# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_1 _database_code_depnum_ccdc_archive 'CCDC 910760' #TrackingRef '91760.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; The two tert-butyl groups were each disordered into two positions with occupancies of 71/29,52/48, respectively, and the temperature factors of all atoms were restrained by using the command DELU/SIMU/ISOR. The subsequent refinement gave good ellipsoid plot. The bond lengths and bond angles of those two tert-butyl groups were restrained by using DFIX. All the hydrogens were added geometrically. The terminal H2O ligand were confirmed by the charge consideration and bond-valence-sum (BVS) calculations, but O6 atoms lies in a special location (O(6)on threefold axis), and may involve in some form of disorde,we failed to added the hydrogens on them, and these six hydrogens were calculated in the reported formula. ; _chemical_name_common ; The two tert-butyl groups were each disordered into two positions with occupancies of 71/29,52/48, respectively, and the temperature factors of all atoms were restrained by using the command DELU/SIMU/ISOR. The subsequent refinement gave good ellipsoid plot. The bond lengths and bond angles of those two tert-butyl groups were restrained by using DFIX. All the hydrogens were added geometrically. Th ; _chemical_melting_point ? _chemical_formula_moiety 'C72 H138 Mn3 N2 Nd4 O33' _chemical_formula_sum 'C72 H138 Mn3 N2 Nd4 O33' _chemical_formula_weight 2301.62 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M R-3c _symmetry_space_group_name_hall '-R 3 2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 17.9410(6) _cell_length_b 17.9410(6) _cell_length_c 57.790(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 16109.2(17) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1886 _cell_measurement_theta_min 2.1960 _cell_measurement_theta_max 27.4797 _exptl_crystal_description prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6942 _exptl_absorpt_coefficient_mu 2.305 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4817 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Corp., 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32266 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0171 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -68 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3150 _reflns_number_gt 2816 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; # start Validation Reply Form _vrf_PLAT041_1 ; PROBLEM:PLAT041_ALERT_1_C Calc. and Reported Sum