 1 d . . . C33 C 0.1727(3) 0.9579(6) 0.2492(4) 0.051(2) Uani 1 1 d . . . C50 C 0.0768(3) 1.1818(8) 0.4191(4) 0.070(3) Uani 1 1 d . . . H50A H 0.0843 1.2000 0.3865 0.084 Uiso 1 1 calc R . . H50B H 0.0637 1.1180 0.4131 0.084 Uiso 1 1 calc R . . C25 C 0.1352(3) 0.5867(7) 0.4961(3) 0.062(2) Uani 1 1 d . . . H25 H 0.1172 0.6086 0.5145 0.075 Uiso 1 1 calc R . . C24 C 0.1590(4) 0.5072(8) 0.5145(4) 0.074(3) Uani 1 1 d . . . H24 H 0.1565 0.4730 0.5450 0.088 Uiso 1 1 calc R . . C38 C 0.2025(4) 1.0252(8) 0.2515(4) 0.073(3) Uani 1 1 d . . . H38 H 0.2274 1.0130 0.2725 0.087 Uiso 1 1 calc R . . O11 O -0.1065(3) 0.6704(10) 0.4163(4) 0.123(4) Uani 1 1 d . . . C46 C 0.0148(4) 1.2500(9) 0.3819(5) 0.081(3) Uani 1 1 d . . . H46A H 0.0235 1.2662 0.3499 0.098 Uiso 1 1 calc R . . H46B H 0.0055 1.1820 0.3783 0.098 Uiso 1 1 calc R . . C35 C 0.1307(4) 1.0656(10) 0.1890(4) 0.089(4) Uani 1 1 d . . . H35 H 0.1061 1.0793 0.1678 0.107 Uiso 1 1 calc R . . C19 C 0.2725(3) 0.7936(8) 0.4105(6) 0.098(5) Uani 1 1 d . . . H19A H 0.2869 0.7729 0.3850 0.147 Uiso 1 1 calc R . . H19B H 0.2776 0.7486 0.4404 0.147 Uiso 1 1 calc R . . H19C H 0.2803 0.8595 0.4228 0.147 Uiso 1 1 calc R . . C49 C 0.1129(4) 1.1713(10) 0.4639(5) 0.089(4) Uani 1 1 d . . . H49A H 0.1261 1.2341 0.4701 0.133 Uiso 1 1 calc R . . H49B H 0.1299 1.1227 0.4541 0.133 Uiso 1 1 calc R . . H49C H 0.1058 1.1503 0.4960 0.133 Uiso 1 1 calc R . . C48 C 0.0659(4) 1.3551(8) 0.4384(5) 0.084(3) Uani 1 1 d . . . H48A H 0.0863 1.3553 0.4712 0.100 Uiso 1 1 calc R . . H48B H 0.0457 1.4000 0.4436 0.100 Uiso 1 1 calc R . . C52 C 0.0367(4) 1.2285(10) 0.4792(5) 0.086(4) Uani 1 1 d . . . H52A H 0.0590 1.2306 0.5096 0.104 Uiso 1 1 calc R . . H52B H 0.0185 1.2786 0.4851 0.104 Uiso 1 1 calc R . . C37 C 0.1941(6) 1.1114(9) 0.2215(6) 0.107(6) Uani 1 1 d . . . H37 H 0.2140 1.1573 0.2230 0.128 Uiso 1 1 calc R . . C47 C 0.0823(5) 1.3945(9) 0.3940(6) 0.109(5) Uani 1 1 d . . . H47A H 0.1072 1.3646 0.3959 0.163 Uiso 1 1 calc R . . H47B H 0.0852 1.4653 0.3975 0.163 Uiso 1 1 calc R . . H47C H 0.0650 1.3788 0.3601 0.163 Uiso 1 1 calc R . . C36 C 0.1601(6) 1.1317(9) 0.1916(5) 0.101(6) Uani 1 1 d . . . H36 H 0.1558 1.1907 0.1722 0.121 Uiso 1 1 calc R . . C51 C 0.0183(5) 1.1313(10) 0.4783(6) 0.104(5) Uani 1 1 d . . . H51A H -0.0047 1.1292 0.4495 0.156 Uiso 1 1 calc R . . H51B H 0.0114 1.1202 0.5117 0.156 Uiso 1 1 calc R . . H51C H 0.0361 1.0807 0.4729 0.156 Uiso 1 1 calc R . . C54 C 0.2030(5) 0.8985(13) 0.0866(6) 0.107(5) Uani 1 1 d . . . C53 C 0.1677(5) 0.8846(12) 0.1020(7) 0.120(6) Uani 1 1 d . . . H53A H 0.1491 0.9334 0.0846 0.180 Uiso 1 1 calc R . . H53B H 0.1722 0.8918 0.1402 0.180 Uiso 1 1 calc R . . H53C H 0.1578 0.8193 0.0917 0.180 Uiso 1 1 calc R . . C45 C -0.0188(4) 1.3166(11) 0.3840(7) 0.113(5) Uani 1 1 d . . . H45A H -0.0267 1.3048 0.4168 0.170 Uiso 1 1 calc R . . H45B H -0.0402 1.3028 0.3540 0.170 Uiso 1 1 calc R . . H45C H -0.0111 1.3847 0.3828 0.170 Uiso 1 1 calc R . . N10 N 0.2300(5) 0.9107(15) 0.0729(6) 0.168(9) Uani 1 1 d . . . C56 C 0.1305(12) 0.3872(18) 0.1305(11) 0.32(4) Uani 1 1 d D . . C55 C 0.0964(8) 0.446(4) 0.1165(15) 0.42(4) Uani 1 1 d D . . H55A H 0.0740 0.4044 0.1127 0.624 Uiso 1 1 calc R . . H55B H 0.0955 0.4796 0.0832 0.624 Uiso 1 1 calc R . . H55C H 0.0967 0.4944 0.1441 0.624 Uiso 1 1 calc R . . N11 N 0.1602(12) 0.361(2) 0.1402(13) 0.34(3) Uani 1 1 d 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 0.02695(14) 0.03542(16) 0.03816(16) 0.00534(11) -0.00289(11) 0.00259(10) Tb1 0.03316(19) 0.0445(2) 0.0394(2) -0.00099(15) 0.00042(14) 0.00455(14) Tb2 0.0251(2) 0.0307(2) 0.0430(3) 0.000 -0.00723(18) 0.000 P1 0.0391(10) 0.0386(10) 0.0450(11) 0.0043(8) -0.0126(8) 0.0021(8) P2 0.0353(10) 0.0390(10) 0.0483(11) 0.0056(9) -0.0059(8) 0.0067(8) P3 0.0259(9) 0.0428(11) 0.0604(13) 0.0034(9) 0.0035(8) 0.0032(8) C2 0.026(3) 0.043(4) 0.040(4) 0.001(3) 0.003(3) -0.004(3) C1 0.042(4) 0.036(4) 0.035(4) 0.002(3) 0.000(3) 0.000(3) N6 0.058(4) 0.051(4) 0.047(4) 0.013(3) 0.003(3) 0.002(3) O13 0.042(3) 0.041(3) 0.064(4) -0.007(3) -0.003(3) -0.003(2) C3 0.029(3) 0.044(4) 0.047(4) 0.008(3) 0.005(3) 0.006(3) O12 0.044(3) 0.050(3) 0.055(3) 0.005(3) 0.000(3) -0.007(3) N1 0.041(4) 0.045(4) 0.038(3) 0.001(3) 0.001(3) -0.003(3) O6 0.061(4) 0.055(4) 0.044(3) -0.002(3) 0.005(3) 0.014(3) C20 0.037(4) 0.053(5) 0.076(6) 0.011(4) -0.012(4) 0.012(4) N8 0.038(4) 0.038(3) 0.071(5) 0.007(3) -0.001(3) -0.001(3) C10 0.034(4) 0.036(4) 0.056(5) 0.002(3) -0.004(3) -0.002(3) C17 0.029(4) 0.051(5) 0.087(7) -0.007(5) -0.003(4) 0.000(3) C13 0.040(4) 0.050(5) 0.072(6) 0.004(4) 0.015(4) -0.009(4) C40 0.039(5) 0.082(7) 0.125(10) -0.040(7) 0.036(6) -0.012(5) O14 0.056(4) 0.053(4) 0.120(7) -0.004(4) 0.016(4) -0.020(3) O10 0.101(6) 0.069(5) 0.052(4) 0.019(3) -0.003(4) 0.013(4) C22 0.073(6) 0.050(5) 0.054(5) 0.006(4) -0.011(5) 0.017(5) C16 0.047(5) 0.051(5) 0.073(6) -0.003(5) -0.027(4) 0.007(4) C26 0.060(5) 0.046(5) 0.043(4) 0.007(4) -0.008(4) 0.003(4) C29 0.045(4) 0.039(4) 0.065(5) -0.004(4) 0.017(4) -0.003(3) C11 0.050(5) 0.051(5) 0.069(6) 0.003(4) -0.020(4) -0.003(4) O5 0.090(5) 0.043(3) 0.048(3) 0.001(3) 0.000(3) -0.003(3) C31 0.058(5) 0.048(5) 0.071(6) 0.013(4) 0.026(5) 0.018(4) C12 0.051(5) 0.055(5) 0.077(7) -0.013(5) -0.003(5) -0.012(4) C4 0.067(6) 0.035(4) 0.038(4) 0.003(3) -0.008(4) -0.001(4) C34 0.063(6) 0.071(6) 0.060(6) 0.018(5) 0.029(5) 0.014(5) C28 0.039(4) 0.039(4) 0.055(5) 0.003(3) 0.008(3) 0.003(3) C15 0.035(4) 0.043(4) 0.049(4) 0.003(3) 0.007(3) 0.001(3) C21 0.051(5) 0.042(4) 0.042(4) 0.004(3) -0.012(4) 0.006(4) C43 