# Supplementary Material (ESI) for Chemical Communications 
# This journal is (c) The Royal Society of Chemistry 2012

data_global
_journal_name_full               ' Chemical Communications '

_journal_coden_Cambridge         ?
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Qi Shen'
_publ_contact_author_email       qshen@suda.edu.cn

_publ_section_title              
;
Highly heteroselective ring-opening polymerization of racemic lactide initiated by bis(phenolate) divalent ytterbium complexes
;
loop_
_publ_author_name 
'Sheng Yang'
'Zhu Du'
'Yong Zhang'
'Qi Shen'

# Attachment 'CC-complex.cif '


data_compound1
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety 
 'C33 H55 N3 O3 Yb'         
_chemical_formula_sum 
 'C33 H55 N3 O3 Yb' 
_chemical_formula_weight          714.84 
 
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' 
 'Yb'  'Yb'  -0.3850   5.5486 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting                 monoclinic
_symmetry_space_group_name_H-M        'P 21/c'
_symmetry_space_group_name_Hall       '-P 2ybc'
_symmetry_Int_Tables_number            14
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    9.792(3) 
_cell_length_b                    23.618(6) 
_cell_length_c                    15.158(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  105.411(6) 
_cell_angle_gamma                 90.00 
_cell_volume                      3379.7(17) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     223(2) 
_cell_measurement_reflns_used     15827
_cell_measurement_theta_min       3.0 
_cell_measurement_theta_max       27.5 
 