Formula Strings Differ ? RESPONSE:The O6 atoms of terminal H2O ligand lies in a special location (O(6)on threefold axis), and may involve in some form of disorder, we failed to added the hydrogens on them. ; _vrf_PLAT094_1 ; PROBLEM: PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.58 RESPONSE:The highest peak on the final difference Fourier map (2.256 e-/A^3^) is in the vicinity of atom c11'. The peak may arise form a disorder of the tert-butly group. The deepest hole (-0.876 e.A^-3^) is located at 0.85 A from Nd2. Attempts to eliminate the peak or name it as H2O molecule proved to be unsuccessful. ; _vrf_PLAT605_1 ; PROBLEM: PLAT605_ALERT_4_G Structure Contains Solvent Accessible VOIDS of . 332 A**3 RESPONSE: The complex contains water and/or methanol (less likely) as solvent molecules, which in a highly disordered fashion are occupying channels extending parallel to the crystallographic c-axis. According to the program SQUEEZE4 of PLATON software package (Vandersluis, P. S., A. L. Acta Crystallogr.; Sect. A 1990, 46, 194.), the solvent accessible volume of the unit cell is 2056 cubic Angstroems with an electron count of 28 electrons per cell. This solvent was subjected to procedure SQUEEZE of program PLATON. It is not contained in chemical formula. ; # end Validation Reply Form # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 344.4 5.4 2 0.000 0.000 0.500 344.4 4.3 3 0.333 0.667 0.167 342.7 4.0 4 0.333 0.667 0.667 342.7 5.0 5 0.667 0.333 0.333 342.2 5.0 6 0.667 0.333 0.833 342.3 4.0 _platon_squeeze_details ; ; _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^)+(0.0863P)^2^+101.3595P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3150 _refine_ls_number_parameters 231 _refine_ls_number_restraints 258 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1429 _refine_ls_wR_factor_gt 0.1365 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.6667 0.3333 0.03646(11) 0.0402(14) Uani 1 3 d S . . Mn1 Mn 0.86928(6) 0.3333 0.0833 0.0402(3) Uani 1 2 d S . . Nd1 Nd 0.6667 0.11314(2) 0.0833 0.04483(19) Uani 1 2 d S . . Nd2 Nd 0.6667 0.3333 0.0833 0.03033(19) Uani 1 6 d S . . O1 O 0.7258(3) 0.0934(3) 0.04679(8) 0.0805(13) Uani 1 1 d . . . O2 O 0.8008(2) 0.2268(2) 0.05804(6) 0.0507(8) Uani 1 1 d . . . O3 O 0.5364(2) -0.0035(2) 0.06712(7) 0.0649(10) Uani 1 1 d . . . O4 O 0.4242(2) 0.0162(2) 0.06458(7) 0.0590(9) Uani 1 1 d . . . O5 O 0.81043(17) 0.40840(19) 0.06620(6) 0.0380(8) Uani 1 1 d . . . O6 O 0.6667 -0.0360(6) 0.0833 0.135(3) Uani 1 2 d SU . . C1 C 0.8243(3) 0.4130(3) 0.04149(10) 