0.052(5) 0.054(5) 0.050(5) 0.000(4) 0.009(4) 0.004(4) C9 0.076(6) 0.057(5) 0.038(4) -0.001(4) 0.004(4) -0.017(5) C27 0.042(4) 0.039(4) 0.043(4) 0.009(3) 0.005(3) 0.008(3) C39 0.029(4) 0.055(5) 0.080(6) 0.003(5) 0.013(4) 0.010(3) C42 0.051(5) 0.066(6) 0.073(6) -0.008(5) 0.010(5) 0.020(5) C5 0.101(8) 0.067(6) 0.042(5) 0.005(5) -0.019(5) 0.018(6) C6 0.129(12) 0.083(8) 0.046(6) 0.015(5) -0.004(7) 0.020(8) C32 0.042(4) 0.044(4) 0.067(6) 0.007(4) 0.004(4) 0.014(4) C8 0.090(8) 0.071(7) 0.051(5) -0.009(5) 0.016(5) -0.023(6) C14 0.056(5) 0.044(4) 0.044(4) 0.003(3) 0.017(4) -0.005(4) C41 0.046(5) 0.105(9) 0.128(11) -0.035(8) 0.044(6) -0.010(6) C7 0.130(12) 0.076(7) 0.050(6) 0.004(5) 0.038(7) -0.011(7) C44 0.039(4) 0.050(5) 0.055(5) 0.012(4) 0.003(4) 0.006(3) C30 0.060(5) 0.039(4) 0.069(6) 0.002(4) 0.021(4) 0.000(4) C18 0.030(4) 0.051(5) 0.092(7) -0.001(5) -0.024(4) 0.005(3) O8 0.039(4) 0.032(4) 0.051(4) 0.000 0.006(3) 0.000 O9 0.068(4) 0.036(3) 0.053(3) -0.001(2) 0.004(3) 0.002(3) O7 0.072(4) 0.046(3) 0.038(3) 0.005(2) 0.014(3) 0.003(3) N2 0.029(3) 0.042(3) 0.051(4) 0.006(3) 0.000(3) 0.004(3) O2 0.124(6) 0.046(3) 0.041(3) 0.004(3) 0.018(4) 0.014(4) N3 0.036(3) 0.059(4) 0.039(3) 0.002(3) 0.005(3) 0.004(3) O3 0.067(4) 0.089(6) 0.056(4) -0.015(4) 0.005(3) 0.001(4) N7 0.038(5) 0.062(6) 0.047(5) 0.000 0.008(4) 0.000 O4 0.071(5) 0.081(5) 0.084(5) 0.032(4) 0.008(4) 0.001(4) N4 0.072(5) 0.044(4) 0.045(4) -0.001(3) 0.006(3) 0.016(4) N5 0.104(8) 0.087(7) 0.046(5) -0.001(5) 0.009(5) 0.013(6) C23 0.108(9) 0.061(6) 0.060(6) 0.016(5) -0.004(6) 0.035(6) O1 0.044(3) 0.040(3) 0.043(3) 0.001(2) -0.002(2) 0.002(2) N9 0.081(6) 0.053(4) 0.053(4) -0.008(4) 0.022(4) -0.003(4) C33 0.054(5) 0.046(4) 0.063(5) 0.005(4) 0.031(4) 0.007(4) C50 0.075(7) 0.070(7) 0.069(6) -0.019(5) 0.026(5) -0.007(5) C25 0.077(6) 0.063(6) 0.037(4) 0.006(4) -0.004(4) 0.004(5) C24 0.097(8) 0.063(6) 0.044(5) 0.012(5) -0.016(5) 0.011(6) C38 0.097(8) 0.067(6) 0.066(6) -0.013(5) 0.043(6) -0.028(6) O11 0.068(5) 0.219(13) 0.090(6) 0.008(7) 0.034(5) 0.002(7) C46 0.090(8) 0.075(7) 0.074(7) -0.019(6) 0.008(6) -0.011(6) C35 0.128(11) 0.092(9) 0.065(7) 0.031(6) 0.055(7) 0.063(8) C19 0.036(5) 0.073(7) 0.155(13) -0.011(7) -0.036(6) 0.013(5) C49 0.085(8) 0.085(8) 0.095(9) -0.016(7) 0.018(7) 0.001(7) C48 0.111(10) 0.066(7) 0.074(7) -0.022(6) 0.023(7) -0.018(7) C52 0.095(9) 0.096(9) 0.081(8) -0.018(7) 0.047(7) -0.008(7) C37 0.205(18) 0.058(7) 0.085(9) -0.018(7) 0.091(11) -0.051(10) C47 0.184(16) 0.060(7) 0.100(10) -0.016(7) 0.067(11) -0.042(9) C36 0.200(18) 0.057(7) 0.068(8) 0.014(6) 0.076(10) 0.014(10) C51 0.123(12) 0.083(9) 0.130(12) 0.002(8) 0.077(10) -0.014(8) C54 0.113(12) 0.118(12) 0.083(9) 0.016(8) 0.006(9) -0.036(10) C53 0.148(15) 0.105(12) 0.121(13) -0.002(10) 0.061(12) 0.028(11) C45 0.088(10) 0.106(11) 0.131(13) -0.041(10) 0.000(9) 0.009(8) N10 0.111(11) 0.25(2) 0.112(11) 0.096(13) -0.028(9) -0.065(13) C56 0.87(11) 0.051(11) 0.12(2) -0.023(13) 0.25(4) -0.02(3) C55 0.28(5) 0.71(12) 0.21(4) -0.15(6) -0.03(3) -0.23(7) N11 0.78(7) 0.12(2) 0.21(2) 0.047(18) 0.32(4) 0.11(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 2.058(8) . ? Re1 C2 2.062(7) . ? Re1 C3 2.073(8) . ? Re1 P3 2.416(2) . ? Re1 P2 2.4221(19) . ? Re1 P1 2.422(2) . ? Tb1 N3 2.402(7) 2 ? Tb1 N1 2.408(7) . ? Tb1 O5 2.449(6) . ? Tb1 O6 2.456(6) . ? Tb1 O4 2.466(8) . ? Tb1 O7 2.506(6) . ? Tb1 O3 2.523(8) . ? Tb1 O2 2.580(7) . ? Tb1 O1 2.606(5) . ? Tb1 O8 2.7608(7) . ? Tb1 N5 2.804(12) . ? Tb1 N6 2.870(7) . ? Tb2 N2 2.400(6) . ? Tb2 N2 2.400(6) 2 ? Tb2 O13 2.445(5) . ? Tb2 O13 2.445(5) 2 ? Tb2 O12 2.445(6) 2 ? Tb2 O12 2.445(6) . ? Tb2 O1 2.583(5) . ? Tb2 O1 2.583(5) 2 ? Tb2 O9 2.604(6) 2 ? Tb2 O9 2.604(6) . ? Tb2 N8 2.864(7) 2 ? Tb2 N8 2.864(7) . ? P1 C4 1.821(10) . ? P1 C16 1.848(9) . ? P1 C10 1.856(8) . ? P2 C27 1.820(8) . ? P2 C21 1.846(9) . ? P2 C20 1.852(9) . ? P3 C33 1.817(9) . ? P3 C17 1.852(8) . ? P3 C39 1.863(10) . ? C2 N2 1.163(9) . ? C1 N1 1.154(10) . ? N6 O10 1.233(9) . ? N6 O5 1.259(9) . ? N6 O6 1.269(9) . ? O13 N8 1.285(10) . ? C3 N3 1.162(10) . ? O12 N8 1.267(9) . ? C20 C18 1.557(13) . ? N8 O14 1.226(9) . ? C10 C15 1.382(11) . ? C10 C11 1.399(11) . ? C17 C18 1.536(14) . ? C13 C12 1.364(14) . ? C13 C14 1.387(12) . ? C40 C41 1.393(15) . ? C40 C39 1.398(13) . ? C22 C23 1.387(15) . ? C22 C21 1.411(11) . ? C16 C18 1.543(16) . ? C26 C21 1.373(13) . ? C26 C25 1.399(12) . ? C29 C28 1.381(11) . ? C29 C30 1.382(12) . ? C11 C12 1.392(13) . ? C31 C32 1.385(13) . ? C31 C30 1.386(13) . ? C4 C9 1.375(13) . ? C4 C5 1.397(11) . ? C34 C33 1.376(13) . ? C34 C35 1.393(14) . ? C28 C27 1.408(11) . ? C15 C14 1.381(11) . ? C43 C42 1.378(13) . ? C43 C44 1.398(12) . ? C9 C8 1.385(14) . ? C27 C32 1.384(11) . ? C39 C44 1.367(13) . ? C42 C41 1.380(16) . ? C5 C6 1.384(18) . ? C6 C7 1.360(18) . ? C8 C7 1.389(16) . ? C18 C19 1.539(11) . ? O8 N7 1.264(12) . ? O8 Tb1 2.7608(7) 2 ? O9 N4 1.259(9) . ? O7 N7 1.263(7) . ? O2 N4 1.238(9) . ? N3 Tb1 2.402(7) 2 ? O3 N5 1.222(13) . ? N7 O7 1.263(7) 2 ? O4 N5 1.268(12) . ? N4 O1 1.293(9) . ? N5 O11 1.340(13) . ? C23 C24 1.367(17) . ? N9 C48 1.482(13) . ? N9 C50 1.483(13) . ? N9 C52 1.523(14) . ? N9 C46 1.559(14) . ? C33 C38 1.411(13) . ? C50 C49 1.541(16) . ? C25 C24 1.402(14) . ? C38 C37 1.414(19) . ? C46 C45 1.532(18) . ? C35 C36 1.39(2) . ? C48 C47 1.525(16) . ? C52 C51 1.488(17) . ? C37 C36 1.32(2) . ? C54 N10 1.13(2) . ? C54 C53 1.44(2) . ? C56 N11 1.102(18) . ? C56 C55 1.447(17) . ? 