Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email MIKE.HILL@IMPERIAL.AC.UK _publ_contact_author_name 'Dr Michael Hill' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Department of Chemistry Imperial College London Exhibition Rd South Kensington London SW7 2AZ UNITED KINGDOM ; _publ_section_title ; Synthesis of a base-free, homoleptic Sm(II) dialkyl ; _publ_requested_category FM loop_ _publ_author_name 'Michael Hill' 'Peter B. Hitchcock' data_apr803 _database_code_depnum_ccdc_archive 'CCDC 222067' _chemical_name_common "'(Sm(MesNPPh2CHPPh2NMes)) 2.5(toluene)'" _audit_creation_date 2003-04-09T09:36:42-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '(C86 H86 N4 P4 Sm1) 2.5(C7 H8)' _chemical_formula_sum 'C103.5 H106 N4 P4 Sm' _chemical_formula_weight 1680.15 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.1670(1) _cell_length_b 15.8289(2) _cell_length_c 22.0330(3) _cell_angle_alpha 68.814(1) _cell_angle_beta 75.887(1) _cell_angle_gamma 75.659(1) _cell_volume 4708.17(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 77755 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1754 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.738 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8223 _exptl_absorpt_correction_T_max 0.9939 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.465947E-1 _diffrn_orient_matrix_ub_12 0.285717E-1 _diffrn_orient_matrix_ub_13 -0.379524E-1 _diffrn_orient_matrix_ub_21 -0.174043E-1 _diffrn_orient_matrix_ub_22 0.577064E-1 _diffrn_orient_matrix_ub_23 0.122122E-1 _diffrn_orient_matrix_ub_31 0.479215E-1 _diffrn_orient_matrix_ub_32 -0.243298E-1 _diffrn_orient_matrix_ub_33 0.291737E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0735 _diffrn_reflns_av_unetI/netI 0.0667 _diffrn_reflns_number 61602 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _reflns_number_total 21366 _reflns_number_gt 16861 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The disordered toluene solvates were poorly defined and refined with constraints, and with hydrogen atoms omitted. The ordered toluene was included with the C6 ring as a rigid body Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0824P)^2^+9.1638P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 21366 _refine_ls_number_parameters 952 _refine_ls_number_restraints 231 _refine_ls_R_factor_all 0.0866 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1749 _refine_ls_wR_factor_gt 0.1609 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.12 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.928 _refine_diff_density_min -1.191 _refine_diff_density_rms 0.108 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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' 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 Sm Sm 0.734383(15) 0.619102(16) 0.723832(12) 0.03142(8) Uani 1 1 d . . . P1 P 0.54777(8) 0.52196(8) 0.79691(6) 0.0326(2) Uani 1 1 d . . . P2 P 0.58825(9) 0.66425(8) 0.85211(6) 0.0355(3) Uani 1 1 d . . . P3 P 0.95321(8) 0.51777(8) 0.69262(6) 0.0324(2) Uani 1 1 d . . . P4 P 0.86202(8) 0.66864(8) 0.57465(6) 0.0326(2) Uani 1 1 d . . . N1 N 0.6057(3) 0.5371(3) 0.7228(2) 0.0350(8) Uani 1 1 d . . . N2 N 0.6342(3) 0.7323(3) 0.7848(2) 0.0452(10) Uani 1 1 d . . . N3 N 0.8921(3) 0.5314(3) 0.7608(2) 0.0365(9) Uani 1 1 d . . . N4 N 0.7954(3) 0.7368(3) 0.6125(2) 0.0377(9) Uani 1 1 d . . . C1 C 0.5992(3) 0.5593(3) 0.8414(2) 0.0352(10) Uani 1 1 d . . . H1 H 0.6427 0.5125 0.865 0.042 Uiso 1 1 calc R . . C2 C 0.4276(3) 0.5790(4) 0.7971(3) 0.0422(11) Uani 1 1 d . . . C3 C 0.4105(4) 0.6737(4) 0.7655(3) 0.0481(13) Uani 1 1 d . . . H3 H 0.4611 0.7052 0.7444 0.058 Uiso 1 1 calc R . . C4 C 0.3215(4) 0.7226(4) 0.7641(3) 0.0599(16) Uani 1 1 d . . . H4 H 0.3109 0.7873 0.743 0.072 Uiso 1 1 calc R . . C5 C 0.2479(5) 0.6761(5) 0.7939(4) 0.079(2) Uani 1 1 d . . . H5 H 0.1864 0.7088 0.7924 0.094 Uiso 1 1 calc R . . C6 C 0.2638(4) 0.5833(5) 0.8254(5) 0.085(3) Uani 1 1 d . . . H6 H 0.213 0.552 0.8458 0.102 Uiso 1 1 calc R . . C7 C 0.3531(4) 0.5340(4) 0.8280(4) 0.0621(17) Uani 1 1 d . . . H7 H 0.363 0.4697 0.8509 0.074 Uiso 1 1 calc R . . C8 C 0.5437(3) 0.4003(3) 