0.0440(12) Uani 1 1 d . . . H1B H 0.8343 0.3669 0.0367 0.065(17) Uiso 1 1 calc R . . H1C H 0.8752 0.4672 0.0377 0.078 Uiso 1 1 calc R . . C2 C 0.7487(4) 0.4057(4) 0.02864(9) 0.0624(14) Uani 1 1 d . . . H2A H 0.7473 0.4587 0.0306 0.075 Uiso 1 1 calc R . . H2B H 0.7558 0.3989 0.0123 0.075 Uiso 1 1 calc R . . C3 C 0.7934(4) 0.1646(4) 0.04566(10) 0.0577(13) Uani 1 1 d . A . C4 C 0.8650(3) 0.1778(3) 0.02922(8) 0.0772(15) Uani 1 1 d DU . . C5 C 0.8384(6) 0.1004(5) 0.01332(18) 0.101(3) Uani 0.710(14) 1 d PDU A 1 H5A H 0.7933 0.0942 0.0032 0.152 Uiso 0.710(14) 1 calc PR A 1 H5B H 0.8181 0.0492 0.0225 0.152 Uiso 0.710(14) 1 calc PR A 1 H5C H 0.8871 0.1090 0.0043 0.152 Uiso 0.710(14) 1 calc PR A 1 C6 C 0.8902(7) 0.2581(5) 0.01458(17) 0.093(3) Uani 0.710(14) 1 d PDU A 1 H6A H 0.8441 0.2471 0.0042 0.139 Uiso 0.710(14) 1 calc PR A 1 H6B H 0.9412 0.2722 0.0059 0.139 Uiso 0.710(14) 1 calc PR A 1 H6C H 0.9012 0.3054 0.0245 0.139 Uiso 0.710(14) 1 calc PR A 1 C7 C 0.9416(5) 0.1922(8) 0.04409(15) 0.085(3) Uani 0.710(14) 1 d PDU A 1 H7A H 0.9939 0.2366 0.0373 0.128 Uiso 0.710(14) 1 calc PR A 1 H7B H 0.9436 0.1398 0.0449 0.128 Uiso 0.710(14) 1 calc PR A 1 H7C H 0.9354 0.2093 0.0594 0.128 Uiso 0.710(14) 1 calc PR A 1 C5' C 0.8503(14) 0.0869(6) 0.0257(5) 0.091(4) Uani 0.290(14) 1 d PDU A 2 H5'A H 0.8054 0.0571 0.0145 0.136 Uiso 0.290(14) 1 calc PR A 2 H5'B H 0.8338 0.0563 0.0401 0.136 Uiso 0.290(14) 1 calc PR A 2 H5'C H 0.9024 0.0903 0.0202 0.136 Uiso 0.290(14) 1 calc PR A 2 C6' C 0.8604(15) 0.2155(16) 0.0059(2) 0.100(4) Uani 0.290(14) 1 d PDU A 2 H6'A H 0.8027 0.1841 0.0000 0.150 Uiso 0.290(14) 1 calc PR A 2 H6'B H 0.8989 0.2113 -0.0048 0.150 Uiso 0.290(14) 1 calc PR A 2 H6'C H 0.8766 0.2749 0.0078 0.150 Uiso 0.290(14) 1 calc PR A 2 C7' C 0.9534(7) 0.2347(13) 0.0402(4) 0.080(4) Uani 0.290(14) 1 d PDU A 2 H7'A H 0.9628 0.2033 0.0521 0.120 Uiso 0.290(14) 1 calc PR A 2 H7'B H 0.9558 0.2851 0.0467 0.120 Uiso 0.290(14) 1 calc PR A 2 H7'C H 0.9972 0.2516 0.0285 0.120 Uiso 0.290(14) 1 calc PR A 2 C8 C 0.4617(4) -0.0252(3) 0.06080(10) 0.0601(13) Uani 1 1 d . B . C9 C 0.4128(4) -0.1090(4) 0.04682(12) 0.1094(17) Uani 1 1 d DU . . C10 C 0.4215(9) -0.0820(8) 0.02140(14) 0.1101(17) Uani 0.524(8) 1 d PDU B 1 H10A H 0.4199 -0.0295 0.0202 0.165 Uiso 0.524(8) 1 calc PR B 1 H10B H 0.3749 -0.1263 0.0127 0.165 Uiso 0.524(8) 1 calc PR B 1 H10C H 0.4752 -0.0733 0.0154 0.165 Uiso 0.524(8) 1 calc PR B 1 C11 C 0.4443(8) -0.1735(7) 0.0500(2) 0.1099(17) Uani 0.524(8) 1 d PDU B 1 H11A H 0.4785 -0.1706 0.0369 0.165 Uiso 0.524(8) 1 calc PR B 1 