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 80.5(3) . . ? C1 Re1 C3 80.1(3) . . ? C2 Re1 C3 80.3(3) . . ? C1 Re1 P3 174.5(2) . . ? C2 Re1 P3 100.0(2) . . ? C3 Re1 P3 94.6(2) . . ? C1 Re1 P2 93.6(2) . . ? C2 Re1 P2 174.0(2) . . ? C3 Re1 P2 99.5(2) . . ? P3 Re1 P2 85.99(7) . . ? C1 Re1 P1 100.8(2) . . ? C2 Re1 P1 93.6(2) . . ? C3 Re1 P1 173.7(2) . . ? P3 Re1 P1 84.65(8) . . ? P2 Re1 P1 86.70(7) . . ? N3 Tb1 N1 140.0(2) 2 . ? N3 Tb1 O5 126.8(2) 2 . ? N1 Tb1 O5 75.2(2) . . ? N3 Tb1 O6 143.1(2) 2 . ? N1 Tb1 O6 76.8(2) . . ? O5 Tb1 O6 52.0(2) . . ? N3 Tb1 O4 72.4(2) 2 . ? N1 Tb1 O4 142.2(2) . . ? O5 Tb1 O4 67.6(3) . . ? O6 Tb1 O4 75.6(2) . . ? N3 Tb1 O7 77.6(2) 2 . ? N1 Tb1 O7 81.9(2) . . ? O5 Tb1 O7 69.4(2) . . ? O6 Tb1 O7 120.84(19) . . ? O4 Tb1 O7 90.6(3) . . ? N3 Tb1 O3 71.8(2) 2 . ? N1 Tb1 O3 139.6(2) . . ? O5 Tb1 O3 107.1(3) . . ? O6 Tb1 O3 74.4(2) . . ? O4 Tb1 O3 52.7(3) . . ? O7 Tb1 O3 137.6(2) . . ? N3 Tb1 O2 113.9(2) 2 . ? N1 Tb1 O2 72.8(2) . . ? O5 Tb1 O2 115.1(2) . . ? O6 Tb1 O2 66.5(2) . . ? O4 Tb1 O2 117.6(3) . . ? O7 Tb1 O2 151.3(2) . . ? O3 Tb1 O2 70.1(3) . . ? N3 Tb1 O1 79.3(2) 2 . ? N1 Tb1 O1 77.21(19) . . ? O5 Tb1 O1 151.8(2) . . ? O6 Tb1 O1 115.48(19) . . ? O4 Tb1 O1 138.6(2) . . ? O7 Tb1 O1 112.28(17) . . ? O3 Tb1 O1 90.3(2) . . ? O2 Tb1 O1 49.62(18) . . ? N3 Tb1 O8 69.09(16) 2 . ? N1 Tb1 O8 71.53(16) . . ? O5 Tb1 O8 111.9(2) . . ? O6 Tb1 O8 147.64(15) . . ? O4 Tb1 O8 128.2(2) . . ? O7 Tb1 O8 48.55(19) . . ? O3 Tb1 O8 136.13(19) . . ? O2 Tb1 O8 109.0(2) . . ? O1 Tb1 O8 63.73(19) . . ? N3 Tb1 N5 70.7(2) 2 . ? N1 Tb1 N5 149.2(2) . . ? O5 Tb1 N5 87.1(3) . . ? O6 Tb1 N5 72.5(2) . . ? O4 Tb1 N5 26.9(3) . . ? O7 Tb1 N5 115.5(3) . . ? O3 Tb1 N5 25.8(3) . . ? O2 Tb1 N5 93.1(3) . . ? O1 Tb1 N5 114.7(3) . . ? O8 Tb1 N5 139.2(2) . . ? N3 Tb1 N6 141.3(2) 2 . ? N1 Tb1 N6 74.1(2) . . ? O5 Tb1 N6 25.9(2) . . ? O6 Tb1 N6 26.1(2) . . ? O4 Tb1 N6 69.7(2) . . ? O7 Tb1 N6 95.0(2) . . ? O3 Tb1 N6 91.1(2) . . ? O2 Tb1 N6 90.8(2) . . ? O1 Tb1 N6 136.77(19) . . ? O8 Tb1 N6 132.34(19) . . ? N5 Tb1 N6 79.0(3) . . ? N2 Tb2 N2 139.6(3) . 2 ? N2 Tb2 O13 73.8(2) . . ? N2 Tb2 O13 145.8(2) 2 . ? N2 Tb2 O13 145.8(2) . 2 ? N2 Tb2 O13 73.8(2) 2 2 ? O13 Tb2 O13 75.0(3) . 2 ? N2 Tb2 O12 129.7(2) . 2 ? N2 Tb2 O12 74.7(2) 2 2 ? O13 Tb2 O12 75.4(2) . 2 ? O13 Tb2 O12 52.6(2) 2 2 ? N2 Tb2 O12 74.7(2) . . ? N2 Tb2 O12 129.7(2) 2 . ? O13 Tb2 O12 52.6(2) . . ? O13 Tb2 O12 75.4(2) 2 . ? O12 Tb2 O12 114.3(3) 2 . ? N2 Tb2 O1 76.3(2) . . ? N2 Tb2 O1 72.3(2) 2 . ? O13 Tb2 O1 123.21(19) . . ? O13 Tb2 O1 134.10(19) 2 . ? O12 Tb2 O1 88.89(19) 2 . ? O12 Tb2 O1 150.40(18) . . ? N2 Tb2 O1 72.3(2) . 2 ? N2 Tb2 O1 76.3(2) 2 2 ? O13 Tb2 O1 134.10(19) . 2 ? O13 Tb2 O1 123.21(19) 2 2 ? O12 Tb2 O1 150.40(18) 2 2 ? O12 Tb2 O1 88.89(19) . 2 ? O1 Tb2 O1 76.7(2) . 2 ? N2 Tb2 O9 106.0(2) . 2 ? N2 Tb2 O9 70.2(2) 2 2 ? O13 Tb2 O9 114.2(2) . 2 ? O13 Tb2 O9 74.6(2) 2 2 ? O12 Tb2 O9 122.71(19) 2 2 ? O12 Tb2 O9 63.79(19) . 2 ? O1 Tb2 O9 119.98(17) . 2 ? O1 Tb2 O9 50.01(17) 2 2 ? N2 Tb2 O9 70.2(2) . . ? N2 Tb2 O9 106.0(2) 2 . ? O13 Tb2 O9 74.6(2) . . ? O13 Tb2 O9 114.2(2) 2 . ? O12 Tb2 O9 63.79(19) 2 . ? O12 Tb2 O9 122.71(19) . . ? O1 Tb2 O9 50.02(17) . . ? O1 Tb2 O9 119.98(17) 2 . ? O9 Tb2 O9 169.5(2) 2 . ? N2 Tb2 N8 145.6(2) . 2 ? N2 Tb2 N8 71.4(2) 2 2 ? O13 Tb2 N8 74.43(19) . 2 ? O13 Tb2 N8 26.5(2) 2 2 ? O12 Tb2 N8 26.1(2) 2 2 ? O12 Tb2 N8 95.9(2) . 2 ? O1 Tb2 N8 111.5(2) . 2 ? O1 Tb2 N8 141.55(18) 2 2 ? O9 Tb2 N8 98.6(2) 2 2 ? O9 Tb2 N8 89.0(2) . 2 ? N2 Tb2 N8 71.4(2) . . ? N2 Tb2 N8 145.6(2) 2 . ? O13 Tb2 N8 26.5(2) . . ? O13 Tb2 N8 74.43(19) 2 . ? O12 Tb2 N8 95.9(2) 2 . ? O12 Tb2 N8 26.1(2) . . ? O1 Tb2 N8 141.55(18) . . ? O1 Tb2 N8 111.5(2) 2 . ? O9 Tb2 N8 89.0(2) 2 . ? O9 Tb2 N8 98.6(2) . . ? N8 Tb2 N8 85.7(3) 2 . ? C4 P1 C16 104.4(5) . . ? C4 P1 C10 100.2(4) . . ? C16 P1 C10 102.9(4) . . ? C4 P1 Re1 116.9(3) . . ? C16 P1 Re1 110.3(3) . . ? C10 P1 Re1 120.3(3) . . ? C27 P2 C21 98.9(4) . . ? C27 P2 C20 105.0(4) . . ? C21 P2 C20 103.4(4) . . ? C27 P2 Re1 115.8(2) . . ? C21 P2 Re1 120.1(3) . . ? C20 P2 Re1 111.8(3) . . ? C33 P3 C17 104.0(4) . . ? C33 P3 C39 100.2(4) . . ? C17 P3 C39 102.4(4) . . ? C33 P3 Re1 117.2(3) . . ? C17 P3 Re1 111.6(3) . . ? C39 P3 Re1 119.3(3) . . ? N2 C2 Re1 170.6(6) . . ? N1 C1 Re1 170.3(6) . . ? O10 N6 O5 123.0(8) . . ? O10 N6 O6 120.6(8) . . ? O5 N6 O6 116.4(7) . . ? O10 N6 Tb1 177.4(7) . . ? O5 N6 Tb1 58.0(4) . . ? O6 N6 Tb1 58.4(4) . . ? N8 O13 Tb2 95.3(4) . . ? N3 C3 Re1 169.2(7) . . ? N8 O12 Tb2 95.7(5) . . ? C1 N1 Tb1 159.7(6) . . ? N6 O6 Tb1 95.5(5) . . ? C18 C20 P2 115.0(6) . . ? O14 N8 O12 122.8(8) . . ? O14 N8 O13 121.0(8) . . ? O12 N8 O13 116.2(6) . . ? O14 N8 Tb2 176.7(6) . . ? O12 N8 Tb2 58.2(4) . . ? O13 N8 Tb2 58.2(4) . . ? C15 C10 C11 118.0(8) . . ? C15 C10 P1 121.2(6) . . ? C11 C10 P1 120.7(6) . . ? C18 C17 P3 116.3(6) . . ? C12 C13 C14 119.3(8) . . ? C41 C40 C39 120.1(10) . . ? C23 C22 C21 119.5(10) . . ? C18 C16 P1 116.1(6) . . ? C21 C26 C25 121.7(8) . . ? C28 C29 C30 119.7(8) . . ? C12 C11 C10 120.2(9) . . ? N6 O5 Tb1 96.1(5) . . ? C32 C31 C30 120.3(8) . . ? C13 C12 C11 120.9(9) . . ? C9 C4 C5 117.9(10) . . ? C9 C4 P1 119.0(6) . . ? C5 C4 P1 123.1(9) . . ? C33 C34 C35 121.5(11) . . ? C29 C28 C27 120.6(8) . . ? C14 C15 C10 121.4(8) . . ? C26 C21 C22 118.9(8) . . ? C26 C21 P2 122.5(6) . . ? C22 C21 P2 118.4(7) . . ? C42 C43 C44 119.8(9) . . ? C4 C9 C8 121.7(9) . . ? C32 C27 C28 119.0(8) . . ? C32 C27 P2 124.8(7) . . ? C28 C27 P2 116.2(6) . . ? C44 C39 C40 119.3(9) . . ? C44 C39 P3 122.1(7) . . ? C40 C39 P3 118.4(7) . . ? C43 C42 C41 120.2(9) . . ? C6 C5 C4 120.2(12) . . ? C7 C6 C5 121.3(11) . . ? C27 C32 C31 120.2(8) . . ? C9 C8 C7 119.6(12) . . ? C15 C14 C13 120.2(8) . . ? C42 C41 C40 119.8(10) . . ? C6 C7 C8 119.3(11) . . ? C39 C44 C43 120.7(8) . . ? C29 C30 C31 120.2(9) . . ? C17 C18 C19 107.2(9) . . ? C17 C18 C16 112.6(7) . . ? C19 C18 C16 106.2(9) . . ? C17 C18 C20 111.5(8) . . ? C19 C18 C20 107.0(7) . . ? C16 C18 C20 112.0(9) . . ? N7 O8 Tb1 90.10(14) . . ? N7 O8 Tb1 90.10(14) . 