_exptl_crystal_description        'block'
_exptl_crystal_colour             'colorless'
_exptl_crystal_size_max           0.60 
_exptl_crystal_size_mid           0.50 
_exptl_crystal_size_min           0.45 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.405 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1472 
_exptl_absorpt_coefficient_mu     2.801 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.202 
_exptl_absorpt_correction_T_max   0.281
_exptl_absorpt_process_details     
 'Jacobson, R. (1998) Private communication'
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       223(2) 
_diffrn_radiation_wavelength      0.71075 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Rigaku Saturn'
_diffrn_measurement_method        ω
_diffrn_detector_area_resol_mean  14.63
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             16360 
_diffrn_reflns_av_R_equivalents   0.0393 
_diffrn_reflns_av_sigmaI/netI     0.0708 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -28 
_diffrn_reflns_limit_k_max        28 
_diffrn_reflns_limit_l_min        -15 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          2.99 
_diffrn_reflns_theta_max          25.50 
_reflns_number_total              6246 
_reflns_number_gt                 5353 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'CrystalClear'
_computing_cell_refinement        'CrystalClear'
_computing_data_reduction         'CrystalStructure'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0442P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          6246 
_refine_ls_number_parameters      375 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0448 
_refine_ls_R_factor_gt            0.0367 
_refine_ls_wR_factor_ref          0.0936 
_refine_ls_wR_factor_gt           0.0871 
_refine_ls_goodness_of_fit_ref    1.138 
_refine_ls_restrained_S_all       1.138 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Yb1 Yb 0.25809(2) 0.342851(7) 0.510261(12) 0.02971(9) Uani 1 1 d . . . 
O1 O 0.3043(3) 0.39848(12) 0.40532(19) 0.0348(7) Uani 1 1 d . . . 
O2 O 0.1512(3) 0.27393(13) 0.4166(2) 0.0436(8) Uani 1 1 d . . . 
O3 O 0.3495(4) 0.27361(15) 0.6353(2) 0.0491(9) Uani 1 1 d . . . 
N1 N 0.4757(4) 0.29515(15) 0.4886(2) 0.0326(8) Uani 1 1 d . . . 
N2 N 0.0500(4) 0.39106(16) 0.5540(3) 0.0390(9) Uani 1 1 d . . . 
N3 N 0.3596(4) 0.42579(16) 0.6319(2) 0.0373(9) Uani 1 1 d . . . 
C1 C 0.3813(4) 0.39499(17) 0.3465(3) 0.0278(9) Uani 1 1 d . . . 
C2 C 0.3358(4) 0.41896(17) 0.2564(3) 0.0276(9) Uani 1 1 d . . . 
C3 C 0.4290(5) 0.41678(18) 0.2009(3) 0.0331(10) Uani 1 1 d . . . 
H3 H 0.4000 0.4334 0.1425 0.040 Uiso 1 1 calc R . . 
C4 C 0.5616(5) 0.39167(18) 0.2267(3) 0.0336(10) Uani 1 1 d . . . 
C5 C 0.6000(4) 0.36575(18) 0.3115(3) 0.0342(10) Uani 1 1 d . . . 
H5 H 0.6872 0.3466 0.3294 0.041 Uiso 1 1 calc R . . 
C6 C 0.5137(4) 0.36711(17) 0.3714(3) 0.0295(10) Uani 1 1 d . . . 
C7 C 0.1881(5) 0.22112(18) 0.4117(3) 0.0346(10) Uani 1 1 d . . . 
C8 C 0.0887(5) 0.1763(2) 0.4010(3) 0.0382(11) Uani 1 1 d . . . 
C9 C 0.1380(5) 0.12086(19) 0.4031(3) 0.0394(11) Uani 1 1 d . . . 
H9 H 0.0721 0.0912 0.3971 0.047 Uiso 1 1 calc R . . 
C10 C 0.2788(6) 0.10705(19) 0.4135(3) 0.0394(11) Uani 1 1 d . . . 
C11 C 0.3732(5) 0.15120(18) 0.4191(3) 0.0365(11) Uani 1 1 d . . . 
H11 H 0.4689 0.1429 0.4243 0.044 Uiso 1 1 calc R . . 
C12 C 0.3311(5) 0.20742(18) 0.4172(3) 0.0347(10) Uani 1 1 d . . . 
C13 C 0.5663(5) 0.33986(17) 0.4647(3) 0.0343(10) Uani 1 1 d . . . 
H13A H 0.6597 0.3234 0.4690 0.041 Uiso 1 1 calc R . . 
H13B H 0.5792 0.3698 0.5110 0.041 Uiso 1 1 calc R . . 
C14 C 0.4356(5) 0.25349(19) 0.4123(3) 0.0379(11) Uani 1 1 d . . . 
H14A H 0.5227 0.2352 0.4067 0.045 Uiso 1 1 calc R . . 
H14B H 0.3968 0.2748 0.3557 0.045 Uiso 1 1 calc R . . 
C15 C 0.5540(6) 0.2699(2) 0.5772(3) 0.0502(13) Uani 1 1 d . . . 