H11B H 0.3956 -0.2305 0.0512 0.165 Uiso 0.524(8) 1 calc PR B 1 H11C H 0.4784 -0.1597 0.0638 0.165 Uiso 0.524(8) 1 calc PR B 1 C12 C 0.3184(5) -0.1506(8) 0.0542(2) 0.1099(17) Uani 0.524(8) 1 d PDU B 1 H12A H 0.2915 -0.1234 0.0461 0.165 Uiso 0.524(8) 1 calc PR B 1 H12B H 0.3152 -0.1438 0.0705 0.165 Uiso 0.524(8) 1 calc PR B 1 H12C H 0.2892 -0.2108 0.0504 0.165 Uiso 0.524(8) 1 calc PR B 1 C10' C 0.4760(7) -0.1040(9) 0.0283(2) 0.1101(17) Uani 0.476(8) 1 d PDU B 2 H10D H 0.4838 -0.0615 0.0169 0.165 Uiso 0.476(8) 1 calc PR B 2 H10E H 0.4535 -0.1591 0.0209 0.165 Uiso 0.476(8) 1 calc PR B 2 H10F H 0.5303 -0.0884 0.0353 0.165 Uiso 0.476(8) 1 calc PR B 2 C11' C 0.3961(10) -0.1806(7) 0.0640(2) 0.1098(18) Uani 0.476(8) 1 d PDU B 2 H11D H 0.4486 -0.1814 0.0667 0.165 Uiso 0.476(8) 1 calc PR B 2 H11E H 0.3535 -0.2351 0.0578 0.165 Uiso 0.476(8) 1 calc PR B 2 H11F H 0.3759 -0.1703 0.0784 0.165 Uiso 0.476(8) 1 calc PR B 2 C12' C 0.3281(6) -0.1282(9) 0.0354(3) 0.1099(17) Uani 0.476(8) 1 d PDU B 2 H12D H 0.3383 -0.0821 0.0251 0.165 Uiso 0.476(8) 1 calc PR B 2 H12E H 0.2878 -0.1334 0.0472 0.165 Uiso 0.476(8) 1 calc PR B 2 H12F H 0.3050 -0.1811 0.0269 0.165 Uiso 0.476(8) 1 calc PR B 2 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 N1 0.043(2) 0.043(2) 0.035(3) 0.000 0.000 0.0213(11) Mn1 0.0375(4) 0.0411(5) 0.0433(6) 0.0013(4) 0.00064(19) 0.0205(3) Nd1 0.0409(2) 0.0364(2) 0.0586(3) 0.00044(7) 0.00087(14) 0.02043(12) Nd2 0.0321(2) 0.0321(2) 0.0269(3) 0.000 0.000 0.01603(12) O1 0.066(3) 0.060(2) 0.100(3) -0.027(2) 0.017(2) 0.020(2) O2 0.054(2) 0.0492(19) 0.0518(19) -0.0059(15) 0.0034(15) 0.0283(16) O3 0.052(2) 0.045(2) 0.094(3) -0.0117(19) -0.002(2) 0.0216(18) O4 0.054(2) 0.0438(19) 0.076(2) -0.0120(17) -0.0092(18) 0.0216(17) O5 0.0384(17) 0.0421(18) 0.0336(18) 0.0044(12) 0.0042(11) 0.0200(14) O6 0.135(3) 0.131(3) 0.139(3) -0.0004(9) -0.0008(18) 0.0677(14) C1 0.048(3) 0.048(3) 0.035(3) 0.0066(19) 0.009(2) 0.023(2) C2 0.067(3) 0.069(4) 0.039(3) 0.008(2) 0.007(2) 0.025(3) C3 0.058(3) 0.058(3) 0.059(3) -0.015(3) -0.001(3) 0.030(3) C4 0.072(3) 0.088(3) 0.081(3) -0.018(3) 0.015(3) 0.047(3) C5 0.094(5) 0.103(5) 0.095(6) -0.037(4) 0.024(5) 0.040(4) C6 0.097(5) 0.102(5) 0.079(5) -0.004(4) 0.028(4) 0.049(4) C7 0.065(4) 0.097(6) 0.099(5) -0.008(5) 0.015(4) 0.045(4) C5' 0.087(6) 0.096(5) 0.089(7) -0.025(6) 0.019(6) 0.046(5) C6' 0.096(7) 0.109(7) 0.085(6) -0.007(6) 0.011(6) 0.043(6) C7' 0.064(5) 0.091(7) 0.093(6) -0.011(6) 0.018(5) 0.045(5) C8 0.065(4) 0.045(3) 0.066(3) -0.001(2) -0.001(3) 0.024(3) C9 0.122(3) 0.084(3) 