0.8406(2) 0.0363(10) Uani 1 1 d . . . C9 C 0.5096(4) 0.3518(3) 0.8124(3) 0.0425(11) Uani 1 1 d . . . H9 H 0.4815 0.3839 0.7743 0.051 Uiso 1 1 calc R . . C10 C 0.5163(4) 0.2574(4) 0.8392(3) 0.0558(15) Uani 1 1 d . . . H10 H 0.4926 0.2252 0.8195 0.067 Uiso 1 1 calc R . . C11 C 0.5570(4) 0.2094(4) 0.8944(3) 0.0605(16) Uani 1 1 d . . . H11 H 0.563 0.1443 0.9122 0.073 Uiso 1 1 calc R . . C12 C 0.5889(4) 0.2573(4) 0.9235(3) 0.0560(15) Uani 1 1 d . . . H12 H 0.6161 0.2249 0.9619 0.067 Uiso 1 1 calc R . . C13 C 0.5817(3) 0.3522(3) 0.8972(3) 0.0427(11) Uani 1 1 d . . . H13 H 0.603 0.3844 0.9182 0.051 Uiso 1 1 calc R . . C14 C 0.4694(3) 0.7094(3) 0.8838(2) 0.0393(11) Uani 1 1 d . . . C15 C 0.4352(4) 0.8031(4) 0.8699(3) 0.0481(13) Uani 1 1 d . . . H15 H 0.4741 0.8463 0.843 0.058 Uiso 1 1 calc R . . C16 C 0.3447(4) 0.8339(4) 0.8950(3) 0.0594(16) Uani 1 1 d . . . H16 H 0.322 0.8981 0.8847 0.071 Uiso 1 1 calc R . . C17 C 0.2873(4) 0.7725(5) 0.9348(3) 0.0640(17) Uani 1 1 d . . . H17 H 0.2252 0.7942 0.9515 0.077 Uiso 1 1 calc R . . C18 C 0.3211(4) 0.6791(5) 0.9500(3) 0.0586(15) Uani 1 1 d . . . H18 H 0.2824 0.6363 0.978 0.07 Uiso 1 1 calc R . . C19 C 0.4109(4) 0.6477(4) 0.9248(3) 0.0479(12) Uani 1 1 d . . . H19 H 0.4332 0.5833 0.9353 0.057 Uiso 1 1 calc R . . C20 C 0.6441(3) 0.6396(3) 0.9225(2) 0.0373(10) Uani 1 1 d . . . C21 C 0.7243(4) 0.5739(4) 0.9318(3) 0.0489(13) Uani 1 1 d . . . H21 H 0.7463 0.5365 0.904 0.059 Uiso 1 1 calc R . . C22 C 0.7725(4) 0.5625(5) 0.9811(3) 0.0587(15) Uani 1 1 d . . . H22 H 0.8269 0.5173 0.9869 0.07 Uiso 1 1 calc R . . C23 C 0.7417(4) 0.6164(5) 1.0215(3) 0.0596(16) Uani 1 1 d . . . H23 H 0.7751 0.6089 1.0549 0.072 Uiso 1 1 calc R . . C24 C 0.6621(5) 0.6812(5) 1.0135(3) 0.0626(16) Uani 1 1 d . . . H24 H 0.6409 0.7186 1.0413 0.075 Uiso 1 1 calc R . . C25 C 0.6131(4) 0.6921(4) 0.9653(3) 0.0519(13) Uani 1 1 d . . . H25 H 0.5575 0.7358 0.961 0.062 Uiso 1 1 calc R . . C26 C 0.5924(3) 0.4913(3) 0.6810(2) 0.0335(9) Uani 1 1 d . . . C27 C 0.6514(3) 0.4079(3) 0.6793(2) 0.0357(10) Uani 1 1 d . . . C28 C 0.6383(4) 0.3610(3) 0.6398(2) 0.0422(11) Uani 1 1 d . . . H28 H 0.679 0.3051 0.6385 0.051 Uiso 1 1 calc R . . C29 C 0.5682(4) 0.3934(4) 0.6027(3) 0.0456(12) Uani 1 1 d . . . C30 C 0.5137(4) 0.4762(4) 0.6028(3) 0.0448(12) Uani 1 1 d . . . H30 H 0.4662 0.5 0.5767 0.054 Uiso 1 1 calc R . . C31 C 0.5251(3) 0.5276(3) 0.6399(2) 0.0372(10) Uani 1 1 d . . . C32 C 0.7291(4) 0.3670(4) 0.7185(3) 0.0475(12) Uani 1 1 d . . . H32A H 0.7665 0.4138 0.71 0.071 Uiso 1 1 calc R . . H32B H 0.7679 0.3149 0.7053 0.071 Uiso 1 1 calc R . . H32C H 0.7035 0.3457 0.7657 0.071 Uiso 1 1 calc R . . C33 C 0.5560(5) 0.3405(5) 0.5613(4) 0.0670(18) Uani 1 1 d . . . H33A H 0.6014 0.2833 0.5678 0.101 Uiso 0.5 1 calc PR . . H33B H 0.565 0.378 0.5145 0.101 Uiso 0.5 1 calc PR . . H33C H 0.4935 0.3258 0.5746 0.101 Uiso 0.5 1 calc PR . . H33D H 0.5052 0.3748 0.5368 0.101 Uiso 0.5 1 calc PR . . H33E H 0.5416 0.2801 0.5901 0.101 Uiso 0.5 1 calc PR . . H33F H 0.6131 0.3322 0.53 0.101 Uiso 0.5 1 calc PR . . C34 C 0.4650(4) 0.6211(4) 0.6329(3) 0.0501(13) Uani 1 1 d . . . H34A H 0.4043 0.6138 0.6606 0.075 Uiso 1 1 calc R . . H34B H 0.4575 0.6522 0.5866 0.075 Uiso 1 1 calc R . . H34C H 0.4942 0.6581 0.6469 0.075 Uiso 1 1 calc R . . C35 C 0.6442(4) 0.8254(3) 0.7696(3) 0.0539(16) Uani 1 1 d . . . C36 C 0.7141(5) 0.8476(4) 0.7896(3) 0.0628(18) Uani 1 1 d . . . C37 C 0.7206(6) 0.9408(5) 0.7715(4) 0.083(3) Uani 1 1 d . . . H37 H 0.7665 0.956 0.7864 0.1 Uiso 1 1 calc R . . C38 C 0.6641(7) 1.0108(5) 0.7335(5) 0.094(3) Uani 1 1 d . . . C39 C 0.5996(6) 0.9874(5) 0.7110(4) 0.086(3) Uani 1 1 d . . . H39 H 0.5616 1.0352 0.6831 0.104 Uiso 1 1 calc R . . C40 C 0.5869(5) 0.8960(4) 0.7272(3) 0.0634(18) Uani 1 1 d . . . C41 C 0.7840(5) 0.7774(5) 0.8259(4) 0.080(2) Uani 1 1 d . . . H41A H 0.7611 0.7621 0.8736 0.121 Uiso 1 1 calc R . . H41B H 0.8414 0.8016 0.8152 0.121 Uiso 1 1 calc R . . H41C H 0.7959 0.7218 0.8132 0.121 Uiso 1 1 calc R . . C42 C 0.6753(9) 1.1105(5) 0.7141(6) 0.137(5) Uani 1 1 d . . . H42A H 0.7243 1.1136 0.7348 0.206 Uiso 0.5 1 calc PR . . H42B H 0.6171 1.1467 0.7291 0.206 Uiso 0.5 1 calc PR . . H42C H 0.6918 1.1354 0.666 0.206 Uiso 0.5 1 calc PR . . H42D H 0.6312 1.1502 0.6852 0.206 Uiso 0.5 1 calc PR . . H42E H 0.7384 1.1171 0.6908 0.206 Uiso 0.5 1 calc PR . . H42F H 0.6637 1.1284 0.754 0.206 Uiso 0.5 1 calc PR . . C43 C 0.5178(6) 0.8759(5) 0.6987(4) 0.079(2) Uani 1 1 d . . . H43A H 0.4621 0.8651 0.732 0.119 Uiso 1 1 calc R . . H43B H 0.544 0.8211 0.6852 0.119 Uiso 1 1 calc R . . H43C H 0.5018 0.9285 0.6602 0.119 Uiso 1 1 calc R . . C44 C 0.8856(3) 0.5612(3) 0.6314(2) 0.0357(10) Uani 1 1 d . . . H44 H 0.8556 0.517 0.6286 0.043 Uiso 1 1 calc R . . C45 C 1.0557(3) 0.5704(4) 0.6663(3) 0.0399(11) Uani 1 1 d . . . C46 C 1.0429(4) 0.6646(4) 0.6542(3) 0.0453(12) Uani 1 1 d . . . H46 H 0.982 0.6979 0.661 0.054 Uiso 1 1 calc R . . C47 C 1.1170(4) 0.7116(4) 0.6324(3) 0.0566(15) Uani 1 1 d . . . H47 H 1.1069 0.7762 0.6241 0.068 Uiso 1 1 calc R . . C48 C 1.2061(4) 0.6624(5) 0.6231(4) 0.0684(19) Uani 1 1 d . . . H48 H 1.2574 0.6933 0.609 0.082 Uiso 1 1 calc R . . C49 C 1.2202(4) 0.5697(5) 0.6341(4) 0.073(2) Uani 1 1 d . . . H49 H 1.2812 0.5369 0.627 0.088 Uiso 1 1 calc R . . C50 C 1.1455(4) 0.5228(4) 0.6556(3) 0.0576(16) Uani 1 1 d . . . H50 H 1.1561 0.4584 0.6629 0.069 Uiso 1 1 calc R . . C51 C 0.9965(3) 0.3955(3) 0.7018(2) 0.0365(10) Uani 1 1 d . . . C52 C 1.0478(4) 0.3424(4) 0.7510(3) 0.0473(13) Uani 1 1 d . . . H52 H 1.0669 0.3711 0.7757 0.057 Uiso 1 1 calc R . . C53 C 1.0716(4) 0.2484(4) 0.7646(3) 0.0603(16) Uani 1 1 d . . . H53 H 1.1059 0.2127 0.799 0.072 Uiso 1 1 calc R . . C54 C 1.0456(4) 0.2056(4) 0.7286(4) 0.0618(17) Uani 1 1 d . . . H54 H 1.0618 0.1407 0.7383 0.074 Uiso 1 1 calc R . . C55 C 0.9966(4) 0.2572(4) 0.6788(4) 0.0579(15) Uani 1 1 d . . . H55 H 0.9786 0.2282 0.6539 0.07 Uiso 1 1 calc R . . C56 C 0.9731(3) 0.3518(4) 0.6646(3) 0.0432(12) Uani 1 1 d . . . H56 H 0.9407 0.3873 0.6291 0.052 Uiso 1 1 calc R . . C57 C 0.8099(3) 0.6501(3) 0.5149(2) 0.0368(10) Uani 1 1 d . . . C58 C 0.8180(4) 0.7080(4) 0.4502(3) 0.0519(14) Uani 1 1 d . . . H58 H 0.856 0.7536 0.4356 0.062 Uiso 1 1 calc R . . C59 C 0.7706(4) 0.6995(5) 0.4064(3) 0.0643(18) Uani 1 1 d . . . H59 H 0.7761 0.7396 0.3621 0.077 Uiso 1 1 calc R . . C60 C 0.7164(4) 0.6339(5) 0.4268(3) 0.0576(15) Uani 1 1 d . . . H60 H 0.6836 0.6291 0.3969 0.069 Uiso 1 1 calc R . . C61 C 0.7090(4) 0.5749(4) 0.4907(3) 0.0540(14) Uani 1 1 d . . . H61 H 0.6723 0.5283 0.5045 0.065 Uiso 1 1 calc R . . C62 C 0.7549(4) 0.5831(4) 0.5348(3) 0.0454(12) Uani 1 1 d . . . H62 H 0.7488 0.5427 0.579 0.054 Uiso 1 1 calc R . . C63 C 0.9662(3) 0.7111(4) 0.5221(2) 0.0394(11) Uani 1 1 d . . . C64 C 0.9709(4) 0.8047(4) 0.4945(3) 0.0482(13) Uani 1 1 d . . . H64 H 0.9182 0.8492 0.502 0.058 Uiso 1 1 calc R . . C65 C 1.0520(4) 0.8333(4) 0.4562(3) 0.0582(15) Uani 1 1 d . . . H65 H 1.0545 0.8971 0.4376 0.07 Uiso 1 1 calc R . . C66 C 1.1291(4) 0.7692(5) 0.4452(3) 0.0618(16) Uani 1 1 d . . . H66 H 1.1853 0.7888 0.4203 0.074 Uiso 1 1 calc R . . C67 C 1.1241(4) 0.6766(5) 0.4704(3) 0.0562(15) Uani 1 1 d . . . H67 H 1.1766 0.6328 0.4614 0.067 Uiso 1 1 calc R . . C68 C 1.0435(3) 0.6470(4) 0.5087(3) 0.0437(12) Uani 1 1 d . . . H68 H 1.0409 0.5831 0.5257 0.052 Uiso 1 1 calc R . . C69 C 0.9215(3) 0.4846(3) 0.8235(2) 0.0374(10) Uani 1 1 d . . . C70 C 0.9774(3) 0.5194(4) 0.8484(3) 0.0415(11) Uani 1 1 d . . . C71 C 1.0047(4) 0.4679(4) 0.9096(3) 0.0490(13) Uani 1 1 d . . . H71 H 1.0443 0.4908 0.925 0.059 Uiso 1 1 calc R . . C72 C 0.9771(4) 0.3863(4) 0.9482(3) 0.0508(13) Uani 1 1 d . . . C73 C 0.9188(4) 0.3545(4) 0.9250(3) 0.0484(13) Uani 1 1 d . . . H73 H 0.8977 0.2986 0.9515 0.058 Uiso 1 1 calc R . . C74 C 0.8902(3) 0.4016(4) 0.8642(3) 0.0412(11) Uani 1 1 d . . . C75 C 1.0077(4) 0.6107(4) 0.8124(3) 0.0546(14) Uani 1 1 d . . . H75A H 1.0122 0.6385 0.8444 0.082 Uiso 1 1 calc R . . H75B H 0.9624 0.6515 0.7847 0.082 Uiso 1 1 calc R . . H75C H 1.0681 0.6018 0.7846 0.082 Uiso 1 1 calc R . . C76 C 1.0061(6) 0.3330(6) 1.0150(3) 0.079(2) Uani 1 1 d . . . H76A H 0.9795 0.2766 1.0347 0.119 Uiso 0.5 1 calc PR . . H76B H 0.9839 0.3711 1.0441 0.119 Uiso 0.5 1 calc PR . . H76C H 1.0736 0.3169 1.0093 0.119 Uiso 0.5 1 calc PR . . H76D H 1.0452 0.3665 1.024 