H15A H 0.6022 0.3003 0.6177 0.060 Uiso 1 1 calc R . . 
H15B H 0.6268 0.2444 0.5665 0.060 Uiso 1 1 calc R . . 
C16 C 0.4631(6) 0.2379(2) 0.6243(3) 0.0515(14) Uani 1 1 d . . . 
H16A H 0.4240 0.2045 0.5882 0.062 Uiso 1 1 calc R . . 
H16B H 0.5200 0.2252 0.6843 0.062 Uiso 1 1 calc R . . 
C17 C 0.2485(7) 0.2409(3) 0.6652(4) 0.076(2) Uani 1 1 d . . . 
H17A H 0.1894 0.2203 0.6138 0.114 Uiso 1 1 calc R . . 
H17B H 0.1899 0.2658 0.6907 0.114 Uiso 1 1 calc R . . 
H17C H 0.2974 0.2143 0.7118 0.114 Uiso 1 1 calc R . . 
C18 C 0.1883(5) 0.4448(2) 0.2226(3) 0.0377(11) Uani 1 1 d . . . 
C19 C 0.1600(6) 0.4686(3) 0.1247(3) 0.0578(15) Uani 1 1 d . . . 
H19A H 0.2271 0.4986 0.1236 0.087 Uiso 1 1 calc R . . 
H19B H 0.0644 0.4835 0.1054 0.087 Uiso 1 1 calc R . . 
H19C H 0.1708 0.4386 0.0834 0.087 Uiso 1 1 calc R . . 
C20 C 0.1702(6) 0.4942(2) 0.2850(3) 0.0460(12) Uani 1 1 d . . . 
H20A H 0.1824 0.4803 0.3468 0.069 Uiso 1 1 calc R . . 
H20B H 0.0762 0.5102 0.2625 0.069 Uiso 1 1 calc R . . 
H20C H 0.2406 0.5230 0.2849 0.069 Uiso 1 1 calc R . . 
C21 C 0.0774(5) 0.3989(2) 0.2225(4) 0.0521(13) Uani 1 1 d . . . 
H21A H 0.0756 0.3720 0.1738 0.078 Uiso 1 1 calc R . . 
H21B H -0.0152 0.4163 0.2127 0.078 Uiso 1 1 calc R . . 
H21C H 0.1016 0.3794 0.2809 0.078 Uiso 1 1 calc R . . 
C22 C 0.6565(6) 0.3906(2) 0.1629(4) 0.0517(13) Uani 1 1 d . . . 
H22A H 0.7091 0.4258 0.1684 0.077 Uiso 1 1 calc R . . 
H22B H 0.5993 0.3861 0.1004 0.077 Uiso 1 1 calc R . . 
H22C H 0.7222 0.3591 0.1788 0.077 Uiso 1 1 calc R . . 
C23 C -0.0684(5) 0.1895(2) 0.3878(4) 0.0500(14) Uani 1 1 d . . . 
C24 C -0.1605(7) 0.1356(3) 0.3726(6) 0.091(3) Uani 1 1 d . . . 
H24A H -0.1310 0.1111 0.4257 0.136 Uiso 1 1 calc R . . 
H24B H -0.1493 0.1157 0.3189 0.136 Uiso 1 1 calc R . . 
H24C H -0.2591 0.1459 0.3635 0.136 Uiso 1 1 calc R . . 
C25 C -0.1242(6) 0.2282(3) 0.3046(4) 0.0666(18) Uani 1 1 d . . . 
H25A H -0.2213 0.2388 0.3007 0.100 Uiso 1 1 calc R . . 
H25B H -0.1206 0.2082 0.2494 0.100 Uiso 1 1 calc R . . 
H25C H -0.0659 0.2619 0.3112 0.100 Uiso 1 1 calc R . . 
C26 C -0.0910(6) 0.2175(2) 0.4740(4) 0.0584(15) Uani 1 1 d . . . 
H26A H -0.1908 0.2258 0.4648 0.088 Uiso 1 1 calc R . . 
H26B H -0.0370 0.2524 0.4861 0.088 Uiso 1 1 calc R . . 
H26C H -0.0595 0.1921 0.5256 0.088 Uiso 1 1 calc R . . 
C27 C 0.3255(7) 0.0460(2) 0.4193(4) 0.0519(14) Uani 1 1 d . . . 
H27A H 0.3499 0.0338 0.4827 0.078 Uiso 1 1 calc R . . 
H27B H 0.4076 0.0422 0.3953 0.078 Uiso 1 1 calc R . . 
H27C H 0.2490 0.0227 0.3837 0.078 Uiso 1 1 calc R . . 
C28 C 0.1028(5) 0.4476(2) 0.5862(4) 0.0452(12) Uani 1 1 d . . . 
H28A H 0.0296 0.4678 0.6071 0.054 Uiso 1 1 calc R . . 
H28B H 0.1208 0.4689 0.5350 0.054 Uiso 1 1 calc R . . 
C29 C 0.2373(5) 0.4456(2) 0.6635(3) 0.0441(12) Uani 1 1 d . . . 
H29A H 0.2575 0.4835 0.6901 0.053 Uiso 1 1 calc R . . 
H29B H 0.2234 0.4201 0.7114 0.053 Uiso 1 1 calc R . . 
C30 C -0.0517(6) 0.3958(2) 0.4642(4) 0.0564(15) Uani 1 1 d . . . 
H30A H -0.1354 0.4157 0.4702 0.085 Uiso 1 1 calc R . . 
H30B H -0.0783 0.3582 0.4397 0.085 Uiso 1 1 calc R . . 
H30C H -0.0091 0.4165 0.4231 0.085 Uiso 1 1 calc R . . 
C31 C -0.0169(7) 0.3639(2) 0.6190(4) 0.0606(16) Uani 1 1 d . . . 
H31A H 0.0502 0.3623 0.6789 0.091 Uiso 1 1 calc R . . 
H31B H -0.0461 0.3259 0.5983 0.091 Uiso 1 1 calc R . . 
H31C H -0.0992 0.3857 0.6227 0.091 Uiso 1 1 calc R . . 
C32 C 0.4723(6) 0.4077(2) 0.7118(3) 0.0558(15) Uani 1 1 d . . . 
H32A H 0.5022 0.4397 0.7525 0.084 Uiso 1 1 calc R . . 
H32B H 0.5522 0.3937 0.6917 0.084 Uiso 1 1 calc R . . 
H32C H 0.4370 0.3779 0.7438 0.084 Uiso 1 1 calc R . . 
C33 C 0.4144(6) 0.4724(2) 0.5857(3) 0.0497(13) Uani 1 1 d . . . 
H33A H 0.3433 0.4829 0.5302 0.075 Uiso 1 1 calc R . . 
H33B H 0.4996 0.4600 0.5702 0.075 Uiso 1 1 calc R . . 
H33C H 0.4361 0.5048 0.6263 0.075 Uiso 1 1 calc R . . 
 