0.120(3) -0.036(3) -0.021(3) 0.049(3) C10 0.122(3) 0.084(3) 0.120(3) -0.036(3) -0.021(3) 0.048(3) C11 0.122(3) 0.084(3) 0.120(3) -0.036(3) -0.021(3) 0.049(3) C12 0.122(3) 0.084(3) 0.120(3) -0.036(3) -0.021(3) 0.048(3) C10' 0.122(3) 0.084(3) 0.120(3) -0.036(3) -0.021(3) 0.048(3) C11' 0.122(3) 0.084(3) 0.120(3) -0.036(3) -0.021(3) 0.049(3) C12' 0.122(3) 0.084(3) 0.120(3) -0.036(3) -0.021(3) 0.048(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 N1 C2 1.465(6) 3_665 ? N1 C2 1.465(6) . ? N1 C2 1.465(6) 2_655 ? N1 Nd2 2.709(6) . ? Mn1 O4 2.107(4) 2_655 ? Mn1 O4 2.107(4) 18_654 ? Mn1 O2 2.225(3) . ? Mn1 O2 2.225(3) 17_554 ? Mn1 O5 2.309(3) . ? Mn1 O5 2.309(3) 17_554 ? Mn1 Nd2 3.6351(11) . ? Nd1 O3 2.414(4) . ? Nd1 O3 2.414(4) 18_654 ? Nd1 O5 2.464(3) 3_665 ? Nd1 O5 2.463(3) 17_554 ? Nd1 O1 2.467(4) . ? Nd1 O1 2.467(4) 18_654 ? Nd1 O6 2.676(10) . ? Nd1 O2 2.680(3) . ? Nd1 O2 2.680(3) 18_654 ? Nd1 C3 2.943(6) . ? Nd1 C3 2.943(6) 18_654 ? Nd1 Nd2 3.9505(4) . ? Nd2 O5 2.444(3) 3_665 ? Nd2 O5 2.444(3) . ? Nd2 O5 2.444(3) 17_554 ? Nd2 O5 2.444(3) 2_655 ? Nd2 O5 2.444(3) 16_544 ? Nd2 O5 2.444(3) 18_654 ? Nd2 N1 2.709(6) 16_544 ? Nd2 Mn1 3.6351(11) 3_665 ? Nd2 Mn1 3.6351(11) 2_655 ? O1 C3 1.248(7) . ? O2 C3 1.275(6) . ? O3 C8 1.250(7) . ? O4 C8 1.245(7) . ? O4 Mn1 2.107(4) 3_665 ? O5 C1 1.445(7) . ? O5 Nd1 2.464(3) 2_655 ? C1 C2 1.494(8) . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.518(7) . ? C4 C7' 1.5298(10) . ? C4 C7 1.5299(10) . ? C4 C6' 1.5296(10) . ? C4 C5 1.5297(10) . ? C4 C5' 1.5301(10) . ? C4 C6 1.5307(10) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C5' H5'A 0.9600 . ? C5' H5'B 0.9600 . ? C5' H5'C 0.9600 . ? C6' H6'A 0.9600 . ? C6' H6'B 0.9600 . ? C6' H6'C 0.9600 . ? C7' H7'A 0.9600 . ? C7' H7'B 0.9600 . ? C7' H7'C 0.9600 . ? C8 C9 1.538(7) . ? C9 C11 1.5294(10) . ? C9 C12' 1.5295(10) . ? C9 C11' 1.5304(10) . ? C9 C10' 1.5303(10) . ? C9 C10 1.5302(10) . ? C9 C12 1.5305(10) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C10' H10D 0.9600 . ? C10' H10E 0.9600 . ? C10' H10F 0.9600 . ? C11' H11D 0.9600 . ? C11' H11E 0.9600 . ? C11' H11F 0.9600 . ? C12' H12D 0.9600 . ? C12' H12E 0.9600 . ? C12' H12F 0.9600 . ? 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 N1 C2 110.9(3) 3_665 . ? C2 N1 C2 110.9(3) 3_665 2_655 ? C2 N1 C2 110.9(3) . 2_655 ? C2 N1 Nd2 108.0(3) 3_665 . ? C2 N1 Nd2 108.0(3) . . ? C2 N1 Nd2 108.0(3) 2_655 . ? O4 Mn1 O4 97.8(2) 2_655 18_654 ? O4 Mn1 O2 98.75(14) 2_655 . ? O4 Mn1 O2 90.50(14) 18_654 . ? O4 Mn1 O2 90.50(14) 2_655 17_554 ? O4 Mn1 O2 98.76(14) 18_654 17_554 ? O2 Mn1 O2 165.93(18) . 