# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address J.W.Walton ; Department of Chemistry Durham University South Rd. Durham DH1 3LE UK ; 'L.di Bari' ; Dipartamento di Chimica Industriale via Risorgimento 35 I-56126 Pisa Italy ; D.Parker ; Department of Chemistry Durham University South Rd. Durham DH1 3LE UK ; H.Puschmann ; Department of Chemistry Durham University South Rd. Durham DH1 3LE UK ; D.S.Yufit ; Department of Chemistry Durham University South Rd. Durham DH1 3LE UK ; _publ_contact_author_address ; Department of Chemistry Durham University South Rd. Durham DH1 3LE UK ; _publ_contact_author_email d.s.yufit@durham.ac.uk _publ_contact_author_name 'Dmitry Yufit' _publ_contact_letter ; The CIF file contains data for the structure [Eu.L^3^] from the paper Structure, resolution and chirooptical analysis of stable lanthanide complexes of a pyridylmethylphosphinate triazacyclonane ligand by J.W.Walton, L. di Bari, D.Parker, H.Puschmann and D.S.Yufit The paper will be submitted to Chem.Commun. shortly ; data_EuL3_130Eu _database_code_depnum_ccdc_archive 'CCDC 836097' #TrackingRef '6390_web_deposit_cif_file_0_DmitryYufit_1311257364.EuL3.cif' _audit_creation_date 2011-07-19 _audit_creation_method ; Olex2 1.1-beta (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H42 Eu N6 O6 P3' _chemical_formula_sum 'C42 H42 Eu N6 O6 P3' _chemical_formula_weight 971.69 _chemical_melting_point ? 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' Eu Eu -0.1578 3.6682 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.0740(7) _cell_length_b 22.6062(5) _cell_length_c 15.9852(7) _cell_angle_alpha 90.00 _cell_angle_beta 112.233(6) _cell_angle_gamma 90.00 _cell_volume 5042.2(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6481 _cell_measurement_temperature 120.0 _cell_measurement_theta_max 28.8554 _cell_measurement_theta_min 2.7106 _exptl_absorpt_coefficient_mu 1.384 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.85808 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1968 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_unetI/netI 0.0340 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 44388 _diffrn_reflns_theta_full 29.00 _diffrn_reflns_theta_max 29.00 _diffrn_reflns_theta_min 2.75 _diffrn_ambient_temperature 120.0 _diffrn_detector CCD _diffrn_detector_area_resol_mean 16.1511 _diffrn_detector_type Sapphire3 _diffrn_measured_fraction_theta_full 0.905 _diffrn_measured_fraction_theta_max 0.905 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -80.00 20.00 1.0000 13.3600 omega____ theta____ kappa____ phi______ frames - -18.0928 0.0000 -180.0000 100 ; _diffrn_measurement_device '3-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method \w-scan _diffrn_orient_matrix_UB_11 -0.0058540000 _diffrn_orient_matrix_UB_12 -0.0203332000 _diffrn_orient_matrix_UB_13 0.0313051000 _diffrn_orient_matrix_UB_21 -0.0206381000 _diffrn_orient_matrix_UB_22 0.0226685000 _diffrn_orient_matrix_UB_23 0.0174736000 _diffrn_orient_matrix_UB_31 -0.0460932000 _diffrn_orient_matrix_UB_32 -0.0075493000 _diffrn_orient_matrix_UB_33 -0.0318317000 _diffrn_radiation_collimation monochromator _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_xray_symbol Mo _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_source_type 'sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 9772 _reflns_number_total 12135 _reflns_odcompleteness_completeness 76.71 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 1.500 _refine_diff_density_min -0.772 _refine_diff_density_rms 0.090 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 492 _refine_ls_number_reflns 12135 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0314 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0020P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.0748 _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. The structure contains a number of severely disordered solvent molecules (H2O, methanol). Their contribution to the structural fctors was taken into account by applying MASK procedure of OLEX2 program package. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Eu1 Eu -0.427742(9) -0.824255(5) -1.177898(9) 0.01273(4) Uani 1 1 d . A . P1 P -0.32450(5) -0.85513(3) -0.94244(5) 0.01586(14) Uani 1 1 d . . . P2 P -0.41956(5) -0.97148(3) -1.25154(5) 0.01751(14) Uani 1 1 d . . . P3 P -0.21963(5) -0.77823(4) -1.21090(5) 0.02395(16) Uani 1 1 d . . . O1 O -0.32194(13) -0.82593(8) -1.02672(12) 0.0180(4) Uani 1 1 d . . . O2 O -0.30637(14) -0.81788(9) -0.86039(13) 0.0243(4) Uani 1 1 d . . . O3 O -0.41461(13) -0.92719(8) -1.17875(12) 0.0173(4) Uani 1 1 d . A . O4 O -0.49507(14) -1.01834(9) -1.27281(14) 0.0256(4) Uani 1 1 d . B . O5 O -0.29156(14) -0.82493(10) -1.21272(14) 0.0264(4) Uani 1 1 d . A . O6B O -0.2193(3) -0.7657(2) -1.3027(3) 0.0208(10) Uiso 0.50 1 d P A 2 N1 N -0.61682(15) -0.83482(10) -1.23279(15) 0.0168(5) Uani 1 1 d . . . N2 N -0.52455(15) -0.75913(10) -1.32597(15) 0.0167(5) Uani 1 1 d . A . N3 N -0.51330(16) -0.72764(10) -1.14714(15) 0.0175(5) Uani 1 1 d . A . N4 N -0.49828(15) -0.87745(9) -1.06814(14) 0.0141(4) Uani 1 1 d . . . N5 N -0.45687(15) -0.86903(10) -1.34131(15) 0.0157(4) Uani 1 1 d . . . N6 N -0.32638(16) -0.72533(10) -1.13297(15) 0.0186(5) Uani 1 1 d . . . C1 C -0.65544(19) -0.83256(12) -1.33357(18) 0.0189(5) Uani 1 1 d . . . H1A H -0.7261 -0.8359 -1.3567 0.023 Uiso 1 1 calc R . . H1B H -0.6306 -0.8669 -1.3565 0.023 Uiso 1 1 calc R . . C2 C -0.62876(19) -0.77611(13) -1.36985(19) 0.0208(6) Uani 1 1 d . . . H2A H -0.6452 -0.7808 -1.4356 0.025 Uiso 1 1 calc R . . H2B H -0.6682 -0.7433 -1.3615 0.025 Uiso 1 1 calc R . . C3 C -0.5167(2) -0.69618(12) -1.29942(19) 0.0208(6) Uani 1 1 d . . . H3A H -0.5546 -0.6720 -1.3526 0.025 Uiso 1 1 calc R . . H3B H -0.4489 -0.6837 -1.2797 0.025 Uiso 1 1 calc R . . C4 C -0.5519(2) -0.68450(11) -1.22382(19) 0.0198(6) Uani 1 1 d . . . H4A H -0.5329 -0.6440 -1.2004 0.024 Uiso 1 1 calc R . . H4B H -0.6228 -0.6864 -1.2485 0.024 Uiso 1 1 calc R . . C5 C -0.5918(2) -0.75016(12) -1.12161(19) 0.0210(6) Uani 1 1 d . . . H5A H -0.6262 -0.7163 -1.1086 0.025 Uiso 1 1 calc R . . H5B H -0.5642 -0.7740 -1.0658 0.025 Uiso 1 1 calc R . . C6 C -0.66274(19) -0.78793(12) -1.19597(19) 0.0209(6) Uani 1 1 d . . . H6A H -0.7071 -0.8072 -1.1719 0.025 Uiso 1 1 calc R . . H6B H -0.7013 -0.7617 -1.2462 0.025 Uiso 1 1 calc R . . C7 C -0.63704(19) -0.89385(12) -1.20456(19) 0.0188(5) Uani 1 1 d . . . H7A H -0.6173 -0.9246 -1.2380 0.023 Uiso 1 1 calc R . . H7B H -0.7068 -0.8979 -1.2200 0.023 Uiso 1 1 calc R . . C8 C -0.58479(18) -0.90331(11) -1.10449(18) 0.0167(5) Uani 1 1 d . . . C9 C -0.6205(2) -0.93932(13) -1.0544(2) 0.0231(6) Uani 1 1 d . . . H9 H -0.6819 -0.9570 -1.0818 0.028 Uiso 1 1 calc R . . C10 C -0.5660(2) -0.94922(14) -0.9640(2) 0.0266(6) Uani 1 1 d . . . H10 H -0.5896 -0.9735 -0.9285 0.032 Uiso 1 1 calc R . . C11 C -0.4762(2) -0.92305(13) -0.92595(19) 0.0219(6) Uani 1 1 d . . . H11 H -0.4375 -0.9291 -0.8640 0.026 Uiso 1 1 calc R . . C12 C -0.44397(18) -0.88782(11) -0.98012(18) 0.0160(5) Uani 1 1 d . . . C13 C -0.24371(19) -0.91726(12) -0.91335(19) 0.0195(6) Uani 1 1 d . . . C14 C -0.2021(2) -0.93735(14) -0.8239(2) 0.0268(6) Uani 1 1 d . . . H14 H -0.2152 -0.9176 -0.7774 0.032 Uiso 1 1 calc R . . C15 C -0.1419(2) -0.98596(15) -0.8033(2) 0.0336(8) Uani 1 1 d . . . H15 H -0.1145 -0.9996 -0.7427 0.040 Uiso 1 1 calc R . . C16 C -0.1215(2) -1.01447(15) -0.8687(3) 0.0351(8) Uani 1 1 d . . . H16 H -0.0795 -1.0475 -0.8533 0.042 Uiso 1 1 calc R . . C17 C -0.1618(2) -0.99545(14) -0.9583(2) 0.0303(7) Uani 1 1 d . . . H17 H -0.1477 -1.0155 -1.0040 0.036 Uiso 1 1 calc R . . C18 C -0.22284(19) -0.94700(13) -0.9802(2) 0.0216(6) Uani 1 1 d . . . H18 H -0.2506 -0.9340 -1.0411 0.026 Uiso 1 1 calc R . . C19 C -0.4770(2) -0.76712(12) -1.39158(19) 0.0202(6) Uani 1 1 d . . . H19A H -0.4134 -0.7477 -1.3678 0.024 Uiso 1 1 calc R B . H19B H -0.5159 -0.7477 -1.4494 0.024 Uiso 1 1 calc R . . C20 C -0.46459(19) -0.83109(12) -1.40853(18) 0.0183(5) Uani 1 1 d . B . C21 C -0.4539(2) -0.84951(14) -1.48703(19) 0.0246(6) Uani 1 1 d . . . H21 H -0.4590 -0.8218 -1.5334 0.030 Uiso 1 1 calc R B . C22 C -0.4358(2) -0.90852(15) -1.4972(2) 0.0300(7) Uani 1 1 d . B . H22 H -0.4296 -0.9221 -1.5510 0.036 Uiso 1 1 calc R . . C23 C -0.4268(2) -0.94742(13) -1.4277(2) 0.0248(6) Uani 1 1 d . . . H23 H -0.4136 -0.9881 -1.4325 0.030 Uiso 1 1 calc R B . C24 C -0.43742(18) -0.92588(12) -1.35077(18) 0.0176(5) Uani 1 1 d . B . C25B C -0.3070(2) -1.00643(18) -1.2192(3) 0.0168(14) Uiso 0.50 1 d PG B 1 C26B C -0.2952(3) -1.06715(18) -1.2061(4) 0.0232(15) Uiso 0.50 1 d PG B 1 H26 H -0.3483 -1.0913 -1.2101 0.028 Uiso 0.50 1 calc PR B 1 C27B C -0.2057(3) -1.09259(14) -1.1870(4) 0.0276(16) Uiso 0.50 1 d PG B 1 H27 H -0.1977 -1.1341 -1.1780 0.033 Uiso 0.50 1 calc PR B 1 C28A C -0.1281(2) -1.05731(18) -1.1811(3) 0.0268(14) Uiso 0.50 1 d PG B 1 H28 H -0.0669 -1.0747 -1.1680 0.032 Uiso 0.50 1 calc PR B 1 C29A C -0.1399(2) -0.99658(18) -1.1942(3) 0.0327(15) Uiso 0.50 1 d PG B 1 H29 H -0.0868 -0.9725 -1.1901 0.039 Uiso 0.50 1 calc PR B 1 C30A C -0.2294(3) -0.97114(14) -1.2133(3) 0.0240(13) Uiso 0.50 1 d PG B 1 H30 H -0.2374 -0.9296 -1.2222 0.029 Uiso 0.50 1 calc PR B 1 C31 C -0.4401(2) -0.69767(13) -1.06783(19) 0.0225(6) Uani 1 1 d . . . H31A H -0.4221 -0.7238 -1.0142 0.027 Uiso 1 1 calc R A . H31B H -0.4672 -0.6607 -1.0541 0.027 Uiso 1 1 calc R . . C32 C -0.3531(2) -0.68376(12) -1.0883(2) 0.0223(6) Uani 1 1 d . A . C33 C -0.2998(2) -0.63173(13) -1.0578(2) 0.0300(7) Uani 1 1 d . . . H33 H -0.3194 -0.6028 -1.0252 0.036 Uiso 1 1 calc R A . C34 C -0.2182(2) -0.62341(14) -1.0762(2) 0.0371(8) Uani 1 1 d . A . H34 H -0.1817 -0.5882 -1.0573 0.044 Uiso 1 1 calc R . . C35 C -0.1899(2) -0.66676(14) -1.1222(2) 0.0307(7) Uani 1 1 d . . . H35 H -0.1336 -0.6620 -1.1349 0.037 Uiso 1 1 calc R A . C36 C -0.2460(2) -0.71756(13) -1.14955(19) 0.0215(6) Uani 1 1 d . A . C37 C -0.1017(2) -0.80487(13) -1.1425(2) 0.0231(6) Uani 1 1 d . A . C38 C -0.0909(2) -0.84901(14) -1.0783(2) 0.0294(7) Uani 1 1 d . . . H38 H -0.1455 -0.8643 -1.0697 0.035 Uiso 1 1 calc R A . C39 C -0.0008(3) -0.87043(15) -1.0273(2) 0.0384(8) Uani 1 1 d . A . H39 H 0.0058 -0.9009 -0.9844 0.046 Uiso 1 1 calc R . . C40 C 0.0792(3) -0.84837(17) -1.0374(3) 0.0418(9) Uani 1 1 d . . . H40 H 0.1408 -0.8634 -1.0014 0.050 Uiso 1 1 calc R A . C41 C 0.0703(2) -0.80365(18) -1.1009(3) 0.0395(8) Uani 1 1 d . A . H41 H 0.1256 -0.7881 -1.1079 0.047 Uiso 1 1 calc R . . C42 C -0.0205(2) -0.78226(15) -1.1536(2) 0.0296(7) Uani 1 1 d . . . H42 H -0.0272 -0.7522 -1.1971 0.035 Uiso 1 1 calc R A . C25A C -0.2974(2) -1.00188(19) -1.2320(3) 0.0180(14) Uiso 0.50 1 d PG B 2 C30B C -0.2284(3) -0.96682(14) -1.2459(3) 0.0265(13) Uiso 0.50 1 d PG B 2 H30A H -0.2428 -0.9270 -1.2653 0.032 Uiso 0.50 1 calc PR B 2 C29B C -0.1384(3) -0.99001(17) -1.2313(3) 0.0315(14) Uiso 0.50 1 d PG B 2 H29A H -0.0912 -0.9661 -1.2408 0.038 Uiso 0.50 1 calc PR B 2 C28B C -0.1173(2) -1.04826(18) -1.2029(3) 0.0240(13) Uiso 0.50 1 d PG B 2 H28A H -0.0557 -1.0641 -1.1929 0.029 Uiso 0.50 1 calc PR B 2 C27A C -0.1862(3) -1.08331(15) -1.1890(3) 0.0197(13) Uiso 0.50 1 d PG B 2 H27A H -0.1718 -1.1231 -1.1696 0.024 Uiso 0.50 1 calc PR B 2 C26A C -0.2763(3) -1.06012(18) -1.2036(3) 0.0193(13) Uiso 0.50 1 d PG B 2 H26A H -0.3234 -1.0841 -1.1941 0.023 Uiso 0.50 1 calc PR B 2 O6A O -0.2235(3) -0.7451(2) -1.2964(3) 0.0220(10) Uiso 0.50 1 d P A 1 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 Eu1 0.01379(6) 0.01126(6) 0.01305(7) 0.00043(5) 0.00499(5) -0.00022(5) P1 0.0150(3) 0.0177(3) 0.0137(3) 0.0002(3) 0.0040(3) -0.0039(3) P2 0.0192(3) 0.0123(3) 0.0174(3) -0.0014(3) 0.0028(3) 0.0013(3) P3 0.0185(4) 0.0370(4) 0.0170(4) 0.0009(3) 0.0075(3) -0.0078(3) O1 0.0194(9) 0.0148(9) 0.0196(9) 0.0010(8) 0.0071(8) -0.0040(7) O2 0.0236(10) 0.0310(11) 0.0176(10) -0.0060(8) 0.0070(9) -0.0073(8) O3 0.0210(10) 0.0163(9) 0.0141(9) 0.0010(7) 0.0060(8) 0.0012(7) O4 0.0282(11) 0.0146(10) 0.0282(11) 0.0010(8) 0.0042(9) -0.0029(8) O5 0.0229(10) 0.0333(11) 0.0274(11) -0.0130(9) 0.0146(9) -0.0122(9) N1 0.0144(10) 0.0204(12) 0.0148(11) 0.0013(9) 0.0045(9) 0.0012(8) N2 0.0168(11) 0.0151(11) 0.0165(11) 0.0026(9) 0.0046(10) 0.0023(8) N3 0.0180(11) 0.0152(11) 0.0173(12) 0.0004(9) 0.0044(10) 0.0016(9) N4 0.0135(10) 0.0148(10) 0.0142(11) -0.0002(8) 0.0055(9) -0.0003(8) N5 0.0151(11) 0.0158(11) 0.0138(11) -0.0015(8) 0.0028(9) 0.0004(8) N6 0.0193(11) 0.0171(11) 0.0153(11) 0.0035(9) 0.0020(10) -0.0020(9) C1 0.0158(12) 0.0225(14) 0.0161(13) 0.0002(11) 0.0034(11) 0.0007(10) C2 0.0182(13) 0.0238(14) 0.0176(14) 0.0011(11) 0.0037(12) 0.0031(11) C3 0.0236(14) 0.0148(12) 0.0196(14) 0.0041(11) 0.0031(12) 0.0021(11) C4 0.0214(13) 0.0125(13) 0.0232(14) 0.0010(10) 0.0059(12) 0.0049(10) C5 0.0241(14) 0.0187(13) 0.0218(15) -0.0009(11) 0.0104(12) 0.0021(11) C6 0.0201(13) 0.0203(14) 0.0240(15) 0.0013(11) 0.0103(12) 0.0036(11) C7 0.0153(13) 0.0176(13) 0.0210(14) -0.0003(11) 0.0042(11) -0.0012(10) C8 0.0160(13) 0.0146(12) 0.0188(14) 0.0016(10) 0.0059(11) 0.0000(10) C9 0.0164(13) 0.0242(15) 0.0271(16) 0.0023(12) 0.0063(12) -0.0058(11) C10 0.0250(15) 0.0326(17) 0.0234(15) 0.0065(12) 0.0105(13) -0.0074(12) C11 0.0214(14) 0.0266(15) 0.0157(14) 0.0032(11) 0.0048(12) -0.0023(11) C12 0.0159(12) 0.0146(12) 0.0175(13) 0.0005(10) 0.0063(11) 0.0001(10) C13 0.0149(13) 0.0184(13) 0.0227(15) 0.0036(11) 0.0043(11) -0.0043(10) C14 0.0243(15) 0.0276(16) 0.0212(15) 0.0018(12) 0.0003(13) -0.0063(12) C15 0.0246(16) 0.0308(17) 0.0299(18) 0.0104(14) -0.0073(14) -0.0040(13) C16 0.0163(14) 0.0263(16) 0.051(2) 0.0046(15) -0.0002(15) 0.0000(12) C17 0.0215(15) 0.0273(16) 0.042(2) 0.0037(14) 0.0122(14) 0.0022(12) C18 0.0174(13) 0.0212(14) 0.0250(15) 0.0058(11) 0.0065(12) -0.0015(11) C19 0.0204(14) 0.0222(14) 0.0165(14) 0.0049(11) 0.0053(12) 0.0023(11) C20 0.0157(12) 0.0218(14) 0.0147(13) -0.0008(11) 0.0028(11) -0.0012(10) C21 0.0262(15) 0.0307(16) 0.0170(14) 0.0040(12) 0.0083(13) 0.0049(12) C22 0.0350(17) 0.0366(18) 0.0200(15) -0.0055(13) 0.0122(14) 0.0046(14) C23 0.0272(15) 0.0238(15) 0.0221(15) -0.0066(12) 0.0080(13) 0.0033(12) C24 0.0141(12) 0.0194(13) 0.0173(13) -0.0015(10) 0.0037(11) -0.0008(10) C31 0.0278(15) 0.0174(13) 0.0204(15) -0.0050(11) 0.0068(13) 0.0011(11) C32 0.0206(14) 0.0162(14) 0.0212(14) 0.0014(11) -0.0020(12) -0.0034(10) C33 0.0320(17) 0.0145(14) 0.0295(17) 0.0019(12) -0.0042(14) -0.0003(12) C34 0.0307(17) 0.0194(15) 0.045(2) 0.0072(14) -0.0041(16) -0.0080(13) C35 0.0219(15) 0.0279(17) 0.0322(17) 0.0144(13) -0.0009(13) -0.0056(12) C36 0.0190(13) 0.0217(14) 0.0170(14) 0.0103(11) -0.0007(12) -0.0016(11) C37 0.0263(15) 0.0215(14) 0.0228(15) -0.0035(11) 0.0109(13) -0.0035(11) C38 0.0377(18) 0.0225(15) 0.0266(17) -0.0003(13) 0.0108(15) -0.0078(13) C39 0.056(2) 0.0247(17) 0.0331(19) 0.0062(14) 0.0150(18) 0.0092(15) C40 0.042(2) 0.038(2) 0.041(2) 0.0055(16) 0.0108(18) 0.0200(16) C41 0.0258(17) 0.050(2) 0.042(2) 0.0029(17) 0.0128(16) 0.0078(15) C42 0.0238(15) 0.0307(17) 0.0353(18) 0.0042(14) 0.0125(14) 0.0002(12) _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 Eu1 P1 3.5557(7) . ? Eu1 P2 3.5480(7) . ? Eu1 P3 3.5291(7) . ? Eu1 O1 2.3385(19) . ? Eu1 O3 2.3359(18) . ? Eu1 O5 2.3213(19) . ? Eu1 N1 2.657(2) . ? Eu1 N2 2.699(2) . ? Eu1 N3 2.675(2) . ? Eu1 N4 2.658(2) . ? Eu1 N5 2.678(2) . ? Eu1 N6 2.650(2) . ? P1 O1 1.5137(19) . ? P1 O2 1.494(2) . ? P1 C12 1.825(3) . ? P1 C13 1.801(3) . ? P2 O3 1.5154(19) . ? P2 O4 1.497(2) . ? P2 C24 1.824(3) . ? P2 C25B 1.762(3) . ? P2 C25A 1.878(3) . ? P3 O5 1.506(2) . ? P3 O6B 1.496(4) . ? P3 C36 1.815(3) . ? P3 C37 1.802(3) . ? P3 O6A 1.540(5) . ? N1 C1 1.492(3) . ? N1 C6 1.502(3) . ? N1 C7 1.477(3) . ? N2 C2 1.508(3) . ? N2 C3 1.477(3) . ? N2 C19 1.489(3) . ? N3 C4 1.501(3) . ? N3 C5 1.481(3) . ? N3 C31 1.492(4) . ? N4 C8 1.344(3) . ? N4 C12 1.354(3) . ? N5 C20 1.345(3) . ? N5 C24 1.339(3) . ? N6 C32 1.331(4) . ? N6 C36 1.346(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 C2 1.518(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.515(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.524(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.507(4) . ? C8 C9 1.386(4) . ? C9 H9 0.9500 . ? C9 C10 1.383(4) . ? C10 H10 0.9500 . ? C10 C11 1.389(4) . ? C11 H11 0.9500 . ? C11 C12 1.393(4) . ? C13 C14 1.402(4) . ? C13 C18 1.395(4) . ? C14 H14 0.9500 . ? C14 C15 1.383(4) . ? C15 H15 0.9500 . ? C15 C16 1.359(5) . ? C16 H16 0.9500 . ? C16 C17 1.396(5) . ? C17 H17 0.9500 . ? C17 C18 1.387(4) . ? C18 H18 0.9500 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19 C20 1.496(4) . ? C20 C21 1.388(4) . ? C21 H21 0.9500 . ? C21 C22 1.383(4) . ? C22 H22 0.9500 . ? C22 C23 1.383(4) . ? C23 H23 0.9500 . ? C23 C24 1.387(4) . ? C25B C26B 1.3900 . ? C25B C30A 1.3900 . ? C26B H26 0.9500 . ? C26B C27B 1.3900 . ? C27B H27 0.9500 . ? C27B C28A 1.3900 . ? C28A H28 0.9500 . ? C28A C29A 1.3900 . ? C29A H29 0.9500 . ? C29A C30A 1.3900 . ? C30A H30 0.9500 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C31 C32 1.501(4) . ? C32 C33 1.404(4) . ? C33 H33 0.9500 . ? C33 C34 1.380(5) . ? C34 H34 0.9500 . ? C34 C35 1.387(5) . ? C35 H35 0.9500 . ? C35 C36 1.395(4) . ? C37 C38 1.396(4) . ? C37 C42 1.398(4) . ? C38 H38 0.9500 . ? C38 C39 1.380(5) . ? C39 H39 0.9500 . ? C39 C40 1.371(5) . ? C40 H40 0.9500 . ? C40 C41 1.402(5) . ? C41 H41 0.9500 . ? C41 C42 1.394(5) . ? C42 H42 0.9500 . ? C25A C30B 1.3900 . ? C25A C26A 1.3900 . ? C30B H30A 0.9500 . ? C30B C29B 1.3900 . ? C29B H29A 0.9500 . ? C29B C28B 1.3900 . ? C28B H28A 0.9500 . ? C28B C27A 1.3900 . ? C27A H27A 0.9500 . ? C27A C26A 1.3900 . ? C26A H26A 0.9500 . ? 