2 ? Tb1 O8 Tb1 179.8(3) . 2 ? N4 O9 Tb2 95.7(5) . . ? N7 O7 Tb1 102.4(5) . . ? C2 N2 Tb2 161.3(6) . . ? N4 O2 Tb1 97.1(5) . . ? C3 N3 Tb1 159.3(6) . 2 ? N5 O3 Tb1 90.1(7) . . ? O7 N7 O7 122.0(10) . 2 ? O7 N7 O8 119.0(5) . . ? O7 N7 O8 119.0(5) 2 . ? N5 O4 Tb1 91.6(7) . . ? O2 N4 O9 123.0(7) . . ? O2 N4 O1 118.6(7) . . ? O9 N4 O1 118.4(7) . . ? O3 N5 O4 125.5(11) . . ? O3 N5 O11 117.1(11) . . ? O4 N5 O11 117.2(12) . . ? O3 N5 Tb1 64.1(6) . . ? O4 N5 Tb1 61.5(6) . . ? O11 N5 Tb1 178.4(9) . . ? C24 C23 C22 121.4(9) . . ? N4 O1 Tb2 95.8(4) . . ? N4 O1 Tb1 94.4(4) . . ? Tb2 O1 Tb1 168.0(2) . . ? C48 N9 C50 113.8(9) . . ? C48 N9 C52 106.9(8) . . ? C50 N9 C52 110.4(9) . . ? C48 N9 C46 112.4(9) . . ? C50 N9 C46 104.8(8) . . ? C52 N9 C46 108.5(9) . . ? C34 C33 C38 118.3(9) . . ? C34 C33 P3 118.2(7) . . ? C38 C33 P3 123.4(8) . . ? N9 C50 C49 113.3(9) . . ? C26 C25 C24 118.7(10) . . ? C23 C24 C25 119.9(10) . . ? C33 C38 C37 117.7(13) . . ? C45 C46 N9 115.9(10) . . ? C36 C35 C34 119.9(13) . . ? N9 C48 C47 115.1(9) . . ? C51 C52 N9 115.7(10) . . ? C36 C37 C38 123.5(14) . . ? C37 C36 C35 119.0(12) . . ? N10 C54 C53 177.7(18) . . ? N11 C56 C55 165(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 5.793 _refine_diff_density_min -2.527 _refine_diff_density_rms 0.161 _database_code_depnum_ccdc_archive 'CCDC 972573' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_F:\MS130Dy\MS130\WORK\130sc.CIF _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Et4N)2[(triphosRe(CN)3)2(Dy(NO3)3)3]?4CH3CN ; _chemical_name_common 3 _chemical_melting_point 300 _chemical_formula_moiety C88H78N15O27P6Re2Dy3,2C8H20N),4(C2H3N) _chemical_formula_sum 'C112 H130 Dy3 N21 O27 P6 Re2' _chemical_formula_weight 3248.09 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 '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 'C 2/c' _symmetry_int_tables_number 15 _chemical_absolute_configuration ? _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 36.167(7) _cell_length_b 13.819(3) _cell_length_c 26.339(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.08(3) _cell_angle_gamma 90.00 _cell_volume 12768(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6412 _exptl_absorpt_coefficient_mu 3.775 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3144 _exptl_absorpt_correction_T_max 0.4305 _exptl_absorpt_process_details 'Bruker AXS Scale, SADABS (Bruker 2008)' _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63978 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0357 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 26.02 _reflns_number_total 12528 _reflns_number_gt 9122 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEXII (Bruker 2008)' _computing_cell_refinement 'SAINT v7.60A (Bruker 2008)' _computing_data_reduction 'SAINT v7.60A, XPREP v2008/2 (Bruker 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond (Pennington, 2013)' _computing_publication_material 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0653P)^2^+232.0954P] 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 12528 _refine_ls_number_parameters 779 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1563 _refine_ls_wR_factor_gt 0.1308 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _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 0.126784(9) 0.70580(2) 0.323610(14) 0.03958(11) Uani 1 1 d . . . Dy1 Dy -0.014600(12) 0.79843(3) 0.348684(17) 0.04459(13) Uani 1 1 d . . . Dy2 Dy 0.0000 0.48125(4) 0.2500 0.03728(15) Uani 1 2 d S . . P1 P 0.16119(7) 0.61562(18) 0.39968(10) 0.0495(6) Uani 1 1 d . . . P2 P 0.17814(7) 0.65669(18) 0.28513(11) 0.0473(6) Uani 1 1 d . . . P3 P 0.16698(7) 0.84252(18) 0.35888(10) 0.0489(6) Uani 1 1 d . . . C2 C 0.0884(2) 0.5941(6) 0.2973(3) 0.042(2) Uani 1 1 d . . . C1 C 0.0810(3) 0.7557(6) 0.3502(3) 0.043(2) Uani 1 1 d . . . C3 C 0.0949(2) 0.7681(6) 0.2558(4) 0.044(2) Uani 1 1 d . . . N1 N 0.0524(2) 0.7813(5) 0.3579(3) 0.0451(18) Uani 1 1 d . . . N4 N 0.0206(3) 0.8966(6) 0.4439(3) 0.058(2) Uani 1 1 d . . . O12 O 0.03891(19) 0.3418(5) 0.2852(3) 0.0541(17) Uani 1 1 d . . . C10 C 0.1717(3) 0.4847(6) 0.3941(4) 0.049(2) Uani 1 1 d . . . O13 O 0.03964(19) 0.3855(5) 0.2062(3) 0.0548(16) Uani 1 1 d . . . O6 O 0.0107(2) 0.8086(5) 0.4434(3) 0.0585(18) Uani 1 1 d . . . N8 N 0.0523(2) 0.3290(6) 0.2446(4) 0.055(2) Uani 1 1 d . . . O14 O 0.0762(2) 0.2667(6) 0.2436(4) 0.084(3) Uani 1 1 d . . . O10 O 0.0365(3) 0.9371(6) 0.4847(3) 0.084(3) Uani 1 1 d . . . C20 C 0.2181(3) 0.8134(7) 0.3680(5) 0.064(3) Uani 1 1 d . . . H20A H 0.2255 0.8271 0.3349 0.077 Uiso 1 1 calc R . . H20B H 0.2332 0.8572 0.3951 0.077 Uiso 1 1 calc R . . C16 C 0.2093(3) 0.6684(8) 0.4247(4) 0.063(3) Uani 1 1 d . . . H16A H 0.2071 0.7224 0.4485 0.076 Uiso 1 1 calc R . . H16B H 0.2257 0.6185 0.4459 0.076 Uiso 1 1 calc R . . C11 C 0.1514(3) 0.4298(7) 0.3523(4) 0.046(2) Uani 1 1 d . . . H11 H 0.1325 0.4599 0.3255 0.055 Uiso 1 1 calc R . . C17 C 0.2294(3) 0.7062(8) 0.3845(5) 0.070(3) Uani 1 1 d . . . C19 C 0.2235(3) 0.6406(8) 0.3354(4) 0.061(3) Uani 1 1 d . . . H19A H 0.2252 0.5723 0.3471 0.073 Uiso 1 1 calc R . . H19B H 0.2449 0.6522 0.3187 0.073 Uiso 1 1 calc R . . C13 C 0.1852(3) 