 
_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 2.201(3) . ? 
Yb1 O2 2.229(3) . ? 
Yb1 O3 2.483(3) . ? 
Yb1 N1 2.508(4) . ? 
Yb1 N2 2.570(4) . ? 
Yb1 N3 2.692(4) . ? 
O1 C1 1.314(5) . ? 
O2 C7 1.306(5) . ? 
O3 C17 1.420(7) . ? 
O3 C16 1.441(6) . ? 
N1 C15 1.482(5) . ? 
N1 C13 1.484(6) . ? 
N1 C14 1.489(5) . ? 
N2 C30 1.462(6) . ? 
N2 C31 1.467(7) . ? 
N2 C28 1.468(6) . ? 
N3 C32 1.469(6) . ? 
N3 C29 1.479(6) . ? 
N3 C33 1.479(6) . ? 
C1 C6 1.413(6) . ? 
C1 C2 1.435(6) . ? 
C2 C3 1.398(6) . ? 
C2 C18 1.526(6) . ? 
C3 C4 1.386(6) . ? 
C3 H3 0.9400 . ? 
C4 C5 1.383(6) . ? 
C4 C22 1.509(7) . ? 
C5 C6 1.396(6) . ? 
C5 H5 0.9400 . ? 
C6 C13 1.514(6) . ? 
C7 C8 1.418(7) . ? 
C7 C12 1.418(7) . ? 
C8 C9 1.393(6) . ? 
C8 C23 1.530(7) . ? 
C9 C10 1.385(7) . ? 
C9 H9 0.9400 . ? 
C10 C11 1.381(7) . ? 
C10 C27 1.508(6) . ? 
C11 C12 1.388(6) . ? 
C11 H11 0.9400 . ? 
C12 C14 1.509(6) . ? 
C13 H13A 0.9800 . ? 
C13 H13B 0.9800 . ? 
C14 H14A 0.9800 . ? 
C14 H14B 0.9800 . ? 
C15 C16 1.486(7) . ? 
C15 H15A 0.9800 . ? 
C15 H15B 0.9800 . ? 
C16 H16A 0.9800 . ? 
C16 H16B 0.9800 . ? 
C17 H17A 0.9700 . ? 
C17 H17B 0.9700 . ? 
C17 H17C 0.9700 . ? 
C18 C21 1.534(7) . ? 
C18 C20 1.540(6) . ? 
C18 C19 1.542(6) . ? 
C19 H19A 0.9700 . ? 
C19 H19B 0.9700 . ? 
C19 H19C 0.9700 . ? 
C20 H20A 0.9700 . ? 
C20 H20B 0.9700 . ? 
C20 H20C 0.9700 . ? 
C21 H21A 0.9700 . ? 
C21 H21B 0.9700 . ? 
C21 H21C 0.9700 . ? 
C22 H22A 0.9700 . ? 
C22 H22B 0.9700 . ? 
C22 H22C 0.9700 . ? 
C23 C26 1.531(7) . ? 
C23 C25 1.535(8) . ? 
C23 C24 1.543(8) . ? 
C24 H24A 0.9700 . ? 
C24 H24B 0.9700 . ? 
C24 H24C 0.9700 . ? 
C25 H25A 0.9700 . ? 
C25 H25B 0.9700 . ? 
C25 H25C 0.9700 . ? 
C26 H26A 0.9700 . ? 
C26 H26B 0.9700 . ? 
C26 H26C 0.9700 . ? 
C27 H27A 0.9700 . ? 
C27 H27B 0.9700 . ? 
C27 H27C 0.9700 . ? 
C28 C29 1.512(7) . ? 
C28 H28A 0.9800 . ? 
C28 H28B 0.9800 . ? 
C29 H29A 0.9800 . ? 
C29 H29B 0.9800 . ? 
C30 H30A 0.9700 . ? 
C30 H30B 0.9700 . ? 
C30 H30C 0.9700 . ? 
C31 H31A 0.9700 . ? 
C31 H31B 0.9700 . ? 
C31 H31C 0.9700 . ? 
C32 H32A 0.9700 . ? 
C32 H32B 0.9700 . ? 
C32 H32C 0.9700 . ? 
C33 H33A 0.9700 . ? 
C33 H33B 0.9700 . ? 
C33 H33C 0.9700 . ? 
 