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 P2 Eu1 P1 96.363(16) . . ? P3 Eu1 P1 99.109(17) . . ? P3 Eu1 P2 94.734(18) . . ? O1 Eu1 P1 17.96(4) . . ? O1 Eu1 P2 103.41(5) . . ? O1 Eu1 P3 82.07(5) . . ? O1 Eu1 N1 124.53(7) . . ? O1 Eu1 N2 147.79(7) . . ? O1 Eu1 N3 90.63(7) . . ? O1 Eu1 N4 66.25(6) . . ? O1 Eu1 N5 142.92(7) . . ? O1 Eu1 N6 68.64(7) . . ? O3 Eu1 P1 78.84(5) . . ? O3 Eu1 P2 18.18(4) . . ? O3 Eu1 P3 102.17(5) . . ? O3 Eu1 O1 87.92(6) . . ? O3 Eu1 N1 89.50(7) . . ? O3 Eu1 N2 123.86(7) . . ? O3 Eu1 N3 149.58(7) . . ? O3 Eu1 N4 66.99(6) . . ? O3 Eu1 N5 66.47(6) . . ? O3 Eu1 N6 143.22(7) . . ? O5 Eu1 P1 100.37(5) . . ? O5 Eu1 P2 76.66(5) . . ? O5 Eu1 P3 18.08(5) . . ? O5 Eu1 O1 85.90(7) . . ? O5 Eu1 O3 84.69(7) . . ? O5 Eu1 N1 148.84(7) . . ? O5 Eu1 N2 91.55(7) . . ? O5 Eu1 N3 125.53(7) . . ? O5 Eu1 N4 140.00(7) . . ? O5 Eu1 N5 66.24(7) . . ? O5 Eu1 N6 66.36(7) . . ? N1 Eu1 P1 108.49(5) . . ? N1 Eu1 P2 88.50(5) . . ? N1 Eu1 P3 151.69(5) . . ? N1 Eu1 N2 66.60(7) . . ? N1 Eu1 N3 66.58(7) . . ? N1 Eu1 N4 61.98(7) . . ? N1 Eu1 N5 83.36(7) . . ? N2 Eu1 P1 155.53(5) . . ? N2 Eu1 P2 107.21(5) . . ? N2 Eu1 P3 85.66(5) . . ? N3 Eu1 P1 90.81(5) . . ? N3 Eu1 P2 155.05(5) . . ? N3 Eu1 P3 107.72(5) . . ? N3 Eu1 N2 65.01(7) . . ? N3 Eu1 N5 125.12(7) . . ? N4 Eu1 P1 48.45(5) . . ? N4 Eu1 P2 82.38(5) . . ? N4 Eu1 P3 146.32(5) . . ? N4 Eu1 N2 127.37(7) . . ? N4 Eu1 N3 84.67(7) . . ? N4 Eu1 N5 120.92(7) . . ? N5 Eu1 P1 143.40(5) . . ? N5 Eu1 P2 48.34(5) . . ? N5 Eu1 P3 78.03(5) . . ? N5 Eu1 N2 61.07(7) . . ? N6 Eu1 P1 84.39(5) . . ? N6 Eu1 P2 142.45(5) . . ? N6 Eu1 P3 48.52(5) . . ? N6 Eu1 N1 127.01(7) . . ? N6 Eu1 N2 80.93(7) . . ? N6 Eu1 N3 61.95(7) . . ? N6 Eu1 N4 122.45(7) . . ? N6 Eu1 N5 116.63(7) . . ? O1 P1 C12 103.72(11) . . ? O1 P1 C13 109.11(12) . . ? O2 P1 O1 118.53(12) . . ? O2 P1 C12 110.35(12) . . ? O2 P1 C13 109.37(13) . . ? C13 P1 C12 104.83(12) . . ? O3 P2 C24 104.03(12) . . ? O3 P2 C25B 107.98(18) . . ? O3 P2 C25A 110.73(17) . . ? O4 P2 O3 117.01(12) . . ? O4 P2 C24 110.67(12) . . ? O4 P2 C25B 108.32(16) . . ? O4 P2 C25A 113.12(16) . . ? C24 P2 C25A 99.43(16) . . ? C25B P2 C24 108.51(18) . . ? C25B P2 C25A 9.1(2) . . ? O5 P3 C36 103.71(12) . . ? O5 P3 C37 108.37(14) . . ? O5 P3 O6A 122.6(2) . . ? O6B P3 O5 112.6(2) . . ? O6B P3 C36 118.0(2) . . ? O6B P3 C37 106.8(2) . . ? O6B P3 O6A 18.4(2) . . ? C37 P3 C36 106.99(13) . . ? O6A P3 C36 99.7(2) . . ? O6A P3 C37 113.47(19) . . ? P1 O1 Eu1 133.60(10) . . ? P2 O3 Eu1 133.08(11) . . ? P3 O5 Eu1 133.34(12) . . ? C1 N1 Eu1 106.56(15) . . ? C1 N1 C6 110.5(2) . . ? C6 N1 Eu1 113.76(16) . . ? C7 N1 Eu1 107.45(15) . . ? C7 N1 C1 108.6(2) . . ? C7 N1 C6 109.8(2) . . ? C2 N2 Eu1 113.05(15) . . ? C3 N2 Eu1 108.40(16) . . ? C3 N2 C2 109.6(2) . . ? C3 N2 C19 108.2(2) . . ? C19 N2 Eu1 107.86(15) . . ? C19 N2 C2 109.7(2) . . ? C4 N3 Eu1 116.46(15) . . ? C5 N3 Eu1 105.14(15) . . ? C5 N3 C4 110.2(2) . . ? C5 N3 C31 109.4(2) . . ? C31 N3 Eu1 105.92(15) . . ? C31 N3 C4 109.4(2) . . ? C8 N4 Eu1 118.45(17) . . ? C8 N4 C12 118.7(2) . . ? C12 N4 Eu1 121.91(16) . . ? C20 N5 Eu1 118.09(17) . . ? C24 N5 Eu1 120.71(17) . . ? C24 N5 C20 118.6(2) . . ? C32 N6 Eu1 118.72(18) . . ? C32 N6 C36 119.4(2) . . ? C36 N6 Eu1 121.76(18) . . ? N1 C1 H1A 109.0 . . ? N1 C1 H1B 109.0 . . ? N1 C1 C2 112.9(2) . . ? H1A C1 H1B 107.8 . . ? C2 C1 H1A 109.0 . . ? C2 C1 H1B 109.0 . . ? N2 C2 C1 114.6(2) . . ? N2 C2 H2A 108.6 . . ? N2 C2 H2B 108.6 . . ? C1 C2 H2A 108.6 . . ? C1 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? N2 C3 H3A 109.1 . . ? N2 C3 H3B 109.1 . . ? N2 C3 C4 112.5(2) . . ? H3A C3 H3B 107.8 . . ? C4 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? N3 C4 C3 113.2(2) . . ? N3 C4 H4A 108.9 . . ? N3 C4 H4B 108.9 . . ? C3 C4 H4A 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.8 . . ? N3 C5 H5A 109.2 . . ? N3 C5 H5B 109.2 . . ? N3 C5 C6 112.1(2) . . ? H5A C5 H5B 107.9 . . ? C6 C5 H5A 109.2 . . ? C6 C5 H5B 109.2 . . ? N1 C6 C5 114.2(2) . . ? N1 C6 H6A 108.7 . . ? N1 C6 H6B 108.7 . . ? C5 C6 H6A 108.7 . . ? C5 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? N1 C7 H7A 109.3 . . ? N1 C7 H7B 109.3 . . ? N1 C7 C8 111.5(2) . . ? H7A C7 H7B 108.0 . . ? C8 C7 H7A 109.3 . . ? C8 C7 H7B 109.3 . . ? N4 C8 C7 115.4(2) . . ? N4 C8 C9 122.1(2) . . ? C9 C8 C7 122.4(2) . . ? C8 C9 H9 120.3 . . ? C10 C9 C8 119.5(3) . . ? C10 C9 H9 120.3 . . ? C9 C10 H10 120.5 . . ? C9 C10 C11 118.9(3) . . ? C11 C10 H10 120.5 . . ? C10 C11 H11 120.6 . . ? C10 C11 C12 118.9(3) . . ? C12 C11 H11 120.6 . . ? N4 C12 P1 113.96(18) . . ? N4 C12 C11 121.9(2) . . ? C11 C12 P1 124.0(2) . . ? C14 C13 P1 120.9(2) . . ? C18 C13 P1 120.3(2) . . ? C18 C13 C14 118.8(3) . . ? C13 C14 H14 120.0 . . ? C15 C14 C13 120.0(3) . . ? C15 C14 H14 120.0 . . ? C14 C15 H15 119.6 . . ? C16 C15 C14 120.9(3) . . ? C16 C15 H15 119.6 . . ? C15 C16 H16 119.8 . . ? C15 C16 C17 120.4(3) . . ? C17 C16 H16 119.8 . . ? C16 C17 H17 120.3 . . ? C18 C17 C16 119.5(3) . . ? C18 C17 H17 120.3 . . ? C13 C18 H18 119.8 . . ? C17 C18 C13 120.5(3) . . ? C17 C18 H18 119.8 . . ? N2 C19 H19A 109.3 . . ? N2 C19 H19B 109.3 . . ? N2 C19 C20 111.8(2) . . ? H19A C19 H19B 107.9 . . ? C20 C19 H19A 109.3 . . ? C20 C19 H19B 109.3 . . ? N5 C20 C19 116.8(2) . . ? N5 C20 C21 121.8(3) . . ? C21 C20 C19 121.3(3) . . ? C20 C21 H21 120.3 . . ? C22 C21 C20 119.4(3) . . ? C22 C21 H21 120.3 . . ? C21 C22 H22 120.6 . . ? C21 C22 C23 118.8(3) . . ? C23 C22 H22 120.6 . . ? C22 C23 H23 120.7 . . ? C22 C23 C24 118.7(3) . . ? C24 C23 H23 120.7 . . ? N5 C24 P2 114.24(19) . . ? N5 C24 C23 122.7(3) . . ? C23 C24 P2 122.9(2) . . ? C26B C25B P2 122.8(2) . . ? C26B C25B C30A 120.0 . . ? C30A C25B P2 117.1(2) . . ? C25B C26B H26 120.0 . . ? C25B C26B C27B 120.0 . . ? C27B C26B H26 120.0 . . ? C26B C27B H27 120.0 . . ? C28A C27B C26B 120.0 . . ? C28A C27B H27 120.0 . . ? C27B C28A H28 120.0 . . ? C29A C28A C27B 120.0 . . ? C29A C28A H28 120.0 . . ? C28A C29A H29 120.0 . . ? C28A C29A C30A 120.0 . . ? C30A C29A H29 120.0 . . ? C25B C30A H30 120.0 . . ? C29A C30A C25B 120.0 . . ? C29A C30A H30 120.0 . . ? N3 C31 H31A 109.7 . . ? N3 C31 H31B 109.7 . . ? N3 C31 C32 109.6(2) . . ? H31A C31 H31B 108.2 . . ? C32 C31 H31A 109.7 . . ? C32 C31 H31B 109.7 . . ? N6 C32 C31 115.9(2) . . ? N6 C32 C33 121.9(3) . . ? C33 C32 C31 122.2(3) . . ? C32 C33 H33 120.7 . . ? C34 C33 C32 118.7(3) . . ? C34 C33 H33 120.7 . . ? C33 C34 H34 120.2 . . ? C33 C34 C35 119.6(3) . . ? C35 C34 H34 120.2 . . ? C34 C35 H35 120.8 . . ? C34 C35 C36 118.4(3) . . ? C36 C35 H35 120.8 . . ? N6 C36 P3 113.9(2) . . ? N6 C36 C35 122.0(3) . . ? C35 C36 P3 124.1(2) . . ? C38 C37 P3 119.9(2) . . ? C38 C37 C42 119.3(3) . . ? C42 C37 P3 120.7(2) . . ? C37 C38 H38 120.0 . . ? C39 C38 C37 120.0(3) . . ? C39 C38 H38 120.0 . . ? C38 C39 H39 119.5 . . ? C40 C39 C38 121.0(3) . . ? C40 C39 H39 119.5 . . ? C39 C40 H40 120.0 . . ? C39 C40 C41 120.0(3) . . ? C41 C40 H40 120.0 . . ? C40 C41 H41 120.3 . . ? C42 C41 C40 119.4(3) . . ? C42 C41 H41 120.3 . . ? C37 C42 H42 119.9 . . ? C41 C42 C37 120.2(3) . . ? C41 C42 H42 119.9 . . ? C30B C25A P2 120.7(2) . . ? C30B C25A C26A 120.0 . . ? C26A C25A P2 119.3(2) . . ? C25A C30B H30A 120.0 . . ? C25A C30B C29B 120.0 . . ? C29B C30B H30A 120.0 . . ? C30B C29B H29A 120.0 . . ? C30B C29B C28B 120.0 . . ? C28B C29B H29A 120.0 . . ? C29B C28B H28A 120.0 . . ? C27A C28B C29B 120.0 . . ? C27A C28B H28A 120.0 . . ? C28B C27A H27A 120.0 . . ? C28B C27A C26A 120.0 . . ? C26A C27A H27A 120.0 . . ? C25A C26A H26A 120.0 . . ? C27A C26A C25A 120.0 . . ? C27A C26A H26A 120.0 . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.588 -0.104 -0.088 1502.7 81.1 ? # start Validation Reply Form _vrf_PLAT602_I ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: The structure contains a number of severely disordered solvent molecules (H2O, methanol). Their contribution to the structural fctors was taken into account by applying MASK procedure of OLEX2 program package. ; _vrf_PLAT029_I ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.905 RESPONSE: This value is 0.966 for the theta equal to 28.00. There is no point to loose a number of reflections in order to satisfy some formal criteria. ; # end Validation Reply Form # Attachment '6391_web_deposit_cif_file_1_DmitryYufit_1311257364.HoL3.cif' data__HoL3_11srv130a _database_code_depnum_ccdc_archive 'CCDC 836098' #TrackingRef '6391_web_deposit_cif_file_1_DmitryYufit_1311257364.HoL3.cif' _audit_creation_date 2011-07-07 _audit_creation_method ; Olex2 1.1-beta (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H42 Ho N6 O6 P3' _chemical_formula_sum 'C42 H42 Ho N6 O6 P3' _chemical_formula_weight 984.66 _chemical_melting_point ? 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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.0447(3) _cell_length_b 22.5125(5) _cell_length_c 15.8446(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.163(10) _cell_angle_gamma 90.00 _cell_volume 4969.96(36) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7843 _cell_measurement_temperature 120 _cell_measurement_theta_max 30.85 _cell_measurement_theta_min 2.28 _exptl_absorpt_coefficient_mu 1.735 _exptl_absorpt_correction_T_max 0.7458 _exptl_absorpt_correction_T_min 0.4965 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2006/1 (Bruker,2006) was used for absorption correction. R(int) was 0.0502 before and 0.0319 after correction. The Ratio of minimum to maximum transmission is 0.665728077233. The \l/2 correction factor is 0.0015 ; _exptl_crystal_colour colourless _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1984 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_special_details ; The data collection nominally covered a full sphere of reciprocal space by a combination of 5 sets of \w scans each set at different \f and/or 2\q angles and each scan (15.00 s exposure) covering -0.200\ degrees in \w. The crystal to detector distance was 4.85 cm. ; _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_unetI/netI 0.0288 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 65106 _diffrn_reflns_theta_full 29.00 _diffrn_reflns_theta_max 29.0 _diffrn_reflns_theta_min 1.59 _diffrn_ambient_temperature 120 _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 5.6 _diffrn_detector_type 'Bruker SMART CCD 6000 area detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART CCD 6000 area detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_xray_symbol K-L~3~ _diffrn_source 'sealed X-ray tube' _diffrn_source_current 35.0 _diffrn_source_power 1.75 _diffrn_source_target Mo _diffrn_source_voltage 50.0 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 10883 _reflns_number_total 13212 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'SAINT v6.45A (Bruker, 2003)' _computing_data_collection 'SMART v5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT v6.45A (Bruker, 2003)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)/Bruker' _refine_diff_density_max 2.149 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.086 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 492 _refine_ls_number_reflns 13212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0286 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.0709 _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. The structure contains a number of severely disordered solvent molecules (H2O, methanol). Their contribution to the structural fctors was taken into account by applying MASK procedure of OLEX2 program package. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Ho1 Ho 0.071776(7) 0.676267(4) 0.321079(7) 0.01878(3) Uani 1 1 d . A . P1 P 0.17435(4) 0.64653(3) 0.55638(4) 0.02076(11) Uani 1 1 d . . . P2 P 0.08146(4) 0.52992(3) 0.24893(4) 0.02307(12) Uani 1 1 d . . . P3 P 0.27813(5) 0.72100(4) 0.28742(4) 0.03213(15) Uani 1 1 d . . . O1 O 0.17704(11) 0.67413(7) 0.47014(11) 0.0212(3) Uani 1 1 d . . . O2 O 0.19221(13) 0.68551(8) 0.63787(12) 0.0284(4) Uani 1 1 d . . . O3 O 0.08622(12) 0.57491(7) 0.32130(11) 0.0235(3) Uani 1 1 d . A . O4 O 0.00649(13) 0.48249(8) 0.22912(13) 0.0321(4) Uani 1 1 d . B . O5 O 0.20646(13) 0.67457(9) 0.28752(13) 0.0331(4) Uani 1 1 d . A . O6A O 0.2736(3) 0.75352(19) 0.2004(2) 0.0245(8) Uiso 0.50 1 d P A 2 O6B O 0.2778(3) 0.7310(2) 0.1939(3) 0.0297(9) Uiso 0.50 1 d P A 1 N1 N -0.11556(14) 0.66519(8) 0.26519(13) 0.0214(4) Uani 1 1 d . . . N2 N -0.02291(14) 0.74159(9) 0.17348(13) 0.0224(4) Uani 1 1 d . A . N3 N -0.01311(14) 0.77157(9) 0.35395(13) 0.0225(4) Uani 1 1 d . A . N4 N 0.00147(13) 0.62294(8) 0.43045(12) 0.0193(4) Uani 1 1 d . . . N5 N 0.04331(13) 0.63244(9) 0.15771(13) 0.0218(4) Uani 1 1 d . . . N6 N 0.17236(14) 0.77413(9) 0.36687(13) 0.0250(4) Uani 1 1 d . . . C1 C -0.15442(16) 0.66787(11) 0.16416(15) 0.0232(5) Uani 1 1 d . . . H1A H -0.2238 0.6648 0.1415 0.028 Uiso 1 1 calc R . . H1B H -0.1304 0.6342 0.1409 0.028 Uiso 1 1 calc R . . C2 C -0.12723(17) 0.72480(11) 0.12859(16) 0.0248(5) Uani 1 1 d . . . H2A H -0.1430 0.7206 0.0636 0.030 Uiso 1 1 calc R . . H2B H -0.1659 0.7570 0.1371 0.030 Uiso 1 1 calc R . . C3 C -0.01471(18) 0.80502(11) 0.20129(16) 0.0256(5) Uani 1 1 d . . . H3A H -0.0514 0.8292 0.1491 0.031 Uiso 1 1 calc R . . H3B H 0.0519 0.8172 0.2215 0.031 Uiso 1 1 calc R . . C4 C -0.05112(18) 0.81557(10) 0.27762(16) 0.0258(5) Uani 1 1 d . . . H4A H -0.0328 0.8552 0.3018 0.031 Uiso 1 1 calc R . . H4B H -0.1207 0.8136 0.2526 0.031 Uiso 1 1 calc R . . C5 C -0.09163(17) 0.74883(11) 0.37931(16) 0.0259(5) Uani 1 1 d . . . H5A H -0.1256 0.7820 0.3923 0.031 Uiso 1 1 calc R . . H5B H -0.0648 0.7250 0.4342 0.031 Uiso 1 1 calc R . . C6 C -0.16239(17) 0.71103(11) 0.30297(17) 0.0256(5) Uani 1 1 d . . . H6A H -0.2058 0.6913 0.3262 0.031 Uiso 1 1 calc R . . H6B H -0.2005 0.7371 0.2539 0.031 Uiso 1 1 calc R . . C7 C -0.13594(16) 0.60532(10) 0.29272(15) 0.0229(4) Uani 1 1 d . . . H7A H -0.1156 0.5753 0.2599 0.027 Uiso 1 1 calc R . . H7B H -0.2045 0.6009 0.2768 0.027 Uiso 1 1 calc R . . C8 C -0.08450(15) 0.59626(10) 0.39335(15) 0.0209(4) Uani 1 1 d . . . C9 C -0.12017(17) 0.55981(11) 0.44422(17) 0.0262(5) Uani 1 1 d . . . H9 H -0.1799 0.5418 0.4171 0.031 Uiso 1 1 calc R . . C10 C -0.06569(18) 0.55067(12) 0.53571(17) 0.0298(5) Uani 1 1 d . . . H10 H -0.0885 0.5266 0.5709 0.036 Uiso 1 1 calc R . . C11 C 0.02320(17) 0.57789(11) 0.57413(16) 0.0259(5) Uani 1 1 d . . . H11 H 0.0608 0.5727 0.6355 0.031 Uiso 1 1 calc R . . C12 C 0.05513(16) 0.61307(10) 0.51932(15) 0.0212(4) Uani 1 1 d . . . C13 C 0.25583(16) 0.58417(11) 0.58852(16) 0.0237(5) Uani 1 1 d . . . C14 C 0.29543(17) 0.56505(12) 0.67935(17) 0.0292(5) Uani 1 1 d . . . H14 H 0.2812 0.5850 0.7241 0.035 Uiso 1 1 calc R . . C15 C 0.35588(19) 0.51623(13) 0.7021(2) 0.0383(7) Uani 1 1 d . . . H15 H 0.3821 0.5035 0.7623 0.046 Uiso 1 1 calc R . . C16 C 0.37753(19) 0.48641(13) 0.6369(2) 0.0398(7) Uani 1 1 d . . . H16 H 0.4179 0.4535 0.6531 0.048 Uiso 1 1 calc R . . C17 C 0.33934(18) 0.50513(12) 0.5463(2) 0.0337(6) Uani 1 1 d . . . H17 H 0.3548 0.4852 0.5023 0.040 Uiso 1 1 calc R . . C18 C 0.27815(17) 0.55357(11) 0.52252(17) 0.0273(5) Uani 1 1 d . . . H18 H 0.2517 0.5658 0.4620 0.033 Uiso 1 1 calc R . . C19 C 0.02495(17) 0.73426(11) 0.10770(16) 0.0248(5) Uani 1 1 d . . . H19A H 0.0875 0.7531 0.1317 0.030 Uiso 1 1 calc R B . H19B H -0.0129 0.7537 0.0509 0.030 Uiso 1 1 calc R . . C20 C 0.03662(16) 0.67011(11) 0.08999(16) 0.0236(5) Uani 1 1 d . B . C21 C 0.04687(18) 0.65158(13) 0.01010(17) 0.0303(5) Uani 1 1 d . . . H21 H 0.0423 0.6787 -0.0356 0.036 Uiso 1 1 calc R B . C22 C 0.0639(2) 0.59215(13) 0.00018(18) 0.0356(6) Uani 1 1 d . B . H22 H 0.0696 0.5786 -0.0530 0.043 Uiso 1 1 calc R . . C23 C 0.07250(19) 0.55300(12) 0.07045(17) 0.0309(5) Uani 1 1 d . . . H23 H 0.0848 0.5129 0.0655 0.037 Uiso 1 1 calc R B . C24 C 0.06241(16) 0.57480(11) 0.14814(16) 0.0234(5) Uani 1 1 d . B . C25A C 0.20315(19) 0.50027(15) 0.2683(3) 0.0190(11) Uiso 0.50 1 d PG B 2 C30B C 0.2710(2) 0.53478(12) 0.2511(3) 0.0270(10) Uiso 0.50 1 d PG B 2 H30 H 0.2563 0.5735 0.2301 0.032 Uiso 0.50 1 calc PR B 2 C29B C 0.3611(2) 0.51140(14) 0.2652(3) 0.0321(11) Uiso 0.50 1 d PG B 2 H29 H 0.4065 0.5345 0.2537 0.039 Uiso 0.50 1 calc PR B 2 C28B C 0.38316(19) 0.45349(15) 0.2966(3) 0.0255(10) Uiso 0.50 1 d PG B 2 H28 H 0.4434 0.4378 0.3061 0.031 Uiso 0.50 1 calc PR B 2 C27A C 0.3153(3) 0.41898(12) 0.3138(3) 0.0222(10) Uiso 0.50 1 d PG B 2 H27 H 0.3301 0.3802 0.3348 0.027 Uiso 0.50 1 calc PR B 2 C26A C 0.2253(2) 0.44237(15) 0.2997(3) 0.0222(10) Uiso 0.50 1 d PG B 2 H26 H 0.1798 0.4193 0.3112 0.027 Uiso 0.50 1 calc PR B 2 C25B C 0.1944(2) 0.49419(18) 0.2811(3) 0.0267(13) Uiso 0.50 1 d PG B 1 C26B C 0.2075(3) 0.43344(17) 0.2965(3) 0.0343(14) Uiso 0.50 1 d PG B 1 H26A H 0.1562 0.4097 0.2944 0.041 Uiso 0.50 1 calc PR B 1 C27B C 0.2972(3) 0.40825(14) 0.3149(3) 0.0361(14) Uiso 0.50 1 d PG B 1 H27A H 0.3059 0.3676 0.3252 0.043 Uiso 0.50 1 calc PR B 1 C28A C 0.3739(2) 0.44380(18) 0.3179(3) 0.0370(13) Uiso 0.50 1 d PG B 1 H28A H 0.4339 0.4269 0.3303 0.044 Uiso 0.50 1 calc PR B 1 C29A C 0.3609(2) 0.50455(17) 0.3026(3) 0.0463(15) Uiso 0.50 1 d PG B 1 H29A H 0.4122 0.5283 0.3046 0.056 Uiso 0.50 1 calc PR B 1 C30A C 0.2711(3) 0.52975(14) 0.2842(3) 0.0377(13) Uiso 0.50 1 d PG B 1 H30A H 0.2624 0.5704 0.2739 0.045 Uiso 0.50 1 calc PR B 1 C31 C 0.05942(19) 0.80137(11) 0.43358(16) 0.0280(5) Uani 1 1 d . . . H31A H 0.0772 0.7755 0.4863 0.034 Uiso 1 1 calc R A . H31B H 0.0325 0.8375 0.4474 0.034 Uiso 1 1 calc R . . C32 C 0.14682(19) 0.81607(11) 0.41352(17) 0.0289(5) Uani 1 1 d . A . C33 C 0.1993(2) 0.86812(12) 0.44239(19) 0.0381(7) Uani 1 1 d . . . H33 H 0.1800 0.8967 0.4743 0.046 Uiso 1 1 calc R A . C34 C 0.2804(2) 0.87682(13) 0.4230(2) 0.0446(8) Uani 1 1 d . A . H34 H 0.3159 0.9116 0.4411 0.054 Uiso 1 1 calc R . . C35 C 0.3084(2) 0.83333(13) 0.3762(2) 0.0393(7) Uani 1 1 d . . . H35 H 0.3633 0.8380 0.3632 0.047 Uiso 1 1 calc R A . C36 C 0.25220(18) 0.78240(11) 0.34915(17) 0.0299(5) Uani 1 1 d . A . C37 C 0.39642(18) 0.69430(12) 0.35515(17) 0.0298(5) Uani 1 1 d . A . C38 C 0.4076(2) 0.65002(13) 0.41973(19) 0.0362(6) Uani 1 1 d . . . H38 H 0.3542 0.6351 0.4286 0.043 Uiso 1 1 calc R A . C39 C 0.4983(3) 0.62817(13) 0.4708(2) 0.0440(7) Uani 1 1 d . A . H39 H 0.5054 0.5982 0.5132 0.053 Uiso 1 1 calc R . . C40 C 0.5782(2) 0.65087(15) 0.4589(2) 0.0468(8) Uani 1 1 d . . . H40 H 0.6389 0.6361 0.4933 0.056 Uiso 1 1 calc R A . C41 C 0.5680(2) 0.69536(15) 0.3958(2) 0.0421(7) Uani 1 1 d . A . H41 H 0.6219 0.7111 0.3887 0.050 Uiso 1 1 calc R . . C42 C 0.47749(19) 0.71659(13) 0.34324(19) 0.0338(6) Uani 1 1 d . . . H42 H 0.4707 0.7458 0.2998 0.041 Uiso 1 1 calc R A . 