0.2856(8) 0.3883(5) 0.062(3) Uani 1 1 d . . . H13 H 0.1897 0.2182 0.3863 0.074 Uiso 1 1 calc R . . C14 C 0.2048(3) 0.3379(8) 0.4293(5) 0.072(3) Uani 1 1 d . . . H14 H 0.2233 0.3067 0.4562 0.086 Uiso 1 1 calc R . . O5 O 0.0133(3) 0.9392(5) 0.3997(3) 0.072(2) Uani 1 1 d . . . C15 C 0.1986(3) 0.4371(8) 0.4331(5) 0.070(3) Uani 1 1 d . . . H15 H 0.2127 0.4724 0.4624 0.084 Uiso 1 1 calc R . . C12 C 0.1584(3) 0.3312(7) 0.3493(4) 0.054(2) Uani 1 1 d . . . H12 H 0.1446 0.2950 0.3202 0.065 Uiso 1 1 calc R . . O9 O 0.0142(2) 0.4995(5) 0.3508(3) 0.0611(19) Uani 1 1 d . . . N3 N 0.0722(2) 0.7945(6) 0.2184(3) 0.0498(19) Uani 1 1 d . . . N2 N 0.0628(2) 0.5423(5) 0.2819(3) 0.0454(18) Uani 1 1 d . . . O2 O 0.0044(3) 0.6327(5) 0.3917(3) 0.080(3) Uani 1 1 d . . . C21 C 0.1724(3) 0.5431(7) 0.2489(4) 0.051(2) Uani 1 1 d . . . N7 N 0.0034(3) 0.5860(6) 0.3508(3) 0.055(2) Uani 1 1 d . . . C33 C 0.1598(3) 0.9532(7) 0.3196(4) 0.050(2) Uani 1 1 d . . . C38 C 0.1215(3) 0.9821(7) 0.2999(4) 0.051(2) Uani 1 1 d . . . H38 H 0.1015 0.9440 0.3071 0.061 Uiso 1 1 calc R . . O1 O -0.00886(18) 0.6281(4) 0.3071(2) 0.0471(15) Uani 1 1 d . . . C32 C 0.1727(3) 0.8189(7) 0.2173(4) 0.055(2) Uani 1 1 d . . . H32 H 0.1510 0.8367 0.2296 0.066 Uiso 1 1 calc R . . C27 C 0.1930(3) 0.7368(8) 0.2368(4) 0.055(3) Uani 1 1 d . . . C44 C 0.1383(3) 0.8664(7) 0.4493(4) 0.060(3) Uani 1 1 d . . . H44 H 0.1221 0.8135 0.4361 0.072 Uiso 1 1 calc R . . C26 C 0.1372(3) 0.5223(9) 0.2174(4) 0.064(3) Uani 1 1 d . . . H26 H 0.1171 0.5675 0.2154 0.077 Uiso 1 1 calc R . . C34 C 0.1887(3) 1.0076(7) 0.3075(5) 0.064(3) Uani 1 1 d . . . H34 H 0.2146 0.9885 0.3198 0.077 Uiso 1 1 calc R . . C39 C 0.1649(3) 0.8962(7) 0.4226(4) 0.056(3) Uani 1 1 d . . . C31 C 0.1835(3) 0.8760(8) 0.1797(4) 0.058(3) Uani 1 1 d . . . H31 H 0.1691 0.9318 0.1663 0.069 Uiso 1 1 calc R . . C4 C 0.1408(3) 0.6120(7) 0.4565(4) 0.057(3) Uani 1 1 d . . . O8 O -0.0666(3) 0.7340(8) 0.3884(3) 0.081(2) Uani 1 1 d . . . O7 O -0.0623(3) 0.8933(8) 0.3789(4) 0.095(3) Uani 1 1 d . . . C40 C 0.1890(4) 0.9743(8) 0.4425(5) 0.073(3) Uani 1 1 d . . . H40 H 0.2074 0.9954 0.4247 0.087 Uiso 1 1 calc R . . N6 N -0.0759(4) 0.8182(12) 0.3939(4) 0.090(4) Uani 1 1 d . . . C9 C 0.1019(4) 0.6041(8) 0.4484(5) 0.071(3) Uani 1 1 d . . . H9 H 0.0869 0.5971 0.4136 0.085 Uiso 1 1 calc R . . C28 C 0.2239(3) 0.7112(10) 0.2179(6) 0.082(4) Uani 1 1 d . . . H28 H 0.2377 0.6540 0.2303 0.099 Uiso 1 1 calc R . . C30 C 0.2152(3) 0.8518(9) 0.1620(5) 0.069(3) Uani 1 1 d . . . H30 H 0.2230 0.8922 0.1374 0.083 Uiso 1 1 calc R . . C41 C 0.1860(4) 1.0202(10) 0.4874(5) 0.085(4) Uani 1 1 d . . . H41 H 0.2026 1.0726 0.5006 0.102 Uiso 1 1 calc R . . C37 C 0.1129(3) 1.0657(7) 0.2703(4) 0.059(3) Uani 1 1 d . . . H37 H 0.0872 1.0855 0.2579 0.071 Uiso 1 1 calc R . . C22 C 0.2018(4) 0.4752(9) 0.2510(5) 0.075(3) Uani 1 1 d . . . H22 H 0.2267 0.4868 0.2721 0.090 Uiso 1 1 calc R . . C35 C 0.1792(3) 1.0919(8) 0.2764(5) 0.066(3) Uani 1 1 d . . . H35 H 0.1988 1.1293 0.2677 0.080 Uiso 1 1 calc R . . C5 C 0.1622(5) 0.6185(10) 0.5079(4) 0.087(4) Uani 1 1 d . . . H5 H 0.1892 0.6228 0.5152 0.105 Uiso 1 1 calc R . . C36 C 0.1419(3) 1.1202(7) 0.2588(5) 0.064(3) Uani 1 1 d . . . H36 H 0.1360 1.1775 0.2386 0.077 Uiso 1 1 calc R . . C42 C 0.1594(4) 0.9914(9) 0.5139(5) 0.084(4) Uani 1 1 d . . . H42 H 0.1574 1.0247 0.5447 0.101 Uiso 1 1 calc R . . C29 C 0.2354(4) 0.7696(12) 0.1798(7) 0.099(5) Uani 1 1 d . . . H29 H 0.2568 0.7518 0.1670 0.118 Uiso 1 1 calc R . . C43 C 0.1349(4) 0.9121(9) 0.4953(4) 0.069(3) Uani 1 1 d . . . H43 H 0.1167 0.8908 0.5135 0.083 Uiso 1 1 calc R . . C8 C 0.0836(4) 0.6059(10) 0.4893(5) 0.082(4) Uani 1 1 d . . . H8 H 0.0566 0.6017 0.4827 0.098 Uiso 1 1 calc R . . O11 O -0.1061(3) 0.8296(13) 0.4153(5) 0.157(6) Uani 1 1 d . . . C18 C 0.2724(3) 0.7068(10) 0.4104(6) 0.098(5) Uani 1 1 d . . . H18A H 0.2776 0.7519 0.4400 0.146 Uiso 1 1 calc R . . H18B H 0.2865 0.7274 0.3848 0.146 Uiso 1 1 calc R . . H18C H 0.2806 0.6416 0.4230 0.146 Uiso 1 1 calc R . . C25 C 0.1298(5) 0.4372(11) 0.1884(5) 0.091(5) Uani 1 1 d . . . H25 H 0.1050 0.4245 0.1672 0.109 Uiso 1 1 calc R . . C6 C 0.1438(6) 0.6186(12) 0.5487(5) 0.101(5) Uani 1 1 d . . . H6 H 0.1587 0.6220 0.5838 0.121 Uiso 1 1 calc R . . N9 N 0.0496(3) 0.2442(7) 0.4300(4) 0.065(2) Uani 1 1 d . . . C49 C 0.0761(4) 0.3184(10) 0.4193(5) 0.080(4) Uani 1 1 d . . . H49A H 0.0628 0.3816 0.4137 0.096 Uiso 1 1 calc R . . H49B H 0.0835 0.3014 0.3867 0.096 Uiso 1 1 calc R . . C23 C 0.1935(7) 0.3906(10) 0.2216(6) 0.109(7) Uani 1 1 d . . . H23 H 0.2134 0.3449 0.2237 0.131 Uiso 1 1 calc R . . C24 C 0.1598(7) 0.3697(10) 0.1911(6) 0.106(7) Uani 1 1 d . . . H24 H 0.1557 0.3114 0.1714 0.128 Uiso 1 1 calc R . . C7 C 0.1063(6) 0.6142(11) 0.5402(6) 0.095(5) Uani 1 1 d . . . H7 H 0.0946 0.6168 0.5688 0.114 Uiso 1 1 calc R . . C51 C 0.0149(4) 0.2496(11) 0.3823(6) 0.096(5) Uani 1 1 d . . . H51A H 0.0056 0.3173 0.3790 0.115 Uiso 1 1 calc R . . H51B H 0.0239 0.2347 0.3505 0.115 Uiso 1 1 calc R . . C50 C 0.1125(5) 0.3283(12) 0.4645(7) 0.105(5) Uani 1 1 d . . . H50A H 0.1058 0.3560 0.4953 0.158 Uiso 1 1 calc R . . H50B H 0.1308 0.3708 0.4535 0.158 Uiso 1 1 calc R . . H50C H 0.1240 0.2643 0.4732 0.158 Uiso 1 1 calc R . . C47 C 0.0660(5) 0.1452(10) 0.4382(6) 0.096(5) Uani 1 1 d . . . H47A H 0.0460 0.1002 0.4434 0.115 Uiso 1 1 calc R . . H47B H 0.0867 0.1450 0.4707 0.115 Uiso 1 1 calc R . . C46 C 0.0365(5) 0.2697(11) 0.4792(6) 0.095(4) Uani 1 1 d . . . H46A H 0.0181 0.2200 0.4845 0.113 Uiso 1 1 calc R . . H46B H 0.0588 0.2667 0.5096 0.113 Uiso 1 1 calc R . . C48 C 0.0823(6) 0.1066(11) 0.3927(7) 0.126(7) Uani 1 1 d . . . H48A H 0.0659 0.1276 0.3592 0.188 Uiso 1 1 calc R . . H48B H 0.0832 0.0357 0.3939 0.188 Uiso 1 1 calc R . . H48C H 0.1081 0.1321 0.3963 0.188 Uiso 1 1 calc R . . C45 C 0.0182(5) 0.3675(12) 0.4783(8) 0.121(6) Uani 1 1 d . . . H45A H 0.0371 0.4179 0.4773 0.181 Uiso 1 1 calc R . . H45B H 0.0087 0.3756 0.5099 0.181 Uiso 1 1 calc R . . H45C H -0.0030 0.3729 0.4472 0.181 Uiso 1 1 calc R . . C52 C -0.0188(5) 0.1840(13) 0.3826(8) 0.127(7) Uani 1 1 d . . . H52A H -0.0109 0.1163 0.3821 0.190 Uiso 1 1 calc R . . H52B H -0.0395 0.1974 0.3516 0.190 Uiso 1 1 calc R . . H52C H -0.0278 0.1962 0.4143 0.190 Uiso 1 1 calc R . . C54 C 0.2033(6) 0.5994(16) 0.0868(7) 0.120(7) Uani 1 1 d . . . C53 C 0.1683(6) 0.6151(14) 0.1018(8) 0.137(7) Uani 1 1 d . . . H53A H 0.1634 0.6848 0.1028 0.205 Uiso 1 1 calc R . . H53B H 0.1702 0.5873 0.1365 0.205 Uiso 1 1 calc R . . H53C H 0.1474 0.5841 0.0763 0.205 Uiso 1 1 calc R . . N10 N 0.2301(6) 0.588(2) 0.0730(8) 0.195(11) Uani 1 1 d . . . C56 C 0.1324(12) 1.1106(18) 0.1314(13) 0.31(4) Uani 1 1 d D . . C55 C 0.0982(9) 1.056(4) 0.1155(16) 0.39(4) Uani 1 1 d D . . H55A H 0.0988 1.0184 0.0842 0.580 Uiso 1 1 calc R . . H55B H 0.0763 1.1001 0.1076 0.580 Uiso 1 1 calc R . . H55C H 0.0959 1.0121 0.1438 0.580 Uiso 1 1 calc R . . N11 N 0.1625(13) 1.138(2) 0.1409(15) 0.37(3) Uani 1 1 d D . . O3 O 0.0000 0.7983(6) 0.2500 0.050(2) Uani 1 2 d S . . O4 O -0.0054(2) 0.9335(5) 0.2899(2) 0.0521(16) Uani 1 1 d . . . N5 N 0.0000 0.8899(9) 0.2500 0.051(3) Uani 1 2 d S . . 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 0.03538(19) 0.03494(19) 0.0424(2) -0.00476(14) -0.00223(14) -0.00249(14) Dy1 0.0395(2) 0.0452(2) 0.0443(2) 0.00233(18) 0.00098(18) -0.00657(18) Dy2 0.0323(3) 0.0281(3) 0.0440(3) 0.000 -0.0053(2) 0.000 P1 0.0502(14) 0.0396(12) 0.0463(13) -0.0037(10) -0.0120(11) -0.0025(11) P2 0.0334(11) 0.0424(13) 0.0613(15) -0.0022(11) 0.0023(11) 0.0001(10) P3 0.0454(13) 0.0391(12) 0.0540(14) -0.0069(11) -0.0037(11) -0.0081(10) C2 0.041(5) 0.044(5) 0.039(5) -0.002(4) 0.005(4) 0.008(4) C1 0.051(5) 0.034(4) 0.037(5) 0.001(4) -0.002(4) 0.000(4) C3 0.032(4) 0.042(5) 0.055(6) -0.011(4) 0.008(4) -0.003(4) N1 0.045(4) 0.042(4) 0.042(4) -0.003(3) -0.001(3) 0.003(3) N4 0.064(5) 0.049(5) 0.054(5) -0.022(4) 0.004(4) -0.005(4) O12 0.051(4) 0.038(3) 0.065(4) 0.007(3) -0.003(3) 0.004(3) C10 0.044(5) 0.037(5) 0.057(6) -0.002(4) -0.005(4) 0.001(4) O13 0.051(4) 0.051(4) 0.057(4) -0.005(3) 0.003(3) 0.006(3) O6 0.070(5) 0.051(4) 0.049(4) -0.001(3) 0.004(3) -0.017(3) N8 0.046(5) 0.035(4) 0.077(6) -0.006(4) 0.001(4) 0.001(4) O14 0.069(5) 0.054(5) 0.127(8) 0.001(5) 0.017(5) 0.026(4) O10 0.105(7) 0.070(5) 0.068(5) -0.020(4) 0.000(5) -0.013(5) C20 0.044(6) 0.049(6) 0.083(8) -0.009(5) -0.014(5) -0.011(5) C16 0.053(6) 0.048(6) 0.069(7) -0.001(5) -0.021(5) -0.006(5) C11 0.046(5) 0.039(5) 0.050(5) -0.001(4) 0.005(4) 0.002(4) C17 0.042(6) 0.052(6) 0.093(9) -0.006(6) -0.026(6) -0.003(5) C19 0.037(5) 0.061(6) 0.076(7) 0.007(5) -0.005(5) -0.004(5) C13 0.056(6) 0.045(6) 0.085(8) 0.004(5) 0.020(6) 0.013(5) C14 0.060(7) 0.053(6) 0.091(9) 0.014(6) -0.005(6) 0.011(5) O5 0.103(6) 0.046(4) 0.059(5) 0.002(4) 0.004(4) 0.005(4) C15 0.063(7) 0.054(6) 0.072(7) -0.003(6) -0.023(6) 0.003(5) C12 0.063(6) 0.048(5) 0.054(6) -0.003(5) 0.017(5) 0.007(5) O9 0.084(5) 0.033(3) 0.062(4) -0.001(3) 0.009(4) -0.006(3) N3 0.042(4) 0.058(5) 0.047(4) 0.001(4) 0.005(4) 0.002(4) N2 0.034(4) 0.040(4) 0.055(5) -0.006(3) -0.002(3) -0.006(3) O2 0.151(8) 0.045(4) 0.047(4) -0.008(3) 0.030(5) -0.018(5) C21 0.051(5) 0.042(5) 0.064(6) -0.004(4) 0.024(5) -0.003(4) N7 0.081(6) 0.035(4) 0.048(5) 0.000(4) 0.013(4) -0.011(4) C33 0.049(5) 0.039(5) 0.058(6) -0.012(4) 0.004(4) -0.007(4) C38 0.055(6) 0.042(5) 0.056(6) -0.001(4) 0.013(5) 0.000(4) O1 0.053(4) 0.042(3) 0.041(3) 0.005(3) 0.002(3) -0.001(3) C32 0.046(5) 0.052(6) 0.064(6) -0.012(5) 0.009(5) -0.004(4) C27 0.034(5) 0.053(6) 0.077(7) -0.002(5) 0.009(5) -0.010(4) C44 0.068(7) 0.047(6) 0.054(6) -0.009(5) -0.006(5) -0.008(5) C26 0.069(7) 0.075(7) 0.057(6) -0.014(6) 0.032(6) -0.015(6) C34 0.063(7) 0.046(6) 0.079(8) -0.010(5) 0.010(6) -0.018(5) C39 0.065(6) 0.045(5) 0.046(5) -0.003(4) -0.010(5) -0.009(5) C31 0.061(6) 0.051(6) 0.060(6) 0.005(5) 0.011(5) -0.004(5) C4 0.076(7) 0.039(5) 0.045(5) -0.003(4) -0.004(5) 0.002(5) O8 0.076(6) 0.102(7) 0.058(5) 0.018(5) 0.004(4) -0.009(5) O7 0.079(6) 0.090(7) 0.105(7) -0.037(6) 0.001(5) -0.006(5) C40 0.079(8) 0.055(6) 0.070(8) -0.012(6) -0.010(6) -0.016(6) N6 0.104(10) 0.106(10) 0.054(6) -0.003(7) 0.008(6) -0.007(9) C9 0.094(9) 0.060(7) 0.053(6) 0.003(5) 0.010(6) 0.017(6) C28 0.047(6) 0.083(9) 0.124(11) 0.033(8) 0.033(7) 0.009(6) C30 0.066(7) 0.065(7) 0.073(8) 0.009(6) 0.012(6) -0.023(6) C41 0.105(11) 0.067(8) 0.072(8) -0.019(7) 0.004(8) -0.029(8) C37 0.055(6) 0.044(5) 0.080(7) 0.003(5) 0.020(5) 0.007(5) C22 0.095(9) 0.074(8) 0.063(7) 0.012(6) 0.030(7) 0.031(7) C35 0.070(7) 0.050(6) 0.087(8) -0.013(6) 0.035(6) -0.021(5) C5 0.117(11) 0.077(8) 0.046(7) -0.004(6) -0.021(7) -0.021(8) C36 0.072(7) 0.040(5) 0.083(8) 0.000(5) 0.023(6) 0.005(5) C42 0.113(11) 0.070(8) 0.052(7) -0.021(6) -0.017(7) 0.002(8) C29 0.049(7) 0.117(12) 0.141(14) 0.040(11) 0.045(8) 0.009(7) C43 0.082(8) 0.071(8) 0.044(6) -0.009(5) -0.004(5) 0.001(6) C8 0.111(11) 0.079(9) 0.055(7) 0.016(6) 0.021(7) 0.028(8) O11 0.072(7) 0.294(19) 0.115(9) -0.022(11) 0.043(7) 0.010(9) C18 0.046(7) 0.086(9) 0.133(13) 0.008(9) -0.032(7) -0.005(6) C25 0.125(12) 0.088(10) 0.075(8) -0.035(7) 