0.119 Uiso 0.5 1 calc PR . . H76E H 1.0407 0.272 1.0147 0.119 Uiso 0.5 1 calc PR . . H76F H 0.951 0.3262 1.0494 0.119 Uiso 0.5 1 calc PR . . C77 C 0.8258(4) 0.3642(4) 0.8431(3) 0.0487(13) Uani 1 1 d . . . H77A H 0.8013 0.3146 0.8805 0.073 Uiso 1 1 calc R . . H77B H 0.8591 0.34 0.8071 0.073 Uiso 1 1 calc R . . H77C H 0.7746 0.4134 0.8278 0.073 Uiso 1 1 calc R . . C78 C 0.7568(3) 0.8315(3) 0.5842(2) 0.0397(11) Uani 1 1 d . . . C79 C 0.6787(4) 0.8585(4) 0.5532(3) 0.0466(12) Uani 1 1 d . . . C80 C 0.6445(4) 0.9521(4) 0.5259(3) 0.0629(17) Uani 1 1 d . . . H80 H 0.592 0.9693 0.505 0.076 Uiso 1 1 calc R . . C81 C 0.6840(5) 1.0211(4) 0.5280(4) 0.0656(18) Uani 1 1 d . . . C82 C 0.7570(4) 0.9927(4) 0.5625(4) 0.0622(17) Uani 1 1 d . . . H82 H 0.7838 1.0383 0.5664 0.075 Uiso 1 1 calc R . . C83 C 0.7931(4) 0.9003(4) 0.5917(3) 0.0452(12) Uani 1 1 d . . . C84 C 0.6255(4) 0.7896(4) 0.5527(4) 0.0589(16) Uani 1 1 d . . . H84A H 0.6454 0.7767 0.5107 0.088 Uiso 1 1 calc R . . H84B H 0.5593 0.815 0.558 0.088 Uiso 1 1 calc R . . H84C H 0.6372 0.7325 0.5892 0.088 Uiso 1 1 calc R . . C85 C 0.6500(7) 1.1205(5) 0.4942(6) 0.118(4) Uani 1 1 d . . . H85A H 0.6865 1.1584 0.501 0.176 Uiso 0.5 1 calc PR . . H85B H 0.5849 1.137 0.5125 0.176 Uiso 0.5 1 calc PR . . H85C H 0.6563 1.1313 0.4467 0.176 Uiso 0.5 1 calc PR . . H85D H 0.5986 1.1261 0.4725 0.176 Uiso 0.5 1 calc PR . . H85E H 0.7002 1.1475 0.461 0.176 Uiso 0.5 1 calc PR . . H85F H 0.6288 1.1532 0.5268 0.176 Uiso 0.5 1 calc PR . . C86 C 0.8690(4) 0.8767(4) 0.6310(3) 0.0593(15) Uani 1 1 d . . . H86A H 0.9284 0.8601 0.6043 0.089 Uiso 1 1 calc R . . H86B H 0.8576 0.8246 0.6711 0.089 Uiso 1 1 calc R . . H86C H 0.8706 0.93 0.6431 0.089 Uiso 1 1 calc R . . C1A C 0.0970(14) 0.9329(13) 0.7256(10) 0.178(6) Uiso 1 1 d . A 1 C2A C 0.1077(13) 0.9661(12) 0.6577(10) 0.176(6) Uiso 1 1 d . A 1 H2A H 0.0695 0.961 0.6313 0.211 Uiso 1 1 calc R A 1 C3A C 0.1806(12) 1.0060(11) 0.6365(9) 0.160(5) Uiso 1 1 d . A 1 H3A H 0.1916 1.0329 0.5898 0.192 Uiso 1 1 calc R A 1 C4A C 0.2424(12) 1.0178(11) 0.6648(9) 0.159(5) Uiso 1 1 d . A 1 H4A H 0.2943 1.0467 0.6418 0.191 Uiso 1 1 calc R A 1 C5A C 0.2214(14) 0.9835(13) 0.7292(10) 0.190(7) Uiso 1 1 d . A 1 H5A H 0.2603 0.9907 0.7542 0.228 Uiso 1 1 calc R A 1 C6A C 0.1569(9) 0.9431(8) 0.7608(6) 0.118(3) Uiso 1 1 d . A 1 H6A H 0.1478 0.9195 0.8077 0.142 Uiso 1 1 calc R A 1 C7A C 0.024(2) 0.890(2) 0.7578(15) 0.317(15) Uiso 1 1 d . A 1 H7A1 H 0.024 0.8691 0.8055 0.475 Uiso 0.5 1 calc PR A 1 H7A2 H 0.0295 0.8367 0.7435 0.475 Uiso 0.5 1 calc PR A 1 H7A3 H -0.0331 0.9327 0.7477 0.475 Uiso 0.5 1 calc PR A 1 H7A4 H -0.0104 0.8899 0.7257 0.475 Uiso 0.5 1 calc PR A 1 H7A5 H -0.0159 0.9223 0.7876 0.475 Uiso 0.5 1 calc PR A 1 H7A6 H 0.0467 0.8263 0.7834 0.475 Uiso 0.5 1 calc PR A 1 C1B C 0.6075(11) -0.0537(14) 0.9639(9) 0.115(7) Uiso 0.5 1 d PD . 1 C2B C 0.5508(13) -0.0437(12) 0.9236(8) 0.192(7) Uiso 1 1 d D B 1 C3B C 0.4625(13) -0.0070(14) 0.9351(9) 0.122(7) Uiso 0.5 1 d PD B 1 C4B C 0.4269(8) 0.0253(9) 0.9840(6) 0.138(4) Uiso 1 1 d D . 1 C5B C 0.5166(8) -0.0198(14) 0.9758(8) 0.114(7) Uiso 0.5 1 d PD . 1 C1C C 1.3475(8) 0.2846(8) 0.7429(6) 0.137(4) Uiso 1 1 d D C 1 C2C C 1.3965(11) 0.2078(13) 0.7220(8) 0.136(8) Uiso 0.5 1 d PD C 1 C3C C 1.3793(14) 0.1255(12) 0.7635(10) 0.258(11) Uiso 1 1 d D C 1 C4C C 1.3176(19) 0.1183(11) 0.8196(11) 0.176(12) Uiso 0.5 1 d PD C 1 C5C C 1.2790(10) 0.1857(9) 0.8401(6) 0.154(5) Uiso 1 1 d D C 1 C6C C 1.285(2) 0.2724(9) 0.8027(12) 0.33(3) Uiso 0.5 1 d PD C 1 C7C C 1.2438(11) 0.3433(10) 0.8182(8) 0.174(6) Uiso 1 1 d D C 1 C8C C 1.3029(13) 0.3534(10) 0.7617(8) 0.104(6) Uiso 0.5 1 d PD C 1 C9C C 1.2293(11) 0.2580(11) 0.8594(7) 0.094(5) Uiso 0.5 1 d PD C 1 C10C C 1.3352(11) 0.2000(8) 0.7803(7) 0.091(5) Uiso 0.5 1 d PD C 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 Sm 0.02335(12) 0.03173(13) 0.03489(13) -0.00891(9) -0.00073(8) -0.00409(8) P1 0.0282(6) 0.0301(6) 0.0368(6) -0.0086(5) -0.0042(5) -0.0051(4) P2 0.0349(6) 0.0309(6) 0.0377(6) -0.0118(5) 0.0020(5) -0.0071(5) P3 0.0237(5) 0.0337(6) 0.0359(6) -0.0087(5) -0.0055(4) -0.0018(4) P4 0.0258(5) 0.0331(6) 0.0336(6) -0.0072(5) -0.0024(4) -0.0038(4) N1 