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 Ho1 0.01904(5) 0.01791(5) 0.01756(5) 0.00072(4) 0.00483(4) -0.00027(4) P1 0.0191(3) 0.0214(3) 0.0186(3) 0.0011(2) 0.0034(2) -0.0028(2) P2 0.0227(3) 0.0188(3) 0.0226(3) -0.0008(2) 0.0028(2) 0.0020(2) P3 0.0228(3) 0.0504(4) 0.0214(3) 0.0026(3) 0.0063(2) -0.0092(3) O1 0.0209(7) 0.0208(8) 0.0197(7) 0.0024(6) 0.0051(6) -0.0027(6) O2 0.0283(9) 0.0316(9) 0.0220(8) -0.0063(7) 0.0059(7) -0.0069(7) O3 0.0275(8) 0.0201(8) 0.0212(8) 0.0024(6) 0.0073(7) 0.0038(6) O4 0.0339(9) 0.0221(9) 0.0331(9) 0.0006(7) 0.0042(8) -0.0030(7) O5 0.0289(9) 0.0446(11) 0.0291(9) -0.0132(8) 0.0147(8) -0.0120(8) N1 0.0224(9) 0.0208(9) 0.0183(9) 0.0026(7) 0.0045(7) 0.0016(7) N2 0.0228(9) 0.0205(9) 0.0210(9) 0.0015(7) 0.0048(7) 0.0003(7) N3 0.0253(9) 0.0204(9) 0.0191(9) 0.0016(7) 0.0052(8) 0.0031(7) N4 0.0180(8) 0.0194(9) 0.0189(9) -0.0003(7) 0.0052(7) 0.0000(7) N5 0.0200(9) 0.0221(9) 0.0199(9) -0.0009(7) 0.0039(7) 0.0008(7) N6 0.0264(10) 0.0216(10) 0.0202(9) 0.0070(7) 0.0010(8) -0.0022(8) C1 0.0193(10) 0.0297(12) 0.0169(10) 0.0013(9) 0.0027(8) 0.0014(9) C2 0.0234(11) 0.0270(12) 0.0215(11) 0.0025(9) 0.0055(9) 0.0024(9) C3 0.0284(12) 0.0195(11) 0.0241(11) 0.0047(9) 0.0046(9) 0.0031(9) C4 0.0302(12) 0.0203(11) 0.0249(11) 0.0026(9) 0.0082(10) 0.0049(9) C5 0.0300(12) 0.0230(11) 0.0257(11) 0.0020(9) 0.0116(10) 0.0063(9) C6 0.0239(11) 0.0263(12) 0.0265(12) 0.0031(9) 0.0095(9) 0.0040(9) C7 0.0198(10) 0.0237(11) 0.0219(11) 0.0013(9) 0.0042(8) -0.0019(8) C8 0.0181(10) 0.0202(10) 0.0220(10) -0.0005(8) 0.0049(8) -0.0005(8) C9 0.0213(11) 0.0256(12) 0.0300(12) 0.0008(10) 0.0078(9) -0.0036(9) C10 0.0274(12) 0.0342(14) 0.0271(12) 0.0064(10) 0.0095(10) -0.0061(10) C11 0.0242(11) 0.0284(12) 0.0228(11) 0.0042(9) 0.0063(9) -0.0010(9) C12 0.0198(10) 0.0215(11) 0.0199(10) 0.0004(8) 0.0048(8) 0.0005(8) C13 0.0185(10) 0.0234(11) 0.0244(11) 0.0037(9) 0.0025(9) -0.0042(8) C14 0.0241(11) 0.0312(13) 0.0248(12) 0.0045(10) 0.0008(9) -0.0060(10) C15 0.0268(13) 0.0345(15) 0.0360(14) 0.0084(12) -0.0083(11) -0.0043(11) C16 0.0242(12) 0.0310(14) 0.0516(17) 0.0044(13) 0.0000(12) 0.0014(10) C17 0.0232(11) 0.0325(14) 0.0443(15) 0.0017(12) 0.0114(11) -0.0006(10) C18 0.0216(11) 0.0278(12) 0.0296(12) 0.0046(10) 0.0066(9) -0.0041(9) C19 0.0276(11) 0.0273(12) 0.0188(10) 0.0042(9) 0.0081(9) -0.0001(9) C20 0.0203(10) 0.0285(12) 0.0195(10) 0.0005(9) 0.0047(8) -0.0015(9) C21 0.0311(13) 0.0362(14) 0.0224(11) 0.0007(10) 0.0086(10) 0.0007(11) C22 0.0410(15) 0.0423(16) 0.0246(12) -0.0055(11) 0.0137(11) 0.0030(12) C23 0.0341(13) 0.0280(13) 0.0279(12) -0.0067(10) 0.0087(10) 0.0012(10) C24 0.0202(10) 0.0246(11) 0.0219(11) -0.0036(9) 0.0038(9) -0.0007(9) C31 0.0361(13) 0.0205(11) 0.0219(11) -0.0008(9) 0.0046(10) 0.0030(10) C32 0.0312(12) 0.0223(12) 0.0227(11) 0.0054(9) -0.0018(9) 0.0005(9) C33 0.0427(15) 0.0213(12) 0.0324(14) 0.0029(10) -0.0061(12) -0.0018(11) C34 0.0387(15) 0.0243(13) 0.0492(17) 0.0099(12) -0.0080(13) -0.0093(11) C35 0.0262(12) 0.0351(15) 0.0428(16) 0.0177(12) -0.0025(11) -0.0084(11) C36 0.0261(12) 0.0279(12) 0.0263(12) 0.0108(10) -0.0008(10) -0.0040(10) C37 0.0289(12) 0.0329(13) 0.0249(12) -0.0026(10) 0.0070(10) -0.0047(10) C38 0.0421(15) 0.0328(14) 0.0312(13) -0.0011(11) 0.0110(12) -0.0104(12) C39 0.065(2) 0.0286(14) 0.0359(15) 0.0065(12) 0.0158(15) 0.0081(14) C40 0.0481(18) 0.0466(18) 0.0417(17) 0.0021(14) 0.0122(14) 0.0203(15) C41 0.0304(14) 0.0540(18) 0.0430(16) 0.0032(14) 0.0152(12) 0.0069(13) C42 0.0281(12) 0.0391(15) 0.0342(14) 0.0048(11) 0.0116(11) 0.0003(11) _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 Ho1 O1 2.2949(16) . ? Ho1 O3 2.2919(16) . ? Ho1 O5 2.2810(18) . ? Ho1 N1 2.628(2) . ? Ho1 N2 2.6735(19) . ? Ho1 N3 2.6470(19) . ? Ho1 N4 2.6356(19) . ? Ho1 N5 2.6497(19) . ? Ho1 N6 2.616(2) . ? P1 O1 1.5154(16) . ? P1 O2 1.4994(18) . ? P1 C12 1.826(2) . ? P1 C13 1.806(2) . ? P2 O3 1.5113(17) . ? P2 O4 1.4978(19) . ? P2 C24 1.819(2) . ? P2 C25A 1.862(2) . ? P2 C25B 1.773(3) . ? P3 O5 1.5022(19) . ? P3 O6A 1.539(4) . ? P3 O6B 1.497(4) . ? P3 C36 1.819(3) . ? P3 C37 1.800(3) . ? N1 C1 1.484(3) . ? N1 C6 1.496(3) . ? N1 C7 1.484(3) . ? N2 C2 1.507(3) . ? N2 C3 1.486(3) . ? N2 C19 1.483(3) . ? N3 C4 1.500(3) . ? N3 C5 1.475(3) . ? N3 C31 1.481(3) . ? N4 C8 1.344(3) . ? N4 C12 1.351(3) . ? N5 C20 1.341(3) . ? N5 C24 1.350(3) . ? N6 C32 1.341(3) . ? N6 C36 1.346(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 C2 1.517(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 C4 1.523(3) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 C6 1.533(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C8 1.501(3) . ? C8 C9 1.392(3) . ? C9 H9 0.9300 . ? C9 C10 1.385(3) . ? C10 H10 0.9300 . ? C10 C11 1.386(3) . ? C11 H11 0.9300 . ? C11 C12 1.388(3) . ? C13 C14 1.402(3) . ? C13 C18 1.395(4) . ? C14 H14 0.9300 . ? C14 C15 1.385(4) . ? C15 H15 0.9300 . ? C15 C16 1.370(5) . ? C16 H16 0.9300 . ? C16 C17 1.394(4) . ? C17 H17 0.9300 . ? C17 C18 1.385(4) . ? C18 H18 0.9300 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 C20 1.494(3) . ? C20 C21 1.395(3) . ? C21 H21 0.9300 . ? C21 C22 1.382(4) . ? C22 H22 0.9300 . ? C22 C23 1.388(4) . ? C23 H23 0.9300 . ? C23 C24 1.386(3) . ? C25A C30B 1.3900 . ? C25A C26A 1.3900 . ? C30B H30 0.9300 . ? C30B C29B 1.3900 . ? C29B H29 0.9300 . ? C29B C28B 1.3900 . ? C28B H28 0.9300 . ? C28B C27A 1.3900 . ? C27A H27 0.9300 . ? C27A C26A 1.3900 . ? C26A H26 0.9300 . ? C25B C26B 1.3900 . ? C25B C30A 1.3900 . ? C26B H26A 0.9300 . ? C26B C27B 1.3900 . ? C27B H27A 0.9300 . ? C27B C28A 1.3900 . ? C28A H28A 0.9300 . ? C28A C29A 1.3900 . ? C29A H29A 0.9300 . ? C29A C30A 1.3900 . ? C30A H30A 0.9300 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 C32 1.502(4) . ? C32 C33 1.390(4) . ? C33 H33 0.9300 . ? C33 C34 1.380(5) . ? C34 H34 0.9300 . ? C34 C35 1.386(5) . ? C35 H35 0.9300 . ? C35 C36 1.393(4) . ? C37 C38 1.393(4) . ? C37 C42 1.396(4) . ? C38 H38 0.9300 . ? C38 C39 1.387(4) . ? C39 H39 0.9300 . ? C39 C40 1.384(5) . ? C40 H40 0.9300 . ? C40 C41 1.381(5) . ? C41 H41 0.9300 . ? C41 C42 1.386(4) . ? C42 H42 0.9300 . ? 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 O1 Ho1 N1 125.51(6) . . ? O1 Ho1 N2 147.66(6) . . ? O1 Ho1 N3 90.65(6) . . ? O1 Ho1 N4 66.80(5) . . ? O1 Ho1 N5 142.38(6) . . ? O1 Ho1 N6 68.27(6) . . ? O3 Ho1 O1 87.10(6) . . ? O3 Ho1 N1 89.71(6) . . ? O3 Ho1 N2 124.60(6) . . ? O3 Ho1 N3 149.21(6) . . ? O3 Ho1 N4 66.85(6) . . ? O3 Ho1 N5 67.11(6) . . ? O3 Ho1 N6 142.52(6) . . ? O5 Ho1 O1 84.88(6) . . ? O5 Ho1 O3 83.78(6) . . ? O5 Ho1 N1 148.64(6) . . ? O5 Ho1 N2 91.85(7) . . ? O5 Ho1 N3 126.61(7) . . ? O5 Ho1 N4 139.27(7) . . ? O5 Ho1 N5 66.20(6) . . ? O5 Ho1 N6 66.86(7) . . ? N1 Ho1 N2 66.90(6) . . ? N1 Ho1 N3 66.89(6) . . ? N1 Ho1 N4 62.16(6) . . ? N1 Ho1 N5 82.99(6) . . ? N3 Ho1 N2 65.72(6) . . ? N3 Ho1 N5 125.58(6) . . ? N4 Ho1 N2 127.75(6) . . ? N4 Ho1 N3 84.07(6) . . ? N4 Ho1 N5 121.04(6) . . ? N5 Ho1 N2 60.91(6) . . ? N6 Ho1 N1 127.45(6) . . ? N6 Ho1 N2 80.85(6) . . ? N6 Ho1 N3 62.25(6) . . ? N6 Ho1 N4 122.34(6) . . ? N6 Ho1 N5 116.62(6) . . ? O1 P1 C12 103.67(10) . . ? O1 P1 C13 109.08(10) . . ? O2 P1 O1 118.65(10) . . ? O2 P1 C12 110.71(11) . . ? O2 P1 C13 109.27(11) . . ? C13 P1 C12 104.47(10) . . ? O3 P2 C24 103.92(10) . . ? O3 P2 C25A 110.67(14) . . ? O3 P2 C25B 108.67(16) . . ? O4 P2 O3 116.95(11) . . ? O4 P2 C24 110.80(11) . . ? O4 P2 C25A 113.25(14) . . ? O4 P2 C25B 107.54(16) . . ? C24 P2 C25A 99.40(14) . . ? C25B P2 C24 108.72(17) . . ? C25B P2 C25A 9.42(19) . . ? O5 P3 O6A 122.84(16) . . ? O5 P3 C36 103.21(11) . . ? O5 P3 C37 108.40(12) . . ? O6A P3 C36 100.01(18) . . ? O6A P3 C37 113.14(16) . . ? O6B P3 O5 111.77(18) . . ? O6B P3 O6A 19.92(18) . . ? O6B P3 C36 119.8(2) . . ? O6B P3 C37 105.90(18) . . ? C37 P3 C36 107.32(12) . . ? P1 O1 Ho1 133.93(9) . . ? P2 O3 Ho1 133.53(9) . . ? P3 O5 Ho1 133.61(12) . . ? C1 N1 Ho1 107.20(13) . . ? C1 N1 C6 110.50(18) . . ? C1 N1 C7 108.25(18) . . ? C6 N1 Ho1 114.00(14) . . ? C7 N1 Ho1 107.55(13) . . ? C7 N1 C6 109.16(18) . . ? C2 N2 Ho1 113.04(13) . . ? C3 N2 Ho1 108.18(13) . . ? C3 N2 C2 109.66(18) . . ? C19 N2 Ho1 108.30(13) . . ? C19 N2 C2 109.62(18) . . ? C19 N2 C3 107.90(18) . . ? C4 N3 Ho1 116.25(14) . . ? C5 N3 Ho1 105.53(13) . . ? C5 N3 C4 110.36(18) . . ? C5 N3 C31 109.47(19) . . ? C31 N3 Ho1 106.24(14) . . ? C31 N3 C4 108.78(18) . . ? C8 N4 Ho1 118.35(14) . . ? C8 N4 C12 118.71(19) . . ? C12 N4 Ho1 121.99(14) . . ? C20 N5 Ho1 118.81(15) . . ? C20 N5 C24 118.2(2) . . ? C24 N5 Ho1 120.32(15) . . ? C32 N6 Ho1 119.31(16) . . ? C32 N6 C36 118.8(2) . . ? C36 N6 Ho1 121.82(17) . . ? N1 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? N1 C1 C2 112.55(19) . . ? H1A C1 H1B 107.8 . . ? C2 C1 H1A 109.1 . . ? C2 C1 H1B 109.1 . . ? N2 C2 C1 114.55(18) . . ? N2 C2 H2A 108.6 . . ? N2 C2 H2B 108.6 . . ? C1 C2 H2A 108.6 . . ? C1 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? N2 C3 H3A 109.3 . . ? N2 C3 H3B 109.3 . . ? N2 C3 C4 111.8(2) . . ? H3A C3 H3B 107.9 . . ? C4 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? N3 C4 C3 113.29(19) . . ? N3 C4 H4A 108.9 . . ? N3 C4 H4B 108.9 . . ? C3 C4 H4A 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? N3 C5 H5A 109.3 . . ? N3 C5 H5B 109.3 . . ? N3 C5 C6 111.52(19) . . ? H5A C5 H5B 108.0 . . ? C6 C5 H5A 109.3 . . ? C6 C5 H5B 109.3 . . ? N1 C6 C5 114.02(19) . . ? N1 C6 H6A 108.7 . . ? N1 C6 H6B 108.7 . . ? C5 C6 H6A 108.7 . . ? C5 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? N1 C7 C8 110.79(18) . . ? H7A C7 H7B 108.1 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? N4 C8 C7 115.4(2) . . ? N4 C8 C9 121.9(2) . . ? C9 C8 C7 122.6(2) . . ? C8 C9 H9 120.4 . . ? C10 C9 C8 119.2(2) . . ? C10 C9 H9 120.4 . . ? C9 C10 H10 120.5 . . ? C9 C10 C11 119.1(2) . . ? C11 C10 H10 120.5 . . ? C10 C11 H11 120.6 . . ? C10 C11 C12 118.8(2) . . ? C12 C11 H11 120.6 . . ? N4 C12 P1 113.29(16) . . ? N4 C12 C11 122.3(2) . . ? C11 C12 P1 124.33(17) . . ? C14 C13 P1 120.6(2) . . ? C18 C13 P1 120.14(18) . . ? C18 C13 C14 119.3(2) . . ? C13 C14 H14 120.2 . . ? C15 C14 C13 119.6(3) . . ? C15 C14 H14 120.2 . . ? C14 C15 H15 119.6 . . ? C16 C15 C14 120.8(3) . . ? C16 C15 H15 119.6 . . ? C15 C16 H16 119.8 . . ? C15 C16 C17 120.3(3) . . ? C17 C16 H16 119.8 . . ? C16 C17 H17 120.3 . . ? C18 C17 C16 119.5(3) . . ? C18 C17 H17 120.3 . . ? C13 C18 H18 119.7 . . ? C17 C18 C13 120.5(2) . . ? C17 C18 H18 119.7 . . ? N2 C19 H19A 109.4 . . ? N2 C19 H19B 109.4 . . ? N2 C19 C20 111.24(19) . . ? H19A C19 H19B 108.0 . . ? C20 C19 H19A 109.4 . . ? C20 C19 H19B 109.4 . . ? N5 C20 C19 116.1(2) . . ? N5 C20 C21 122.4(2) . . ? C21 C20 C19 121.4(2) . . ? C20 C21 H21 120.6 . . ? C22 C21 C20 118.8(2) . . ? C22 C21 H21 120.6 . . ? C21 C22 H22 120.4 . . ? C21 C22 C23 119.3(2) . . ? C23 C22 H22 120.4 . . ? C22 C23 H23 120.7 . . ? C24 C23 C22 118.7(2) . . ? C24 C23 H23 120.7 . . ? N5 C24 P2 113.89(17) . . ? N5 C24 C23 122.7(2) . . ? C23 C24 P2 123.33(19) . . ? C30B C25A P2 121.12(19) . . ? C30B C25A C26A 120.0 . . ? C26A C25A P2 118.87(19) . . ? C25A C30B H30 120.0 . . ? C29B C30B C25A 120.0 . . ? C29B C30B H30 120.0 . . ? C30B C29B H29 120.0 . . ? C28B C29B C30B 120.0 . . ? C28B C29B H29 120.0 . . ? C29B C28B H28 120.0 . . ? C29B C28B C27A 120.0 . . ? C27A C28B H28 120.0 . . ? C28B C27A H27 120.0 . . ? C26A C27A C28B 120.0 . . ? C26A C27A H27 120.0 . . ? C25A C26A H26 120.0 . . ? C27A C26A C25A 120.0 . . ? C27A C26A H26 120.0 . . ? C26B C25B P2 123.6(2) . . ? C26B C25B C30A 120.0 . . ? C30A C25B P2 116.2(2) . . ? C25B C26B H26A 120.0 . . ? C27B C26B C25B 120.0 . . ? C27B C26B H26A 120.0 . . ? C26B C27B H27A 120.0 . . ? C26B C27B C28A 120.0 . . ? C28A C27B H27A 120.0 . . ? C27B C28A H28A 120.0 . . ? C27B C28A C29A 120.0 . . ? C29A C28A H28A 120.0 . . ? C28A C29A H29A 120.0 . . ? C30A C29A C28A 120.0 . . ? C30A C29A H29A 120.0 . . ? C25B C30A H30A 120.0 . . ? C29A C30A C25B 120.0 . . ? C29A C30A H30A 120.0 . . ? N3 C31 H31A 109.7 . . ? N3 C31 H31B 109.7 . . ? N3 C31 C32 110.0(2) . . ? H31A C31 H31B 108.2 . . ? C32 C31 H31A 109.7 . . ? C32 C31 H31B 109.7 . . ? N6 C32 C31 114.7(2) . . ? N6 C32 C33 122.0(3) . . ? C33 C32 C31 123.4(3) . . ? C32 C33 H33 120.5 . . ? C34 C33 C32 119.1(3) . . ? C34 C33 H33 120.5 . . ? C33 C34 H34 120.3 . . ? C33 C34 C35 119.4(3) . . ? C35 C34 H34 120.3 . . ? C34 C35 H35 120.8 . . ? C34 C35 C36 118.3(3) . . ? C36 C35 H35 120.8 . . ? N6 C36 P3 113.36(18) . . ? N6 C36 C35 122.4(3) . . ? C35 C36 P3 124.3(2) . . ? C38 C37 P3 119.7(2) . . ? C38 C37 C42 119.2(3) . . ? C42 C37 P3 121.1(2) . . ? C37 C38 H38 119.9 . . ? C39 C38 C37 120.1(3) . . ? C39 C38 H38 119.9 . . ? C38 C39 H39 119.9 . . ? C40 C39 C38 120.2(3) . . ? C40 C39 H39 119.9 . . ? C39 C40 H40 120.0 . . ? C41 C40 C39 120.1(3) . . ? C41 C40 H40 120.0 . . ? C40 C41 H41 120.0 . . ? C40 C41 C42 120.1(3) . . ? C42 C41 H41 120.0 . . ? C37 C42 H42 119.8 . . ? C41 C42 C37 120.3(3) . . ? C41 C42 H42 119.8 . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.863 -0.502 -0.363 1401.3 367.7 ? # start Validation Reply Form _vrf_PLAT602_I ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: The structure contains a number of severely disordered solvent molecules (H2O, methanol). Their contribution to the structural fctors was taken into account by applying MASK procedure of OLEX2 program package. ; # end Validation Reply Form # Attachment '6392_web_deposit_cif_file_2_DmitryYufit_1311257364.NdL3.cif' data_NdL3_11srv130e _database_code_depnum_ccdc_archive 'CCDC 836099' #TrackingRef '6392_web_deposit_cif_file_2_DmitryYufit_1311257364.NdL3.cif' _audit_creation_date 2011-07-18 _audit_creation_method ; Olex2 1.1-beta (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H42 N6 Nd O6 P3' _chemical_formula_sum 'C42 H42 N6 Nd O6 P3' _chemical_formula_weight 963.97 _chemical_melting_point ? _chemical_oxdiff_formula 'C42 H42 N6 O6 P3 Nb1' 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' Nd Nd -0.1943 3.0179 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.1667(5) _cell_length_b 22.6624(6) _cell_length_c 15.9874(6) _cell_angle_alpha 90.00 _cell_angle_beta 112.584(4) _cell_angle_gamma 90.00 _cell_volume 5073.7(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 14367 _cell_measurement_temperature 120.0 _cell_measurement_theta_max 33.0681 _cell_measurement_theta_min 2.5732 _exptl_absorpt_coefficient_mu 1.163 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.80617 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.10 (release 06-04-2011 CrysAlis171 .NET) (compiled Apr 6 2011,09:17:13) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1956 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0704 _diffrn_reflns_av_unetI/netI 0.0668 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 56906 _diffrn_reflns_theta_full 29.00 _diffrn_reflns_theta_max 29.00 _diffrn_reflns_theta_min 2.76 _diffrn_ambient_temperature 120.0 _diffrn_detector CCD _diffrn_detector_area_resol_mean 16.1511 _diffrn_detector_type Sapphire3 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -102.00 -75.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - -27.1651 179.0000 30.0000 54 #__ type_ start__ end____ width___ exp.time_ 2 omega -99.00 -8.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - -27.1651 -38.0000 -120.0000 182 #__ type_ start__ end____ width___ exp.time_ 3 omega -87.00 41.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - -27.1651 0.0000 -90.0000 256 #__ type_ start__ end____ width___ exp.time_ 4 omega 65.00 103.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 27.9463 179.0000 -30.0000 76 #__ type_ start__ end____ width___ exp.time_ 5 omega -97.00 3.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - -27.1651 -77.0000 150.0000 200 #__ type_ start__ end____ width___ exp.time_ 6 omega -42.00 56.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 27.9463 -77.0000 30.0000 196 #__ type_ start__ end____ width___ exp.time_ 7 omega 56.00 104.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 27.9463 179.0000 60.0000 96 ; _diffrn_measurement_device '3-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method \w-scan _diffrn_orient_matrix_UB_11 0.0351170000 _diffrn_orient_matrix_UB_12 -0.0179086000 _diffrn_orient_matrix_UB_13 -0.0067230000 _diffrn_orient_matrix_UB_21 -0.0054946000 _diffrn_orient_matrix_UB_22 -0.0214155000 _diffrn_orient_matrix_UB_23 0.0299567000 _diffrn_orient_matrix_UB_31 -0.0360264000 _diffrn_orient_matrix_UB_32 -0.0141227000 _diffrn_orient_matrix_UB_33 -0.0370206000 _diffrn_radiation_collimation monochromator _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_xray_symbol Mo _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_source_type 'sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 10869 _reflns_number_total 13469 _reflns_odcompleteness_completeness 99.92 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 30.93 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.10 (release 06-04-2011 CrysAlis171 .NET) (compiled Apr 6 2011,09:17:13) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.10 (release 06-04-2011 CrysAlis171 .NET) (compiled Apr 6 2011,09:17:13) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.10 (release 06-04-2011 CrysAlis171 .NET) (compiled Apr 6 2011,09:17:13) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)/Bruker' _refine_diff_density_max 2.454 _refine_diff_density_min -1.458 _refine_diff_density_rms 0.134 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 492 _refine_ls_number_reflns 13469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0457 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1259 _refine_ls_wR_factor_ref 0.1320 _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. The structure contains a number of severely disordered solvent molecules (H2O, methanol). Their contribution to the structural fctors was taken into account by applying MASK procedure of OLEX2 program package. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Nd1 Nd -0.573729(11) -0.324261(7) -0.824158(11) 0.01507(6) Uani 1 1 d . A . P1 P -0.67674(6) -0.35626(4) -1.06218(5) 0.01854(16) Uani 1 1 d . . . P2 P -0.58245(6) -0.47237(4) -0.74890(6) 0.01930(16) Uani 1 1 d . . . P3 P -0.78106(6) -0.27498(4) -0.79061(6) 0.02572(19) Uani 1 1 d . . . O1 O -0.68065(17) -0.32605(9) -0.97911(16) 0.0191(5) Uani 1 1 d . . . O2 O -0.69522(18) -0.31991(10) -1.14555(17) 0.0252(5) Uani 1 1 d . . . O3 O -0.58773(16) -0.42892(10) -0.82263(15) 0.0208(5) Uani 1 1 d . A . O4 O -0.50735(17) -0.51926(10) -0.72642(17) 0.0261(5) Uani 1 1 d . B . O5 O -0.70989(19) -0.32265(10) -0.78690(18) 0.0279(6) Uani 1 1 d . A . O6B O -0.7797(4) -0.2611(3) -0.6989(4) 0.0306(15) Uiso 0.50 1 d P A 2 N1 N -0.3830(2) -0.33457(12) -0.76893(19) 0.0191(5) Uani 1 1 d . . . N2 N -0.47397(19) -0.25948(12) -0.67350(18) 0.0196(5) Uani 1 1 d . A . N3 N -0.48654(19) -0.22640(11) -0.85327(18) 0.0197(5) Uani 1 1 d . A . N4 N -0.50344(18) -0.37804(11) -0.93493(17) 0.0167(5) Uani 1 1 d . . . N5 N -0.54316(18) -0.36939(11) -0.65912(17) 0.0178(5) Uani 1 1 d . . . N6 N -0.67411(19) -0.22398(12) -0.87003(18) 0.0209(5) Uani 1 1 d . . . C1 C -0.3446(2) -0.33248(14) -0.6682(2) 0.0199(6) Uani 1 1 d . . . H1A H -0.2742 -0.3362 -0.6448 0.024 Uiso 1 1 calc R . . H1B H -0.3696 -0.3667 -0.6457 0.024 Uiso 1 1 calc R . . C2 C -0.3699(2) -0.27635(15) -0.6307(2) 0.0225(6) Uani 1 1 d . . . H2A H -0.3522 -0.2813 -0.5647 0.027 Uiso 1 1 calc R . . H2B H -0.3311 -0.2436 -0.6395 0.027 Uiso 1 1 calc R . . C3 C -0.4823(3) -0.19638(15) -0.7002(2) 0.0230(7) Uani 1 1 d . . . H3A H -0.4448 -0.1723 -0.6467 0.028 Uiso 1 1 calc R . . H3B H -0.5500 -0.1842 -0.7203 0.028 Uiso 1 1 calc R . . C4 C -0.4473(3) -0.18402(14) -0.7757(2) 0.0214(6) Uani 1 1 d . . . H4A H -0.4660 -0.1434 -0.7984 0.026 Uiso 1 1 calc R . . H4B H -0.3767 -0.1861 -0.7508 0.026 Uiso 1 1 calc R . . C5 C -0.4092(2) -0.24974(15) -0.8797(2) 0.0223(6) Uani 1 1 d . . . H5A H -0.3748 -0.2163 -0.8933 0.027 Uiso 1 1 calc R . . H5B H -0.4379 -0.2736 -0.9355 0.027 Uiso 1 1 calc R . . C6 C -0.3385(2) -0.28753(15) -0.8057(2) 0.0221(6) Uani 1 1 d . . . H6A H -0.2945 -0.3065 -0.8300 0.027 Uiso 1 1 calc R . . H6B H -0.2998 -0.2615 -0.7552 0.027 Uiso 1 1 calc R . . C7 C -0.3637(2) -0.39365(14) -0.7973(2) 0.0201(6) Uani 1 1 d . . . H7A H -0.3829 -0.4242 -0.7634 0.024 Uiso 1 1 calc R . . H7B H -0.2943 -0.3979 -0.7822 0.024 Uiso 1 1 calc R . . C8 C -0.4167(2) -0.40348(14) -0.8973(2) 0.0195(6) Uani 1 1 d . . . C9 C -0.3804(2) -0.43971(15) -0.9472(2) 0.0245(7) Uani 1 1 d . . . H9 H -0.3192 -0.4572 -0.9193 0.029 Uiso 1 1 calc R . . C10 C -0.4350(3) -0.44972(17) -1.0378(2) 0.0296(8) Uani 1 1 d . . . H10 H -0.4114 -0.4741 -1.0729 0.036 Uiso 1 1 calc R . . C11 C -0.5257(2) -0.42365(16) -1.0775(2) 0.0255(7) Uani 1 1 d . . . H11 H -0.5644 -0.4297 -1.1396 0.031 Uiso 1 1 calc R . . C12 C -0.5570(2) -0.38871(14) -1.0229(2) 0.0184(6) Uani 1 1 d . . . C13 C -0.7569(2) -0.41855(14) -1.0905(2) 0.0227(6) Uani 1 1 d . . . C14 C -0.7972(2) -0.43942(16) -1.1798(2) 0.0288(8) Uani 1 1 d . . . H14 H -0.7836 -0.4202 -1.2263 0.035 Uiso 1 1 calc R . . C15 C -0.8571(3) -0.48837(18) -1.2001(3) 0.0381(10) Uani 1 1 d . . . H15 H -0.8840 -0.5025 -1.2607 0.046 Uiso 1 1 calc R . . C16 C -0.8780(3) -0.51669(18) -1.1339(3) 0.0381(9) Uani 1 1 d . . . H16 H -0.9195 -0.5499 -1.1489 0.046 Uiso 1 1 calc R . . C17 C -0.8383(3) -0.49663(17) -1.0452(3) 0.0327(8) Uani 1 1 d . . . H17 H -0.8521 -0.5164 -0.9993 0.039 Uiso 1 1 calc R . . C18 C -0.7782(2) -0.44747(15) -1.0232(3) 0.0258(7) Uani 1 1 d . . . H18 H -0.7518 -0.4336 -0.9625 0.031 Uiso 1 1 calc R . . C19 C -0.5205(2) -0.26762(14) -0.6083(2) 0.0217(6) Uani 1 1 d . . . H19A H -0.5833 -0.2476 -0.6316 0.026 Uiso 1 1 calc R B . H19B H -0.4808 -0.2488 -0.5500 0.026 Uiso 1 1 calc R . . C20 C -0.5346(2) -0.33197(14) -0.5918(2) 0.0210(6) Uani 1 1 d . B . C21 C -0.5446(3) -0.34990(16) -0.5132(2) 0.0266(7) Uani 1 1 d . . . H21 H -0.5383 -0.3221 -0.4668 0.032 Uiso 1 1 calc R B . C22 C -0.5639(3) -0.40820(17) -0.5026(3) 0.0330(8) Uani 1 1 d . B . H22 H -0.5701 -0.4212 -0.4486 0.040 Uiso 1 1 calc R . . C23 C -0.5741(3) -0.44784(17) -0.5728(2) 0.0283(7) Uani 1 1 d . . . H23 H -0.5878 -0.4883 -0.5679 0.034 Uiso 1 1 calc R B . C24 C -0.5637(2) -0.42631(14) -0.6500(2) 0.0194(6) Uani 1 1 d . B . C25B C -0.6965(3) -0.5062(3) -0.7804(5) 0.023(2) Uiso 0.50 1 d PG B 1 C26B C -0.7092(4) -0.5668(3) -0.7927(5) 0.026(2) Uiso 0.50 1 d PG B 1 H26 H -0.6567 -0.5913 -0.7878 0.031 Uiso 0.50 1 calc PR B 1 C27B C -0.7989(5) -0.59149(19) -0.8123(5) 0.031(2) Uiso 0.50 1 d PG B 1 H27 H -0.8076 -0.6329 -0.8207 0.037 Uiso 0.50 1 calc PR B 1 C28B C -0.8758(3) -0.5556(2) -0.8195(4) 0.0313(19) Uiso 0.50 1 d PG B 1 H28 H -0.9370 -0.5725 -0.8329 0.038 Uiso 0.50 1 calc PR B 1 C29B C -0.8631(3) -0.4950(2) -0.8072(4) 0.0336(17) Uiso 0.50 1 d PG B 1 H29 H -0.9156 -0.4705 -0.8122 0.040 Uiso 0.50 1 calc PR B 1 C30B C -0.7735(4) -0.47031(19) -0.7877(4) 0.0260(15) Uiso 0.50 1 d PG B 1 H30 H -0.7648 -0.4289 -0.7792 0.031 Uiso 0.50 1 calc PR B 1 C31 C -0.5592(3) -0.19625(16) -0.9325(2) 0.0256(7) Uani 1 1 d . . . H31A H -0.5318 -0.1594 -0.9456 0.031 Uiso 1 1 calc R A . H31B H -0.5769 -0.2221 -0.9864 0.031 Uiso 1 1 calc R . . C32 C -0.6455(3) -0.18221(15) -0.9139(2) 0.0247(7) Uani 1 1 d . A . C33 C -0.6984(3) -0.12990(15) -0.9433(3) 0.0332(9) Uani 1 1 d . . . H33 H -0.6778 -0.1006 -0.9743 0.040 Uiso 1 1 calc R A . C34 C -0.7807(3) -0.12137(16) -0.9267(3) 0.0376(9) Uani 1 1 d . A . H34 H -0.8171 -0.0863 -0.9467 0.045 Uiso 1 1 calc R . . C35 C -0.8096(3) -0.16403(16) -0.8810(3) 0.0319(8) Uani 1 1 d . . . H35 H -0.8652 -0.1586 -0.8682 0.038 Uiso 1 1 calc R A . C36 C -0.7545(2) -0.21562(15) -0.8538(2) 0.0253(7) Uani 1 1 d . A . C37 C -0.8979(2) -0.30246(15) -0.8584(2) 0.0246(7) Uani 1 1 d . A . C38 C -0.9080(3) -0.34735(17) -0.9212(3) 0.0310(8) Uani 1 1 d . . . H38 H -0.8531 -0.3626 -0.9287 0.037 Uiso 1 1 calc R A . C39 C -0.9968(3) -0.36978(17) -0.9723(3) 0.0412(10) Uani 1 1 d . A . H39 H -1.0026 -0.4006 -1.0144 0.049 Uiso 1 1 calc R . . C40 C -1.0770(3) -0.3479(2) -0.9629(3) 0.0433(10) Uani 1 1 d . . . H40 H -1.1381 -0.3635 -0.9987 0.052 Uiso 1 1 calc R A . C41 C -1.0691(3) -0.3029(2) -0.9009(3) 0.0395(9) Uani 1 1 d . A . H41 H -1.1246 -0.2876 -0.8947 0.047 Uiso 1 1 calc R . . C42 C -0.9794(3) -0.28051(17) -0.8482(3) 0.0302(8) Uani 1 1 d . . . H42 H -0.9736 -0.2503 -0.8053 0.036 Uiso 1 1 calc R A . C25A C -0.7023(3) -0.5032(3) -0.7697(4) 0.0188(19) Uiso 0.50 1 d PG B 2 C30A C -0.7720(4) -0.46732(19) -0.7596(4) 0.0277(16) Uiso 0.50 1 d PG B 2 H30A H -0.7580 -0.4273 -0.7420 0.033 Uiso 0.50 1 calc PR B 2 C29A C -0.8620(3) -0.4901(2) -0.7752(4) 0.0319(17) Uiso 0.50 1 d PG B 2 H29A H -0.9096 -0.4656 -0.7683 0.038 Uiso 0.50 1 calc PR B 2 C28A C -0.8824(3) -0.5487(2) -0.8009(4) 0.0254(16) Uiso 0.50 1 d PG B 2 H28A H -0.9440 -0.5643 -0.8116 0.030 Uiso 0.50 1 calc PR B 2 C27A C -0.8128(4) -0.58457(19) -0.8110(5) 0.026(2) Uiso 0.50 1 d PG B 2 H27A H -0.8268 -0.6246 -0.8285 0.031 Uiso 0.50 1 calc PR B 2 C26A C -0.7228(4) -0.5618(3) -0.7953(5) 0.024(2) Uiso 0.50 1 d PG B 2 H26A H -0.6752 -0.5863 -0.8022 0.029 Uiso 0.50 1 calc PR B 2 O6A O -0.7786(4) -0.2418(3) -0.7072(4) 0.0210(12) Uiso 0.50 1 d P A 1 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 Nd1 0.01762(10) 0.01077(9) 0.01764(10) -0.00065(5) 0.00767(7) 0.00009(5) P1 0.0186(4) 0.0170(4) 0.0194(4) -0.0008(3) 0.0066(3) 0.0026(3) P2 0.0217(4) 0.0118(4) 0.0236(4) 0.0004(3) 0.0079(3) -0.0013(3) P3 0.0220(4) 0.0343(5) 0.0226(4) -0.0024(4) 0.0105(3) 0.0064(4) O1 0.0210(11) 0.0154(11) 0.0196(11) -0.0008(8) 0.0065(9) 0.0029(8) O2 0.0259(12) 0.0264(13) 0.0229(12) 0.0038(9) 0.0089(10) 0.0042(9) O3 0.0258(11) 0.0149(11) 0.0231(11) -0.0005(8) 0.0110(10) -0.0016(9) O4 0.0283(12) 0.0139(11) 0.0322(13) 0.0009(9) 0.0074(11) 0.0036(9) O5 0.0270(13) 0.0300(14) 0.0334(14) 0.0135(10) 0.0190(11) 0.0103(10) N1 0.0208(13) 0.0163(12) 0.0203(13) -0.0020(10) 0.0080(11) -0.0018(10) N2 0.0233(13) 0.0153(12) 0.0206(13) -0.0026(10) 0.0088(11) -0.0024(10) N3 0.0236(13) 0.0123(12) 0.0223(13) -0.0005(10) 0.0078(11) -0.0018(10) N4 0.0199(12) 0.0118(12) 0.0190(12) -0.0005(9) 0.0082(10) 0.0010(10) N5 0.0191(12) 0.0148(12) 0.0185(12) -0.0001(10) 0.0061(10) -0.0009(10) N6 0.0228(13) 0.0157(12) 0.0210(13) -0.0053(10) 0.0050(11) 0.0011(10) C1 0.0205(15) 0.0181(15) 0.0210(15) -0.0010(12) 0.0077(13) -0.0017(12) C2 0.0256(16) 0.0191(15) 0.0204(15) -0.0044(12) 0.0061(13) -0.0024(13) C3 0.0290(17) 0.0147(15) 0.0227(16) -0.0056(12) 0.0070(14) -0.0019(13) C4 0.0268(17) 0.0123(14) 0.0247(16) -0.0026(12) 0.0096(14) -0.0044(12) C5 0.0238(16) 0.0183(15) 0.0247(16) -0.0019(12) 0.0094(13) -0.0030(12) C6 0.0214(15) 0.0204(16) 0.0253(16) -0.0006(13) 0.0099(13) -0.0018(12) C7 0.0190(14) 0.0166(15) 0.0229(15) 0.0008(12) 0.0062(12) 0.0022(12) C8 0.0208(15) 0.0156(14) 0.0239(15) -0.0020(12) 0.0108(13) -0.0006(12) C9 0.0230(16) 0.0211(16) 0.0303(17) -0.0050(13) 0.0112(14) 0.0033(13) C10 0.0270(17) 0.034(2) 0.0288(18) -0.0094(15) 0.0123(15) 0.0072(15) C11 0.0243(16) 0.0290(18) 0.0227(16) -0.0050(14) 0.0084(13) 0.0021(14) C12 0.0178(14) 0.0159(14) 0.0229(15) 0.0003(12) 0.0095(12) 0.0000(11) C13 0.0194(15) 0.0179(15) 0.0297(17) -0.0027(13) 0.0083(13) 0.0038(12) C14 0.0244(17) 0.0264(18) 0.0298(18) -0.0037(14) 0.0041(15) 0.0030(14) C15 0.032(2) 0.031(2) 0.037(2) -0.0092(17) -0.0039(17) 0.0009(16) C16 0.0271(18) 0.0257(19) 0.052(2) -0.0070(18) 0.0048(18) -0.0045(15) C17 0.0218(16) 0.0269(18) 0.050(2) -0.0042(17) 0.0137(16) -0.0022(14) C18 0.0242(16) 0.0204(16) 0.0337(18) -0.0042(14) 0.0123(14) 0.0025(13) C19 0.0281(16) 0.0140(14) 0.0249(16) -0.0037(12) 0.0122(14) -0.0017(12) C20 0.0216(15) 0.0190(15) 0.0213(16) -0.0025(12) 0.0071(13) 0.0003(12) C21 0.0294(17) 0.0278(18) 0.0236(16) -0.0041(14) 0.0113(14) -0.0018(14) C22 0.042(2) 0.033(2) 0.0276(18) 0.0025(15) 0.0178(16) -0.0072(17) C23 0.0355(19) 0.0252(18) 0.0238(16) 0.0023(14) 0.0108(15) -0.0059(15) C24 0.0199(14) 0.0149(14) 0.0227(15) 0.0029(12) 0.0076(12) 0.0013(12) C31 0.0318(18) 0.0218(16) 0.0216(16) 0.0027(13) 0.0086(14) -0.0019(14) C32 0.0236(16) 0.0176(16) 0.0250(17) -0.0002(12) 0.0005(14) 0.0018(12) C33 0.041(2) 0.0147(16) 0.0332(19) 0.0007(14) 0.0022(17) 0.0026(15) C34 0.035(2) 0.0174(17) 0.047(2) -0.0018(16) 0.0006(18) 0.0082(15) C35 0.0265(18) 0.0198(17) 0.040(2) -0.0114(15) 0.0026(16) 0.0056(14) C36 0.0259(16) 0.0218(16) 0.0240(16) -0.0087(13) 0.0049(14) 0.0043(13) C37 0.0274(17) 0.0206(16) 0.0272(17) 0.0026(13) 0.0120(14) 0.0041(13) C38 0.038(2) 0.0231(18) 0.0309(19) -0.0006(15) 0.0121(16) 0.0062(15) C39 0.062(3) 0.0205(19) 0.041(2) -0.0069(16) 0.019(2) -0.0073(18) C40 0.044(2) 0.040(2) 0.041(2) -0.0016(19) 0.010(2) -0.022(2) C41 0.0270(19) 0.045(2) 0.048(2) -0.001(2) 0.0160(18) -0.0060(18) C42 0.0249(17) 0.0300(19) 0.038(2) -0.0062(16) 0.0140(15) -0.0047(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O1 2.384(2) . ? Nd1 O3 2.382(2) . ? Nd1 O5 2.359(2) . ? Nd1 N1 2.691(3) . ? Nd1 N2 2.729(3) . ? Nd1 N3 2.712(3) . ? Nd1 N4 2.685(3) . ? Nd1 N5 2.699(3) . ? Nd1 N6 2.676(3) . ? P1 O1 1.515(2) . ? P1 O2 1.499(3) . ? P1 C12 1.833(3) . ? P1 C13 1.803(3) . ? P2 O3 1.514(2) . ? P2 O4 1.497(2) . ? P2 C24 1.823(3) . ? P2 C25B 1.779(4) . ? P2 C25A 1.855(4) . ? P3 O5 1.512(2) . ? P3 O6B 1.492(6) . ? P3 C36 1.818(4) . ? P3 C37 1.796(4) . ? P3 O6A 1.519(5) . ? N1 C1 1.489(4) . ? N1 C6 1.497(4) . ? N1 C7 1.479(4) . ? N2 C2 1.509(4) . ? N2 C3 1.484(4) . ? N2 C19 1.478(4) . ? N3 C4 1.499(4) . ? N3 C5 1.489(4) . ? N3 C31 1.487(4) . ? N4 C8 1.348(4) . ? N4 C12 1.349(4) . ? N5 C20 1.337(4) . ? N5 C24 1.348(4) . ? N6 C32 1.345(5) . ? N6 C36 1.353(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 C2 1.517(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.519(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.520(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.504(4) . ? C8 C9 1.396(4) . ? C9 H9 0.9500 . ? C9 C10 1.384(5) . ? C10 H10 0.9500 . ? C10 C11 1.405(5) . ? C11 H11 0.9500 . ? C11 C12 1.389(4) . ? C13 C14 1.403(5) . ? C13 C18 1.399(5) . ? C14 H14 0.9500 . ? C14 C15 1.391(5) . ? C15 H15 0.9500 . ? C15 C16 1.375(6) . ? C16 H16 0.9500 . ? C16 C17 1.388(6) . ? C17 H17 0.9500 . ? C17 C18 1.396(5) . ? C18 H18 0.9500 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19 C20 1.512(4) . ? C20 C21 1.383(5) . ? C21 H21 0.9500 . ? C21 C22 1.378(5) . ? C22 H22 0.9500 . ? C22 C23 1.399(5) . ? C23 H23 0.9500 . ? C23 C24 1.391(4) . ? C25B C26B 1.3900 . ? C25B C30B 1.3900 . ? C26B H26 0.9500 . ? C26B C27B 1.3900 . ? C27B H27 0.9500 . ? C27B C28B 1.3900 . ? C28B H28 0.9500 . ? C28B C29B 1.3900 . ? C29B H29 0.9500 . ? C29B C30B 1.3900 . ? C30B H30 0.9500 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C31 C32 1.485(5) . ? C32 C33 1.407(5) . ? C33 H33 0.9500 . ? C33 C34 1.386(6) . ? C34 H34 0.9500 . ? C34 C35 1.380(6) . ? C35 H35 0.9500 . ? C35 C36 1.405(5) . ? C37 C38 1.396(5) . ? C37 C42 1.399(5) . ? C38 H38 0.9500 . ? C38 C39 1.376(6) . ? C39 H39 0.9500 . ? C39 C40 1.375(7) . ? C40 H40 0.9500 . ? C40 C41 1.395(6) . ? C41 H41 0.9500 . ? C41 C42 1.391(5) . ? C42 H42 0.9500 . ? C25A C30A 1.3900 . ? C25A C26A 1.3900 . ? C30A H30A 0.9500 . ? C30A C29A 1.3900 . ? C29A H29A 0.9500 . ? C29A C28A 1.3900 . ? C28A H28A 0.9500 . ? C28A C27A 1.3900 . ? C27A H27A 0.9500 . ? C27A C26A 1.3900 . ? C26A H26A 0.9500 . ? 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 O1 Nd1 N1 123.78(8) . . ? O1 Nd1 N2 148.40(8) . . ? O1 Nd1 N3 91.00(8) . . ? O1 Nd1 N4 65.84(8) . . ? O1 Nd1 N5 143.37(8) . . ? O1 Nd1 N6 68.98(7) . . ? O3 Nd1 O1 88.05(7) . . ? O3 Nd1 N1 89.95(8) . . ? O3 Nd1 N2 123.23(8) . . ? O3 Nd1 N3 150.12(8) . . ? O3 Nd1 N4 67.31(7) . . ? O3 Nd1 N5 66.12(8) . . ? O3 Nd1 N6 143.58(8) . . ? O5 Nd1 O1 87.17(9) . . ? O5 Nd1 O3 85.56(8) . . ? O5 Nd1 N1 148.59(9) . . ? O5 Nd1 N2 90.64(9) . . ? O5 Nd1 N3 124.22(8) . . ? O5 Nd1 N4 141.39(9) . . ? O5 Nd1 N5 66.26(8) . . ? O5 Nd1 N6 66.11(8) . . ? N1 Nd1 N2 66.13(8) . . ? N1 Nd1 N3 66.03(8) . . ? N1 Nd1 N5 83.51(8) . . ? N3 Nd1 N2 64.53(8) . . ? N4 Nd1 N1 61.83(8) . . ? N4 Nd1 N2 126.90(8) . . ? N4 Nd1 N3 85.11(8) . . ? N4 Nd1 N5 120.68(8) . . ? N5 Nd1 N2 60.80(8) . . ? N5 Nd1 N3 124.44(8) . . ? N6 Nd1 N1 126.18(8) . . ? N6 Nd1 N2 81.33(8) . . ? N6 Nd1 N3 61.46(8) . . ? N6 Nd1 N4 122.20(8) . . ? N6 Nd1 N5 117.11(8) . . ? O1 P1 C12 104.39(14) . . ? O1 P1 C13 108.91(15) . . ? O2 P1 O1 118.30(13) . . ? O2 P1 C12 110.31(14) . . ? O2 P1 C13 109.23(15) . . ? C13 P1 C12 104.82(14) . . ? O3 P2 C24 104.29(14) . . ? O3 P2 C25B 107.8(2) . . ? O3 P2 C25A 110.5(2) . . ? O4 P2 O3 117.15(14) . . ? O4 P2 C24 110.32(14) . . ? O4 P2 C25B 109.2(2) . . ? O4 P2 C25A 112.3(2) . . ? C24 P2 C25A 100.7(2) . . ? C25B P2 C24 107.6(2) . . ? C25B P2 C25A 6.9(3) . . ? O5 P3 C36 104.07(15) . . ? O5 P3 C37 107.45(16) . . ? O5 P3 O6A 122.9(2) . . ? O6B P3 O5 111.8(3) . . ? O6B P3 C36 117.9(3) . . ? O6B P3 C37 107.7(3) . . ? O6B P3 O6A 17.5(3) . . ? C37 P3 C36 107.42(16) . . ? O6A P3 C36 100.7(3) . . ? O6A P3 C37 112.7(2) . . ? P1 O1 Nd1 132.73(13) . . ? P2 O3 Nd1 132.62(13) . . ? P3 O5 Nd1 133.00(14) . . ? C1 N1 Nd1 106.09(19) . . ? C1 N1 C6 110.7(2) . . ? C6 N1 Nd1 113.54(19) . . ? C7 N1 Nd1 107.00(18) . . ? C7 N1 C1 108.6(2) . . ? C7 N1 C6 110.6(2) . . ? C2 N2 Nd1 113.11(18) . . ? C3 N2 Nd1 107.89(18) . . ? C3 N2 C2 109.5(3) . . ? C19 N2 Nd1 107.61(18) . . ? C19 N2 C2 110.4(2) . . ? C19 N2 C3 108.2(2) . . ? C4 N3 Nd1 116.51(19) . . ? C5 N3 Nd1 104.33(18) . . ? C5 N3 C4 110.9(3) . . ? C31 N3 Nd1 105.74(19) . . ? C31 N3 C4 109.8(3) . . ? C31 N3 C5 109.1(3) . . ? C8 N4 Nd1 117.81(19) . . ? C8 N4 C12 118.8(3) . . ? C12 N4 Nd1 122.46(19) . . ? C20 N5 Nd1 118.3(2) . . ? C20 N5 C24 118.4(3) . . ? C24 N5 Nd1 120.5(2) . . ? C32 N6 Nd1 118.5(2) . . ? C32 N6 C36 119.7(3) . . ? C36 N6 Nd1 121.7(2) . . ? N1 C1 H1A 108.8 . . ? N1 C1 H1B 108.8 . . ? N1 C1 C2 113.6(3) . . ? H1A C1 H1B 107.7 . . ? C2 C1 H1A 108.8 . . ? C2 C1 H1B 108.8 . . ? N2 C2 C1 114.4(3) . . ? N2 C2 H2A 108.7 . . ? N2 C2 H2B 108.7 . . ? C1 C2 H2A 108.7 . . ? C1 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? N2 C3 H3A 109.0 . . ? N2 C3 H3B 109.0 . . ? N2 C3 C4 112.9(3) . . ? H3A C3 H3B 107.8 . . ? C4 C3 H3A 109.0 . . ? C4 C3 H3B 109.0 . . ? N3 C4 C3 113.0(3) . . ? N3 C4 H4A 109.0 . . ? N3 C4 H4B 109.0 . . ? C3 C4 H4A 109.0 . . ? C3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? N3 C5 H5A 109.2 . . ? N3 C5 H5B 109.2 . . ? N3 C5 C6 112.1(3) . . ? H5A C5 H5B 107.9 . . ? C6 C5 H5A 109.2 . . ? C6 C5 H5B 109.2 . . ? N1 C6 C5 114.7(3) . . ? N1 C6 H6A 108.6 . . ? N1 C6 H6B 108.6 . . ? C5 C6 H6A 108.6 . . ? C5 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? N1 C7 H7A 109.2 . . ? N1 C7 H7B 109.2 . . ? N1 C7 C8 111.9(3) . . ? H7A C7 H7B 107.9 . . ? C8 C7 H7A 109.2 . . ? C8 C7 H7B 109.2 . . ? N4 C8 C7 116.3(3) . . ? N4 C8 C9 121.8(3) . . ? C9 C8 C7 121.8(3) . . ? C8 C9 H9 120.5 . . ? C10 C9 C8 119.1(3) . . ? C10 C9 H9 120.5 . . ? C9 C10 H10 120.2 . . ? C9 C10 C11 119.5(3) . . ? C11 C10 H10 120.2 . . ? C10 C11 H11 121.1 . . ? C12 C11 C10 117.8(3) . . ? C12 C11 H11 121.1 . . ? N4 C12 P1 113.9(2) . . ? N4 C12 C11 122.9(3) . . ? C11 C12 P1 123.1(3) . . ? C14 C13 P1 120.5(3) . . ? C18 C13 P1 120.4(3) . . ? C18 C13 C14 119.1(3) . . ? C13 C14 H14 120.1 . . ? C15 C14 C13 119.8(4) . . ? C15 C14 H14 120.1 . . ? C14 C15 H15 119.5 . . ? C16 C15 C14 121.0(4) . . ? C16 C15 H15 119.5 . . ? C15 C16 H16 120.1 . . ? C15 C16 C17 119.7(4) . . ? C17 C16 H16 120.1 . . ? C16 C17 H17 119.9 . . ? C16 C17 C18 120.3(4) . . ? C18 C17 H17 119.9 . . ? C13 C18 H18 120.0 . . ? C17 C18 C13 120.1(3) . . ? C17 C18 H18 120.0 . . ? N2 C19 H19A 109.1 . . ? N2 C19 H19B 109.1 . . ? N2 C19 C20 112.4(3) . . ? H19A C19 H19B 107.9 . . ? C20 C19 H19A 109.1 . . ? C20 C19 H19B 109.1 . . ? N5 C20 C19 116.6(3) . . ? N5 C20 C21 122.3(3) . . ? C21 C20 C19 120.9(3) . . ? C20 C21 H21 120.1 . . ? C22 C21 C20 119.8(3) . . ? C22 C21 H21 120.1 . . ? C21 C22 H22 120.7 . . ? C21 C22 C23 118.7(3) . . ? C23 C22 H22 120.7 . . ? C22 C23 H23 120.9 . . ? C24 C23 C22 118.1(3) . . ? C24 C23 H23 120.9 . . ? N5 C24 P2 114.8(2) . . ? N5 C24 C23 122.8(3) . . ? C23 C24 P2 122.4(3) . . ? C26B C25B P2 122.2(3) . . ? C26B C25B C30B 120.0 . . ? C30B C25B P2 117.7(3) . . ? C25B C26B H26 120.0 . . ? C25B C26B C27B 120.0 . . ? C27B C26B H26 120.0 . . ? C26B C27B H27 120.0 . . ? C28B C27B C26B 120.0 . . ? C28B C27B H27 120.0 . . ? C27B C28B H28 120.0 . . ? C29B C28B C27B 120.0 . . ? C29B C28B H28 120.0 . . ? C28B C29B H29 120.0 . . ? C30B C29B C28B 120.0 . . ? C30B C29B H29 120.0 . . ? C25B C30B H30 120.0 . . ? C29B C30B C25B 120.0 . . ? C29B C30B H30 120.0 . . ? N3 C31 H31A 109.6 . . ? N3 C31 H31B 109.6 . . ? H31A C31 H31B 108.1 . . ? C32 C31 N3 110.5(3) . . ? C32 C31 H31A 109.6 . . ? C32 C31 H31B 109.6 . . ? N6 C32 C31 116.1(3) . . ? N6 C32 C33 120.7(4) . . ? C33 C32 C31 123.2(3) . . ? C32 C33 H33 120.2 . . ? C34 C33 C32 119.5(4) . . ? C34 C33 H33 120.2 . . ? C33 C34 H34 120.1 . . ? C35 C34 C33 119.7(3) . . ? C35 C34 H34 120.1 . . ? C34 C35 H35 120.8 . . ? C34 C35 C36 118.3(4) . . ? C36 C35 H35 120.8 . . ? N6 C36 P3 114.3(2) . . ? N6 C36 C35 122.0(4) . . ? C35 C36 P3 123.7(3) . . ? C38 C37 P3 119.8(3) . . ? C38 C37 C42 119.0(3) . . ? C42 C37 P3 121.2(3) . . ? C37 C38 H38 119.7 . . ? C39 C38 C37 120.6(4) . . ? C39 C38 H38 119.7 . . ? C38 C39 H39 119.8 . . ? C40 C39 C38 120.5(4) . . ? C40 C39 H39 119.8 . . ? C39 C40 H40 119.9 . . ? C39 C40 C41 120.1(4) . . ? C41 C40 H40 119.9 . . ? C40 C41 H41 120.2 . . ? C42 C41 C40 119.7(4) . . ? C42 C41 H41 120.2 . . ? C37 C42 H42 119.9 . . ? C41 C42 C37 120.1(4) . . ? C41 C42 H42 119.9 . . ? C30A C25A P2 119.7(3) . . ? C30A C25A C26A 120.0 . . ? C26A C25A P2 120.3(3) . . ? C25A C30A H30A 120.0 . . ? C25A C30A C29A 120.0 . . ? C29A C30A H30A 120.0 . . ? C30A C29A H29A 120.0 . . ? C28A C29A C30A 120.0 . . ? C28A C29A H29A 120.0 . . ? C29A C28A H28A 120.0 . . ? C27A C28A C29A 120.0 . . ? C27A C28A H28A 120.0 . . ? C28A C27A H27A 120.0 . . ? C26A C27A C28A 120.0 . . ? C26A C27A H27A 120.0 . . ? C25A C26A H26A 120.0 . . ? C27A C26A C25A 120.0 . . ? C27A C26A H26A 120.0 . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.084 -0.449 -0.584 1481.9 84.9 ? # start Validation Reply Form _vrf_PLAT602_I ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: The structure contains a number of severely disordered solvent molecules (H2O, methanol). Their contribution to the structural fctors was taken into account by applying MASK procedure of OLEX2 program package. ; # end Validation Reply Form # Attachment '6393_web_deposit_cif_file_3_DmitryYufit_1311257364.SmL3.cif' data_SmL3_11srv130b _database_code_depnum_ccdc_archive 'CCDC 836100' #TrackingRef '6393_web_deposit_cif_file_3_DmitryYufit_1311257364.SmL3.cif' _audit_creation_date 2011-07-08 _audit_creation_method ; Olex2 1.1-beta (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H42 N6 O6 P3 Sm' _chemical_formula_sum 'C42 H42 N6 O6 P3 Sm' _chemical_formula_weight 970.08 _chemical_melting_point ? 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.0707(4) _cell_length_b 22.5655(5) _cell_length_c 15.9329(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.336(10) _cell_angle_gamma 90.00 _cell_volume 5011.9(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9804 _cell_measurement_temperature 120 _cell_measurement_theta_max 28.07 _cell_measurement_theta_min 2.27 _exptl_absorpt_coefficient_mu 1.313 _exptl_absorpt_correction_T_max 0.8621 _exptl_absorpt_correction_T_min 0.2803 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2006/1 (Bruker,2006) was used for absorption correction. R(int) was 0.0521 before and 0.0410 after correction. The Ratio of minimum to maximum transmission is 0.325136295093. The \l/2 correction factor is 0.0015 ; _exptl_crystal_colour less _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1964 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.07 _exptl_special_details ; The data collection nominally covered a full sphere of reciprocal space by a combination of 4 sets of \w scans each set at different \f and/or 2\q angles and each scan (15.00 s exposure) covering -0.300\ degrees in \w. The crystal to detector distance was 4.85 cm. ; _diffrn_reflns_av_R_equivalents 0.0635 _diffrn_reflns_av_unetI/netI 0.0583 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 54782 _diffrn_reflns_theta_full 29.00 _diffrn_reflns_theta_max 29.00 _diffrn_reflns_theta_min 1.58 _diffrn_ambient_temperature 120 _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 5.6 _diffrn_detector_type 'Bruker SMART CCD 6000 area detector' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART CCD 6000 area detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_xray_symbol K-L~3~ _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40.0 _diffrn_source_power 2.0 _diffrn_source_target Mo _diffrn_source_voltage 50.0 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 9473 _reflns_number_total 13297 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'SAINT v6.45A (Bruker, 2003)' _computing_data_collection 'SMART v5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT v6.45A (Bruker, 2003)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)/Bruker' _refine_diff_density_max 2.550 _refine_diff_density_min -1.213 _refine_diff_density_rms 0.114 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 492 _refine_ls_number_reflns 13297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0398 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+2.4000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0886 _refine_ls_wR_factor_ref 0.0965 _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. The structure contains a number of severely disordered solvent molecules (H2O, methanol). Their contribution to the structural fctors was taken into account by applying MASK procedure of OLEX2 program package. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Sm1 Sm 0.927108(11) 0.675977(7) 0.676934(10) 0.01826(5) Uani 1 1 d . A . P1 P 0.82417(6) 0.64444(4) 0.44024(5) 0.02122(17) Uani 1 1 d . . . P2 P 0.91890(6) 0.52831(4) 0.75157(5) 0.02213(17) Uani 1 1 d . . . P3 P 0.71908(6) 0.72288(5) 0.71037(6) 0.0309(2) Uani 1 1 d . . . O1 O 0.82055(15) 0.67400(9) 0.52399(14) 0.0214(4) Uani 1 1 d . . . O2 O 0.80597(17) 0.68146(10) 0.35716(15) 0.0283(5) Uani 1 1 d . . . O3 O 0.91410(15) 0.57231(9) 0.67850(14) 0.0220(5) Uani 1 1 d . A . O4 O 0.99415(17) 0.48130(10) 0.77322(16) 0.0306(5) Uani 1 1 d . B . O5 O 0.79092(17) 0.67587(11) 0.71251(16) 0.0316(5) Uani 1 1 d . A . O6A O 0.7225(3) 0.7560(2) 0.7951(3) 0.0228(11) Uiso 0.50 1 d P A 1 O6B O 0.7203(4) 0.7335(3) 0.8034(4) 0.0330(13) Uiso 0.50 1 d P A 2 N1 N 1.11698(19) 0.66610(11) 0.73218(17) 0.0218(6) Uani 1 1 d . . . N2 N 1.02483(19) 0.74159(11) 0.82643(17) 0.0220(6) Uani 1 1 d . A . N3 N 1.01295(19) 0.77322(11) 0.64646(17) 0.0227(6) Uani 1 1 d . A . N4 N 0.99815(18) 0.62211(11) 0.56679(16) 0.0194(5) Uani 1 1 d . . . N5 N 0.95705(18) 0.63116(11) 0.84152(17) 0.0214(5) Uani 1 1 d . . . N6 N 0.82578(19) 0.77526(12) 0.63177(18) 0.0257(6) Uani 1 1 d . . . C1 C 1.1559(2) 0.66815(13) 0.8327(2) 0.0216(6) Uani 1 1 d . . . H1A H 1.2253 0.6650 0.8552 0.026 Uiso 1 1 calc R . . H1B H 1.1321 0.6342 0.8552 0.026 Uiso 1 1 calc R . . C2 C 1.1291(2) 0.72462(14) 0.8702(2) 0.0246(7) Uani 1 1 d . . . H2A H 1.1454 0.7196 0.9348 0.030 Uiso 1 1 calc R . . H2B H 1.1677 0.7570 0.8624 0.030 Uiso 1 1 calc R . . C3 C 1.0161(3) 0.80462(14) 0.7992(2) 0.0267(7) Uani 1 1 d . . . H3A H 1.0527 0.8286 0.8514 0.032 Uiso 1 1 calc R . . H3B H 0.9494 0.8165 0.7793 0.032 Uiso 1 1 calc R . . C4 C 1.0518(2) 0.81627(14) 0.7235(2) 0.0258(7) Uani 1 1 d . . . H4A H 1.0335 0.8561 0.7005 0.031 Uiso 1 1 calc R . . H4B H 1.1213 0.8142 0.7481 0.031 Uiso 1 1 calc R . . C5 C 1.0908(2) 0.75075(14) 0.6199(2) 0.0269(7) Uani 1 1 d . . . H5A H 1.1241 0.7840 0.6068 0.032 Uiso 1 1 calc R . . H5B H 1.0631 0.7273 0.5650 0.032 Uiso 1 1 calc R . . C6 C 1.1634(2) 0.71243(14) 0.6949(2) 0.0255(7) Uani 1 1 d . . . H6A H 1.2059 0.6931 0.6704 0.031 Uiso 1 1 calc R . . H6B H 1.2022 0.7380 0.7440 0.031 Uiso 1 1 calc R . . C7 C 1.1371(2) 0.60656(14) 0.7037(2) 0.0226(6) Uani 1 1 d . . . H7A H 1.1179 0.5764 0.7367 0.027 Uiso 1 1 calc R . . H7B H 1.2056 0.6025 0.7187 0.027 Uiso 1 1 calc R . . C8 C 1.0847(2) 0.59707(13) 0.6037(2) 0.0209(6) Uani 1 1 d . . . C9 C 1.1205(2) 0.56049(15) 0.5540(2) 0.0268(7) Uani 1 1 d . . . H9 H 1.1805 0.5430 0.5815 0.032 Uiso 1 1 calc R . . C10 C 1.0661(2) 0.55002(16) 0.4627(2) 0.0317(8) Uani 1 1 d . . . H10 H 1.0892 0.5260 0.4282 0.038 Uiso 1 1 calc R . . C11 C 0.9759(2) 0.57658(15) 0.4245(2) 0.0249(7) Uani 1 1 d . . . H11 H 0.9378 0.5707 0.3636 0.030 Uiso 1 1 calc R . . C12 C 0.9442(2) 0.61170(13) 0.4784(2) 0.0215(6) Uani 1 1 d . . . C13 C 0.7430(2) 0.58183(14) 0.4112(2) 0.0248(7) Uani 1 1 d . . . C14 C 0.7034(2) 0.56166(15) 0.3215(2) 0.0295(8) Uani 1 1 d . . . H14 H 0.7179 0.5805 0.2763 0.035 Uiso 1 1 calc R . . C15 C 0.6423(3) 0.51310(16) 0.3010(3) 0.0383(9) Uani 1 1 d . . . H15 H 0.6152 0.4997 0.2414 0.046 Uiso 1 1 calc R . . C16 C 0.6209(3) 0.48451(17) 0.3672(3) 0.0420(10) Uani 1 1 d . . . H16 H 0.5800 0.4519 0.3522 0.050 Uiso 1 1 calc R . . C17 C 0.6605(2) 0.50434(16) 0.4567(3) 0.0348(8) Uani 1 1 d . . . H17 H 0.6461 0.4854 0.5017 0.042 Uiso 1 1 calc R . . C18 C 0.7218(2) 0.55278(15) 0.4776(2) 0.0279(7) Uani 1 1 d . . . H18 H 0.7491 0.5659 0.5373 0.034 Uiso 1 1 calc R . . C19 C 0.9777(2) 0.73307(14) 0.8916(2) 0.0237(7) Uani 1 1 d . . . H19A H 0.9156 0.7524 0.8683 0.028 Uiso 1 1 calc R B . H19B H 1.0161 0.7520 0.9485 0.028 Uiso 1 1 calc R . . C20 C 0.9644(2) 0.66911(14) 0.9091(2) 0.0216(6) Uani 1 1 d . B . C21 C 0.9540(3) 0.65068(16) 0.9880(2) 0.0301(8) Uani 1 1 d . . . H21 H 0.9593 0.6778 1.0336 0.036 Uiso 1 1 calc R B . C22 C 0.9357(3) 0.59216(16) 0.9979(2) 0.0333(8) Uani 1 1 d . B . H22 H 0.9291 0.5791 1.0506 0.040 Uiso 1 1 calc R . . C23 C 0.9269(2) 0.55261(15) 0.9284(2) 0.0293(7) Uani 1 1 d . . . H23 H 0.9144 0.5127 0.9336 0.035 Uiso 1 1 calc R B . C24 C 0.9374(2) 0.57395(14) 0.8512(2) 0.0218(6) Uani 1 1 d . B . C25A C 0.7965(3) 0.4982(2) 0.7323(4) 0.0223(19) Uiso 0.50 1 d PG B 1 C30A C 0.7278(4) 0.53268(17) 0.7478(4) 0.0305(16) Uiso 0.50 1 d PG B 1 H30 H 0.7419 0.5716 0.7678 0.037 Uiso 0.50 1 calc PR B 1 C29A C 0.6380(3) 0.5090(2) 0.7333(4) 0.0372(18) Uiso 0.50 1 d PG B 1 H29 H 0.5920 0.5321 0.7437 0.045 Uiso 0.50 1 calc PR B 1 C28A C 0.6169(3) 0.4509(2) 0.7034(4) 0.0289(17) Uiso 0.50 1 d PG B 1 H28 H 0.5569 0.4351 0.6937 0.035 Uiso 0.50 1 calc PR B 1 C27A C 0.6856(4) 0.41647(18) 0.6879(4) 0.0251(18) Uiso 0.50 1 d PG B 1 H27 H 0.6716 0.3776 0.6679 0.030 Uiso 0.50 1 calc PR B 1 C26A C 0.7754(4) 0.4401(2) 0.7024(5) 0.0272(19) Uiso 0.50 1 d PG B 1 H26 H 0.8214 0.4171 0.6920 0.033 Uiso 0.50 1 calc PR B 1 C25B C 0.8058(3) 0.4938(2) 0.7207(4) 0.0197(17) Uiso 0.50 1 d PG B 2 C26B C 0.7920(3) 0.4332(2) 0.7056(5) 0.0275(19) Uiso 0.50 1 d PG B 2 H26A H 0.8430 0.4091 0.7079 0.033 Uiso 0.50 1 calc PR B 2 C27B C 0.7020(4) 0.40852(17) 0.6870(5) 0.031(2) Uiso 0.50 1 d PG B 2 H27A H 0.6928 0.3680 0.6769 0.037 Uiso 0.50 1 calc PR B 2 C28B C 0.6258(3) 0.4444(2) 0.6835(4) 0.0296(17) Uiso 0.50 1 d PG B 2 H28A H 0.5655 0.4279 0.6711 0.036 Uiso 0.50 1 calc PR B 2 C29B C 0.6395(3) 0.5050(2) 0.6986(4) 0.0326(16) Uiso 0.50 1 d PG B 2 H29A H 0.5885 0.5291 0.6963 0.039 Uiso 0.50 1 calc PR B 2 C30B C 0.7295(3) 0.52969(17) 0.7172(4) 0.0278(15) Uiso 0.50 1 d PG B 2 H30A H 0.7387 0.5702 0.7273 0.033 Uiso 0.50 1 calc PR B 2 C31 C 0.9404(3) 0.80318(15) 0.5672(2) 0.0290(8) Uani 1 1 d . . . H31A H 0.9230 0.7776 0.5144 0.035 Uiso 1 1 calc R A . H31B H 0.9672 0.8394 0.5540 0.035 Uiso 1 1 calc R . . C32 C 0.8526(3) 0.81744(14) 0.5866(2) 0.0286(8) Uani 1 1 d . A . C33 C 0.8001(3) 0.86957(15) 0.5568(2) 0.0378(9) Uani 1 1 d . . . H33 H 0.8194 0.8981 0.5252 0.045 Uiso 1 1 calc R A . C34 C 0.7185(3) 0.87760(16) 0.5757(3) 0.0422(10) Uani 1 1 d . A . H34 H 0.6829 0.9123 0.5577 0.051 Uiso 1 1 calc R . . C35 C 0.6897(3) 0.83423(16) 0.6212(3) 0.0371(9) Uani 1 1 d . . . H35 H 0.6343 0.8388 0.6331 0.045 Uiso 1 1 calc R A . C36 C 0.7458(2) 0.78349(15) 0.6486(2) 0.0286(8) Uani 1 1 d . A . C37 C 0.6014(2) 0.69601(16) 0.6425(2) 0.0280(7) Uani 1 1 d . A . C38 C 0.5910(3) 0.65130(16) 0.5787(2) 0.0358(9) Uani 1 1 d . . . H38 H 0.6448 0.6365 0.5707 0.043 Uiso 1 1 calc R A . C39 C 0.5013(3) 0.62904(17) 0.5274(3) 0.0431(10) Uani 1 1 d . A . H39 H 0.4950 0.5989 0.4858 0.052 Uiso 1 1 calc R . . C40 C 0.4206(3) 0.65176(19) 0.5380(3) 0.0474(11) Uani 1 1 d . . . H40 H 0.3602 0.6368 0.5034 0.057 Uiso 1 1 calc R A . C41 C 0.4299(3) 0.69666(19) 0.6000(3) 0.0420(9) Uani 1 1 d . A . H41 H 0.3757 0.7125 0.6061 0.050 Uiso 1 1 calc R . . C42 C 0.5197(3) 0.71783(17) 0.6528(2) 0.0336(8) Uani 1 1 d . . . H42 H 0.5258 0.7470 0.6958 0.040 Uiso 1 1 calc R A . 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 Sm1 0.01809(8) 0.01838(7) 0.01593(7) -0.00091(6) 0.00379(6) 0.00035(6) P1 0.0188(4) 0.0246(4) 0.0171(4) -0.0008(3) 0.0033(3) 0.0031(3) P2 0.0224(4) 0.0185(4) 0.0210(4) 0.0004(3) 0.0032(3) -0.0012(3) P3 0.0223(4) 0.0478(6) 0.0201(4) -0.0038(4) 0.0055(4) 0.0082(4) O1 0.0198(10) 0.0232(10) 0.0182(10) -0.0039(9) 0.0037(8) 0.0024(9) O2 0.0261(12) 0.0353(13) 0.0203(11) 0.0059(10) 0.0053(9) 0.0087(10) O3 0.0260(12) 0.0183(10) 0.0195(10) -0.0015(8) 0.0060(9) -0.0016(9) O4 0.0317(13) 0.0233(12) 0.0312(13) -0.0029(10) 0.0057(11) 0.0036(10) O5 0.0271(12) 0.0429(14) 0.0288(12) 0.0133(11) 0.0151(10) 0.0123(11) N1 0.0209(13) 0.0240(14) 0.0171(12) -0.0038(10) 0.0033(10) -0.0024(10) N2 0.0233(13) 0.0186(12) 0.0217(13) -0.0002(10) 0.0059(11) -0.0002(10) N3 0.0268(14) 0.0204(13) 0.0196(13) -0.0016(10) 0.0071(11) -0.0040(11) N4 0.0175(12) 0.0208(12) 0.0176(12) -0.0017(10) 0.0039(10) 0.0002(10) N5 0.0193(13) 0.0229(13) 0.0183(12) 0.0027(10) 0.0030(10) 0.0003(10) N6 0.0235(14) 0.0247(14) 0.0218(13) -0.0065(11) 0.0006(11) 0.0009(11) C1 0.0180(14) 0.0268(16) 0.0173(14) -0.0018(12) 0.0036(12) -0.0017(12) C2 0.0212(15) 0.0265(16) 0.0221(15) -0.0023(12) 0.0036(13) -0.0046(13) C3 0.0287(17) 0.0203(15) 0.0251(16) -0.0105(12) 0.0034(14) -0.0043(13) C4 0.0282(17) 0.0222(16) 0.0235(16) -0.0024(12) 0.0060(14) -0.0042(13) C5 0.0285(17) 0.0246(16) 0.0266(17) -0.0009(13) 0.0095(14) -0.0056(14) C6 0.0248(16) 0.0275(16) 0.0230(16) -0.0020(13) 0.0076(13) -0.0050(13) C7 0.0200(15) 0.0236(15) 0.0207(15) -0.0016(12) 0.0038(12) 0.0021(12) C8 0.0195(15) 0.0206(14) 0.0217(15) 0.0027(12) 0.0066(12) 0.0023(12) C9 0.0219(16) 0.0290(17) 0.0275(17) 0.0001(13) 0.0070(14) 0.0050(13) C10 0.0258(17) 0.040(2) 0.0270(17) -0.0110(15) 0.0073(14) 0.0040(15) C11 0.0226(16) 0.0334(17) 0.0182(15) -0.0070(13) 0.0073(13) -0.0007(14) C12 0.0219(15) 0.0208(15) 0.0189(14) -0.0003(11) 0.0044(12) 0.0004(12) C13 0.0177(15) 0.0256(16) 0.0236(16) -0.0033(12) -0.0005(13) 0.0043(12) C14 0.0245(17) 0.0318(18) 0.0238(16) -0.0050(13) -0.0004(14) 0.0058(14) C15 0.0279(19) 0.035(2) 0.033(2) -0.0058(16) -0.0095(16) 0.0040(15) C16 0.0227(18) 0.032(2) 0.056(3) -0.0044(18) -0.0014(17) 0.0010(15) C17 0.0227(17) 0.0330(19) 0.046(2) 0.0014(16) 0.0098(16) 0.0029(15) C18 0.0218(16) 0.0285(17) 0.0315(18) -0.0017(14) 0.0079(14) 0.0027(13) C19 0.0252(16) 0.0252(16) 0.0197(15) -0.0031(12) 0.0074(13) 0.0004(13) C20 0.0178(14) 0.0286(16) 0.0173(14) -0.0014(12) 0.0054(12) 0.0019(12) C21 0.0322(19) 0.0350(18) 0.0203(16) -0.0031(14) 0.0070(14) -0.0025(15) C22 0.041(2) 0.0367(19) 0.0226(16) 0.0043(14) 0.0123(16) -0.0028(16) C23 0.0313(18) 0.0249(16) 0.0282(17) 0.0053(13) 0.0074(15) -0.0019(14) C24 0.0188(15) 0.0216(15) 0.0193(14) 0.0034(12) 0.0007(12) 0.0012(12) C31 0.039(2) 0.0216(15) 0.0191(15) 0.0017(12) 0.0034(14) -0.0024(14) C32 0.0302(18) 0.0244(16) 0.0211(15) -0.0031(13) -0.0015(14) -0.0008(14) C33 0.041(2) 0.0227(17) 0.0298(18) -0.0059(14) -0.0083(16) 0.0038(15) C34 0.036(2) 0.0243(18) 0.046(2) -0.0113(16) -0.0074(18) 0.0098(16) C35 0.0231(17) 0.037(2) 0.039(2) -0.0163(16) -0.0017(16) 0.0061(15) C36 0.0230(16) 0.0289(17) 0.0237(16) -0.0111(13) -0.0027(13) 0.0041(14) C37 0.0255(17) 0.0333(17) 0.0211(16) 0.0016(13) 0.0041(14) 0.0059(14) C38 0.046(2) 0.0295(18) 0.0269(18) 0.0022(14) 0.0088(17) 0.0090(17) C39 0.057(3) 0.032(2) 0.037(2) -0.0036(16) 0.013(2) -0.0069(19) C40 0.049(3) 0.047(2) 0.041(2) -0.0037(19) 0.011(2) -0.021(2) C41 0.030(2) 0.051(2) 0.044(2) -0.0026(19) 0.0128(18) -0.0052(18) C42 0.0264(18) 0.039(2) 0.0325(19) -0.0073(15) 0.0079(15) -0.0010(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O1 2.355(2) . ? Sm1 O3 2.348(2) . ? Sm1 O5 2.328(2) . ? Sm1 N1 2.664(3) . ? Sm1 N2 2.714(3) . ? Sm1 N3 2.684(3) . ? Sm1 N4 2.671(3) . ? Sm1 N5 2.684(3) . ? Sm1 N6 2.652(3) . ? P1 O1 1.511(2) . ? P1 O2 1.500(2) . ? P1 C12 1.831(3) . ? P1 C13 1.810(3) . ? P2 O3 1.511(2) . ? P2 O4 1.494(2) . ? P2 C24 1.823(3) . ? P2 C25A 1.878(4) . ? P2 C25B 1.766(4) . ? P3 O5 1.507(2) . ? P3 O6A 1.526(5) . ? P3 O6B 1.495(6) . ? P3 C36 1.817(4) . ? P3 C37 1.796(4) . ? N1 C1 1.483(4) . ? N1 C6 1.501(4) . ? N1 C7 1.486(4) . ? N2 C2 1.507(4) . ? N2 C3 1.478(4) . ? N2 C19 1.476(4) . ? N3 C4 1.499(4) . ? N3 C5 1.480(4) . ? N3 C31 1.482(4) . ? N4 C8 1.336(4) . ? N4 C12 1.353(4) . ? N5 C20 1.347(4) . ? N5 C24 1.346(4) . ? N6 C32 1.345(4) . ? N6 C36 1.344(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 C2 1.525(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 C4 1.519(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 C6 1.542(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C8 1.500(4) . ? C8 C9 1.388(5) . ? C9 H9 0.9300 . ? C9 C10 1.391(5) . ? C10 H10 0.9300 . ? C10 C11 1.396(5) . ? C11 H11 0.9300 . ? C11 C12 1.381(4) . ? C13 C14 1.400(4) . ? C13 C18 1.381(5) . ? C14 H14 0.9300 . ? C14 C15 1.389(5) . ? C15 H15 0.9300 . ? C15 C16 1.375(6) . ? C16 H16 0.9300 . ? C16 C17 1.394(6) . ? C17 H17 0.9300 . ? C17 C18 1.387(5) . ? C18 H18 0.9300 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 C20 1.498(4) . ? C20 C21 1.388(5) . ? C21 H21 0.9300 . ? C21 C22 1.371(5) . ? C22 H22 0.9300 . ? C22 C23 1.389(5) . ? C23 H23 0.9300 . ? C23 C24 1.385(5) . ? C25A C30A 1.3900 . ? C25A C26A 1.3900 . ? C30A H30 0.9300 . ? C30A C29A 1.3900 . ? C29A H29 0.9300 . ? C29A C28A 1.3900 . ? C28A H28 0.9300 . ? C28A C27A 1.3900 . ? C27A H27 0.9300 . ? C27A C26A 1.3900 . ? C26A H26 0.9300 . ? C25B C26B 1.3900 . ? C25B C30B 1.3900 . ? C26B H26A 0.9300 . ? C26B C27B 1.3900 . ? C27B H27A 0.9300 . ? C27B C28B 1.3900 . ? C28B H28A 0.9300 . ? C28B C29B 1.3900 . ? C29B H29A 0.9300 . ? C29B C30B 1.3900 . ? C30B H30A 0.9300 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 C32 1.503(5) . ? C32 C33 1.396(5) . ? C33 H33 0.9300 . ? C33 C34 1.385(6) . ? C34 H34 0.9300 . ? C34 C35 1.383(6) . ? C35 H35 0.9300 . ? C35 C36 1.392(5) . ? C37 C38 1.399(5) . ? C37 C42 1.392(5) . ? C38 H38 0.9300 . ? C38 C39 1.381(6) . ? C39 H39 0.9300 . ? C39 C40 1.389(6) . ? C40 H40 0.9300 . ? C40 C41 1.385(6) . ? C41 H41 0.9300 . ? C41 C42 1.379(5) . ? C42 H42 0.9300 . ? 