0.054(8) -0.055(9) C6 0.146(15) 0.097(11) 0.050(8) -0.018(7) 0.005(9) -0.020(11) N9 0.084(7) 0.056(5) 0.058(5) 0.013(4) 0.023(5) -0.001(5) C49 0.086(9) 0.078(9) 0.074(8) 0.018(7) 0.018(7) 0.003(7) C23 0.21(2) 0.058(8) 0.081(10) 0.012(7) 0.074(12) 0.056(11) C24 0.22(2) 0.052(8) 0.062(9) -0.015(7) 0.067(12) -0.020(11) C7 0.144(15) 0.087(10) 0.063(8) -0.005(7) 0.044(10) 0.016(10) C51 0.106(11) 0.087(10) 0.087(10) 0.033(8) 0.005(8) -0.003(9) C50 0.107(12) 0.088(10) 0.114(13) 0.013(9) 0.013(10) -0.008(9) C47 0.126(13) 0.062(8) 0.098(11) 0.028(7) 0.025(9) 0.015(8) C46 0.110(12) 0.094(10) 0.091(10) 0.022(8) 0.046(9) 0.010(9) C48 0.21(2) 0.073(10) 0.116(13) 0.009(9) 0.075(14) 0.047(12) C45 0.140(15) 0.099(12) 0.148(16) 0.007(11) 0.085(13) 0.018(11) C52 0.097(12) 0.110(13) 0.154(17) 0.040(12) -0.009(11) -0.018(10) C54 0.113(15) 0.144(17) 0.084(11) -0.032(11) -0.010(11) 0.032(13) C53 0.17(2) 0.111(14) 0.142(17) 0.014(13) 0.064(15) -0.031(14) N10 0.135(16) 0.29(3) 0.130(15) -0.103(17) -0.021(12) 0.061(18) C56 0.78(11) 0.055(13) 0.17(3) 0.032(17) 0.29(6) 0.05(3) C55 0.22(4) 0.67(12) 0.24(4) 0.20(6) 0.00(3) 0.17(6) N11 0.86(9) 0.14(3) 0.22(3) -0.04(2) 0.33(5) -0.14(4) O3 0.054(5) 0.032(5) 0.062(6) 0.000 0.009(5) 0.000 O4 0.072(4) 0.046(4) 0.040(3) -0.006(3) 0.017(3) -0.002(3) N5 0.046(6) 0.059(7) 0.049(7) 0.000 0.011(5) 0.000 _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 C3 2.065(10) . ? Re1 C1 2.065(10) . ? Re1 C2 2.079(9) . ? Re1 P2 2.419(3) . ? Re1 P3 2.427(2) . ? Re1 P1 2.430(2) . ? Dy1 N3 2.381(8) 2 ? Dy1 N1 2.387(8) . ? Dy1 O5 2.440(8) . ? Dy1 O6 2.442(7) . ? Dy1 O7 2.447(10) . ? Dy1 O4 2.499(6) . ? Dy1 O8 2.528(9) . ? Dy1 O2 2.573(8) . ? Dy1 O1 2.626(6) . ? Dy1 N6 2.775(14) . ? Dy1 O3 2.7753(7) . ? Dy1 N4 2.862(8) . ? Dy2 N2 2.375(7) 2 ? Dy2 N2 2.375(7) . ? Dy2 O12 2.433(6) 2 ? Dy2 O12 2.433(6) . ? Dy2 O13 2.438(7) . ? Dy2 O13 2.438(7) 2 ? Dy2 O9 2.591(7) 2 ? Dy2 O9 2.591(7) . ? Dy2 O1 2.591(6) 2 ? Dy2 O1 2.591(6) . ? Dy2 N8 2.855(8) 2 ? Dy2 N8 2.855(8) . ? P1 C4 1.823(12) . ? P1 C16 1.854(10) . ? P1 C10 1.862(9) . ? P2 C21 1.823(10) . ? P2 C19 1.855(10) . ? P2 C27 1.862(11) . ? P3 C33 1.829(10) . ? P3 C20 1.851(11) . ? P3 C39 1.853(11) . ? C2 N2 1.164(11) . ? C1 N1 1.159(12) . ? C3 N3 1.176(12) . ? N4 O10 1.225(10) . ? N4 O6 1.267(10) . ? N4 O5 1.272(11) . ? O12 N8 1.288(11) . ? C10 C11 1.390(12) . ? C10 C15 1.396(13) . ? O13 N8 1.271(11) . ? N8 O14 1.224(10) . ? C20 C17 1.571(15) . ? C16 C17 1.515(18) . ? C11 C12 1.391(13) . ? C17 C18 1.539(14) . ? C17 C19 1.550(16) . ? C13 C14 1.349(17) . ? C13 C12 1.381(15) . ? C14 C15 1.396(15) . ? O9 N7 1.258(10) . ? N3 Dy1 2.381(8) 2 ? O2 N7 1.249(10) . ? C21 C26 1.369(15) . ? C21 C22 1.409(15) . ? N7 O1 1.269(10) . ? C33 C34 1.388(14) . ? C33 C38 1.412(13) . ? C38 C37 1.386(14) . ? C32 C27 1.381(14) . ? C32 C31 1.395(15) . ? C27 C28 1.377(15) . ? C44 C39 1.383(15) . ? C44 C43 1.398(15) . ? C26 C25 1.392(16) . ? C34 C35 1.417(16) . ? C39 C40 1.407(14) . ? C31 C30 1.377(16) . ? C4 C9 1.373(16) . ? C4 C5 1.391(14) . ? O8 N6 1.229(15) . ? O7 N6 1.254(15) . ? C40 C41 1.369(18) . ? N6 O11 1.355(16) . ? C9 C8 1.395(17) . ? C28 C29 1.424(18) . ? C30 C29 1.370(18) . ? C41 C42 1.38(2) . ? C37 C36 1.382(15) . ? C22 C23 1.39(2) . ? C35 C36 1.370(16) . ? C5 C6 1.39(2) . ? C42 C43 1.419(17) . ? C8 C7 1.40(2) . ? C25 C24 1.42(2) . ? C6 C7 1.32(2) . ? N9 C49 1.477(15) . ? N9 C47 1.486(15) . ? N9 C46 1.525(16) . ? N9 C51 1.547(16) . ? C49 C50 1.552(19) . ? C23 C24 1.32(2) . ? C51 C52 1.52(2) . ? C47 C48 1.55(2) . ? C46 C45 1.50(2) . ? C54 N10 1.13(2) . ? C54 C53 1.43(3) . ? C56 N11 1.125(17) . ? C56 C55 1.422(17) . ? O3 N5 1.266(14) . ? O3 Dy1 2.7754(7) 2 ? O4 N5 1.268(8) . ? N5 O4 1.268(8) 2 ? 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 C3 Re1 C1 80.1(3) . . ? C3 Re1 C2 80.4(3) . . ? C1 Re1 C2 80.6(3) . . ? C3 Re1 P2 94.6(3) . . ? C1 Re1 P2 174.6(2) . . ? C2 Re1 P2 99.8(2) . . ? C3 Re1 P3 99.4(2) . . ? C1 Re1 P3 93.7(3) . . ? C2 Re1 P3 174.3(2) . . ? P2 Re1 P3 85.95(9) . . ? C3 Re1 P1 173.7(2) . . ? C1 Re1 P1 100.6(2) . . ? C2 Re1 P1 93.5(2) . . ? P2 Re1 P1 84.84(9) . . ? P3 Re1 P1 86.83(9) . . ? N3 Dy1 N1 139.1(3) 2 . ? N3 Dy1 O5 126.7(3) 2 . ? N1 Dy1 O5 75.5(3) . . ? N3 Dy1 O6 143.2(3) 2 . ? N1 Dy1 O6 77.5(3) . . ? O5 Dy1 O6 52.4(2) . . ? N3 Dy1 O7 72.3(3) 2 . ? N1 Dy1 O7 142.9(3) . . ? O5 Dy1 O7 67.9(3) . . ? O6 Dy1 O7 75.9(3) . . ? N3 Dy1 O4 77.4(3) 2 . ? N1 Dy1 O4 81.5(2) . . ? O5 Dy1 O4 69.2(2) . . ? O6 Dy1 O4 121.1(2) . . ? O7 Dy1 O4 90.7(3) . . ? N3 Dy1 O8 72.2(3) 2 . ? N1 Dy1 O8 139.7(3) . . ? O5 Dy1 O8 107.6(3) . . ? O6 Dy1 O8 74.3(3) . . ? O7 Dy1 O8 53.1(4) . . ? O4 Dy1 O8 138.1(3) . . ? N3 Dy1 O2 113.4(3) 2 . ? N1 Dy1 O2 73.2(3) . . ? O5 Dy1 O2 115.9(3) . . ? O6 Dy1 O2 66.9(2) . . ? O7 Dy1 O2 117.9(4) . . ? O4 Dy1 O2 151.2(3) . . ? O8 Dy1 O2 69.5(3) . . ? N3 Dy1 O1 79.2(2) 2 . ? N1 Dy1 O1 76.8(2) . . ? O5 Dy1 O1 151.7(2) . . ? O6 Dy1 O1 115.5(2) . . ? O7 Dy1 O1 138.5(3) . . ? O4 Dy1 O1 112.04(19) . . ? O8 Dy1 O1 90.0(3) . . ? O2 Dy1 O1 49.2(2) . . ? N3 Dy1 N6 71.0(3) 2 . ? N1 Dy1 N6 149.8(3) . . ? O5 Dy1 N6 87.2(4) . . ? O6 Dy1 N6 72.3(3) . . ? O7 Dy1 N6 26.9(3) . . ? O4 Dy1 N6 115.7(4) . . ? O8 Dy1 N6 26.3(3) . . ? O2 Dy1 N6 93.1(4) . . ? O1 Dy1 N6 114.8(4) . . ? N3 Dy1 O3 68.69(19) 2 . ? N1 Dy1 O3 71.04(18) . . ? O5 Dy1 O3 111.7(2) . . ? O6 Dy1 O3 147.89(18) . . ? O7 Dy1 O3 127.9(3) . . ? O4 Dy1 O3 48.4(2) . . ? O8 Dy1 O3 135.9(2) . . ? O2 Dy1 O3 108.7(2) . . ? O1 Dy1 O3 63.6(2) . . ? N6 Dy1 O3 139.1(2) . . ? N3 Dy1 N4 141.5(3) 2 . ? N1 Dy1 N4 74.6(3) . . ? O5 Dy1 N4 26.3(2) . . ? O6 Dy1 N4 26.1(2) . . ? O7 Dy1 N4 70.1(3) . . ? O4 Dy1 N4 95.2(2) . . ? O8 Dy1 N4 91.2(3) . . ? O2 Dy1 N4 91.3(3) . . ? O1 Dy1 N4 136.6(2) . . ? N6 Dy1 N4 79.0(3) . . ? O3 Dy1 N4 132.5(2) . . ? N2 Dy2 N2 138.4(4) 2 . ? N2 Dy2 O12 74.5(2) 2 2 ? N2 Dy2 O12 146.1(2) . 