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 O2 97.34(12) . . ? 
O1 Yb1 O3 147.48(12) . . ? 
O2 Yb1 O3 91.03(12) . . ? 
O1 Yb1 N1 80.12(11) . . ? 
O2 Yb1 N1 81.97(12) . . ? 
O3 Yb1 N1 69.98(12) . . ? 
O1 Yb1 N2 104.57(12) . . ? 
O2 Yb1 N2 102.56(12) . . ? 
O3 Yb1 N2 104.14(13) . . ? 
N1 Yb1 N2 172.84(12) . . ? 
O1 Yb1 N3 87.19(11) . . ? 
O2 Yb1 N3 172.99(12) . . ? 
O3 Yb1 N3 87.94(12) . . ? 
N1 Yb1 N3 104.16(12) . . ? 
N2 Yb1 N3 71.02(12) . . ? 
C1 O1 Yb1 135.9(3) . . ? 
C7 O2 Yb1 130.1(3) . . ? 
C17 O3 C16 110.1(4) . . ? 
C17 O3 Yb1 117.5(3) . . ? 
C16 O3 Yb1 115.4(3) . . ? 
C15 N1 C13 108.0(3) . . ? 
C15 N1 C14 113.8(4) . . ? 
C13 N1 C14 109.4(3) . . ? 
C15 N1 Yb1 108.3(3) . . ? 
C13 N1 Yb1 107.2(2) . . ? 
C14 N1 Yb1 109.9(3) . . ? 
C30 N2 C31 110.0(4) . . ? 
C30 N2 C28 109.5(4) . . ? 
C31 N2 C28 110.8(4) . . ? 
C30 N2 Yb1 100.6(3) . . ? 
C31 N2 Yb1 120.4(3) . . ? 
C28 N2 Yb1 104.8(3) . . ? 
C32 N3 C29 108.7(4) . . ? 
C32 N3 C33 108.6(4) . . ? 
C29 N3 C33 110.2(4) . . ? 
C32 N3 Yb1 114.4(3) . . ? 
C29 N3 Yb1 105.6(3) . . ? 
C33 N3 Yb1 109.4(3) . . ? 
O1 C1 C6 119.9(4) . . ? 
O1 C1 C2 122.1(4) . . ? 
C6 C1 C2 118.0(4) . . ? 
C3 C2 C1 118.1(4) . . ? 
C3 C2 C18 121.6(4) . . ? 
C1 C2 C18 120.3(4) . . ? 
C4 C3 C2 124.0(4) . . ? 
C4 C3 H3 118.0 . . ? 
C2 C3 H3 118.0 . . ? 
C5 C4 C3 117.1(4) . . ? 
C5 C4 C22 121.8(4) . . ? 
C3 C4 C22 121.1(4) . . ? 
C4 C5 C6 122.2(4) . . ? 
C4 C5 H5 118.9 . . ? 
C6 C5 H5 118.9 . . ? 
C5 C6 C1 120.5(4) . . ? 
C5 C6 C13 118.9(4) . . ? 
C1 C6 C13 120.5(4) . . ? 
O2 C7 C8 121.9(4) . . ? 
O2 C7 C12 119.9(4) . . ? 
C8 C7 C12 118.2(4) . . ? 
C9 C8 C7 118.4(4) . . ? 
C9 C8 C23 121.7(4) . . ? 
C7 C8 C23 119.9(4) . . ? 
C10 C9 C8 123.6(5) . . ? 
C10 C9 H9 118.2 . . ? 
C8 C9 H9 118.2 . . ? 
C11 C10 C9 117.3(4) . . ? 
C11 C10 C27 122.1(5) . . ? 
C9 C10 C27 120.6(5) . . ? 
C10 C11 C12 122.1(5) . . ? 
C10 C11 H11 119.0 . . ? 
C12 C11 H11 119.0 . . ? 
C11 C12 C7 120.2(4) . . ? 
C11 C12 C14 119.3(4) . . ? 
C7 C12 C14 120.3(4) . . ? 
N1 C13 C6 117.0(3) . . ? 
N1 C13 H13A 108.1 . . ? 
C6 C13 H13A 108.1 . . ? 
N1 C13 H13B 108.1 . . ? 
C6 C13 H13B 108.1 . . ? 
H13A C13 H13B 107.3 . . ? 
N1 C14 C12 118.8(4) . . ? 
N1 C14 H14A 107.6 . . ? 
C12 C14 H14A 107.6 . . ? 
N1 C14 H14B 107.6 . . ? 
C12 C14 H14B 107.6 . . ? 
H14A C14 H14B 107.1 . . ? 
N1 C15 C16 114.1(4) . . ? 
N1 C15 H15A 108.7 . . ? 
C16 C15 H15A 108.7 . . ? 
N1 C15 H15B 108.7 . . ? 
C16 C15 H15B 108.7 . . ? 
H15A C15 H15B 107.6 . . ? 
O3 C16 C15 109.8(4) . . ? 
O3 C16 H16A 109.7 . . ? 
C15 C16 H16A 109.7 . . ? 
O3 C16 H16B 109.7 . . ? 
C15 C16 H16B 109.7 . . ? 
H16A C16 H16B 108.2 . . ? 
O3 C17 H17A 109.5 . . ? 
O3 C17 H17B 109.5 . . ? 
H17A C17 H17B 109.5 . . ? 
O3 C17 H17C 109.5 . . ? 
H17A C17 H17C 109.5 . . ? 
H17B C17 H17C 109.5 . . ? 
C2 C18 C21 108.9(4) . . ? 
C2 C18 C20 110.5(4) . . ? 
C21 C18 C20 109.8(4) . . ? 
C2 C18 C19 112.4(4) . . ? 
C21 C18 C19 108.1(4) . . ? 
C20 C18 C19 107.2(4) . . ? 
C18 C19 H19A 109.5 . . ? 
C18 C19 H19B 109.5 . . ? 
H19A C19 H19B 109.5 . . ? 
C18 C19 H19C 109.5 . . ? 
H19A C19 H19C 109.5 . . ? 
H19B C19 H19C 109.5 . . ? 
C18 C20 H20A 109.5 . . ? 
C18 C20 H20B 109.5 . . ? 
H20A C20 H20B 109.5 . . ? 
C18 C20 H20C 109.5 . . ? 
H20A C20 H20C 109.5 . . ? 
H20B C20 H20C 109.5 . . ? 
C18 C21 H21A 109.5 . . ? 
C18 C21 H21B 109.5 . . ? 
H21A C21 H21B 109.5 . . ? 
C18 C21 H21C 109.5 . . ? 
H21A C21 H21C 109.5 . . ? 
H21B C21 H21C 109.5 . . ? 
C4 C22 H22A 109.5 . . ? 
C4 C22 H22B 109.5 . . ? 
H22A C22 H22B 109.5 . . ? 
C4 C22 H22C 109.5 . . ? 
H22A C22 H22C 109.5 . . ? 
H22B C22 H22C 109.5 . . ? 
C8 C23 C26 110.2(4) . . ? 
C8 C23 C25 110.8(5) . . ? 
C26 C23 C25 110.1(5) . . ? 
C8 C23 C24 112.2(5) . . ? 
C26 C23 C24 105.9(5) . . ? 
C25 C23 C24 107.6(5) . . ? 
C23 C24 H24A 109.5 . . ? 
C23 C24 H24B 109.5 . . ? 
H24A C24 H24B 109.5 . . ? 
C23 C24 H24C 109.5 . . ? 
H24A C24 H24C 109.5 . . ? 
H24B C24 H24C 109.5 . . ? 
C23 C25 H25A 109.5 . . ? 
C23 C25 H25B 109.5 . . ? 
H25A C25 H25B 109.5 . . ? 
C23 C25 H25C 109.5 . . ? 
H25A C25 H25C 109.5 . . ? 
H25B C25 H25C 109.5 . . ? 
C23 C26 H26A 109.5 . . ? 
C23 C26 H26B 109.5 . . ? 
H26A C26 H26B 109.5 . . ? 
C23 C26 H26C 109.5 . . ? 
H26A C26 H26C 109.5 . . ? 
H26B C26 H26C 109.5 . . ? 
C10 C27 H27A 109.5 . . ? 
C10 C27 H27B 109.5 . . ? 
H27A C27 H27B 109.5 . . ? 
C10 C27 H27C 109.5 . . ? 
H27A C27 H27C 109.5 . . ? 
H27B C27 H27C 109.5 . . ? 
N2 C28 C29 112.7(4) . . ? 
N2 C28 H28A 109.0 . . ? 
C29 C28 H28A 109.0 . . ? 
N2 C28 H28B 109.0 . . ? 
C29 C28 H28B 109.0 . . ? 
H28A C28 H28B 107.8 . . ? 
N3 C29 C28 111.9(4) . . ? 
N3 C29 H29A 109.2 . . ? 
C28 C29 H29A 109.2 . . ? 
N3 C29 H29B 109.2 . . ? 
C28 C29 H29B 109.2 . . ? 
H29A C29 H29B 107.9 . . ? 
N2 C30 H30A 109.5 . . ? 
N2 C30 H30B 109.5 . . ? 
H30A C30 H30B 109.5 . . ? 
N2 C30 H30C 109.5 . . ? 
H30A C30 H30C 109.5 . . ? 
H30B C30 H30C 109.5 . . ? 
N2 C31 H31A 109.5 . . ? 
N2 C31 H31B 109.5 . . ? 
H31A C31 H31B 109.5 . . ? 
N2 C31 H31C 109.5 . . ? 
H31A C31 H31C 109.5 . . ? 
H31B C31 H31C 109.5 . . ? 
N3 C32 H32A 109.5 . . ? 
N3 C32 H32B 109.5 . . ? 
H32A C32 H32B 109.5 . . ? 
N3 C32 H32C 109.5 . . ? 
H32A C32 H32C 109.5 . . ? 
H32B C32 H32C 109.5 . . ? 
N3 C33 H33A 109.5 . . ? 
N3 C33 H33B 109.5 . . ? 
H33A C33 H33B 109.5 . . ? 
N3 C33 H33C 109.5 . . ? 
H33A C33 H33C 109.5 . . ? 
H33B C33 H33C 109.5 . . ? 
 