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 O1 Sm1 N1 124.39(8) . . ? O1 Sm1 N2 147.95(7) . . ? O1 Sm1 N3 90.82(8) . . ? O1 Sm1 N4 66.26(7) . . ? O1 Sm1 N5 143.06(8) . . ? O1 Sm1 N6 68.86(7) . . ? O3 Sm1 O1 88.01(7) . . ? O3 Sm1 N1 89.81(8) . . ? O3 Sm1 N2 123.62(7) . . ? O3 Sm1 N3 149.81(8) . . ? O3 Sm1 N4 67.02(8) . . ? O3 Sm1 N5 66.30(7) . . ? O3 Sm1 N6 143.38(8) . . ? O5 Sm1 O1 86.23(8) . . ? O5 Sm1 O3 84.92(8) . . ? O5 Sm1 N1 148.78(8) . . ? O5 Sm1 N2 91.23(9) . . ? O5 Sm1 N3 125.12(8) . . ? O5 Sm1 N4 140.39(8) . . ? O5 Sm1 N5 66.30(8) . . ? O5 Sm1 N6 66.23(9) . . ? N1 Sm1 N2 66.38(8) . . ? N1 Sm1 N3 66.24(8) . . ? N1 Sm1 N4 62.00(8) . . ? N1 Sm1 N5 83.40(8) . . ? N3 Sm1 N2 64.83(8) . . ? N3 Sm1 N5 124.84(8) . . ? N4 Sm1 N2 127.27(8) . . ? N4 Sm1 N3 84.95(8) . . ? N4 Sm1 N5 120.67(8) . . ? N5 Sm1 N2 60.95(8) . . ? N6 Sm1 N1 126.56(8) . . ? N6 Sm1 N2 80.89(8) . . ? N6 Sm1 N3 61.81(9) . . ? N6 Sm1 N4 122.65(8) . . ? N6 Sm1 N5 116.68(8) . . ? O1 P1 C12 104.34(13) . . ? O1 P1 C13 108.81(15) . . ? O2 P1 O1 118.53(13) . . ? O2 P1 C12 110.11(14) . . ? O2 P1 C13 109.28(14) . . ? C13 P1 C12 104.85(14) . . ? O3 P2 C24 104.27(13) . . ? O3 P2 C25A 110.8(2) . . ? O3 P2 C25B 108.5(2) . . ? O4 P2 O3 117.02(14) . . ? O4 P2 C24 110.40(14) . . ? O4 P2 C25A 113.2(2) . . ? O4 P2 C25B 108.6(2) . . ? C24 P2 C25A 99.3(2) . . ? C25B P2 C24 107.7(2) . . ? C25B P2 C25A 8.4(3) . . ? O5 P3 O6A 122.8(2) . . ? O5 P3 C36 103.71(15) . . ? O5 P3 C37 108.22(16) . . ? O6A P3 C36 99.8(2) . . ? O6A P3 C37 113.0(2) . . ? O6B P3 O5 110.7(2) . . ? O6B P3 O6A 20.1(2) . . ? O6B P3 C36 119.6(3) . . ? O6B P3 C37 106.7(3) . . ? C37 P3 C36 107.45(15) . . ? P1 O1 Sm1 133.07(12) . . ? P2 O3 Sm1 133.08(12) . . ? P3 O5 Sm1 133.33(14) . . ? C1 N1 Sm1 106.78(19) . . ? C1 N1 C6 110.7(2) . . ? C1 N1 C7 108.4(2) . . ? C6 N1 Sm1 114.50(18) . . ? C7 N1 Sm1 107.06(17) . . ? C7 N1 C6 109.2(3) . . ? C2 N2 Sm1 112.94(18) . . ? C3 N2 Sm1 108.02(17) . . ? C3 N2 C2 109.9(2) . . ? C19 N2 Sm1 107.50(18) . . ? C19 N2 C2 109.7(2) . . ? C19 N2 C3 108.6(2) . . ? C4 N3 Sm1 116.55(19) . . ? C5 N3 Sm1 105.11(18) . . ? C5 N3 C4 110.5(3) . . ? C5 N3 C31 108.7(3) . . ? C31 N3 Sm1 106.07(19) . . ? C31 N3 C4 109.5(2) . . ? C8 N4 Sm1 118.12(19) . . ? C8 N4 C12 119.0(3) . . ? C12 N4 Sm1 122.1(2) . . ? C20 N5 Sm1 118.3(2) . . ? C24 N5 Sm1 120.7(2) . . ? C24 N5 C20 118.2(3) . . ? C32 N6 Sm1 118.9(2) . . ? C36 N6 Sm1 122.0(2) . . ? C36 N6 C32 119.0(3) . . ? N1 C1 H1A 108.9 . . ? N1 C1 H1B 108.9 . . ? N1 C1 C2 113.2(2) . . ? H1A C1 H1B 107.8 . . ? C2 C1 H1A 108.9 . . ? C2 C1 H1B 108.9 . . ? N2 C2 C1 114.6(2) . . ? N2 C2 H2A 108.6 . . ? N2 C2 H2B 108.6 . . ? C1 C2 H2A 108.6 . . ? C1 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? N2 C3 H3A 109.1 . . ? N2 C3 H3B 109.1 . . ? N2 C3 C4 112.4(3) . . ? H3A C3 H3B 107.9 . . ? C4 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? N3 C4 C3 113.1(3) . . ? N3 C4 H4A 109.0 . . ? N3 C4 H4B 109.0 . . ? C3 C4 H4A 109.0 . . ? C3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? N3 C5 H5A 109.2 . . ? N3 C5 H5B 109.2 . . ? N3 C5 C6 112.2(3) . . ? H5A C5 H5B 107.9 . . ? C6 C5 H5A 109.2 . . ? C6 C5 H5B 109.2 . . ? N1 C6 C5 113.4(3) . . ? N1 C6 H6A 108.9 . . ? N1 C6 H6B 108.9 . . ? C5 C6 H6A 108.9 . . ? C5 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? N1 C7 H7A 109.3 . . ? N1 C7 H7B 109.3 . . ? N1 C7 C8 111.5(2) . . ? H7A C7 H7B 108.0 . . ? C8 C7 H7A 109.3 . . ? C8 C7 H7B 109.3 . . ? N4 C8 C7 116.1(3) . . ? N4 C8 C9 121.7(3) . . ? C9 C8 C7 122.0(3) . . ? C8 C9 H9 120.1 . . ? C8 C9 C10 119.7(3) . . ? C10 C9 H9 120.1 . . ? C9 C10 H10 120.9 . . ? C9 C10 C11 118.2(3) . . ? C11 C10 H10 120.9 . . ? C10 C11 H11 120.5 . . ? C12 C11 C10 119.0(3) . . ? C12 C11 H11 120.5 . . ? N4 C12 P1 113.7(2) . . ? N4 C12 C11 122.3(3) . . ? C11 C12 P1 123.9(2) . . ? C14 C13 P1 119.9(3) . . ? C18 C13 P1 120.4(2) . . ? C18 C13 C14 119.7(3) . . ? C13 C14 H14 120.5 . . ? C15 C14 C13 119.0(4) . . ? C15 C14 H14 120.5 . . ? C14 C15 H15 119.4 . . ? C16 C15 C14 121.2(3) . . ? C16 C15 H15 119.4 . . ? C15 C16 H16 120.0 . . ? C15 C16 C17 120.0(4) . . ? C17 C16 H16 120.0 . . ? C16 C17 H17 120.5 . . ? C18 C17 C16 119.1(4) . . ? C18 C17 H17 120.5 . . ? C13 C18 C17 121.1(3) . . ? C13 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? N2 C19 H19A 109.0 . . ? N2 C19 H19B 109.0 . . ? N2 C19 C20 113.0(3) . . ? H19A C19 H19B 107.8 . . ? C20 C19 H19A 109.0 . . ? C20 C19 H19B 109.0 . . ? N5 C20 C19 116.1(3) . . ? N5 C20 C21 122.0(3) . . ? C21 C20 C19 121.8(3) . . ? C20 C21 H21 120.3 . . ? C22 C21 C20 119.4(3) . . ? C22 C21 H21 120.3 . . ? C21 C22 H22 120.4 . . ? C21 C22 C23 119.3(3) . . ? C23 C22 H22 120.4 . . ? C22 C23 H23 120.8 . . ? C24 C23 C22 118.5(3) . . ? C24 C23 H23 120.8 . . ? N5 C24 P2 114.2(2) . . ? N5 C24 C23 122.6(3) . . ? C23 C24 P2 123.1(2) . . ? C30A C25A P2 121.4(3) . . ? C30A C25A C26A 120.0 . . ? C26A C25A P2 118.6(3) . . ? C25A C30A H30 120.0 . . ? C29A C30A C25A 120.0 . . ? C29A C30A H30 120.0 . . ? C30A C29A H29 120.0 . . ? C30A C29A C28A 120.0 . . ? C28A C29A H29 120.0 . . ? C29A C28A H28 120.0 . . ? C27A C28A C29A 120.0 . . ? C27A C28A H28 120.0 . . ? C28A C27A H27 120.0 . . ? C28A C27A C26A 120.0 . . ? C26A C27A H27 120.0 . . ? C25A C26A H26 120.0 . . ? C27A C26A C25A 120.0 . . ? C27A C26A H26 120.0 . . ? C26B C25B P2 123.2(3) . . ? C26B C25B C30B 120.0 . . ? C30B C25B P2 116.7(3) . . ? C25B C26B H26A 120.0 . . ? C25B C26B C27B 120.0 . . ? C27B C26B H26A 120.0 . . ? C26B C27B H27A 120.0 . . ? C26B C27B C28B 120.0 . . ? C28B C27B H27A 120.0 . . ? C27B C28B H28A 120.0 . . ? C29B C28B C27B 120.0 . . ? C29B C28B H28A 120.0 . . ? C28B C29B H29A 120.0 . . ? C30B C29B C28B 120.0 . . ? C30B C29B H29A 120.0 . . ? C25B C30B H30A 120.0 . . ? C29B C30B C25B 120.0 . . ? C29B C30B H30A 120.0 . . ? N3 C31 H31A 109.6 . . ? N3 C31 H31B 109.6 . . ? N3 C31 C32 110.2(3) . . ? H31A C31 H31B 108.1 . . ? C32 C31 H31A 109.6 . . ? C32 C31 H31B 109.6 . . ? N6 C32 C31 115.2(3) . . ? N6 C32 C33 122.1(4) . . ? C33 C32 C31 122.7(3) . . ? C32 C33 H33 120.9 . . ? C34 C33 C32 118.2(4) . . ? C34 C33 H33 120.9 . . ? C33 C34 H34 119.9 . . ? C35 C34 C33 120.2(3) . . ? C35 C34 H34 119.9 . . ? C34 C35 H35 120.9 . . ? C34 C35 C36 118.2(4) . . ? C36 C35 H35 120.9 . . ? N6 C36 P3 113.9(2) . . ? N6 C36 C35 122.4(4) . . ? C35 C36 P3 123.8(3) . . ? C38 C37 P3 119.5(3) . . ? C42 C37 P3 121.7(3) . . ? C42 C37 C38 118.8(3) . . ? C37 C38 H38 119.8 . . ? C39 C38 C37 120.4(4) . . ? C39 C38 H38 119.8 . . ? C38 C39 H39 120.0 . . ? C38 C39 C40 120.0(4) . . ? C40 C39 H39 120.0 . . ? C39 C40 H40 120.0 . . ? C41 C40 C39 120.1(4) . . ? C41 C40 H40 120.0 . . ? C40 C41 H41 120.0 . . ? C42 C41 C40 119.9(4) . . ? C42 C41 H41 120.0 . . ? C37 C42 H42 119.6 . . ? C41 C42 C37 120.8(4) . . ? C41 C42 H42 119.6 . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 0.000 0.000 10.5 0.0 ? 2 -0.586 -0.096 -0.086 1635.3 372.4 ? 3 0.500 0.500 0.500 10.5 0.0 ? # start Validation Reply Form _vrf_PLAT602_I ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: The structure contains a number of severely disordered solvent molecules (H2O, methanol). Their contribution to the structural fctors was taken into account by applying MASK procedure of OLEX2 program package. ; # end Validation Reply Form # Attachment '6394_web_deposit_cif_file_4_DmitryYufit_1311257364.TmL3.cif' data_TmL3_11srv130c _database_code_depnum_ccdc_archive 'CCDC 836101' #TrackingRef '6394_web_deposit_cif_file_4_DmitryYufit_1311257364.TmL3.cif' _audit_creation_date 2011-07-11 _audit_creation_method ; Olex2 1.1-beta (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H42 N6 O6 P3 Tm' _chemical_formula_sum 'C42 H42 N6 O6 P3 Tm' _chemical_formula_weight 988.66 _chemical_melting_point ? 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' Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.9636(4) _cell_length_b 22.5457(6) _cell_length_c 15.8430(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.991(10) _cell_angle_gamma 90.00 _cell_volume 4956.0(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7555 _cell_measurement_temperature 120 _cell_measurement_theta_max 30.86 _cell_measurement_theta_min 2.33 _exptl_absorpt_coefficient_mu 1.933 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.4530 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2006/1 (Bruker,2006) was used for absorption correction. R(int) was 0.0561 before and 0.0380 after correction. The Ratio of minimum to maximum transmission is 0.607157217531. The \l/2 correction factor is 0.0015 ; _exptl_crystal_colour colourless _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1992 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.14 _exptl_special_details ; The data collection nominally covered a full sphere of reciprocal space by a combination of 5 sets of \w scans each set at different \f and/or 2\q angles and each scan (10.00 s exposure) covering -0.300\ degrees in \w. The crystal to detector distance was 4.85 cm. ; _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_unetI/netI 0.0289 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 81026 _diffrn_reflns_theta_full 29.00 _diffrn_reflns_theta_max 29.00 _diffrn_reflns_theta_min 0.90 _diffrn_ambient_temperature 120 _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 5.6 _diffrn_detector_type 'Bruker SMART CCD 6000 area detector' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART CCD 6000 area detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_xray_symbol K-L~3~ _diffrn_source 'sealed X-ray tube' _diffrn_source_current 10.0 _diffrn_source_power 0.3 _diffrn_source_target Mo _diffrn_source_voltage 30.0 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 11129 _reflns_number_total 13155 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'SAINT v6.45A (Bruker, 2003)' _computing_data_collection 'SMART v5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT v6.45A (Bruker, 2003)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)/Bruker' _refine_diff_density_max 4.603 _refine_diff_density_min -1.348 _refine_diff_density_rms 0.142 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 492 _refine_ls_number_reflns 13155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0434 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+26.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1176 _refine_ls_wR_factor_ref 0.1219 _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. The structure contains a number of severely disordered solvent molecules (H2O, methanol). Their contribution to the structural fctors was taken into account by applying MASK procedure of OLEX2 program package. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Tm1 Tm 0.571663(12) 0.175885(7) 0.819790(11) 0.01765(6) Uani 1 1 d . A . P1 P 0.67434(7) 0.14670(5) 1.05335(7) 0.02032(19) Uani 1 1 d . . . P2 P 0.58066(8) 0.03044(5) 0.74792(7) 0.0244(2) Uani 1 1 d . . . P3 P 0.77904(8) 0.21827(6) 0.78660(8) 0.0294(2) Uani 1 1 d . . . O1 O 0.6756(2) 0.17374(12) 0.9663(2) 0.0224(6) Uani 1 1 d . . . O2 O 0.6927(2) 0.18590(15) 1.1338(2) 0.0284(6) Uani 1 1 d . . . O3 O 0.5849(2) 0.07577(13) 0.81997(18) 0.0224(6) Uani 1 1 d . A . O4 O 0.5054(3) -0.01678(14) 0.7292(2) 0.0339(7) Uani 1 1 d . B . O5 O 0.7064(2) 0.17236(15) 0.7879(2) 0.0295(7) Uani 1 1 d . A . O6B O 0.7786(5) 0.2283(3) 0.6928(4) 0.0216(13) Uiso 0.50 1 d P A 1 N1 N 0.3851(2) 0.16475(15) 0.7644(2) 0.0208(6) Uani 1 1 d . . . N2 N 0.4786(2) 0.24161(15) 0.6732(2) 0.0215(6) Uani 1 1 d . A . N3 N 0.4880(3) 0.27043(15) 0.8533(2) 0.0232(7) Uani 1 1 d . A . N4 N 0.5008(2) 0.12296(15) 0.9286(2) 0.0194(6) Uani 1 1 d . . . N5 N 0.5437(2) 0.13236(16) 0.6567(2) 0.0227(7) Uani 1 1 d . . . N6 N 0.6728(3) 0.27276(16) 0.8642(2) 0.0235(7) Uani 1 1 d . . . C1 C 0.3467(3) 0.16799(19) 0.6635(3) 0.0215(7) Uani 1 1 d . . . H1A H 0.2770 0.1650 0.6407 0.026 Uiso 1 1 calc R . . H1B H 0.3708 0.1344 0.6400 0.026 Uiso 1 1 calc R . . C2 C 0.3743(3) 0.22470(19) 0.6281(3) 0.0242(8) Uani 1 1 d . . . H2A H 0.3591 0.2204 0.5633 0.029 Uiso 1 1 calc R . . H2B H 0.3352 0.2568 0.6362 0.029 Uiso 1 1 calc R . . C3 C 0.4861(3) 0.30454(19) 0.7013(3) 0.0247(8) Uani 1 1 d . . . H3A H 0.4492 0.3287 0.6493 0.030 Uiso 1 1 calc R . . H3B H 0.5530 0.3169 0.7214 0.030 Uiso 1 1 calc R . . C4 C 0.4496(3) 0.31499(18) 0.7775(3) 0.0238(8) Uani 1 1 d . . . H4A H 0.4682 0.3545 0.8021 0.029 Uiso 1 1 calc R . . H4B H 0.3797 0.3132 0.7527 0.029 Uiso 1 1 calc R . . C5 C 0.4085(3) 0.24818(19) 0.8784(3) 0.0247(8) Uani 1 1 d . . . H5A H 0.3744 0.2815 0.8911 0.030 Uiso 1 1 calc R . . H5B H 0.4348 0.2244 0.9333 0.030 Uiso 1 1 calc R . . C6 C 0.3379(3) 0.21062(19) 0.8020(3) 0.0249(8) Uani 1 1 d . . . H6A H 0.2938 0.1910 0.8249 0.030 Uiso 1 1 calc R . . H6B H 0.3001 0.2367 0.7529 0.030 Uiso 1 1 calc R . . C7 C 0.3641(3) 0.10509(19) 0.7916(3) 0.0232(8) Uani 1 1 d . . . H7A H 0.3847 0.0751 0.7589 0.028 Uiso 1 1 calc R . . H7B H 0.2951 0.1008 0.7755 0.028 Uiso 1 1 calc R . . C8 C 0.4150(3) 0.09595(18) 0.8921(3) 0.0216(7) Uani 1 1 d . . . C9 C 0.3789(3) 0.05990(19) 0.9428(3) 0.0262(8) Uani 1 1 d . . . H9 H 0.3189 0.0420 0.9157 0.031 Uiso 1 1 calc R . . C10 C 0.4334(3) 0.0509(2) 1.0343(3) 0.0291(9) Uani 1 1 d . . . H10 H 0.4103 0.0269 1.0695 0.035 Uiso 1 1 calc R . . C11 C 0.5234(3) 0.0783(2) 1.0730(3) 0.0250(8) Uani 1 1 d . . . H11 H 0.5611 0.0734 1.1343 0.030 Uiso 1 1 calc R . . C12 C 0.5550(3) 0.11302(18) 1.0174(3) 0.0208(7) Uani 1 1 d . . . C13 C 0.7561(3) 0.08443(19) 1.0850(3) 0.0234(8) Uani 1 1 d . . . C14 C 0.7963(3) 0.0660(2) 1.1757(3) 0.0294(9) Uani 1 1 d . . . H14 H 0.7824 0.0863 1.2205 0.035 Uiso 1 1 calc R . . C15 C 0.8579(4) 0.0169(2) 1.1986(4) 0.0401(12) Uani 1 1 d . . . H15 H 0.8843 0.0044 1.2589 0.048 Uiso 1 1 calc R . . C16 C 0.8797(4) -0.0128(2) 1.1344(4) 0.0391(12) Uani 1 1 d . . . H16 H 0.9220 -0.0448 1.1510 0.047 Uiso 1 1 calc R . . C17 C 0.8388(3) 0.0047(2) 1.0434(4) 0.0330(10) Uani 1 1 d . . . H17 H 0.8526 -0.0162 0.9991 0.040 Uiso 1 1 calc R . . C18 C 0.7773(3) 0.05335(19) 1.0190(3) 0.0258(8) Uani 1 1 d . . . H18 H 0.7504 0.0652 0.9584 0.031 Uiso 1 1 calc R . . C19 C 0.5264(3) 0.23438(19) 0.6075(3) 0.0248(8) Uani 1 1 d . . . H19A H 0.5895 0.2529 0.6316 0.030 Uiso 1 1 calc R B . H19B H 0.4887 0.2541 0.5509 0.030 Uiso 1 1 calc R . . C20 C 0.5372(3) 0.16998(19) 0.5893(3) 0.0239(8) Uani 1 1 d . B . C21 C 0.5483(3) 0.1519(2) 0.5096(3) 0.0305(9) Uani 1 1 d . . . H21 H 0.5446 0.1791 0.4644 0.037 Uiso 1 1 calc R B . C22 C 0.5650(4) 0.0921(2) 0.4994(3) 0.0330(10) Uani 1 1 d . B . H22 H 0.5708 0.0784 0.4463 0.040 Uiso 1 1 calc R . . C23 C 0.5729(3) 0.0532(2) 0.5699(3) 0.0299(9) Uani 1 1 d . . . H23 H 0.5854 0.0132 0.5653 0.036 Uiso 1 1 calc R B . C24 C 0.5618(3) 0.07506(18) 0.6470(3) 0.0227(8) Uani 1 1 d . B . C25B C 0.6920(4) -0.0057(3) 0.7810(5) 0.031(2) Uiso 0.50 1 d PG B 1 C26B C 0.7042(5) -0.0664(3) 0.7963(6) 0.035(2) Uiso 0.50 1 d PG B 1 H26 H 0.6523 -0.0898 0.7944 0.042 Uiso 0.50 1 calc PR B 1 C27B C 0.7939(5) -0.0921(3) 0.8145(6) 0.039(2) Uiso 0.50 1 d PG B 1 H27 H 0.8020 -0.1328 0.8248 0.047 Uiso 0.50 1 calc PR B 1 C28A C 0.8715(4) -0.0572(3) 0.8174(6) 0.040(2) Uiso 0.50 1 d PG B 1 H28 H 0.9315 -0.0744 0.8296 0.048 Uiso 0.50 1 calc PR B 1 C29A C 0.8593(5) 0.0035(3) 0.8021(6) 0.056(3) Uiso 0.50 1 d PG B 1 H29 H 0.9112 0.0270 0.8040 0.067 Uiso 0.50 1 calc PR B 1 C30A C 0.7696(5) 0.0293(2) 0.7839(6) 0.043(2) Uiso 0.50 1 d PG B 1 H30 H 0.7615 0.0699 0.7736 0.052 Uiso 0.50 1 calc PR B 1 C31 C 0.5612(3) 0.30029(19) 0.9329(3) 0.0265(8) Uani 1 1 d . . . H31A H 0.5792 0.2745 0.9857 0.032 Uiso 1 1 calc R A . H31B H 0.5345 0.3365 0.9469 0.032 Uiso 1 1 calc R . . C32 C 0.6481(3) 0.31449(19) 0.9116(3) 0.0266(9) Uani 1 1 d . A . C33 C 0.7016(4) 0.3664(2) 0.9409(3) 0.0342(10) Uani 1 1 d . . . H33 H 0.6832 0.3948 0.9738 0.041 Uiso 1 1 calc R A . C34 C 0.7825(4) 0.3749(2) 0.9199(4) 0.0410(12) Uani 1 1 d . A . H34 H 0.8182 0.4097 0.9369 0.049 Uiso 1 1 calc R . . C35 C 0.8098(3) 0.3309(2) 0.8730(4) 0.0350(11) Uani 1 1 d . . . H35 H 0.8650 0.3351 0.8598 0.042 Uiso 1 1 calc R A . C36 C 0.7532(3) 0.2804(2) 0.8463(3) 0.0288(9) Uani 1 1 d . A . C37 C 0.8975(3) 0.1924(2) 0.8549(3) 0.0279(9) Uani 1 1 d . A . C38 C 0.9090(4) 0.1486(2) 0.9200(3) 0.0337(10) Uani 1 1 d . . . H38 H 0.8554 0.1332 0.9287 0.040 Uiso 1 1 calc R A . C39 C 1.0007(5) 0.1277(2) 0.9722(4) 0.0415(12) Uani 1 1 d . A . H39 H 1.0079 0.0981 1.0151 0.050 Uiso 1 1 calc R . . C40 C 1.0806(5) 0.1504(3) 0.9607(4) 0.0462(14) Uani 1 1 d . . . H40 H 1.1416 0.1363 0.9959 0.055 Uiso 1 1 calc R A . C41 C 1.0700(4) 0.1949(3) 0.8959(4) 0.0406(12) Uani 1 1 d . A . H41 H 1.1239 0.2106 0.8883 0.049 Uiso 1 1 calc R . . C42 C 0.9787(3) 0.2153(2) 0.8433(3) 0.0330(10) Uani 1 1 d . . . H42 H 0.9715 0.2445 0.7998 0.040 Uiso 1 1 calc R A . O6A O 0.7751(5) 0.2498(4) 0.6988(5) 0.0308(16) Uiso 0.50 1 d P A 2 C25A C 0.7043(3) 0.0009(2) 0.7677(4) 0.0170(16) Uiso 0.50 1 d PG B 2 C30B C 0.7718(4) 0.03432(18) 0.7475(4) 0.0212(15) Uiso 0.50 1 d PG B 2 H30A H 0.7570 0.0728 0.7254 0.025 Uiso 0.50 1 calc PR B 2 C29B C 0.8615(3) 0.0103(2) 0.7604(4) 0.0292(18) Uiso 0.50 1 d PG B 2 H29A H 0.9067 0.0326 0.7469 0.035 Uiso 0.50 1 calc PR B 2 C28B C 0.8837(3) -0.0472(2) 0.7934(4) 0.0219(15) Uiso 0.50 1 d PG B 2 H28A H 0.9437 -0.0633 0.8021 0.026 Uiso 0.50 1 calc PR B 2 C27A C 0.8162(4) -0.08060(19) 0.8136(4) 0.0202(16) Uiso 0.50 1 d PG B 2 H27A H 0.8310 -0.1190 0.8357 0.024 Uiso 0.50 1 calc PR B 2 C26A C 0.7265(4) -0.0566(2) 0.8007(4) 0.0188(15) Uiso 0.50 1 d PG B 2 H26A H 0.6813 -0.0789 0.8142 0.023 Uiso 0.50 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 Tm1 0.01871(9) 0.01668(9) 0.01649(8) 0.00058(6) 0.00535(6) 0.00007(6) P1 0.0197(4) 0.0220(5) 0.0177(4) 0.0007(4) 0.0053(4) -0.0030(4) P2 0.0260(5) 0.0187(5) 0.0221(5) -0.0014(4) 0.0017(4) 0.0020(4) P3 0.0228(5) 0.0449(7) 0.0196(5) 0.0020(5) 0.0069(4) -0.0075(5) O1 0.0172(13) 0.0195(13) 0.0288(15) 0.0011(11) 0.0065(11) -0.0038(10) O2 0.0278(15) 0.0338(17) 0.0225(14) -0.0052(12) 0.0082(12) -0.0063(13) O3 0.0280(14) 0.0192(13) 0.0173(13) 0.0008(10) 0.0056(11) 0.0021(11) O4 0.0381(18) 0.0208(15) 0.0327(17) 0.0019(12) 0.0018(14) -0.0054(13) O5 0.0238(15) 0.0388(18) 0.0282(16) -0.0105(13) 