2 ? N2 Dy2 O12 146.1(2) 2 . ? N2 Dy2 O12 74.5(2) . . ? O12 Dy2 O12 75.2(3) 2 . ? N2 Dy2 O13 130.3(2) 2 . ? N2 Dy2 O13 74.9(2) . . ? O12 Dy2 O13 75.0(2) 2 . ? O12 Dy2 O13 53.0(2) . . ? N2 Dy2 O13 74.9(2) 2 2 ? N2 Dy2 O13 130.3(2) . 2 ? O12 Dy2 O13 53.0(2) 2 2 ? O12 Dy2 O13 75.0(2) . 2 ? O13 Dy2 O13 114.2(3) . 2 ? N2 Dy2 O9 70.6(3) 2 2 ? N2 Dy2 O9 105.2(3) . 2 ? O12 Dy2 O9 74.6(2) 2 2 ? O12 Dy2 O9 114.8(2) . 2 ? O13 Dy2 O9 63.9(2) . 2 ? O13 Dy2 O9 123.0(2) 2 2 ? N2 Dy2 O9 105.2(3) 2 . ? N2 Dy2 O9 70.6(3) . . ? O12 Dy2 O9 114.8(2) 2 . ? O12 Dy2 O9 74.6(2) . . ? O13 Dy2 O9 123.0(2) . . ? O13 Dy2 O9 63.9(2) 2 . ? O9 Dy2 O9 168.8(3) 2 . ? N2 Dy2 O1 76.1(2) 2 2 ? N2 Dy2 O1 71.6(2) . 2 ? O12 Dy2 O1 122.8(2) 2 2 ? O12 Dy2 O1 134.4(2) . 2 ? O13 Dy2 O1 88.9(2) . 2 ? O13 Dy2 O1 150.4(2) 2 2 ? O9 Dy2 O1 49.54(19) 2 2 ? O9 Dy2 O1 119.77(19) . 2 ? N2 Dy2 O1 71.6(2) 2 . ? N2 Dy2 O1 76.1(2) . . ? O12 Dy2 O1 134.4(2) 2 . ? O12 Dy2 O1 122.8(2) . . ? O13 Dy2 O1 150.4(2) . . ? O13 Dy2 O1 88.9(2) 2 . ? O9 Dy2 O1 119.77(19) 2 . ? O9 Dy2 O1 49.54(19) . . ? O1 Dy2 O1 76.9(3) 2 . ? N2 Dy2 N8 72.1(2) 2 2 ? N2 Dy2 N8 146.2(2) . 2 ? O12 Dy2 N8 26.7(2) 2 2 ? O12 Dy2 N8 74.1(2) . 2 ? O13 Dy2 N8 95.5(3) . 2 ? O13 Dy2 N8 26.3(2) 2 2 ? O9 Dy2 N8 98.9(3) 2 2 ? O9 Dy2 N8 89.4(3) . 2 ? O1 Dy2 N8 141.5(2) 2 2 ? O1 Dy2 N8 111.8(2) . 2 ? N2 Dy2 N8 146.2(2) 2 . ? N2 Dy2 N8 72.1(2) . . ? O12 Dy2 N8 74.1(2) 2 . ? O12 Dy2 N8 26.7(2) . . ? O13 Dy2 N8 26.3(2) . . ? O13 Dy2 N8 95.5(3) 2 . ? O9 Dy2 N8 89.4(3) 2 . ? O9 Dy2 N8 98.9(3) . . ? O1 Dy2 N8 111.8(2) 2 . ? O1 Dy2 N8 141.5(2) . . ? N8 Dy2 N8 85.1(3) 2 . ? C4 P1 C16 104.6(5) . . ? C4 P1 C10 99.8(5) . . ? C16 P1 C10 102.6(5) . . ? C4 P1 Re1 117.5(3) . . ? C16 P1 Re1 109.8(4) . . ? C10 P1 Re1 120.4(3) . . ? C21 P2 C19 103.9(5) . . ? C21 P2 C27 99.7(5) . . ? C19 P2 C27 102.0(5) . . ? C21 P2 Re1 117.4(3) . . ? C19 P2 Re1 111.7(4) . . ? C27 P2 Re1 119.9(3) . . ? C33 P3 C20 104.8(5) . . ? C33 P3 C39 98.3(4) . . ? C20 P3 C39 103.3(5) . . ? C33 P3 Re1 116.4(3) . . ? C20 P3 Re1 111.6(3) . . ? C39 P3 Re1 120.4(4) . . ? N2 C2 Re1 169.7(7) . . ? N1 C1 Re1 170.2(7) . . ? N3 C3 Re1 169.5(8) . . ? C1 N1 Dy1 160.4(7) . . ? O10 N4 O6 121.2(10) . . ? O10 N4 O5 122.7(9) . . ? O6 N4 O5 116.1(8) . . ? O10 N4 Dy1 178.2(8) . . ? O6 N4 Dy1 58.1(4) . . ? O5 N4 Dy1 58.0(5) . . ? N8 O12 Dy2 95.2(5) . . ? C11 C10 C15 117.7(9) . . ? C11 C10 P1 121.0(7) . . ? C15 C10 P1 121.2(8) . . ? N8 O13 Dy2 95.4(6) . . ? N4 O6 Dy1 95.8(5) . . ? O14 N8 O13 122.2(10) . . ? O14 N8 O12 121.5(9) . . ? O13 N8 O12 116.2(8) . . ? O14 N8 Dy2 176.7(7) . . ? O13 N8 Dy2 58.2(5) . . ? O12 N8 Dy2 58.1(4) . . ? C17 C20 P3 115.1(7) . . ? C17 C16 P1 117.1(7) . . ? C10 C11 C12 120.8(9) . . ? C16 C17 C18 107.3(11) . . ? C16 C17 C19 112.9(9) . . ? C18 C17 C19 107.0(11) . . ? C16 C17 C20 112.5(10) . . ? C18 C17 C20 106.4(9) . . ? C19 C17 C20 110.3(10) . . ? C17 C19 P2 116.3(7) . . ? C14 C13 C12 119.3(10) . . ? C13 C14 C15 121.3(11) . . ? N4 O5 Dy1 95.7(5) . . ? C10 C15 C14 120.4(10) . . ? C13 C12 C11 120.6(10) . . ? N7 O9 Dy2 96.2(5) . . ? C3 N3 Dy1 159.2(7) . 2 ? C2 N2 Dy2 162.5(7) . . ? N7 O2 Dy1 97.6(6) . . ? C26 C21 C22 117.7(11) . . ? C26 C21 P2 118.0(8) . . ? C22 C21 P2 124.3(9) . . ? O2 N7 O9 123.2(8) . . ? O2 N7 O1 118.4(8) . . ? O9 N7 O1 118.4(8) . . ? C34 C33 C38 119.3(10) . . ? C34 C33 P3 124.8(8) . . ? C38 C33 P3 115.9(7) . . ? C37 C38 C33 120.5(10) . . ? N7 O1 Dy2 95.9(5) . . ? N7 O1 Dy1 94.4(5) . . ? Dy2 O1 Dy1 167.8(3) . . ? C27 C32 C31 120.8(10) . . ? C28 C27 C32 118.8(10) . . ? C28 C27 P2 119.3(9) . . ? C32 C27 P2 121.8(8) . . ? C39 C44 C43 121.7(10) . . ? C21 C26 C25 122.5(13) . . ? C33 C34 C35 119.1(11) . . ? C44 C39 C40 118.8(10) . . ? C44 C39 P3 121.9(7) . . ? C40 C39 P3 119.1(9) . . ? C30 C31 C32 120.2(10) . . ? C9 C4 C5 117.6(12) . . ? C9 C4 P1 118.6(8) . . ? C5 C4 P1 123.8(11) . . ? N6 O8 Dy1 88.1(8) . . ? N6 O7 Dy1 91.3(9) . . ? C41 C40 C39 120.4(13) . . ? O8 N6 O7 127.3(14) . . ? O8 N6 O11 115.4(15) . . ? O7 N6 O11 117.1(15) . . ? O8 N6 Dy1 65.6(8) . . ? O7 N6 Dy1 61.8(7) . . ? O11 N6 Dy1 178.8(12) . . ? C4 C9 C8 122.6(12) . . ? C27 C28 C29 120.7(12) . . ? C29 C30 C31 120.3(11) . . ? C40 C41 C42 120.9(12) . . ? C36 C37 C38 120.0(10) . . ? C23 C22 C21 118.5(14) . . ? C36 C35 C34 120.7(10) . . ? C4 C5 C6 119.5(15) . . ? C35 C36 C37 120.4(10) . . ? C41 C42 C43 120.2(12) . . ? C30 C29 C28 119.2(12) . . ? C44 C43 C42 117.9(12) . . ? C9 C8 C7 117.7(14) . . ? C26 C25 C24 119.0(14) . . ? C7 C6 C5 122.0(14) . . ? C49 N9 C47 114.3(11) . . ? C49 N9 C46 110.6(11) . . ? C47 N9 C46 106.5(10) . . ? C49 N9 C51 104.3(9) . . ? C47 N9 C51 112.3(11) . . ? C46 N9 C51 108.7(11) . . ? N9 C49 C50 112.5(11) . . ? C24 C23 C22 124.3(15) . . ? C23 C24 C25 117.9(13) . . ? C6 C7 C8 120.4(14) . . ? C52 C51 N9 117.4(11) . . ? N9 C47 C48 114.7(11) . . ? C45 C46 N9 114.9(12) . . ? N10 C54 C53 177(2) . . ? N11 C56 C55 167(5) . . ? N5 O3 Dy1 89.95(17) . . ? N5 O3 Dy1 89.95(17) . 2 ? Dy1 O3 Dy1 179.9(3) . 2 ? N5 O4 Dy1 103.2(6) . . ? O3 N5 O4 118.4(6) . . ? O3 N5 O4 118.4(6) . 2 ? O4 N5 O4 123.2(12) . 2 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 6.530 _refine_diff_density_min -2.641 _refine_diff_density_rms 0.164 _database_code_depnum_ccdc_archive 'CCDC 972574'