0.0313(19) 0.036(2) 0.040(2) -0.0121(17) -0.0055(16) -0.0094(16) N2 0.051(3) 0.029(2) 0.046(2) -0.0121(18) 0.011(2) -0.0106(18) N3 0.0279(19) 0.039(2) 0.040(2) -0.0124(17) -0.0059(16) -0.0020(16) N4 0.036(2) 0.032(2) 0.036(2) -0.0073(16) 0.0006(17) -0.0030(16) C1 0.034(2) 0.031(2) 0.038(2) -0.0100(19) -0.0047(19) -0.0045(18) C2 0.035(2) 0.043(3) 0.045(3) -0.014(2) -0.009(2) 0.001(2) C3 0.043(3) 0.046(3) 0.052(3) -0.017(2) -0.008(2) 0.002(2) C4 0.055(4) 0.044(3) 0.074(4) -0.020(3) -0.018(3) 0.011(3) C5 0.040(3) 0.073(5) 0.117(6) -0.028(4) -0.027(4) 0.010(3) C6 0.034(3) 0.074(5) 0.133(7) -0.019(5) -0.014(4) -0.008(3) C7 0.032(3) 0.055(3) 0.089(5) -0.016(3) -0.005(3) -0.007(2) C8 0.030(2) 0.033(2) 0.042(3) -0.010(2) -0.0009(19) -0.0086(18) C9 0.039(3) 0.040(3) 0.048(3) -0.011(2) -0.004(2) -0.015(2) C10 0.057(3) 0.042(3) 0.071(4) -0.019(3) 0.000(3) -0.021(3) C11 0.062(4) 0.036(3) 0.074(4) -0.001(3) -0.008(3) -0.019(3) C12 0.053(3) 0.041(3) 0.061(4) 0.003(3) -0.013(3) -0.013(3) C13 0.039(3) 0.039(3) 0.047(3) -0.007(2) -0.007(2) -0.012(2) C14 0.035(2) 0.042(3) 0.038(3) -0.015(2) -0.001(2) -0.004(2) C15 0.045(3) 0.042(3) 0.050(3) -0.014(2) 0.000(2) -0.004(2) C16 0.053(3) 0.048(3) 0.061(4) -0.018(3) -0.002(3) 0.011(3) C17 0.035(3) 0.083(5) 0.065(4) -0.029(4) 0.003(3) 0.003(3) C18 0.043(3) 0.068(4) 0.059(4) -0.017(3) 0.005(3) -0.017(3) C19 0.044(3) 0.049(3) 0.047(3) -0.016(2) -0.001(2) -0.009(2) C20 0.033(2) 0.040(3) 0.038(2) -0.014(2) 0.0019(19) -0.011(2) C21 0.039(3) 0.054(3) 0.060(3) -0.029(3) -0.006(2) -0.004(2) C22 0.041(3) 0.065(4) 0.074(4) -0.032(3) -0.015(3) 0.003(3) C23 0.050(3) 0.084(4) 0.061(4) -0.039(3) -0.016(3) -0.009(3) C24 0.057(4) 0.081(4) 0.063(4) -0.046(4) -0.007(3) -0.005(3) C25 0.042(3) 0.061(3) 0.058(3) -0.032(3) -0.004(3) -0.003(3) C26 0.031(2) 0.035(2) 0.033(2) -0.0097(19) -0.0018(18) -0.0100(18) C27 0.029(2) 0.036(2) 0.038(2) -0.011(2) 0.0011(19) -0.0078(18) C28 0.047(3) 0.037(3) 0.040(3) -0.014(2) 0.002(2) -0.009(2) C29 0.053(3) 0.049(3) 0.038(3) -0.016(2) -0.006(2) -0.014(2) C30 0.042(3) 0.052(3) 0.040(3) -0.010(2) -0.012(2) -0.011(2) C31 0.032(2) 0.039(2) 0.036(2) -0.009(2) -0.0030(19) -0.0060(19) C32 0.037(3) 0.044(3) 0.056(3) -0.014(2) -0.009(2) -0.001(2) C33 0.083(5) 0.066(4) 0.067(4) -0.033(3) -0.022(4) -0.013(4) C34 0.049(3) 0.047(3) 0.052(3) -0.013(2) -0.021(3) 0.005(2) C35 0.065(4) 0.027(2) 0.053(3) -0.012(2) 0.023(3) -0.013(2) C36 0.061(4) 0.046(3) 0.073(4) -0.025(3) 0.026(3) -0.023(3) C37 0.089(5) 0.056(4) 0.104(6) -0.039(4) 0.036(5) -0.042(4) C38 0.108(7) 0.033(3) 0.110(7) -0.023(4) 0.044(5) -0.022(4) C39 0.103(6) 0.035(3) 0.085(5) -0.010(3) 0.031(5) -0.008(4) C40 0.072(4) 0.036(3) 0.058(4) -0.010(3) 0.020(3) -0.005(3) C41 0.063(4) 0.073(5) 0.110(6) -0.034(4) 0.012(4) -0.041(4) C42 0.172(11) 0.045(4) 0.170(11) -0.037(6) 0.042(9) -0.042(6) C43 0.095(6) 0.056(4) 0.061(4) -0.001(3) -0.009(4) 0.001(4) C44 0.031(2) 0.032(2) 0.041(3) -0.008(2) -0.0087(19) -0.0043(18) C45 0.031(2) 0.045(3) 0.043(3) -0.010(2) -0.009(2) -0.009(2) C46 0.035(3) 0.045(3) 0.053(3) -0.012(2) -0.011(2) -0.006(2) C47 0.052(3) 0.051(3) 0.065(4) -0.004(3) -0.018(3) -0.019(3) C48 0.040(3) 0.072(4) 0.087(5) -0.007(4) -0.013(3) -0.024(3) C49 0.025(3) 0.069(4) 0.112(6) -0.014(4) -0.008(3) -0.009(3) C50 0.030(3) 0.048(3) 0.084(4) -0.016(3) -0.005(3) -0.002(2) C51 0.025(2) 0.034(2) 0.045(3) -0.012(2) -0.0002(19) -0.0014(18) C52 0.036(3) 0.046(3) 0.053(3) -0.013(2) -0.010(2) 0.003(2) C53 0.054(3) 0.046(3) 0.061(4) -0.004(3) -0.015(3) 0.012(3) C54 0.055(4) 0.035(3) 0.082(5) -0.016(3) -0.007(3) 0.006(3) C55 0.044(3) 0.044(3) 0.085(5) -0.028(3) -0.010(3) 0.002(2) C56 0.033(2) 0.044(3) 0.049(3) -0.019(2) -0.006(2) 0.004(2) C57 0.025(2) 0.042(3) 0.036(2) -0.008(2) -0.0025(18) -0.0027(19) C58 0.046(3) 0.061(3) 0.042(3) -0.005(3) -0.005(2) -0.017(3) C59 0.056(4) 0.091(5) 0.037(3) -0.001(3) -0.014(3) -0.018(3) C60 0.044(3) 0.086(4) 0.046(3) -0.019(3) -0.013(3) -0.017(3) C61 0.046(3) 0.064(4) 0.057(3) -0.016(3) -0.012(3) -0.020(3) C62 0.043(3) 0.048(3) 0.040(3) -0.005(2) -0.009(2) -0.012(2) C63 0.028(2) 0.049(3) 0.038(3) -0.011(2) 0.0009(19) -0.011(2) C64 0.042(3) 