17_554 ? O4 Mn1 O5 89.62(13) 2_655 . ? O4 Mn1 O5 172.34(13) 18_654 . ? O2 Mn1 O5 90.14(12) . . ? O2 Mn1 O5 79.29(13) 17_554 . ? O4 Mn1 O5 172.33(13) 2_655 17_554 ? O4 Mn1 O5 89.62(13) 18_654 17_554 ? O2 Mn1 O5 79.29(13) . 17_554 ? O2 Mn1 O5 90.14(12) 17_554 17_554 ? O5 Mn1 O5 83.00(15) . 17_554 ? O4 Mn1 Nd2 131.08(11) 2_655 . ? O4 Mn1 Nd2 131.09(11) 18_654 . ? O2 Mn1 Nd2 82.97(9) . . ? O2 Mn1 Nd2 82.97(9) 17_554 . ? O5 Mn1 Nd2 41.50(7) . . ? O5 Mn1 Nd2 41.50(7) 17_554 . ? O3 Nd1 O3 135.00(18) . 18_654 ? O3 Nd1 O5 77.85(11) . 3_665 ? O3 Nd1 O5 145.88(11) 18_654 3_665 ? O3 Nd1 O5 145.88(11) . 17_554 ? O3 Nd1 O5 77.85(11) 18_654 17_554 ? O5 Nd1 O5 72.44(14) 3_665 17_554 ? O3 Nd1 O1 80.95(14) . . ? O3 Nd1 O1 83.26(16) 18_654 . ? O5 Nd1 O1 96.13(15) 3_665 . ? O5 Nd1 O1 118.17(12) 17_554 . ? O3 Nd1 O1 83.27(16) . 18_654 ? O3 Nd1 O1 80.95(14) 18_654 18_654 ? O5 Nd1 O1 118.17(12) 3_665 18_654 ? O5 Nd1 O1 96.13(15) 17_554 18_654 ? O1 Nd1 O1 138.0(2) . 18_654 ? O3 Nd1 O6 67.50(9) . . ? O3 Nd1 O6 67.50(9) 18_654 . ? O5 Nd1 O6 143.78(7) 3_665 . ? O5 Nd1 O6 143.78(7) 17_554 . ? O1 Nd1 O6 68.98(11) . . ? O1 Nd1 O6 68.97(11) 18_654 . ? O3 Nd1 O2 124.05(12) . . ? O3 Nd1 O2 71.26(12) 18_654 . ? O5 Nd1 O2 82.31(10) 3_665 . ? O5 Nd1 O2 68.32(11) 17_554 . ? O1 Nd1 O2 49.86(12) . . ? O1 Nd1 O2 150.28(13) 18_654 . ? O6 Nd1 O2 108.17(7) . . ? O3 Nd1 O2 71.26(12) . 18_654 ? O3 Nd1 O2 124.05(12) 18_654 18_654 ? O5 Nd1 O2 68.32(11) 3_665 18_654 ? O5 Nd1 O2 82.31(10) 17_554 18_654 ? O1 Nd1 O2 150.28(13) . 18_654 ? O1 Nd1 O2 49.86(12) 18_654 18_654 ? O6 Nd1 O2 108.17(7) . 18_654 ? O2 Nd1 O2 143.66(14) . 18_654 ? O3 Nd1 C3 104.24(14) . . ? O3 Nd1 C3 72.45(15) 18_654 . ? O5 Nd1 C3 92.93(14) 3_665 . ? O5 Nd1 C3 93.78(13) 17_554 . ? O1 Nd1 C3 24.73(14) . . ? O1 Nd1 C3 148.90(15) 18_654 . ? O6 Nd1 C3 85.84(11) . . ? O2 Nd1 C3 25.67(13) . . ? O2 Nd1 C3 161.18(14) 18_654 . ? O3 Nd1 C3 72.45(15) . 18_654 ? O3 Nd1 C3 104.24(14) 18_654 18_654 ? O5 Nd1 C3 93.79(13) 3_665 18_654 ? O5 Nd1 C3 92.93(14) 17_554 18_654 ? O1 Nd1 C3 148.90(15) . 18_654 ? O1 Nd1 C3 24.73(14) 18_654 18_654 ? O6 Nd1 C3 85.84(11) . 18_654 ? O2 Nd1 C3 161.19(14) . 18_654 ? O2 Nd1 C3 25.67(13) 18_654 18_654 ? C3 Nd1 C3 171.7(2) . 18_654 ? O3 Nd1 Nd2 112.50(9) . . ? O3 Nd1 Nd2 112.50(9) 18_654 . ? O5 Nd1 Nd2 36.22(7) 3_665 . ? O5 Nd1 Nd2 36.22(7) 17_554 . ? O1 Nd1 Nd2 111.02(11) . . ? O1 Nd1 Nd2 111.03(11) 18_654 . ? O6 Nd1 Nd2 180.0 . . ? O2 Nd1 Nd2 71.83(7) . . ? O2 Nd1 Nd2 71.83(7) 18_654 . ? C3 Nd1 Nd2 94.16(11) . . ? C3 Nd1 Nd2 94.16(11) 18_654 . ? O5 Nd2 O5 104.70(10) 3_665 . ? O5 Nd2 O5 73.12(16) 3_665 17_554 ? O5 Nd2 O5 77.51(15) . 