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
O2 Yb1 O1 C1 -63.1(4) . . . . ? 
O3 Yb1 O1 C1 40.5(5) . . . . ? 
N1 Yb1 O1 C1 17.4(4) . . . . ? 
N2 Yb1 O1 C1 -168.2(4) . . . . ? 
N3 Yb1 O1 C1 122.3(4) . . . . ? 
O1 Yb1 O2 C7 116.0(4) . . . . ? 
O3 Yb1 O2 C7 -32.5(4) . . . . ? 
N1 Yb1 O2 C7 37.2(4) . . . . ? 
N2 Yb1 O2 C7 -137.2(4) . . . . ? 
N3 Yb1 O2 C7 -114.0(9) . . . . ? 
O1 Yb1 O3 C17 -164.9(4) . . . . ? 
O2 Yb1 O3 C17 -59.5(4) . . . . ? 
N1 Yb1 O3 C17 -140.5(4) . . . . ? 
N2 Yb1 O3 C17 43.8(4) . . . . ? 
N3 Yb1 O3 C17 113.6(4) . . . . ? 
O1 Yb1 O3 C16 -32.3(4) . . . . ? 
O2 Yb1 O3 C16 73.1(3) . . . . ? 
N1 Yb1 O3 C16 -7.9(3) . . . . ? 
N2 Yb1 O3 C16 176.4(3) . . . . ? 
N3 Yb1 O3 C16 -113.8(3) . . . . ? 
O1 Yb1 N1 C15 147.9(3) . . . . ? 
O2 Yb1 N1 C15 -113.2(3) . . . . ? 
O3 Yb1 N1 C15 -19.1(3) . . . . ? 
N2 Yb1 N1 C15 16.5(11) . . . . ? 
N3 Yb1 N1 C15 63.4(3) . . . . ? 
O1 Yb1 N1 C13 31.6(2) . . . . ? 
O2 Yb1 N1 C13 130.6(3) . . . . ? 
O3 Yb1 N1 C13 -135.4(3) . . . . ? 
N2 Yb1 N1 C13 -99.8(9) . . . . ? 
N3 Yb1 N1 C13 -52.9(3) . . . . ? 
O1 Yb1 N1 C14 -87.2(3) . . . . ? 
O2 Yb1 N1 C14 11.8(3) . . . . ? 
O3 Yb1 N1 C14 105.9(3) . . . . ? 
N2 Yb1 N1 C14 141.4(9) . . . . ? 
N3 Yb1 N1 C14 -171.7(3) . . . . ? 
O1 Yb1 N2 C30 55.1(3) . . . . ? 
O2 Yb1 N2 C30 -46.1(3) . . . . ? 
O3 Yb1 N2 C30 -140.4(3) . . . . ? 
N1 Yb1 N2 C30 -174.7(8) . . . . ? 
N3 Yb1 N2 C30 136.9(3) . . . . ? 
O1 Yb1 N2 C31 176.0(4) . . . . ? 
O2 Yb1 N2 C31 74.9(4) . . . . ? 
O3 Yb1 N2 C31 -19.4(4) . . . . ? 
N1 Yb1 N2 C31 -53.7(11) . . . . ? 
N3 Yb1 N2 C31 -102.2(4) . . . . ? 
O1 Yb1 N2 C28 -58.5(3) . . . . ? 
O2 Yb1 N2 C28 -159.6(3) . . . . ? 
O3 Yb1 N2 C28 106.0(3) . . . . ? 
N1 Yb1 N2 C28 71.8(10) . . . . ? 
N3 Yb1 N2 C28 23.3(3) . . . . ? 
O1 Yb1 N3 C32 -126.1(3) . . . . ? 
O2 Yb1 N3 C32 103.5(9) . . . . ? 
O3 Yb1 N3 C32 21.8(3) . . . . ? 
N1 Yb1 N3 C32 -47.0(4) . . . . ? 
N2 Yb1 N3 C32 127.5(4) . . . . ? 
O1 Yb1 N3 C29 114.4(3) . . . . ? 
O2 Yb1 N3 C29 -16.0(11) . . . . ? 
O3 Yb1 N3 C29 -97.7(3) . . . . ? 
N1 Yb1 N3 C29 -166.5(3) . . . . ? 
N2 Yb1 N3 C29 8.0(3) . . . . ? 
O1 Yb1 N3 C33 -4.1(3) . . . . ? 
O2 Yb1 N3 C33 -134.6(9) . . . . ? 
O3 Yb1 N3 C33 143.8(3) . . . . ? 
N1 Yb1 N3 C33 75.0(3) . . . . ? 
N2 Yb1 N3 C33 -110.5(3) . . . . ? 
Yb1 O1 C1 C6 -37.3(6) . . . . ? 
Yb1 O1 C1 C2 142.8(3) . . . . ? 
O1 C1 C2 C3 175.5(4) . . . . ? 
C6 C1 C2 C3 -4.4(6) . . . . ? 
O1 C1 C2 C18 -5.7(6) . . . . ? 
C6 C1 C2 C18 174.4(4) . . . . ? 
C1 C2 C3 C4 1.6(6) . . . . ? 
C18 C2 C3 C4 -177.2(4) . . . . ? 
C2 C3 C4 C5 2.3(6) . . . . ? 
C2 C3 C4 C22 179.6(4) . . . . ? 
C3 C4 C5 C6 -3.4(6) . . . . ? 
C22 C4 C5 C6 179.2(4) . . . . ? 
C4 C5 C6 C1 0.6(6) . . . . ? 
C4 C5 C6 C13 -177.4(4) . . . . ? 
O1 C1 C6 C5 -176.5(4) . . . . ? 
C2 C1 C6 C5 3.3(6) . . . . ? 
O1 C1 C6 C13 1.5(6) . . . . ? 
C2 C1 C6 C13 -178.7(4) . . . . ? 
Yb1 O2 C7 C8 136.3(4) . . . . ? 
Yb1 O2 C7 C12 -43.6(6) . . . . ? 
O2 C7 C8 C9 -175.3(4) . . . . ? 
C12 C7 C8 C9 4.6(6) . . . . ? 
O2 C7 C8 C23 4.6(7) . . . . ? 
C12 C7 C8 C23 -175.6(4) . . . . ? 
C7 C8 C9 C10 -1.1(7) . . . . ? 
C23 C8 C9 C10 179.0(4) . . . . ? 
C8 C9 C10 C11 -2.1(7) . . . . ? 
C8 C9 C10 C27 177.2(4) . . . . ? 
C9 C10 C11 C12 1.8(7) . . . . ? 
C27 C10 C11 C12 -177.5(4) . . . . ? 
C10 C11 C12 C7 1.6(7) . . . . ? 
C10 C11 C12 C14 -172.8(4) . . . . ? 
O2 C7 C12 C11 175.0(4) . . . . ? 
C8 C7 C12 C11 -4.9(6) . . . . ? 
O2 C7 C12 C14 -10.6(6) . . . . ? 
C8 C7 C12 C14 169.5(4) . . . . ? 
C15 N1 C13 C6 173.6(4) . . . . ? 
C14 N1 C13 C6 49.2(5) . . . . ? 
Yb1 N1 C13 C6 -69.9(4) . . . . ? 
C5 C6 C13 N1 -123.3(4) . . . . ? 
C1 C6 C13 N1 58.7(5) . . . . ? 
C15 N1 C14 C12 65.4(5) . . . . ? 
C13 N1 C14 C12 -173.8(4) . . . . ? 
Yb1 N1 C14 C12 -56.4(4) . . . . ? 
C11 C12 C14 N1 -118.5(5) . . . . ? 
C7 C12 C14 N1 67.1(5) . . . . ? 
C13 N1 C15 C16 161.9(4) . . . . ? 
C14 N1 C15 C16 -76.4(6) . . . . ? 
Yb1 N1 C15 C16 46.1(5) . . . . ? 
C17 O3 C16 C15 169.8(4) . . . . ? 
Yb1 O3 C16 C15 33.8(5) . . . . ? 
N1 C15 C16 O3 -54.7(6) . . . . ? 
C3 C2 C18 C21 118.1(5) . . . . ? 
C1 C2 C18 C21 -60.7(5) . . . . ? 
C3 C2 C18 C20 -121.3(4) . . . . ? 
C1 C2 C18 C20 60.0(5) . . . . ? 
C3 C2 C18 C19 -1.7(6) . . . . ? 
C1 C2 C18 C19 179.6(4) . . . . ? 
C9 C8 C23 C26 114.7(5) . . . . ? 
C7 C8 C23 C26 -65.2(6) . . . . ? 
C9 C8 C23 C25 -123.3(5) . . . . ? 
C7 C8 C23 C25 56.9(6) . . . . ? 
C9 C8 C23 C24 -3.0(7) . . . . ? 
C7 C8 C23 C24 177.1(5) . . . . ? 
C30 N2 C28 C29 -163.1(4) . . . . ? 
C31 N2 C28 C29 75.4(5) . . . . ? 
Yb1 N2 C28 C29 -55.9(4) . . . . ? 
C32 N3 C29 C28 -162.2(4) . . . . ? 
C33 N3 C29 C28 78.9(5) . . . . ? 
Yb1 N3 C29 C28 -39.0(4) . . . . ? 
N2 C28 C29 N3 69.8(5) . . . . ? 
 