0.044(3) 0.051(3) -0.011(2) 0.003(2) -0.011(2) C65 0.048(3) 0.053(3) 0.065(4) -0.012(3) 0.007(3) -0.020(3) C66 0.042(3) 0.069(4) 0.066(4) -0.020(3) 0.011(3) -0.018(3) C67 0.033(3) 0.072(4) 0.054(3) -0.019(3) 0.004(2) -0.004(3) C68 0.034(2) 0.046(3) 0.045(3) -0.015(2) 0.000(2) -0.003(2) C69 0.023(2) 0.046(3) 0.039(3) -0.015(2) -0.0056(18) 0.0024(19) C70 0.032(2) 0.050(3) 0.044(3) -0.022(2) -0.005(2) -0.001(2) C71 0.039(3) 0.068(4) 0.046(3) -0.026(3) -0.015(2) -0.001(3) C72 0.049(3) 0.060(3) 0.041(3) -0.018(3) -0.015(2) 0.004(3) C73 0.047(3) 0.047(3) 0.043(3) -0.010(2) -0.005(2) -0.004(2) C74 0.031(2) 0.044(3) 0.047(3) -0.014(2) -0.008(2) -0.003(2) C75 0.054(3) 0.060(4) 0.059(4) -0.023(3) -0.011(3) -0.017(3) C76 0.098(6) 0.083(5) 0.055(4) -0.010(4) -0.038(4) -0.005(4) C77 0.037(3) 0.052(3) 0.052(3) -0.009(3) -0.007(2) -0.012(2) C78 0.035(2) 0.034(2) 0.038(3) -0.005(2) 0.003(2) -0.0025(19) C79 0.034(3) 0.044(3) 0.052(3) -0.012(2) -0.001(2) -0.003(2) C80 0.046(3) 0.053(3) 0.074(4) -0.011(3) -0.017(3) 0.012(3) C81 0.058(4) 0.039(3) 0.082(5) -0.009(3) -0.008(3) 0.005(3) C82 0.058(4) 0.034(3) 0.086(5) -0.020(3) 0.003(3) -0.007(3) C83 0.040(3) 0.039(3) 0.050(3) -0.015(2) 0.001(2) -0.005(2) C84 0.031(3) 0.059(4) 0.088(5) -0.030(3) -0.015(3) 0.004(2) C85 0.115(7) 0.038(4) 0.168(10) -0.005(5) -0.041(7) 0.017(4) C86 0.059(4) 0.053(3) 0.071(4) -0.028(3) -0.011(3) -0.006(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Sm N2 2.592(4) . ? Sm N4 2.605(4) . ? Sm N1 2.606(4) . ? Sm N3 2.608(4) . ? Sm C44 2.877(5) . ? Sm C1 2.900(5) . ? P1 N1 1.617(4) . ? P1 C1 1.714(5) . ? P1 C2 1.822(5) . ? P1 C8 1.825(5) . ? P2 N2 1.600(4) . ? P2 C1 1.724(5) . ? P2 C20 1.820(5) . ? P2 C14 1.832(5) . ? P3 N3 1.618(4) . ? P3 C44 1.731(5) . ? P3 C45 1.817(5) . ? P3 C51 1.835(5) . ? P4 N4 1.607(4) . ? P4 C44 1.722(5) . ? P4 C57 1.829(5) . ? P4 C63 1.833(5) . ? N1 C26 1.436(6) . ? N2 C35 1.427(6) . ? N3 C69 1.432(6) . ? N4 C78 1.430(6) . ? C2 C7 1.385(8) . ? C2 C3 1.393(7) . ? C3 C4 1.382(8) . ? C4 C5 1.385(10) . ? C5 C6 1.367(10) . ? C6 C7 1.388(8) . ? C8 C13 1.383(7) . ? C8 C9 1.394(7) . ? C9 C10 1.382(7) . ? C10 C11 1.380(9) . ? C11 C12 1.378(9) . ? C12 C13 1.388(7) . ? C14 C15 1.390(7) . ? C14 C19 1.398(7) . ? C15 C16 1.385(8) . ? C16 C17 1.380(9) . ? C17 C18 1.382(9) . ? C18 C19 1.380(8) . ? C20 C21 1.395(7) . ? C20 C25 1.398(7) . ? C21 C22 1.389(8) . ? C22 C23 1.373(9) . ? C23 C24 1.379(9) . ? C24 C25 1.378(9) . ? C26 C27 1.407(7) . ? C26 C31 1.406(7) . ? C27 C28 1.405(7) . ? C27 C32 1.506(7) . ? C28 C29 1.382(8) . ? C29 C30 1.366(8) . ? C29 C33 1.510(8) . ? C30 C31 1.407(7) . ? C31 C34 1.511(7) . ? C35 C36 1.401(10) . ? C35 C40 1.427(9) . ? C36 C37 1.404(8) . ? C36 C41 1.480(11) . ? C37 C38 1.369(13) . ? C38 C39 1.373(14) . ? C38 C42 1.520(10) . ? C39 C40 1.411(9) . ? C40 C43 1.492(11) . ? C45 C46 1.388(7) . ? C45 C50 1.394(7) . ? C46 C47 1.393(8) . ? C47 C48 1.391(9) . ? C48 C49 1.366(10) . ? C49 C50 1.400(8) . ? C51 C52 1.386(7) . ? C51 C56 1.397(7) . ? C52 C53 1.378(8) . ? C53 C54 1.385(10) . ? C54 C55 1.369(9) . ? C55 C56 1.384(8) . ? C57 C58 1.383(7) . ? C57 C62 1.392(7) . ? C58 C59 1.396(9) . ? C59 C60 1.364(9) . ? C60 C61 1.375(8) . ? C61 C62 1.382(8) . ? C63 C64 1.397(7) . ? C63 C68 1.397(7) . ? C64 C65 1.386(8) . ? C65 C66 1.381(9) . ? C66 C67 1.382(9) . ? C67 C68 1.386(7) . ? C69 C70 1.416(7) . ? C69 C74 1.416(7) . ? C70 C71 1.402(7) . ? C70 C75 1.501(8) . ? C71 C72 1.366(9) . ? C72 C73 1.386(8) . ? C72 C76 1.518(8) . ? C73 C74 1.392(7) . ? C74 C77 1.494(7) . ? C78 C83 1.410(8) . ? C78 C79 1.409(7) . ? C79 C80 1.398(8) . ? C79 C84 1.513(8) . ? C80 C81 1.389(10) . ? C81 C82 1.386(10) . ? C81 C85 1.495(9) . ? C82 C83 1.395(8) . ? C83 C86 1.501(8) . ? C1A C7A 1.35(3) . ? C1A C2A 1.38(2) . ? C1A C6A 1.40(2) . ? C2A C3A 1.31(2) . ? C3A C4A 1.326(19) . ? C4A C5A 1.31(2) . ? C5A C6A 1.227(19) . ? C1B C4B 1.324(14) 2_657 ? C1B C2B 1.327(14) . ? C1B C5B 1.349(15) . ? C2B C5B 1.290(14) . ? C2B C3B 1.323(14) . ? C3B C5B 1.290(15) . ? C3B C4B 1.301(14) . ? C4B C1B 1.324(14) 2_657 ? C4B C5B 1.342(13) 2_657 ? C4B C5B 1.372(13) . ? C5B C4B 1.342(13) 2_657 ? C5B C5B 1.36(3) 2_657 ? C1C C8C 1.281(13) . ? C1C C10C 1.326(11) . ? C1C C6C 1.407(12) . ? C1C C2C 1.424(13) . ? C2C C3C 1.339(14) . ? C2C C10C 1.374(12) . ? C3C C10C 1.335(14) . ? C3C C4C 1.343(14) . ? C4C C5C 1.263(14) . ? C4C C10C 1.320(13) . ? C5C C6C 1.332(12) . ? C5C C9C 1.351(13) . ? C5C C10C 1.358(11) . ? C6C C7C 1.260(12) . ? C6C C9C 1.303(12) . ? C6C C8C 1.325(13) . ? C6C C10C 1.390(12) . ? C7C C8C 1.327(13) . ? C7C C9C 1.364(13) . ? 