17_554 ? O5 Nd2 O5 104.70(10) 3_665 2_655 ? O5 Nd2 O5 104.70(10) . 2_655 ? O5 Nd2 O5 177.32(15) 17_554 2_655 ? O5 Nd2 O5 177.31(15) 3_665 16_544 ? O5 Nd2 O5 73.12(16) . 16_544 ? O5 Nd2 O5 104.71(10) 17_554 16_544 ? O5 Nd2 O5 77.51(15) 2_655 16_544 ? O5 Nd2 O5 77.51(15) 3_665 18_654 ? O5 Nd2 O5 177.32(14) . 18_654 ? O5 Nd2 O5 104.71(10) 17_554 18_654 ? O5 Nd2 O5 73.12(16) 2_655 18_654 ? O5 Nd2 O5 104.71(10) 16_544 18_654 ? O5 Nd2 N1 66.10(8) 3_665 . ? O5 Nd2 N1 66.10(8) . . ? O5 Nd2 N1 113.89(8) 17_554 . ? O5 Nd2 N1 66.10(8) 2_655 . ? O5 Nd2 N1 113.90(8) 16_544 . ? O5 Nd2 N1 113.90(8) 18_654 . ? O5 Nd2 N1 113.90(8) 3_665 16_544 ? O5 Nd2 N1 113.90(8) . 16_544 ? O5 Nd2 N1 66.10(8) 17_554 16_544 ? O5 Nd2 N1 113.90(8) 2_655 16_544 ? O5 Nd2 N1 66.11(8) 16_544 16_544 ? O5 Nd2 N1 66.11(8) 18_654 16_544 ? N1 Nd2 N1 180.0 . 16_544 ? O5 Nd2 Mn1 88.66(7) 3_665 . ? O5 Nd2 Mn1 38.76(7) . . ? O5 Nd2 Mn1 38.75(7) 17_554 . ? O5 Nd2 Mn1 143.44(8) 2_655 . ? O5 Nd2 Mn1 88.66(7) 16_544 . ? O5 Nd2 Mn1 143.44(8) 18_654 . ? N1 Nd2 Mn1 90.0 . . ? N1 Nd2 Mn1 90.0 16_544 . ? O5 Nd2 Mn1 38.76(7) 3_665 3_665 ? O5 Nd2 Mn1 143.44(8) . 3_665 ? O5 Nd2 Mn1 88.66(7) 17_554 3_665 ? O5 Nd2 Mn1 88.66(7) 2_655 3_665 ? O5 Nd2 Mn1 143.44(8) 16_544 3_665 ? O5 Nd2 Mn1 38.75(7) 18_654 3_665 ? N1 Nd2 Mn1 90.0 . 3_665 ? N1 Nd2 Mn1 90.0 16_544 3_665 ? Mn1 Nd2 Mn1 120.0 . 3_665 ? O5 Nd2 Mn1 143.44(8) 3_665 2_655 ? O5 Nd2 Mn1 88.66(7) . 2_655 ? O5 Nd2 Mn1 143.44(8) 17_554 2_655 ? O5 Nd2 Mn1 38.76(7) 2_655 2_655 ? O5 Nd2 Mn1 38.76(7) 16_544 2_655 ? O5 Nd2 Mn1 88.66(7) 18_654 2_655 ? N1 Nd2 Mn1 90.0 . 2_655 ? N1 Nd2 Mn1 90.0 16_544 2_655 ? Mn1 Nd2 Mn1 120.0 . 2_655 ? Mn1 Nd2 Mn1 120.0 3_665 2_655 ? O5 Nd2 Nd1 36.56(8) 3_665 . ? O5 Nd2 Nd1 91.34(7) . . ? O5 Nd2 Nd1 36.56(8) 17_554 . ? O5 Nd2 Nd1 141.24(7) 2_655 . ? O5 Nd2 Nd1 141.24(7) 16_544 . ? O5 Nd2 Nd1 91.34(7) 18_654 . ? N1 Nd2 Nd1 90.0 . . ? N1 Nd2 Nd1 90.0 16_544 . ? Mn1 Nd2 Nd1 60.0 . . ? Mn1 Nd2 Nd1 60.0 3_665 . ? Mn1 Nd2 Nd1 180.0 2_655 . ? C3 O1 Nd1 99.5(3) . . ? C3 O2 Mn1 153.1(4) . . ? C3 O2 Nd1 88.8(3) . . ? Mn1 O2 Nd1 101.26(12) . . ? C8 O3 Nd1 143.8(3) . . ? C8 O4 Mn1 130.6(4) . 3_665 ? C1 O5 Mn1 109.9(3) . . ? C1 O5 Nd2 122.4(3) . . ? Mn1 O5 Nd2 99.74(12) . . ? C1 O5 Nd1 110.4(3) . 2_655 ? Mn1 O5 Nd1 105.60(13) . 2_655 ? Nd2 O5 Nd1 107.22(13) . 