_diffrn_measured_fraction_theta_max    0.992 
_diffrn_reflns_theta_full              25.50 
_diffrn_measured_fraction_theta_full   0.992 
_refine_diff_density_max    0.785 
_refine_diff_density_min   -2.128 
_refine_diff_density_rms    0.196 
#==========================================================end
 
data_compound2
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety 
 'C18 H52 N4 Si4 Yb'         
_chemical_formula_sum 
 'C18 H52 N4 Si4 Yb' 
_chemical_formula_weight          610.04 
 
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' 
 'Si'  'Si'   0.0817   0.0704 
 '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' 
 
_symmetry_cell_setting                 monoclinic
_symmetry_space_group_name_H-M        'C 2/c'
_symmetry_space_group_name_Hall       '-C 2yc'
_symmetry_Int_Tables_number            15
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 
 
_cell_length_a                    8.649(3) 
_cell_length_b                    17.753(5) 
_cell_length_c                    20.315(7) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  102.324(8) 
_cell_angle_gamma                 90.00 
_cell_volume                      3047.6(16) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     223(2) 
_cell_measurement_reflns_used     7147 
_cell_measurement_theta_min       3.0 
_cell_measurement_theta_max       27.6 
 
_exptl_crystal_description        'prism'
_exptl_crystal_colour             'purple'
_exptl_crystal_size_max           0.40 
_exptl_crystal_size_mid           0.15 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.330 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1256 
_exptl_absorpt_coefficient_mu     3.236 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.143
_exptl_absorpt_correction_T_max   0.724
_exptl_absorpt_process_details   
 'Jacobson, R. (1998) Private communication'
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       223(2) 
_diffrn_radiation_wavelength      0.71075 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Rigaku Saturn'
_diffrn_measurement_method        ω
_diffrn_detector_area_resol_mean  14.63
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             7606 
_diffrn_reflns_av_R_equivalents   0.1302 
_diffrn_reflns_av_sigmaI/netI     0.1660 
_diffrn_reflns_limit_h_min        -8 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -21 
_diffrn_reflns_limit_k_max        21 
_diffrn_reflns_limit_l_min        -24 
_diffrn_reflns_limit_l_max        22 
_diffrn_reflns_theta_min          3.04 
_diffrn_reflns_theta_max          25.50 
_reflns_number_total              2825 
_reflns_number_gt                 1828 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'CrystalClear'
_computing_cell_refinement        'CrystalClear'
_computing_data_reduction         'CrystalStructure'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.1039P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          2825 
_refine_ls_number_parameters      132 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1067 
_refine_ls_R_factor_gt            0.0880 
_refine_ls_wR_factor_ref          0.2110 
_refine_ls_wR_factor_gt           0.2037 
_refine_ls_goodness_of_fit_ref    0.940 
_refine_ls_restrained_S_all       0.940 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Yb1 Yb 0.5000 0.69524(4) 0.2500 0.0369(3) Uani 1 2 d S . . 
Si1 Si 0.3045(4) 0.5775(2) 0.13167(18) 0.0405(9) Uani 1 1 d . . . 
Si2 Si 0.6058(4) 0.6378(2) 0.09884(19) 0.0399(9) Uani 1 1 d . . . 
N1 N 0.4699(13) 0.6288(6) 0.1484(5) 0.040(3) Uani 1 1 d . . . 
N2 N 0.6570(13) 0.8150(6) 0.2994(6) 0.047(3) Uani 1 1 d . . . 
C1 C 0.1977(17) 0.5930(9) 0.2028(8) 0.057(4) Uani 1 1 d . . . 
H1A H 0.2591 0.5713 0.2440 0.085 Uiso 1 1 calc R . . 
H1B H 0.0946 0.5691 0.1917 0.085 Uiso 1 1 calc R . . 
H1C H 0.1847 0.6466 0.2091 0.085 Uiso 1 1 calc R . . 
C2 C 0.336(2) 0.4718(8) 0.1294(10) 0.072(5) Uani 1 1 d . . . 
H2A H 0.4127 0.4607 0.1023 0.109 Uiso 1 1 calc R . . 
H2B H 0.2363 0.4473 0.1099 0.109 Uiso 1 1 calc R . . 
H2C H 0.3746 0.4533 0.1749 0.109 Uiso 1 1 calc R . . 
C3 C 0.1613(18) 0.6002(10) 0.0519(7) 0.063(4) Uani 1 1 d . . . 
H3A H 0.1412 0.6540 0.0496 0.094 Uiso 1 1 calc R . . 
H3B H 0.0629 0.5734 0.0506 0.094 Uiso 1 1 calc R . . 
H3C H 0.2051 0.5849 0.0138 0.094 Uiso 1 1 calc R . . 
C4 C 0.523(2) 0.6714(10) 0.0105(8) 0.069(5) Uani 1 1 d . . . 
H4A H 0.4408 0.6372 -0.0115 0.104 Uiso 1 1 calc R . . 
H4B H 0.6071 0.6727 -0.0145 0.104 Uiso 1 1 calc R . . 
H4C H 0.4795 0.7215 0.0119 0.104 Uiso 1 1 calc R . . 
C5 C 0.712(2) 0.5466(8) 0.0894(9) 0.068(5) Uani 1 1 d . . . 
H5A H 0.7348 0.5202 0.1322 0.101 Uiso 1 1 calc R . . 
H5B H 0.8098 0.5574 0.0753 0.101 Uiso 1 1 calc R . . 
H5C H 0.6450 0.5153 0.0557 0.101 Uiso 1 1 calc R . . 
C6 C 0.7662(18) 0.7066(9) 0.1347(9) 0.064(4) Uani 1 1 d . . . 
H6A H 0.7192 0.7547 0.1420 0.096 Uiso 1 1 calc R . . 
H6B H 0.8355 0.7132 0.1033 0.096 Uiso 1 1 calc R . . 
H6C H 0.8268 0.6877 0.1772 0.096 Uiso 1 1 calc R . . 
C7 C 0.588(2) 0.8819(9) 0.2578(9) 0.080(6) Uani 1 1 d . . . 
H7A H 0.6259 0.9282 0.2821 0.096 Uiso 1 1 calc R . . 
H7B H 0.6249 0.8818 0.2154 0.096 Uiso 1 1 calc R . . 
C8 C 0.8314(18) 0.8139(11) 0.3043(10) 0.083(6) Uani 1 1 d . . . 
H8A H 0.8766 0.8615 0.3224 0.125 Uiso 1 1 calc R . . 
H8B H 0.8529 0.8063 0.2598 0.125 Uiso 1 1 calc R . . 
H8C H 0.8781 0.7732 0.3337 0.125 Uiso 1 1 calc R . . 
C9 C 0.6304(19) 0.8224(8) 0.3681(7) 0.054(4) Uani 1 1 d . . . 
H9A H 0.6833 0.7816 0.3957 0.080 Uiso 1 1 calc R . . 
H9B H 0.5178 0.8204 0.3669 0.080 Uiso 1 1 calc R . . 
H9C H 0.6725 0.8702 0.3870 0.080 Uiso 1 1 calc R . . 
 
 
_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 N1 2.344(10) . ? 
Yb1 N1 2.344(10) 2_655 ? 
Yb1 N2 2.607(11) . ? 
Yb1 N2 2.607(11) 2_655 ? 
Yb1 C1 3.159(16) 2_655 ? 
Yb1 Si1 3.358(4) . ? 
Yb1 Si1 3.358(4) 2_655 ? 
Yb1 Si2 3.537(4) . ? 
Yb1 Si2 3.537(4) 2_655 ? 
Si1 N1 1.669(12) . ? 
Si1 C3 1.863(14) . ? 
Si1 C1 1.894(15) . ? 
Si1 C2 1.897(14) . ? 
Si2 N1 1.710(12) . ? 
Si2 C6 1.875(15) . ? 
Si2 C4 1.881(15) . ? 
Si2 C5 1.890(14) . ? 
N2 C9 1.467(19) . ? 
N2 C8 1.491(19) . ? 
N2 C7 1.506(19) . ? 
C1 H1A 0.9700 . ? 
C1 H1B 0.9700 . ? 
C1 H1C 0.9700 . ? 
C2 H2A 0.9700 . ? 
C2 H2B 0.9700 . ? 
C2 H2C 0.9700 . ? 
C3 H3A 0.9700 . ? 
C3 H3B 0.9700 . ? 
C3 H3C 0.9700 . ? 
C4 H4A 0.9700 . ? 
C4 H4B 0.9700 . ? 
C4 H4C 0.9700 . ? 
C5 H5A 0.9700 . ? 
C5 H5B 0.9700 . ? 
C5 H5C 0.9700 . ? 
C6 H6A 0.9700 . ? 
C6 H6B 0.9700 . ? 
C6 H6C 0.9700 . ? 
C7 C7 1.48(4) 2_655 ? 
C7 H7A 0.9800 . ? 
C7 H7B 0.9800 . ? 
C8 H8A 0.9700 . ? 
C8 H8B 0.9700 . ? 
C8 H8C 0.9700 . ? 
C9 H9A 0.9700 . ? 
C9 H9B 0.9700 . ? 
C9 H9C 0.9700 . ? 
 