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 N2 Sm N4 99.58(12) . . ? N2 Sm N1 98.87(13) . . ? N4 Sm N1 116.88(13) . . ? N2 Sm N3 117.37(14) . . ? N4 Sm N3 98.91(12) . . ? N1 Sm N3 123.56(12) . . ? N2 Sm C44 154.97(13) . . ? N4 Sm C44 58.94(12) . . ? N1 Sm C44 102.47(13) . . ? N3 Sm C44 59.67(13) . . ? N2 Sm C1 58.47(13) . . ? N4 Sm C1 153.87(13) . . ? N1 Sm C1 59.26(13) . . ? N3 Sm C1 103.87(13) . . ? C44 Sm C1 145.52(13) . . ? N1 P1 C1 110.3(2) . . ? N1 P1 C2 112.1(2) . . ? C1 P1 C2 110.4(2) . . ? N1 P1 C8 111.1(2) . . ? C1 P1 C8 107.3(2) . . ? C2 P1 C8 105.4(2) . . ? N1 P1 Sm 49.95(14) . . ? C1 P1 Sm 60.43(16) . . ? C2 P1 Sm 126.87(17) . . ? C8 P1 Sm 127.65(15) . . ? N2 P2 C1 108.4(2) . . ? N2 P2 C20 114.4(2) . . ? C1 P2 C20 105.3(2) . . ? N2 P2 C14 114.6(2) . . ? C1 P2 C14 112.9(2) . . ? C20 P2 C14 101.0(2) . . ? N2 P2 Sm 49.71(15) . . ? C1 P2 Sm 60.76(16) . . ? C20 P2 Sm 112.76(16) . . ? C14 P2 Sm 146.23(17) . . ? N3 P3 C44 109.7(2) . . ? N3 P3 C45 112.7(2) . . ? C44 P3 C45 110.5(2) . . ? N3 P3 C51 111.4(2) . . ? C44 P3 C51 107.3(2) . . ? C45 P3 C51 105.1(2) . . ? N3 P3 Sm 50.07(14) . . ? C44 P3 Sm 59.66(16) . . ? C45 P3 Sm 127.52(17) . . ? C51 P3 Sm 127.32(15) . . ? N4 P4 C44 108.8(2) . . ? N4 P4 C57 113.9(2) . . ? C44 P4 C57 104.8(2) . . ? N4 P4 C63 114.6(2) . . ? C44 P4 C63 113.0(2) . . ? C57 P4 C63 101.2(2) . . ? N4 P4 Sm 50.63(14) . . ? C44 P4 Sm 60.33(16) . . ? C57 P4 Sm 111.92(15) . . ? C63 P4 Sm 146.88(17) . . ? C26 N1 P1 121.5(3) . . ? C26 N1 Sm 135.0(3) . . ? P1 N1 Sm 101.69(18) . . ? C35 N2 P2 129.5(4) . . ? C35 N2 Sm 125.5(3) . . ? P2 N2 Sm 102.20(19) . . ? C69 N3 P3 122.7(3) . . ? C69 N3 Sm 134.3(3) . . ? P3 N3 Sm 101.53(18) . . ? C78 N4 P4 127.5(3) . . ? C78 N4 Sm 128.4(3) . . ? P4 N4 Sm 100.90(18) . . ? P1 C1 P2 133.3(3) . . ? P1 C1 Sm 88.64(19) . . ? P2 C1 Sm 88.00(18) . . ? C7 C2 C3 118.7(5) . . ? C7 C2 P1 123.9(4) . . ? C3 C2 P1 117.5(4) . . ? C4 C3 C2 121.3(6) . . ? C3 C4 C5 119.2(6) . . ? C6 C5 C4 120.0(6) . . ? C5 C6 C7 121.1(7) . . ? C2 C7 C6 119.7(6) . . ? C13 C8 C9 118.6(5) . . ? C13 C8 P1 122.4(4) . . ? C9 C8 P1 118.8(4) . . ? C10 C9 C8 120.6(5) . . ? C11 C10 C9 120.5(6) . . ? C10 C11 C12 119.1(5) . . ? C11 C12 C13 120.8(6) . . ? C8 C13 C12 120.4(5) . . ? C15 C14 C19 118.3(5) . . ? C15 C14 P2 122.5(4) . . ? C19 C14 P2 119.2(4) . . ? C16 C15 C14 120.3(5) . . ? C17 C16 C15 120.9(6) . . ? C16 C17 C18 119.2(5) . . ? C19 C18 C17 120.4(6) . . ? C18 C19 C14 120.8(5) . . ? C21 C20 C25 117.7(5) . . ? C21 C20 P2 121.0(4) . . ? C25 C20 P2 121.0(4) . . ? C22 C21 C20 120.9(5) . . ? C23 C22 C21 120.2(6) . . ? C22 C23 C24 119.8(6) . . ? C23 C24 C25 120.3(6) . . ? C24 C25 C20 121.0(5) . . ? C27 C26 C31 118.4(4) . . ? C27 C26 N1 118.6(4) . . ? C31 C26 N1 123.0(4) . . ? C28 C27 C26 119.5(5) . . ? C28 C27 C32 118.5(5) . . ? C26 C27 C32 122.0(5) . . ? C29 C28 C27 122.2(5) . . ? C30 C29 C28 117.7(5) . . ? C30 C29 C33 121.7(5) . . ? C28 C29 C33 120.6(5) . . ? C29 C30 C31 122.7(5) . . ? C30 C31 C26 119.4(5) . . ? C30 C31 C34 118.2(5) . . ? C26 C31 C34 122.4(5) . . ? C36 C35 N2 121.8(6) . . ? C36 C35 C40 119.9(5) . . ? N2 C35 C40 118.0(6) . . ? C35 C36 C37 118.3(7) . . ? C35 C36 C41 123.1(5) . . ? C37 C36 C41 118.5(7) . . ? C38 C37 C36 123.3(8) . . ? C37 C38 C39 117.5(7) . . ? C37 C38 C42 121.2(11) . . ? C39 C38 C42 121.2(10) . . ? C38 C39 C40 123.4(8) . . ? C39 C40 C35 117.3(8) . . ? C39 C40 C43 120.1(7) . . ? C35 C40 C43 122.6(6) . . ? P4 C44 P3 132.7(3) . . ? P4 C44 Sm 88.34(18) . . ? P3 C44 Sm 89.05(19) . . ? C46 C45 C50 118.4(5) . . ? C46 C45 P3 117.4(4) . . ? C50 C45 P3 124.1(4) . . ? C45 C46 C47 121.7(5) . . ? C48 C47 C46 118.9(6) . . ? C49 C48 C47 120.3(6) . . ? C48 C49 C50 120.7(6) . . ? C45 C50 C49 120.0(6) . . ? C52 