0.0122(13) -0.0100(13) N1 0.0203(15) 0.0228(16) 0.0178(15) 0.0022(12) 0.0054(13) 0.0026(12) N2 0.0200(15) 0.0218(16) 0.0205(15) 0.0017(12) 0.0050(13) 0.0021(13) N3 0.0283(17) 0.0202(16) 0.0188(15) 0.0026(12) 0.0063(13) 0.0045(13) N4 0.0202(15) 0.0186(15) 0.0185(15) 0.0009(12) 0.0062(12) 0.0023(12) N5 0.0214(16) 0.0246(17) 0.0179(15) -0.0030(13) 0.0027(13) 0.0003(13) N6 0.0237(16) 0.0227(16) 0.0185(15) 0.0059(13) 0.0014(13) -0.0014(13) C1 0.0177(17) 0.029(2) 0.0159(17) 0.0010(14) 0.0042(14) 0.0014(15) C2 0.0245(19) 0.0252(19) 0.0192(18) -0.0003(15) 0.0039(15) 0.0022(16) C3 0.028(2) 0.0205(18) 0.0216(18) 0.0049(15) 0.0047(16) 0.0010(16) C4 0.026(2) 0.0182(18) 0.0255(19) 0.0034(15) 0.0079(16) 0.0047(15) C5 0.0255(19) 0.0216(19) 0.028(2) -0.0011(15) 0.0110(16) 0.0022(15) C6 0.0239(19) 0.027(2) 0.0248(19) 0.0034(16) 0.0103(16) 0.0041(16) C7 0.0180(17) 0.0245(19) 0.0225(19) 0.0028(15) 0.0022(15) -0.0017(14) C8 0.0217(18) 0.0199(18) 0.0220(18) 0.0009(14) 0.0069(15) 0.0002(14) C9 0.0214(19) 0.025(2) 0.030(2) 0.0004(16) 0.0068(16) -0.0035(15) C10 0.026(2) 0.031(2) 0.030(2) 0.0061(17) 0.0101(17) -0.0050(17) C11 0.0216(19) 0.030(2) 0.0218(19) 0.0025(16) 0.0061(15) -0.0027(16) C12 0.0231(18) 0.0202(18) 0.0182(17) -0.0015(14) 0.0068(15) -0.0008(14) C13 0.0178(17) 0.0249(19) 0.0235(19) 0.0060(15) 0.0031(15) -0.0040(15) C14 0.026(2) 0.031(2) 0.023(2) 0.0059(17) -0.0003(16) -0.0024(17) C15 0.030(2) 0.039(3) 0.036(3) 0.013(2) -0.006(2) -0.003(2) C16 0.027(2) 0.030(2) 0.047(3) 0.005(2) -0.003(2) -0.0022(18) C17 0.026(2) 0.030(2) 0.040(3) 0.0024(19) 0.0084(19) 0.0018(18) C18 0.0198(18) 0.027(2) 0.027(2) 0.0063(16) 0.0047(16) 0.0009(15) C19 0.027(2) 0.027(2) 0.0200(18) 0.0047(15) 0.0087(16) 0.0022(16) C20 0.0224(19) 0.026(2) 0.0183(18) -0.0009(15) 0.0025(15) -0.0008(15) C21 0.031(2) 0.035(2) 0.023(2) 0.0012(18) 0.0079(17) 0.0024(19) C22 0.037(2) 0.040(3) 0.022(2) -0.0061(18) 0.0108(18) 0.002(2) C23 0.029(2) 0.030(2) 0.028(2) -0.0080(17) 0.0089(17) 0.0031(17) C24 0.0202(18) 0.0228(19) 0.0219(18) -0.0032(15) 0.0041(15) -0.0006(14) C31 0.032(2) 0.0201(19) 0.0213(19) -0.0023(15) 0.0027(16) 0.0020(16) C32 0.025(2) 0.0216(19) 0.0214(19) 0.0005(15) -0.0055(16) -0.0021(15) C33 0.036(2) 0.025(2) 0.028(2) 0.0022(17) -0.0045(19) -0.0041(18) C34 0.037(3) 0.023(2) 0.049(3) 0.007(2) -0.001(2) -0.0073(19) C35 0.023(2) 0.031(2) 0.041(3) 0.0126(19) 0.0008(19) -0.0069(17) C36 0.026(2) 0.028(2) 0.027(2) 0.0117(17) 0.0031(17) -0.0031(17) C37 0.028(2) 0.030(2) 0.024(2) 0.0008(17) 0.0081(17) -0.0020(17) C38 0.039(3) 0.033(2) 0.027(2) 0.0003(18) 0.0101(19) -0.007(2) C39 0.058(3) 0.030(2) 0.036(3) 0.005(2) 0.016(2) 0.007(2) C40 0.048(3) 0.049(3) 0.038(3) 0.005(2) 0.012(2) 0.024(3) C41 0.030(2) 0.053(3) 0.040(3) 0.008(2) 0.014(2) 0.009(2) C42 0.027(2) 0.037(2) 0.035(2) 0.0034(19) 0.0107(19) 0.0021(18) _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 Tm1 O1 2.260(3) . ? Tm1 O3 2.266(3) . ? Tm1 O5 2.255(3) . ? Tm1 N1 2.607(3) . ? Tm1 N2 2.666(3) . ? Tm1 N3 2.626(3) . ? Tm1 N4 2.625(3) . ? Tm1 N5 2.646(3) . ? Tm1 N6 2.599(4) . ? P1 O1 1.515(3) . ? P1 O2 1.489(3) . ? P1 C12 1.825(4) . ? P1 C13 1.805(4) . ? P2 O3 1.516(3) . ? P2 O4 1.496(3) . ? P2 C24 1.820(4) . ? P2 C25B 1.750(5) . ? P2 C25A 1.879(4) . ? P3 O5 1.507(3) . ? P3 O6B 1.501(6) . ? P3 C36 1.812(5) . ? P3 C37 1.794(5) . ? P3 O6A 1.544(7) . ? N1 C1 1.485(5) . ? N1 C6 1.495(5) . ? N1 C7 1.482(5) . ? N2 C2 1.502(5) . ? N2 C3 1.479(5) . ? N2 C19 1.475(5) . ? N3 C4 1.505(5) . ? N3 C5 1.475(6) . ? N3 C31 1.486(5) . ? N4 C8 1.341(5) . ? N4 C12 1.353(5) . ? N5 C20 1.339(5) . ? N5 C24 1.341(5) . ? N6 C32 1.339(6) . ? N6 C36 1.347(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 C2 1.515(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 C4 1.519(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 C6 1.530(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C8 1.499(6) . ? C8 C9 1.386(6) . ? C9 H9 0.9300 . ? C9 C10 1.387(6) . ? C10 H10 0.9300 . ? C10 C11 1.398(6) . ? C11 H11 0.9300 . ? C11 C12 1.387(6) . ? C13 C14 1.397(6) . ? C13 C18 1.392(6) . ? C14 H14 0.9300 . ? C14 C15 1.398(7) . ? C15 H15 0.9300 . ? C15 C16 1.357(8) . ? C16 H16 0.9300 . ? C16 C17 1.395(7) . ? C17 H17 0.9300 . ? C17 C18 1.390(6) . ? C18 H18 0.9300 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 C20 1.501(6) . ? C20 C21 1.394(6) . ? C21 H21 0.9300 . ? C21 C22 1.390(7) . ? C22 H22 0.9300 . ? C22 C23 1.390(7) . ? C23 H23 0.9300 . ? C23 C24 1.384(6) . ? C25B C26B 1.3900 . ? C25B C30A 1.3900 . ? C26B H26 0.9300 . ? C26B C27B 1.3900 . ? C27B H27 0.9300 . ? C27B C28A 1.3900 . ? C28A H28 0.9300 . ? C28A C29A 1.3900 . ? C29A H29 0.9300 . ? C29A C30A 1.3900 . ? C30A H30 0.9300 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 C32 1.495(7) . ? C32 C33 1.395(6) . ? C33 H33 0.9300 . ? C33 C34 1.384(8) . ? C34 H34 0.9300 . ? C34 C35 1.390(8) . ? C35 H35 0.9300 . ? C35 C36 1.386(6) . ? C37 C38 1.392(6) . ? C37 C42 1.393(7) . ? C38 H38 0.9300 . ? C38 C39 1.392(8) . ? C39 H39 0.9300 . ? C39 C40 1.373(9) . ? C40 H40 0.9300 . ? C40 C41 1.400(8) . ? C41 H41 0.9300 . ? C41 C42 1.386(7) . ? C42 H42 0.9300 . ? C25A C30B 1.3900 . ? C25A C26A 1.3900 . ? C30B H30A 0.9300 . ? C30B C29B 1.3900 . ? C29B H29A 0.9300 . ? C29B C28B 1.3900 . ? C28B H28A 0.9300 . ? C28B C27A 1.3900 . ? C27A H27A 0.9300 . ? C27A C26A 1.3900 . ? C26A H26A 0.9300 . ? 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 O1 Tm1 O3 87.20(10) . . ? O1 Tm1 N1 125.61(11) . . ? O1 Tm1 N2 147.24(10) . . ? O1 Tm1 N3 90.37(11) . . ? O1 Tm1 N4 66.89(10) . . ? O1 Tm1 N5 142.30(11) . . ? O1 Tm1 N6 68.47(10) . . ? O3 Tm1 N1 89.24(11) . . ? O3 Tm1 N2 124.86(10) . . ? O3 Tm1 N3 148.95(11) . . ? O3 Tm1 N4 66.62(10) . . ? O3 Tm1 N5 67.27(10) . . ? O3 Tm1 N6 142.65(11) . . ? O5 Tm1 O1 84.25(11) . . ? O5 Tm1 O3 83.11(11) . . ? O5 Tm1 N1 148.86(11) . . ? O5 Tm1 N2 92.50(12) . . ? O5 Tm1 N3 127.44(12) . . ? O5 Tm1 N4 138.22(12) . . ? O5 Tm1 N5 66.19(11) . . ? O5 Tm1 N6 67.15(12) . . ? N1 Tm1 N2 67.43(11) . . ? N1 Tm1 N3 67.31(11) . . ? N1 Tm1 N4 62.10(10) . . ? N1 Tm1 N5 83.00(11) . . ? N3 Tm1 N2 65.93(10) . . ? N3 Tm1 N5 125.86(11) . . ? N4 Tm1 N2 128.12(10) . . ? N4 Tm1 N3 84.00(11) . . ? N4 Tm1 N5 121.18(11) . . ? N5 Tm1 N2 61.01(11) . . ? N6 Tm1 N1 127.84(11) . . ? N6 Tm1 N2 80.20(11) . . ? N6 Tm1 N3 62.38(12) . . ? N6 Tm1 N4 122.79(11) . . ? N6 Tm1 N5 116.03(11) . . ? O1 P1 C12 103.17(17) . . ? O1 P1 C13 109.15(18) . . ? O2 P1 O1 118.61(18) . . ? O2 P1 C12 111.07(18) . . ? O2 P1 C13 109.6(2) . . ? C13 P1 C12 104.20(19) . . ? O3 P2 C24 103.77(18) . . ? O3 P2 C25B 108.8(3) . . ? O3 P2 C25A 110.6(2) . . ? O4 P2 O3 116.4(2) . . ? O4 P2 C24 111.22(19) . . ? O4 P2 C25B 106.8(3) . . ? O4 P2 C25A 113.7(2) . . ? C24 P2 C25A 99.3(2) . . ? C25B P2 C24 109.7(3) . . ? C25B P2 C25A 10.6(3) . . ? O5 P3 C36 103.2(2) . . ? O5 P3 C37 108.9(2) . . ? O5 P3 O6A 123.0(3) . . ? O6B P3 O5 112.5(3) . . ? O6B P3 C36 118.5(3) . . ? O6B P3 C37 106.4(3) . . ? O6B P3 O6A 18.8(3) . . ? C37 P3 C36 107.0(2) . . ? O6A P3 C36 99.8(3) . . ? O6A P3 C37 112.9(3) . . ? P1 O1 Tm1 134.85(16) . . ? P2 O3 Tm1 133.78(17) . . ? P3 O5 Tm1 133.5(2) . . ? C1 N1 Tm1 106.9(2) . . ? C1 N1 C6 110.2(3) . . ? C6 N1 Tm1 113.9(2) . . ? C7 N1 Tm1 107.9(2) . . ? C7 N1 C1 108.6(3) . . ? C7 N1 C6 109.2(3) . . ? C2 N2 Tm1 112.6(2) . . ? C3 N2 Tm1 108.3(2) . . ? C3 N2 C2 109.6(3) . . ? C19 N2 Tm1 108.7(2) . . ? C19 N2 C2 109.2(3) . . ? C19 N2 C3 108.4(3) . . ? C4 N3 Tm1 116.6(2) . . ? C5 N3 Tm1 105.8(2) . . ? C5 N3 C4 109.7(3) . . ? C5 N3 C31 109.8(3) . . ? C31 N3 Tm1 106.4(2) . . ? C31 N3 C4 108.3(3) . . ? C8 N4 Tm1 118.7(3) . . ? C8 N4 C12 118.5(3) . . ? C12 N4 Tm1 121.7(3) . . ? C20 N5 Tm1 118.8(3) . . ? C20 N5 C24 118.4(4) . . ? C24 N5 Tm1 120.3(3) . . ? C32 N6 Tm1 119.2(3) . . ? C32 N6 C36 118.9(4) . . ? C36 N6 Tm1 121.8(3) . . ? N1 C1 H1A 109.0 . . ? N1 C1 H1B 109.0 . . ? N1 C1 C2 113.0(3) . . ? H1A C1 H1B 107.8 . . ? C2 C1 H1A 109.0 . . ? C2 C1 H1B 109.0 . . ? N2 C2 C1 114.7(3) . . ? N2 C2 H2A 108.6 . . ? N2 C2 H2B 108.6 . . ? C1 C2 H2A 108.6 . . ? C1 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? N2 C3 H3A 109.2 . . ? N2 C3 H3B 109.2 . . ? N2 C3 C4 112.3(3) . . ? H3A C3 H3B 107.9 . . ? C4 C3 H3A 109.2 . . ? C4 C3 H3B 109.2 . . ? N3 C4 C3 112.8(3) . . ? N3 C4 H4A 109.0 . . ? N3 C4 H4B 109.0 . . ? C3 C4 H4A 109.0 . . ? C3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? N3 C5 H5A 109.4 . . ? N3 C5 H5B 109.4 . . ? N3 C5 C6 111.3(3) . . ? H5A C5 H5B 108.0 . . ? C6 C5 H5A 109.4 . . ? C6 C5 H5B 109.4 . . ? N1 C6 C5 114.1(3) . . ? N1 C6 H6A 108.7 . . ? N1 C6 H6B 108.7 . . ? C5 C6 H6A 108.7 . . ? C5 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? N1 C7 C8 110.8(3) . . ? H7A C7 H7B 108.1 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? N4 C8 C7 114.8(3) . . ? N4 C8 C9 122.3(4) . . ? C9 C8 C7 122.8(4) . . ? C8 C9 H9 120.4 . . ? C8 C9 C10 119.2(4) . . ? C10 C9 H9 120.4 . . ? C9 C10 H10 120.5 . . ? C9 C10 C11 119.1(4) . . ? C11 C10 H10 120.5 . . ? C10 C11 H11 120.9 . . ? C12 C11 C10 118.2(4) . . ? C12 C11 H11 120.9 . . ? N4 C12 P1 113.0(3) . . ? N4 C12 C11 122.7(4) . . ? C11 C12 P1 124.2(3) . . ? C14 C13 P1 120.2(4) . . ? C18 C13 P1 120.3(3) . . ? C18 C13 C14 119.4(4) . . ? C13 C14 H14 120.3 . . ? C13 C14 C15 119.4(5) . . ? C15 C14 H14 120.3 . . ? C14 C15 H15 119.5 . . ? C16 C15 C14 121.1(5) . . ? C16 C15 H15 119.5 . . ? C15 C16 H16 120.0 . . ? C15 C16 C17 120.0(5) . . ? C17 C16 H16 120.0 . . ? C16 C17 H17 120.1 . . ? C18 C17 C16 119.8(5) . . ? C18 C17 H17 120.1 . . ? C13 C18 H18 119.9 . . ? C17 C18 C13 120.2(4) . . ? C17 C18 H18 119.9 . . ? N2 C19 H19A 109.4 . . ? N2 C19 H19B 109.4 . . ? N2 C19 C20 111.0(3) . . ? H19A C19 H19B 108.0 . . ? C20 C19 H19A 109.4 . . ? C20 C19 H19B 109.4 . . ? N5 C20 C19 116.1(4) . . ? N5 C20 C21 122.6(4) . . ? C21 C20 C19 121.1(4) . . ? C20 C21 H21 120.7 . . ? C22 C21 C20 118.5(4) . . ? C22 C21 H21 120.7 . . ? C21 C22 H22 120.6 . . ? C23 C22 C21 118.9(4) . . ? C23 C22 H22 120.6 . . ? C22 C23 H23 120.6 . . ? C24 C23 C22 118.9(4) . . ? C24 C23 H23 120.6 . . ? N5 C24 P2 113.8(3) . . ? N5 C24 C23 122.7(4) . . ? C23 C24 P2 123.3(3) . . ? C26B C25B P2 124.0(4) . . ? C26B C25B C30A 120.0 . . ? C30A C25B P2 115.8(4) . . ? C25B C26B H26 120.0 . . ? C25B C26B C27B 120.0 . . ? C27B C26B H26 120.0 . . ? C26B C27B H27 120.0 . . ? C26B C27B C28A 120.0 . . ? C28A C27B H27 120.0 . . ? C27B C28A H28 120.0 . . ? C29A C28A C27B 120.0 . . ? C29A C28A H28 120.0 . . ? C28A C29A H29 120.0 . . ? C30A C29A C28A 120.0 . . ? C30A C29A H29 120.0 . . ? C25B C30A H30 120.0 . . ? C29A C30A C25B 120.0 . . ? C29A C30A H30 120.0 . . ? N3 C31 H31A 109.8 . . ? N3 C31 H31B 109.8 . . ? N3 C31 C32 109.5(3) . . ? H31A C31 H31B 108.2 . . ? C32 C31 H31A 109.8 . . ? C32 C31 H31B 109.8 . . ? N6 C32 C31 114.9(4) . . ? N6 C32 C33 122.1(5) . . ? C33 C32 C31 122.9(4) . . ? C32 C33 H33 120.6 . . ? C34 C33 C32 118.8(5) . . ? C34 C33 H33 120.6 . . ? C33 C34 H34 120.4 . . ? C33 C34 C35 119.2(4) . . ? C35 C34 H34 120.4 . . ? C34 C35 H35 120.6 . . ? C36 C35 C34 118.8(5) . . ? C36 C35 H35 120.6 . . ? N6 C36 P3 113.1(3) . . ? N6 C36 C35 122.2(5) . . ? C35 C36 P3 124.6(4) . . ? C38 C37 P3 119.8(4) . . ? C38 C37 C42 119.3(4) . . ? C42 C37 P3 120.9(4) . . ? C37 C38 H38 120.0 . . ? C39 C38 C37 120.0(5) . . ? C39 C38 H38 120.0 . . ? C38 C39 H39 119.7 . . ? C40 C39 C38 120.5(5) . . ? C40 C39 H39 119.7 . . ? C39 C40 H40 120.0 . . ? C39 C40 C41 119.9(5) . . ? C41 C40 H40 120.0 . . ? C40 C41 H41 120.2 . . ? C42 C41 C40 119.6(5) . . ? C42 C41 H41 120.2 . . ? C37 C42 H42 119.7 . . ? C41 C42 C37 120.6(5) . . ? C41 C42 H42 119.7 . . ? C30B C25A P2 121.7(3) . . ? C30B C25A C26A 120.0 . . ? C26A C25A P2 118.3(3) . . ? C25A C30B H30A 120.0 . . ? C25A C30B C29B 120.0 . . ? C29B C30B H30A 120.0 . . ? C30B C29B H29A 120.0 . . ? C28B C29B C30B 120.0 . . ? C28B C29B H29A 120.0 . . ? C29B C28B H28A 120.0 . . ? C29B C28B C27A 120.0 . . ? C27A C28B H28A 120.0 . . ? C28B C27A H27A 120.0 . . ? C26A C27A C28B 120.0 . . ? C26A C27A H27A 120.0 . . ? C25A C26A H26A 120.0 . . ? C27A C26A C25A 120.0 . . ? C27A C26A H26A 120.0 . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.281 -0.986 -0.781 1407.5 381.0 ? # start Validation Reply Form _vrf_PLAT602_I ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: The structure contains a number of severely disordered solvent molecules (H2O, methanol). Their contribution to the structural fctors was taken into account by applying MASK procedure of OLEX2 program package. ; # end Validation Reply Form # Attachment 'web_deposit_cif_file_5_DmitryYufit_1311257364.YbL3.cif' data_YbL3_11srv130d _database_code_depnum_ccdc_archive 'CCDC 836102' #TrackingRef 'web_deposit_cif_file_5_DmitryYufit_1311257364.YbL3.cif' _audit_creation_date 2011-07-13 _audit_creation_method ; Olex2 1.1-beta (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H42 N6 O6 P3 Yb' _chemical_formula_sum 'C42 H42 N6 O6 P3 Yb' _chemical_formula_weight 992.77 _chemical_melting_point ? 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.9462(4) _cell_length_b 22.5220(6) _cell_length_c 15.8151(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.917(10) _cell_angle_gamma 90.00 _cell_volume 4938.9(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9794 _cell_measurement_temperature 120 _cell_measurement_theta_max 31.20 _cell_measurement_theta_min 2.28 _exptl_absorpt_coefficient_mu 2.037 _exptl_absorpt_correction_T_max 0.7435 _exptl_absorpt_correction_T_min 0.5411 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2006/1 (Bruker,2006) was used for absorption correction. R(int) was 0.0473 before and 0.0330 after correction. The Ratio of minimum to maximum transmission is 0.727774041695. The \l/2 correction factor is 0.0015 ; _exptl_crystal_colour less _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1996 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_special_details ; The data collection nominally covered a full sphere of reciprocal space by a combination of 5 sets of \w scans each set at different \f and/or 2\q angles and each scan (15.00 s exposure) covering -0.300\ degrees in \w. The crystal to detector distance was 4.85 cm. ; _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_unetI/netI 0.0252 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 81281 _diffrn_reflns_theta_full 29.00 _diffrn_reflns_theta_max 29.00 _diffrn_reflns_theta_min 1.60 _diffrn_ambient_temperature 120 _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 5.6 _diffrn_detector_type 'Bruker SMART CCD 6000 area detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART CCD 6000 area detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_xray_symbol K-L~3~ _diffrn_source 'sealed X-ray tube' _diffrn_source_current 10.0 _diffrn_source_power 0.3 _diffrn_source_target Mo _diffrn_source_voltage 30.0 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 10508 _reflns_number_total 13133 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'SAINT v6.45A (Bruker, 2003)' _computing_data_collection 'SMART v5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT v6.45A (Bruker, 2003)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)/Bruker' _refine_diff_density_max 2.273 _refine_diff_density_min -1.081 _refine_diff_density_rms 0.126 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 492 _refine_ls_number_reflns 13133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0322 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0896 _refine_ls_wR_factor_ref 0.0954 _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. The structure contains a number of severely disordered solvent molecules (H2O, methanol). Their contribution to the structural fctors was taken into account by applying MASK procedure of OLEX2 program package. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Yb1 Yb 0.071776(8) 0.675954(5) 0.319544(7) 0.01910(5) Uani 1 1 d . A . P1 P 0.17398(5) 0.64711(3) 0.55315(5) 0.02136(14) Uani 1 1 d . A . P2 P 0.08066(5) 0.53089(3) 0.24766(5) 0.02516(15) Uani 1 1 d . . . P3 P 0.27871(6) 0.71801(4) 0.28549(5) 0.03144(18) Uani 1 1 d . . . O1 O 0.17594(14) 0.67374(8) 0.46611(13) 0.0216(4) Uani 1 1 d . . . O2 O 0.19219(16) 0.68691(10) 0.63353(15) 0.0298(5) Uani 1 1 d . . . O3 O 0.08486(14) 0.57639(9) 0.31949(12) 0.0235(4) Uani 1 1 d . A . O4 O 0.00581(17) 0.48369(10) 0.22850(15) 0.0357(5) Uani 1 1 d . B . O5 O 0.20588(16) 0.67249(9) 0.28750(16) 0.0317(5) Uani 1 1 d . A . O6 O 0.2737(3) 0.7488(2) 0.1968(3) 0.0310(11) Uiso 0.50 1 d P A 1 O6A O 0.2787(3) 0.7272(2) 0.1922(3) 0.0229(9) Uiso 0.50 1 d P A 2 N1 N -0.11481(18) 0.66497(10) 0.26373(17) 0.0231(5) Uani 1 1 d . . . N2 N -0.02134(17) 0.74175(10) 0.17311(16) 0.0227(5) Uani 1 1 d . . . N3 N -0.01200(17) 0.77034(10) 0.35351(16) 0.0236(5) Uani 1 1 d . . . N4 N 0.00086(16) 0.62319(10) 0.42876(15) 0.0200(4) Uani 1 1 d . . . N5 N 0.04428(17) 0.63290(11) 0.15651(16) 0.0229(5) Uani 1 1 d . . . N6 N 0.17284(17) 0.77265(10) 0.36405(16) 0.0249(5) Uani 1 1 d . . . C1 C -0.1539(2) 0.66812(13) 0.16323(19) 0.0232(6) Uani 1 1 d . A . H1A H -0.2236 0.6654 0.1410 0.028 Uiso 1 1 calc R . . H1B H -0.1304 0.6344 0.1393 0.028 Uiso 1 1 calc R . . C2 C -0.1259(2) 0.72475(13) 0.12804(19) 0.0251(6) Uani 1 1 d . A . H2A H -0.1410 0.7205 0.0631 0.030 Uiso 1 1 calc R . . H2B H -0.1650 0.7569 0.1362 0.030 Uiso 1 1 calc R . . C3 C -0.0134(2) 0.80472(13) 0.20107(19) 0.0249(6) Uani 1 1 d . A . H3A H -0.0504 0.8290 0.1491 0.030 Uiso 1 1 calc R . . H3B H 0.0535 0.8170 0.2212 0.030 Uiso 1 1 calc R . . C4 C -0.0502(2) 0.81479(12) 0.2775(2) 0.0263(6) Uani 1 1 d . A . H4A H -0.0319 0.8543 0.3022 0.032 Uiso 1 1 calc R . . H4B H -0.1201 0.8128 0.2526 0.032 Uiso 1 1 calc R . . C5 C -0.0913(2) 0.74793(13) 0.3783(2) 0.0264(6) Uani 1 1 d . A . H5A H -0.1251 0.7812 0.3917 0.032 Uiso 1 1 calc R . . H5B H -0.0650 0.7239 0.4330 0.032 Uiso 1 1 calc R . . C6 C -0.1626(2) 0.71075(13) 0.3022(2) 0.0259(6) Uani 1 1 d . A . H6A H -0.2061 0.6908 0.3256 0.031 Uiso 1 1 calc R . . H6B H -0.2009 0.7370 0.2535 0.031 Uiso 1 1 calc R . . C7 C -0.1355(2) 0.60494(12) 0.29098(19) 0.0236(5) Uani 1 1 d . A . H7A H -0.1141 0.5750 0.2586 0.028 Uiso 1 1 calc R . . H7B H -0.2045 0.6004 0.2744 0.028 Uiso 1 1 calc R . . C8 C -0.08513(19) 0.59607(12) 0.39181(19) 0.0217(5) Uani 1 1 d . A . C9 C -0.1214(2) 0.55965(13) 0.4427(2) 0.0271(6) Uani 1 1 d . . . H9 H -0.1813 0.5415 0.4157 0.032 Uiso 1 1 calc R A . C10 C -0.0664(2) 0.55096(14) 0.5347(2) 0.0304(6) Uani 1 1 d . A . H10 H -0.0893 0.5272 0.5704 0.036 Uiso 1 1 calc R . . C11 C 0.0227(2) 0.57812(13) 0.57222(19) 0.0256(6) Uani 1 1 d . . . H11 H 0.0609 0.5728 0.6334 0.031 Uiso 1 1 calc R A . C12 C 0.05442(19) 0.61342(12) 0.51727(18) 0.0215(5) Uani 1 1 d . A . C13 C 0.2556(2) 0.58503(13) 0.58555(19) 0.0239(6) Uani 1 1 d . . . C14 C 0.2955(2) 0.56640(14) 0.6768(2) 0.0297(6) Uani 1 1 d . A . H14 H 0.2809 0.5866 0.7213 0.036 Uiso 1 1 calc R . . C15 C 0.3570(2) 0.51745(15) 0.7003(2) 0.0386(8) Uani 1 1 d . . . H15 H 0.3831 0.5049 0.7606 0.046 Uiso 1 1 calc R A . C16 C 0.3792(2) 0.48768(15) 0.6348(3) 0.0402(8) Uani 1 1 d . A . H16 H 0.4211 0.4554 0.6512 0.048 Uiso 1 1 calc R . . C17 C 0.3396(2) 0.50552(15) 0.5446(2) 0.0351(7) Uani 1 1 d . . . H17 H 0.3545 0.4852 0.5004 0.042 Uiso 1 1 calc R A . C18 C 0.2778(2) 0.55366(13) 0.5204(2) 0.0273(6) Uani 1 1 d . A . H18 H 0.2507 0.5652 0.4596 0.033 Uiso 1 1 calc R . . C19 C 0.0269(2) 0.73466(13) 0.10729(19) 0.0256(6) Uani 1 1 d . A . H19A H 0.0899 0.7534 0.1314 0.031 Uiso 1 1 calc R . . H19B H -0.0108 0.7543 0.0506 0.031 Uiso 1 1 calc R . . C20 C 0.0383(2) 0.67044(12) 0.0891(2) 0.0243(6) Uani 1 1 d . A . C21 C 0.0485(2) 0.65176(15) 0.0094(2) 0.0300(6) Uani 1 1 d . . . H21 H 0.0443 0.6788 -0.0364 0.036 Uiso 1 1 calc R A . C22 C 0.0650(2) 0.59214(16) -0.0009(2) 0.0360(7) Uani 1 1 d . A . H22 H 0.0708 0.5785 -0.0541 0.043 Uiso 1 1 calc R . . C23 C 0.0727(2) 0.55335(14) 0.0691(2) 0.0315(7) Uani 1 1 d . . . H23 H 0.0846 0.5132 0.0641 0.038 Uiso 1 1 calc R A . C24 C 0.0624(2) 0.57492(13) 0.14629(19) 0.0246(6) Uani 1 1 d . A . C25B C 0.1923(3) 0.4943(2) 0.2808(4) 0.0318(15) Uiso 0.50 1 d PG B 1 C26B C 0.2050(3) 0.4337(2) 0.2974(4) 0.0403(17) Uiso 0.50 1 d PG B 1 H26 H 0.1534 0.4102 0.2964 0.048 Uiso 0.50 1 calc PR B 1 C27B C 0.2949(4) 0.40806(18) 0.3154(4) 0.0457(19) Uiso 0.50 1 d PG B 1 H27 H 0.3034 0.3675 0.3265 0.055 Uiso 0.50 1 calc PR B 1 C28A C 0.3720(3) 0.4431(2) 0.3168(4) 0.0458(18) Uiso 0.50 1 d PG B 1 H28 H 0.4321 0.4260 0.3289 0.055 Uiso 0.50 1 calc PR B 1 C29A C 0.3593(3) 0.5037(2) 0.3003(4) 0.060(2) Uiso 0.50 1 d PG B 1 H29 H 0.4109 0.5271 0.3012 0.072 Uiso 0.50 1 calc PR B 1 C30A C 0.2694(4) 0.52931(17) 0.2823(4) 0.0486(19) Uiso 0.50 1 d PG B 1 H30 H 0.2609 0.5699 0.2712 0.058 Uiso 0.50 1 calc PR B 1 C31 C 0.0610(2) 0.80005(13) 0.4328(2) 0.0286(6) Uani 1 1 d . A . H31A H 0.0791 0.7741 0.4856 0.034 Uiso 1 1 calc R . . H31B H 0.0341 0.8362 0.4471 0.034 Uiso 1 1 calc R . . C32 C 0.1480(2) 0.81465(13) 0.4118(2) 0.0282(6) Uani 1 1 d . A . C33 C 0.2013(3) 0.86685(14) 0.4402(2) 0.0361(8) Uani 1 1 d . . . H33 H 0.1824 0.8955 0.4725 0.043 Uiso 1 1 calc R A . C34 C 0.2821(3) 0.87530(15) 0.4198(3) 0.0446(9) Uani 1 1 d . A . H34 H 0.3179 0.9100 0.4374 0.054 Uiso 1 1 calc R . . C35 C 0.3099(2) 0.83108(14) 0.3724(3) 0.0379(8) Uani 1 1 d . . . H35 H 0.3651 0.8354 0.3590 0.046 Uiso 1 1 calc R A . C36 C 0.2528(2) 0.78067(14) 0.3460(2) 0.0295(6) Uani 1 1 d . A . C37 C 0.3974(2) 0.69211(15) 0.3538(2) 0.0295(6) Uani 1 1 d . A . C38 C 0.4092(3) 0.64852(15) 0.4193(2) 0.0357(7) Uani 1 1 d . . . H38 H 0.3556 0.6333 0.4283 0.043 Uiso 1 1 calc R A . C39 C 0.5004(3) 0.62767(16) 0.4712(3) 0.0455(9) Uani 1 1 d . A . H39 H 0.5078 0.5980 0.5143 0.055 Uiso 1 1 calc R . . C40 C 0.5814(3) 0.65104(18) 0.4591(3) 0.0448(9) Uani 1 1 d . . . H40 H 0.6427 0.6372 0.4940 0.054 Uiso 1 1 calc R A . C41 C 0.5694(3) 0.69478(18) 0.3949(3) 0.0428(8) Uani 1 1 d . A . H41 H 0.6232 0.7109 0.3872 0.051 Uiso 1 1 calc R . . C42 C 0.4787(2) 0.71506(16) 0.3418(2) 0.0345(7) Uani 1 1 d . . . H42 H 0.4716 0.7441 0.2979 0.041 Uiso 1 1 calc R A . C25A C 0.2044(2) 0.50114(16) 0.2666(3) 0.0157(11) Uiso 0.50 1 d PG B 2 C30B C 0.2718(3) 0.53436(12) 0.2457(3) 0.0225(11) Uiso 0.50 1 d PG B 2 H30A H 0.2566 0.5726 0.2226 0.027 Uiso 0.50 1 calc PR B 2 C29B C 0.3619(2) 0.51044(15) 0.2593(3) 0.0288(12) Uiso 0.50 1 d PG B 2 H29A H 0.4069 0.5327 0.2453 0.035 Uiso 0.50 1 calc PR B 2 C28B C 0.3846(2) 0.45330(16) 0.2939(3) 0.0220(11) Uiso 0.50 1 d PG B 2 H28A H 0.4448 0.4373 0.3030 0.026 Uiso 0.50 1 calc PR B 2 C27A C 0.3172(3) 0.42007(13) 0.3148(3) 0.0170(10) Uiso 0.50 1 d PG B 2 H27A H 0.3324 0.3818 0.3380 0.020 Uiso 0.50 1 calc PR B 2 C26A C 0.2271(2) 0.44399(15) 0.3012(3) 0.0178(11) Uiso 0.50 1 d PG B 2 H26A H 0.1820 0.4218 0.3152 0.021 Uiso 0.50 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 Yb1 0.01918(7) 0.01765(7) 0.01817(7) 0.00047(4) 0.00430(5) 0.00010(4) P1 0.0195(3) 0.0220(3) 0.0197(3) 0.0007(3) 0.0040(3) -0.0037(3) P2 0.0258(4) 0.0193(3) 0.0233(3) -0.0015(3) 0.0009(3) 0.0028(3) P3 0.0233(4) 0.0476(5) 0.0213(3) 0.0014(3) 0.0058(3) -0.0080(3) O1 0.0210(10) 0.0212(10) 0.0204(9) 0.0023(7) 0.0053(8) -0.0028(7) O2 0.0299(11) 0.0334(11) 0.0246(10) -0.0056(9) 0.0085(9) -0.0080(9) O3 0.0280(10) 0.0201(10) 0.0192(9) 0.0002(7) 0.0051(8) 0.0037(7) O4 0.0413(13) 0.0239(11) 0.0329(12) 0.0002(9) 0.0037(10) -0.0046(9) O5 0.0274(11) 0.0402(13) 0.0293(11) -0.0106(9) 0.0127(9) -0.0091(9) N1 0.0244(12) 0.0202(11) 0.0227(11) 0.0040(9) 0.0066(10) 0.0019(9) N2 0.0225(11) 0.0209(11) 0.0222(11) 0.0011(9) 0.0054(9) 0.0025(9) N3 0.0255(12) 0.0216(11) 0.0206(11) 0.0020(9) 0.0051(9) 0.0027(9) N4 0.0190(11) 0.0194(11) 0.0195(10) -0.0016(8) 0.0046(9) -0.0017(8) N5 0.0201(11) 0.0247(12) 0.0213(11) -0.0006(9) 0.0048(9) 0.0025(9) N6 0.0259(12) 0.0212(11) 0.0209(11) 0.0049(9) 0.0011(9) -0.0020(9) C1 0.0169(12) 0.0287(15) 0.0193(13) 0.0003(10) 0.0013(10) 0.0007(10) C2 0.0244(14) 0.0240(14) 0.0234(13) 0.0028(11) 0.0048(11) 0.0039(11) C3 0.0275(14) 0.0203(13) 0.0225(13) 0.0054(11) 0.0044(11) 0.0021(11) C4 0.0309(15) 0.0206(13) 0.0259(14) 0.0038(11) 0.0088(12) 0.0065(11) C5 0.0292(15) 0.0237(14) 0.0268(14) 0.0010(11) 0.0110(12) 0.0039(11) C6 0.0239(14) 0.0264(14) 0.0276(14) 0.0037(11) 0.0099(11) 0.0032(11) C7 0.0195(13) 0.0235(13) 0.0236(13) 0.0007(11) 0.0033(10) -0.0003(10) C8 0.0182(12) 0.0200(13) 0.0236(13) -0.0009(10) 0.0039(10) -0.0003(10) C9 0.0214(14) 0.0258(14) 0.0313(15) 0.0020(12) 0.0067(12) -0.0020(11) C10 0.0259(15) 0.0337(16) 0.0305(15) 0.0073(13) 0.0094(12) -0.0038(12) C11 0.0241(14) 0.0284(15) 0.0222(13) 0.0039(11) 0.0062(11) 0.0002(11) C12 0.0201(13) 0.0219(13) 0.0213(13) -0.0007(10) 0.0062(10) -0.0001(10) C13 0.0189(13) 0.0234(13) 0.0252(13) 0.0043(11) 0.0033(10) -0.0039(10) C14 0.0261(15) 0.0313(16) 0.0248(14) 0.0028(12) 0.0015(12) -0.0052(12) C15 0.0295(17) 0.0333(17) 0.0358(17) 0.0073(14) -0.0077(13) -0.0058(13) C16 0.0238(16) 0.0312(17) 0.051(2) 0.0030(15) -0.0023(14) 0.0025(13) C17 0.0248(15) 0.0315(16) 0.0455(19) -0.0007(14) 0.0092(14) -0.0009(12) C18 0.0218(14) 0.0268(14) 0.0301(15) 0.0053(12) 0.0060(11) -0.0032(11) C19 0.0265(14) 0.0262(14) 0.0211(13) 0.0045(11) 0.0052(11) 0.0031(11) C20 0.0211(13) 0.0281(15) 0.0208(13) -0.0001(11) 0.0044(11) -0.0013(11) C21 0.0276(15) 0.0377(17) 0.0220(14) -0.0002(13) 0.0061(12) 0.0009(13) C22 0.0388(18) 0.0433(19) 0.0259(15) -0.0067(14) 0.0120(13) 0.0017(14) C23 0.0308(16) 0.0285(15) 0.0312(15) -0.0104(12) 0.0069(13) 0.0006(12) C24 0.0203(13) 0.0245(14) 0.0241(13) -0.0039(11) 0.0027(11) -0.0011(10) C31 0.0355(16) 0.0212(14) 0.0242(14) -0.0029(11) 0.0055(12) 0.0025(12) C32 0.0312(16) 0.0220(14) 0.0222(14) 0.0050(11) -0.0007(12) 0.0007(11) C33 0.0411(19) 0.0235(15) 0.0278(15) 0.0043(12) -0.0055(13) -0.0021(13) C34 0.0380(19) 0.0266(17) 0.049(2) 0.0118(15) -0.0070(16) -0.0105(14) C35 0.0260(16) 0.0308(17) 0.046(2) 0.0145(14) 0.0007(14) -0.0058(12) C36 0.0261(15) 0.0299(15) 0.0237(14) 0.0110(12) -0.0009(11) -0.0033(12) C37 0.0289(15) 0.0331(15) 0.0259(14) -0.0026(12) 0.0095(12) -0.0035(12) C38 0.0374(18) 0.0332(17) 0.0344(17) -0.0043(14) 0.0111(14) -0.0080(14) C39 0.062(3) 0.0288(18) 0.041(2) 0.0051(14) 0.0149(18) 0.0064(16) C40 0.043(2) 0.049(2) 0.0383(19) 0.0010(17) 0.0101(16) 0.0179(17) C41 0.0313(18) 0.054(2) 0.045(2) 0.0047(17) 0.0163(16) 0.0079(16) C42 0.0291(16) 0.0425(19) 0.0325(16) 0.0056(14) 0.0120(13) 0.0025(13) _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 Yb1 O1 2.259(2) . ? Yb1 O3 2.251(2) . ? Yb1 O5 2.245(2) . ? Yb1 N1 2.604(2) . ? Yb1 N2 2.663(2) . ? Yb1 N3 2.623(2) . ? Yb1 N4 2.624(2) . ? Yb1 N5 2.639(2) . ? Yb1 N6 2.594(2) . ? P1 O1 1.512(2) . ? P1 O2 1.495(2) . ? P1 C12 1.826(3) . ? P1 C13 1.800(3) . ? P2 O3 1.514(2) . ? P2 O4 1.490(2) . ? P2 C24 1.817(3) . ? P2 C25B 1.756(4) . ? P2 C25A 1.883(3) . ? P3 O5 1.504(2) . ? P3 O6 1.541(5) . ? P3 O6A 1.490(4) . ? P3 C36 1.826(3) . ? P3 C37 1.795(3) . ? N1 C1 1.476(4) . ? N1 C6 1.507(4) . ? N1 C7 1.486(4) . ? N2 C2 1.505(4) . ? N2 C3 1.477(4) . ? N2 C19 1.480(4) . ? N3 C4 1.503(4) . ? N3 C5 1.471(4) . ? N3 C31 1.480(4) . ? N4 C8 1.344(3) . ? N4 C12 1.346(3) . ? N5 C20 1.337(4) . ? N5 C24 1.355(4) . ? N6 C32 1.346(4) . ? N6 C36 1.340(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 C2 1.512(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 C4 1.520(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 C6 1.526(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C8 1.501(4) . ? C8 C9 1.393(4) . ? C9 H9 0.9300 . ? C9 C10 1.393(4) . ? C10 H10 0.9300 . ? C10 C11 1.382(4) . ? C11 H11 0.9300 . ? C11 C12 1.385(4) . ? C13 C14 1.404(4) . ? C13 C18 1.387(4) . ? C14 H14 0.9300 . ? C14 C15 1.394(5) . ? C15 H15 0.9300 . ? C15 C16 1.375(5) . ? C16 H16 0.9300 . ? C16 C17 1.385(5) . ? C17 H17 0.9300 . ? C17 C18 1.382(4) . ? C18 H18 0.9300 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 C20 1.497(4) . ? C20 C21 1.391(4) . ? C21 H21 0.9300 . ? C21 C22 1.385(5) . ? C22 H22 0.9300 . ? C22 C23 1.381(5) . ? C23 H23 0.9300 . ? C23 C24 1.375(4) . ? C25B C26B 1.3900 . ? C25B C30A 1.3900 . ? C26B H26 0.9300 . ? C26B C27B 1.3900 . ? C27B H27 0.9300 . ? C27B C28A 1.3900 . ? C28A H28 0.9300 . ? C28A C29A 1.3900 . ? C29A H29 0.9300 . ? C29A C30A 1.3900 . ? C30A H30 0.9300 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 C32 1.494(5) . ? C32 C33 1.397(4) . ? C33 H33 0.9300 . ? C33 C34 1.373(5) . ? C34 H34 0.9300 . ? C34 C35 1.400(6) . ? C35 H35 0.9300 . ? C35 C36 1.388(4) . ? C37 C38 1.390(5) . ? C37 C42 1.397(4) . ? C38 H38 0.9300 . ? C38 C39 1.385(5) . ? C39 H39 0.9300 . ? C39 C40 1.397(6) . ? C40 H40 0.9300 . ? C40 C41 1.378(5) . ? C41 H41 0.9300 . ? C41 C42 1.379(5) . ? C42 H42 0.9300 . ? C25A C30B 1.3900 . ? C25A C26A 1.3900 . ? C30B H30A 0.9300 . ? C30B C29B 1.3900 . ? C29B H29A 0.9300 . ? C29B C28B 1.3900 . ? C28B H28A 0.9300 . ? C28B C27A 1.3900 . ? C27A H27A 0.9300 . ? C27A C26A 1.3900 . ? C26A H26A 0.9300 . ? 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 O1 Yb1 N1 125.90(7) . . ? O1 Yb1 N2 147.23(7) . . ? O1 Yb1 N3 90.38(7) . . ? O1 Yb1 N4 66.90(7) . . ? O1 Yb1 N5 142.23(7) . . ? O1 Yb1 N6 68.38(7) . . ? O3 Yb1 O1 87.23(6) . . ? O3 Yb1 N1 89.28(7) . . ? O3 Yb1 N2 124.84(7) . . ? O3 Yb1 N3 148.85(7) . . ? O3 Yb1 N4 66.77(7) . . ? O3 Yb1 N5 67.39(7) . . ? O3 Yb1 N6 142.63(7) . . ? O5 Yb1 O1 84.23(8) . . ? O5 Yb1 O3 83.12(7) . . ? O5 Yb1 N1 148.63(8) . . ? O5 Yb1 N2 92.52(8) . . ? O5 Yb1 N3 127.54(8) . . ? O5 Yb1 N4 138.33(8) . . ? O5 Yb1 N5 66.00(8) . . ? O5 Yb1 N6 67.16(8) . . ? N1 Yb1 N2 67.17(7) . . ? N1 Yb1 N3 67.27(7) . . ? N1 Yb1 N4 62.32(7) . . ? N1 Yb1 N5 82.96(8) . . ? N3 Yb1 N2 65.95(7) . . ? N3 Yb1 N4 83.75(7) . . ? N3 Yb1 N5 125.86(7) . . ? N4 Yb1 N2 128.03(7) . . ? N4 Yb1 N5 121.52(7) . . ? N5 Yb1 N2 60.96(7) . . ? N6 Yb1 N1 127.83(7) . . ? N6 Yb1 N2 80.28(7) . . ? N6 Yb1 N3 62.48(8) . . ? N6 Yb1 N4 122.62(7) . . ? N6 Yb1 N5 115.86(8) . . ? O1 P1 Yb1 27.41(8) . . ? O1 P1 C12 103.37(12) . . ? O1 P1 C13 109.01(12) . . ? O2 P1 Yb1 131.07(9) . . ? O2 P1 O1 118.50(12) . . ? O2 P1 C12 111.09(13) . . ? O2 P1 C13 109.56(13) . . ? C12 P1 Yb1 75.97(9) . . ? C13 P1 Yb1 115.34(10) . . ? C13 P1 C12 104.28(13) . . ? O3 P2 Yb1 27.71(7) . . ? O3 P2 C24 104.07(12) . . ? O3 P2 C25B 109.0(2) . . ? O3 P2 C25A 111.00(15) . . ? O4 P2 Yb1 128.26(10) . . ? O4 P2 O3 116.95(13) . . ? O4 P2 C24 110.85(13) . . ? O4 P2 C25B 106.5(2) . . ? O4 P2 C25A 113.38(15) . . ? C24 P2 Yb1 76.36(9) . . ? C24 P2 C25A 98.61(15) . . ? C25B P2 Yb1 119.42(18) . . ? C25B P2 C24 109.4(2) . . ? C25B P2 C25A 11.0(2) . . ? C25A P2 Yb1 115.93(12) . . ? O5 P3 Yb1 27.76(9) . . ? O5 P3 O6 122.4(2) . . ? O5 P3 C36 102.64(13) . . ? O5 P3 C37 109.02(15) . . ? O6 P3 Yb1 121.44(18) . . ? O6 P3 C36 100.4(2) . . ? O6 P3 C37 113.3(2) . . ? O6A P3 Yb1 121.45(17) . . ? O6A P3 O5 112.5(2) . . ? O6A P3 O6 19.0(2) . . ? O6A P3 C36 119.3(2) . . ? O6A P3 C37 106.1(2) . . ? C36 P3 Yb1 75.72(10) . . ? C37 P3 Yb1 123.81(11) . . ? C37 P3 C36 106.91(14) . . ? P1 O1 Yb1 134.65(11) . . ? P2 O3 Yb1 134.07(11) . . ? P3 O5 Yb1 134.05(13) . . ? C1 N1 Yb1 107.66(17) . . ? C1 N1 C6 110.2(2) . . ? C1 N1 C7 108.3(2) . . ? C6 N1 Yb1 114.06(17) . . ? C7 N1 Yb1 107.50(16) . . ? C7 N1 C6 108.9(2) . . ? C2 N2 Yb1 112.57(16) . . ? C3 N2 Yb1 108.45(16) . . ? C3 N2 C2 109.8(2) . . ? C3 N2 C19 108.0(2) . . ? C19 N2 Yb1 108.54(16) . . ? C19 N2 C2 109.4(2) . . ? C4 N3 Yb1 116.36(17) . . ? C5 N3 Yb1 105.71(16) . . ? C5 N3 C4 109.8(2) . . ? C5 N3 C31 110.0(2) . . ? C31 N3 Yb1 106.42(16) . . ? C31 N3 C4 108.4(2) . . ? C8 N4 Yb1 118.39(17) . . ? C8 N4 C12 118.6(2) . . ? C12 N4 Yb1 121.94(17) . . ? C20 N5 Yb1 119.09(18) . . ? C20 N5 C24 118.1(2) . . ? C24 N5 Yb1 120.35(18) . . ? C32 N6 Yb1 119.2(2) . . ? C36 N6 Yb1 122.0(2) . . ? C36 N6 C32 118.6(3) . . ? N1 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? N1 C1 C2 112.6(2) . . ? H1A C1 H1B 107.8 . . ? C2 C1 H1A 109.1 . . ? C2 C1 H1B 109.1 . . ? N2 C2 C1 114.9(2) . . ? N2 C2 H2A 108.5 . . ? N2 C2 H2B 108.5 . . ? C1 C2 H2A 108.5 . . ? C1 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? N2 C3 H3A 109.3 . . ? N2 C3 H3B 109.3 . . ? N2 C3 C4 111.6(2) . . ? H3A C3 H3B 108.0 . . ? C4 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? N3 C4 C3 113.2(2) . . ? N3 C4 H4A 108.9 . . ? N3 C4 H4B 108.9 . . ? C3 C4 H4A 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? N3 C5 H5A 109.2 . . ? N3 C5 H5B 109.2 . . ? N3 C5 C6 111.9(2) . . ? H5A C5 H5B 107.9 . . ? C6 C5 H5A 109.2 . . ? C6 C5 H5B 109.2 . . ? N1 C6 C5 113.4(2) . . ? N1 C6 H6A 108.9 . . ? N1 C6 H6B 108.9 . . ? C5 C6 H6A 108.9 . . ? C5 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? N1 C7 C8 110.7(2) . . ? H7A C7 H7B 108.1 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? N4 C8 C7 114.9(2) . . ? N4 C8 C9 122.1(3) . . ? C9 C8 C7 122.9(2) . . ? C8 C9 H9 120.6 . . ? C8 C9 C10 118.8(3) . . ? C10 C9 H9 120.6 . . ? C9 C10 H10 120.5 . . ? C11 C10 C9 119.0(3) . . ? C11 C10 H10 120.5 . . ? C10 C11 H11 120.5 . . ? C10 C11 C12 119.0(3) . . ? C12 C11 H11 120.5 . . ? N4 C12 P1 112.8(2) . . ? N4 C12 C11 122.4(3) . . ? C11 C12 P1 124.6(2) . . ? C14 C13 P1 120.5(2) . . ? C18 C13 P1 120.6(2) . . ? C18 C13 C14 118.9(3) . . ? C13 C14 H14 120.2 . . ? C15 C14 C13 119.7(3) . . ? C15 C14 H14 120.2 . . ? C14 C15 H15 119.8 . . ? C16 C15 C14 120.4(3) . . ? C16 C15 H15 119.8 . . ? C15 C16 H16 119.9 . . ? C15 C16 C17 120.3(3) . . ? C17 C16 H16 119.9 . . ? C16 C17 H17 120.1 . . ? C18 C17 C16 119.8(3) . . ? C18 C17 H17 120.1 . . ? C13 C18 H18 119.5 . . ? C17 C18 C13 120.9(3) . . ? C17 C18 H18 119.5 . . ? N2 C19 H19A 109.4 . . ? N2 C19 H19B 109.4 . . ? N2 C19 C20 111.1(2) . . ? H19A C19 H19B 108.0 . . ? C20 C19 H19A 109.4 . . ? C20 C19 H19B 109.4 . . ? N5 C20 C19 115.9(2) . . ? N5 C20 C21 122.3(3) . . ? C21 C20 C19 121.7(3) . . ? C20 C21 H21 120.5 . . ? C22 C21 C20 118.9(3) . . ? C22 C21 H21 120.5 . . ? C21 C22 H22 120.5 . . ? C23 C22 C21 119.0(3) . . ? C23 C22 H22 120.5 . . ? C22 C23 H23 120.5 . . ? C24 C23 C22 119.0(3) . . ? C24 C23 H23 120.5 . . ? N5 C24 P2 113.0(2) . . ? N5 C24 C23 122.7(3) . . ? C23 C24 P2 124.1(2) . . ? C26B C25B P2 124.4(3) . . ? C26B C25B C30A 120.0 . . ? C30A C25B P2 115.3(3) . . ? C25B C26B H26 120.0 . . ? C27B C26B C25B 120.0 . . ? C27B C26B H26 120.0 . . ? C26B C27B H27 120.0 . . ? C26B C27B C28A 120.0 . . ? C28A C27B H27 120.0 . . ? C27B C28A H28 120.0 . . ? C29A C28A C27B 120.0 . . ? C29A C28A H28 120.0 . . ? C28A C29A H29 120.0 . . ? C28A C29A C30A 120.0 . . ? C30A C29A H29 120.0 . . ? C25B C30A H30 120.0 . . ? C29A C30A C25B 120.0 . . ? C29A C30A H30 120.0 . . ? N3 C31 H31A 109.7 . . ? N3 C31 H31B 109.7 . . ? N3 C31 C32 109.8(2) . . ? H31A C31 H31B 108.2 . . ? C32 C31 H31A 109.7 . . ? C32 C31 H31B 109.7 . . ? N6 C32 C31 114.5(3) . . ? N6 C32 C33 121.9(3) . . ? C33 C32 C31 123.6(3) . . ? C32 C33 H33 120.4 . . ? C34 C33 C32 119.2(3) . . ? C34 C33 H33 120.4 . . ? C33 C34 H34 120.3 . . ? C33 C34 C35 119.3(3) . . ? C35 C34 H34 120.3 . . ? C34 C35 H35 121.0 . . ? C36 C35 C34 118.1(3) . . ? C36 C35 H35 121.0 . . ? N6 C36 P3 112.8(2) . . ? N6 C36 C35 122.9(3) . . ? C35 C36 P3 124.2(3) . . ? C38 C37 P3 120.0(2) . . ? C38 C37 C42 119.2(3) . . ? C42 C37 P3 120.8(2) . . ? C37 C38 H38 119.9 . . ? C39 C38 C37 120.3(3) . . ? C39 C38 H38 119.9 . . ? C38 C39 H39 119.9 . . ? C38 C39 C40 120.2(3) . . ? C40 C39 H39 119.9 . . ? C39 C40 H40 120.3 . . ? C41 C40 C39 119.3(3) . . ? C41 C40 H40 120.3 . . ? C40 C41 H41 119.6 . . ? C40 C41 C42 120.9(4) . . ? C42 C41 H41 119.6 . . ? C37 C42 H42 119.9 . . ? C41 C42 C37 120.1(3) . . ? C41 C42 H42 119.9 . . ? C30B C25A P2 121.76(19) . . ? C30B C25A C26A 120.0 . . ? C26A C25A P2 118.23(19) . . ? C25A C30B H30A 120.0 . . ? C29B C30B C25A 120.0 . . ? C29B C30B H30A 120.0 . . ? C30B C29B H29A 120.0 . . ? C30B C29B C28B 120.0 . . ? C28B C29B H29A 120.0 . . ? C29B C28B H28A 120.0 . . ? C29B C28B C27A 120.0 . . ? C27A C28B H28A 120.0 . . ? C28B C27A H27A 120.0 . . ? C26A C27A C28B 120.0 . . ? C26A C27A H27A 120.0 . . ? C25A C26A H26A 120.0 . . ? C27A C26A C25A 120.0 . . ? C27A C26A H26A 120.0 . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.994 -0.150 -0.494 1387.6 571.7 ? # start Validation Reply Form _vrf_PLAT602_I ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: The structure contains a number of severely disordered solvent molecules (H2O, methanol). Their contribution to the structural fctors was taken into account by applying MASK procedure of OLEX2 program package. ; # end Validation Reply Form