2_655 ? O5 C1 C2 111.3(4) . . ? O5 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? O5 C1 H1C 109.4 . . ? C2 C1 H1C 109.4 . . ? H1B C1 H1C 108.0 . . ? N1 C2 C1 113.0(4) . . ? N1 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? N1 C2 H2B 109.0 . . ? C1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? O1 C3 O2 119.3(5) . . ? O1 C3 C4 120.4(5) . . ? O2 C3 C4 120.3(5) . . ? O1 C3 Nd1 55.8(3) . . ? O2 C3 Nd1 65.6(3) . . ? C4 C3 Nd1 166.6(4) . . ? C3 C4 C7' 111.1(9) . . ? C3 C4 C7 107.1(5) . . ? C7' C4 C7 27.2(8) . . ? C3 C4 C6' 113.1(9) . . ? C7' C4 C6' 109.66(15) . . ? C7 C4 C6' 131.6(9) . . ? C3 C4 C5 112.3(5) . . ? C7' C4 C5 127.1(10) . . ? C7 C4 C5 109.66(15) . . ? C6' C4 C5 79.1(8) . . ? C3 C4 C5' 103.6(9) . . ? C7' C4 C5' 109.56(15) . . ? C7 C4 C5' 85.2(8) . . ? C6' C4 C5' 109.61(15) . . ? C5 C4 C5' 30.9(8) . . ? C3 C4 C6 108.8(5) . . ? C7' C4 C6 83.1(8) . . ? C7 C4 C6 109.47(15) . . ? C6' C4 C6 32.1(8) . . ? C5 C4 C6 109.51(15) . . ? C5' C4 C6 137.9(9) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C5' H5'A 109.5 . . ? C4 C5' H5'B 109.5 . . ? H5'A C5' H5'B 109.5 . . ? C4 C5' H5'C 109.5 . . ? H5'A C5' H5'C 109.5 . . ? H5'B C5' H5'C 109.5 . . ? C4 C6' H6'A 109.5 . . ? C4 C6' H6'B 109.5 . . ? H6'A C6' H6'B 109.5 . . ? C4 C6' H6'C 109.5 . . ? H6'A C6' H6'C 109.5 . . ? H6'B C6' H6'C 109.5 . . ? C4 C7' H7'A 109.5 . . ? C4 C7' H7'B 109.5 . . ? H7'A C7' H7'B 109.5 . . ? C4 C7' H7'C 109.5 . . ? H7'A C7' H7'C 109.5 . . ? H7'B C7' H7'C 109.5 . . ? O4 C8 O3 125.3(5) . . ? O4 C8 C9 117.5(5) . . ? O3 C8 C9 117.2(5) . . ? C11 C9 C12' 125.6(8) . . ? C11 C9 C11' 44.0(6) . . ? C12' C9 C11' 109.60(15) . . ? C11 C9 C10' 65.5(6) . . ? C12' C9 C10' 109.59(15) . . ? C11' C9 C10' 109.45(15) . . ? C11 C9 C10 109.62(15) . . ? C12' C9 C10 65.8(6) . . ? C11' C9 C10 146.7(7) . . ? C10' C9 C10 49.7(6) . . ? C11 C9 C12 109.59(15) . . ? C12' C9 C12 43.6(6) . . ? C11' C9 C12 72.9(6) . . ? C10' C9 C12 146.0(7) . . ? C10 C9 C12 109.43(15) . . ? C11 C9 C8 115.6(6) . . ? C12' C9 C8 117.5(7) . . ? C11' C9 C8 104.9(7) . . ? C10' C9 C8 105.5(6) . . ? C10 C9 C8 106.0(6) . . ? C12 C9 C8 106.4(7) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C10' H10D 109.5 . . ? C9 C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C9 C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? C9 C11' H11D 109.5 . . ? C9 C11' H11E 109.5 . . ? H11D C11' H11E 109.5 . . ? C9 C11' H11F 109.5 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? C9 C12' H12D 109.5 . . ? C9 C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? C9 C12' H12F 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.256 _refine_diff_density_min -0.876 _refine_diff_density_rms 0.104