C51 C56 118.2(5) . . ? C52 C51 P3 119.1(4) . . ? C56 C51 P3 122.4(4) . . ? C53 C52 C51 120.6(6) . . ? C52 C53 C54 120.5(6) . . ? C55 C54 C53 119.7(6) . . ? C54 C55 C56 120.0(6) . . ? C55 C56 C51 120.9(5) . . ? C58 C57 C62 118.8(5) . . ? C58 C57 P4 120.2(4) . . ? C62 C57 P4 120.8(4) . . ? C57 C58 C59 120.0(5) . . ? C60 C59 C58 120.4(5) . . ? C59 C60 C61 120.1(6) . . ? C60 C61 C62 120.1(5) . . ? C61 C62 C57 120.6(5) . . ? C64 C63 C68 118.9(5) . . ? C64 C63 P4 122.7(4) . . ? C68 C63 P4 118.4(4) . . ? C65 C64 C63 120.5(5) . . ? C66 C65 C64 120.2(6) . . ? C65 C66 C67 119.7(5) . . ? C66 C67 C68 120.7(5) . . ? C67 C68 C63 119.9(5) . . ? C70 C69 C74 117.7(5) . . ? C70 C69 N3 123.0(5) . . ? C74 C69 N3 119.2(4) . . ? C71 C70 C69 119.2(5) . . ? C71 C70 C75 118.2(5) . . ? C69 C70 C75 122.5(5) . . ? C72 C71 C70 123.1(5) . . ? C71 C72 C73 117.4(5) . . ? C71 C72 C76 121.9(6) . . ? C73 C72 C76 120.6(6) . . ? C72 C73 C74 122.4(5) . . ? C73 C74 C69 120.0(5) . . ? C73 C74 C77 119.4(5) . . ? C69 C74 C77 120.7(5) . . ? C83 C78 C79 118.4(5) . . ? C83 C78 N4 119.4(5) . . ? C79 C78 N4 122.1(5) . . ? C80 C79 C78 119.5(5) . . ? C80 C79 C84 118.1(5) . . ? C78 C79 C84 122.2(5) . . ? C81 C80 C79 122.9(6) . . ? C82 C81 C80 116.4(5) . . ? C82 C81 C85 122.1(7) . . ? C80 C81 C85 121.5(7) . . ? C81 C82 C83 123.2(6) . . ? C82 C83 C78 119.3(5) . . ? C82 C83 C86 119.1(5) . . ? C78 C83 C86 121.7(5) . . ? C7A C1A C2A 117(2) . . ? C7A C1A C6A 120(2) . . ? C2A C1A C6A 122.8(19) . . ? C3A C2A C1A 107.0(19) . . ? C2A C3A C4A 135.2(19) . . ? C5A C4A C3A 109.9(18) . . ? C6A C5A C4A 127(2) . . ? C5A C6A C1A 117.9(17) . . ? C4B C1B C2B 117.8(12) 2_657 . ? C4B C1B C5B 60.3(8) 2_657 . ? C2B C1B C5B 57.6(8) . . ? C5B C2B C3B 59.2(8) . . ? C5B C2B C1B 62.0(8) . . ? C3B C2B C1B 121.1(12) . . ? C5B C3B C4B 64.0(8) . . ? C5B C3B C2B 59.2(8) . . ? C4B C3B C2B 122.9(12) . . ? C3B C4B C1B 176.9(18) . 2_657 ? C3B C4B C5B 117.4(13) . 2_657 ? C1B C4B C5B 60.8(8) 2_657 2_657 ? C3B C4B C5B 57.6(8) . . ? C1B C4B C5B 120.3(13) 2_657 . ? C5B C4B C5B 60.0(13) 2_657 . ? C3B C5B C2B 61.7(8) . . ? C3B C5B C4B 175(2) . 2_657 ? C2B C5B C4B 119.2(11) . 2_657 ? C3B C5B C1B 122.0(12) . . ? C2B C5B C1B 60.3(8) . . ? C4B C5B C1B 59.0(7) 2_657 . ? C3B C5B C5B 117.1(13) . 2_657 ? C2B C5B C5B 170(3) . 2_657 ? C4B C5B C5B 61.1(10) 2_657 2_657 ? C1B C5B C5B 119.5(13) . 2_657 ? C3B C5B C4B 58.4(7) . . ? C2B C5B C4B 119.9(11) . . ? C4B C5B C4B 120.0(13) 2_657 . ? C1B C5B C4B 173(2) . . ? C5B C5B C4B 58.9(9) 2_657 . ? C8C C1C C10C 119.9(9) . . ? C8C C1C C6C 58.9(6) . . ? C10C C1C C6C 61.0(6) . . ? C8C C1C C2C 179.5(12) . . ? C10C C1C C2C 59.8(6) . . ? C6C C1C C2C 120.8(8) . . ? C3C C2C C10C 58.9(7) . . ? C3C C2C C1C 115.5(9) . . ? C10C C2C C1C 56.5(5) . . ? C10C C3C C2C 61.9(7) . . ? C10C C3C C4C 59.1(7) . . ? C2C C3C C4C 120.9(11) . . ? C5C C4C C10C 63.4(7) . . ? C5C C4C C3C 123.4(11) . . ? C10C C4C C3C 60.1(8) . . ? C4C C5C C6C 122.2(10) . . ? C4C C5C C9C 174(2) . . ? C6C C5C C9C 58.1(6) . . ? C4C C5C C10C 60.3(7) . . ? C6C C5C C10C 62.2(6) . . ? C9C C5C C10C 120.2(9) . . ? C7C C6C C9C 64.3(7) . . ? C7C C6C C8C 61.7(7) . . ? C9C C6C C8C 126.0(10) . . ? C7C C6C C5C 125.9(10) . . ? C9C C6C C5C 61.7(7) . . ? C8C C6C C5C 171(2) . . ? C7C C6C C10C 174.1(14) . . ? C9C C6C C10C 121.5(10) . . ? C8C C6C C10C 112.4(9) . . ? C5C C6C C10C 59.8(6) . . ? C7C C6C C1C 117.5(10) . . ? C9C C6C C1C 177(3) . . ? C8C C6C C1C 55.8(7) . . ? C5C C6C C1C 116.3(8) . . ? C10C C6C C1C 56.6(5) . . ? C6C C7C C8C 61.6(7) . . ? C6C C7C C9C 59.4(7) . . ? C8C C7C C9C 120.9(9) . . ? C1C C8C C6C 65.3(7) . . ? C1C C8C C7C 122.0(10) . . ? C6C C8C C7C 56.7(6) . . ? C6C C9C C5C 60.2(7) . . ? C6C C9C C7C 56.3(6) . . ? C5C C9C C7C 116.5(9) . . ? C4C C10C C1C 176.1(13) . . ? C4C C10C C3C 60.8(7) . . ? C1C C10C C3C 122.8(10) . . ? C4C C10C C5C 56.2(7) . . ? C1C C10C C5C 120.2(8) . . ? C3C C10C C5C 116.9(9) . . ? C4C C10C C2C 120.0(9) . . ? C1C C10C C2C 63.6(7) . . ? C3C C10C C2C 59.2(7) . . ? C5C C10C C2C 175.4(13) . . ? C4C C10C C6C 114.0(9) . . ? C1C C10C C6C 62.4(6) . . ? C3C C10C C6C 174.7(11) . . ? C5C C10C C6C 58.0(6) . . ? C2C C10C C6C 126.0(9) . . ? #===END