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 
N1 Yb1 N1 119.6(5) . 2_655 ? 
N1 Yb1 N2 134.5(4) . . ? 
N1 Yb1 N2 96.9(3) 2_655 . ? 
N1 Yb1 N2 96.9(3) . 2_655 ? 
N1 Yb1 N2 134.5(4) 2_655 2_655 ? 
N2 Yb1 N2 70.6(5) . 2_655 ? 
N1 Yb1 C1 84.7(4) . 2_655 ? 
N1 Yb1 C1 60.9(4) 2_655 2_655 ? 
N2 Yb1 C1 91.3(4) . 2_655 ? 
N2 Yb1 C1 156.2(4) 2_655 2_655 ? 
N1 Yb1 Si1 27.3(3) . . ? 
N1 Yb1 Si1 105.2(2) 2_655 . ? 
N2 Yb1 Si1 157.7(3) . . ? 
N2 Yb1 Si1 95.2(3) 2_655 . ? 
C1 Yb1 Si1 96.7(3) 2_655 . ? 
N1 Yb1 Si1 105.2(2) . 2_655 ? 
N1 Yb1 Si1 27.3(3) 2_655 2_655 ? 
N2 Yb1 Si1 95.2(3) . 2_655 ? 
N2 Yb1 Si1 157.7(3) 2_655 2_655 ? 
C1 Yb1 Si1 33.6(3) 2_655 2_655 ? 
Si1 Yb1 Si1 102.97(13) . 2_655 ? 
N1 Yb1 Si2 24.6(3) . . ? 
N1 Yb1 Si2 128.3(3) 2_655 . ? 
N2 Yb1 Si2 111.1(3) . . ? 
N2 Yb1 Si2 96.4(3) 2_655 . ? 
C1 Yb1 Si2 75.4(3) 2_655 . ? 
Si1 Yb1 Si2 51.90(9) . . ? 
Si1 Yb1 Si2 104.94(9) 2_655 . ? 
N1 Yb1 Si2 128.3(3) . 2_655 ? 
N1 Yb1 Si2 24.6(3) 2_655 2_655 ? 
N2 Yb1 Si2 96.4(3) . 2_655 ? 
N2 Yb1 Si2 111.1(3) 2_655 2_655 ? 
C1 Yb1 Si2 85.5(3) 2_655 2_655 ? 
Si1 Yb1 Si2 104.94(9) . 2_655 ? 
Si1 Yb1 Si2 51.90(9) 2_655 2_655 ? 
Si2 Yb1 Si2 146.47(12) . 2_655 ? 
N1 Si1 C3 116.1(7) . . ? 
N1 Si1 C1 107.6(6) . . ? 
C3 Si1 C1 106.9(7) . . ? 
N1 Si1 C2 115.1(6) . . ? 
C3 Si1 C2 105.4(8) . . ? 
C1 Si1 C2 104.9(7) . . ? 
N1 Si1 Yb1 40.1(4) . . ? 
C3 Si1 Yb1 128.9(6) . . ? 
C1 Si1 Yb1 67.4(5) . . ? 
C2 Si1 Yb1 125.5(6) . . ? 
N1 Si2 C6 112.1(7) . . ? 
N1 Si2 C4 115.0(7) . . ? 
C6 Si2 C4 105.2(8) . . ? 
N1 Si2 C5 112.9(6) . . ? 
C6 Si2 C5 105.3(8) . . ? 
C4 Si2 C5 105.5(8) . . ? 
N1 Si2 Yb1 34.7(3) . . ? 
C6 Si2 Yb1 77.4(6) . . ? 
C4 Si2 Yb1 128.4(6) . . ? 
C5 Si2 Yb1 123.8(5) . . ? 
Si1 N1 Si2 126.8(6) . . ? 
Si1 N1 Yb1 112.5(6) . . ? 
Si2 N1 Yb1 120.7(5) . . ? 
C9 N2 C8 107.5(12) . . ? 
C9 N2 C7 109.9(12) . . ? 
C8 N2 C7 108.9(14) . . ? 
C9 N2 Yb1 105.3(8) . . ? 
C8 N2 Yb1 116.8(9) . . ? 
C7 N2 Yb1 108.3(8) . . ? 
Si1 C1 H1A 109.5 . . ? 
Si1 C1 H1B 109.5 . . ? 
H1A C1 H1B 109.5 . . ? 
Si1 C1 H1C 109.5 . . ? 
H1A C1 H1C 109.5 . . ? 
H1B C1 H1C 109.5 . . ? 
Si1 C2 H2A 109.5 . . ? 
Si1 C2 H2B 109.5 . . ? 
H2A C2 H2B 109.5 . . ? 
Si1 C2 H2C 109.5 . . ? 
H2A C2 H2C 109.5 . . ? 
H2B C2 H2C 109.5 . . ? 
Si1 C3 H3A 109.5 . . ? 
Si1 C3 H3B 109.5 . . ? 
H3A C3 H3B 109.5 . . ? 
Si1 C3 H3C 109.5 . . ? 
H3A C3 H3C 109.5 . . ? 
H3B C3 H3C 109.5 . . ? 
Si2 C4 H4A 109.5 . . ? 
Si2 C4 H4B 109.5 . . ? 
H4A C4 H4B 109.5 . . ? 
Si2 C4 H4C 109.5 . . ? 
H4A C4 H4C 109.5 . . ? 
H4B C4 H4C 109.5 . . ? 
Si2 C5 H5A 109.5 . . ? 
Si2 C5 H5B 109.5 . . ? 
H5A C5 H5B 109.5 . . ? 
Si2 C5 H5C 109.5 . . ? 
H5A C5 H5C 109.5 . . ? 
H5B C5 H5C 109.5 . . ? 
Si2 C6 H6A 109.5 . . ? 
Si2 C6 H6B 109.5 . . ? 
H6A C6 H6B 109.5 . . ? 
Si2 C6 H6C 109.5 . . ? 
H6A C6 H6C 109.5 . . ? 
H6B C6 H6C 109.5 . . ? 
C7 C7 N2 112.7(13) 2_655 . ? 
C7 C7 H7A 109.1 2_655 . ? 
N2 C7 H7A 109.1 . . ? 
C7 C7 H7B 109.1 2_655 . ? 
N2 C7 H7B 109.1 . . ? 
H7A C7 H7B 107.8 . . ? 
N2 C8 H8A 109.5 . . ? 
N2 C8 H8B 109.5 . . ? 
H8A C8 H8B 109.5 . . ? 
N2 C8 H8C 109.5 . . ? 
H8A C8 H8C 109.5 . . ? 
H8B C8 H8C 109.5 . . ? 
N2 C9 H9A 109.5 . . ? 
N2 C9 H9B 109.5 . . ? 
H9A C9 H9B 109.5 . . ? 
N2 C9 H9C 109.5 . . ? 
H9A C9 H9C 109.5 . . ? 
H9B C9 H9C 109.5 . . ? 
 
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
N1 Yb1 Si1 N1 -126.1(6) 2_655 . . . ? 
N2 Yb1 Si1 N1 45.9(9) . . . . ? 
N2 Yb1 Si1 N1 95.0(6) 2_655 . . . ? 
C1 Yb1 Si1 N1 -64.5(6) 2_655 . . . ? 
Si1 Yb1 Si1 N1 -98.0(5) 2_655 . . . ? 
Si2 Yb1 Si1 N1 0.9(5) . . . . ? 
Si2 Yb1 Si1 N1 -151.6(5) 2_655 . . . ? 
N1 Yb1 Si1 C3 -85.5(9) . . . . ? 
N1 Yb1 Si1 C3 148.4(8) 2_655 . . . ? 
N2 Yb1 Si1 C3 -39.6(10) . . . . ? 
N2 Yb1 Si1 C3 9.5(7) 2_655 . . . ? 
C1 Yb1 Si1 C3 -149.9(7) 2_655 . . . ? 
Si1 Yb1 Si1 C3 176.5(7) 2_655 . . . ? 
Si2 Yb1 Si1 C3 -84.5(7) . . . . ? 
Si2 Yb1 Si1 C3 123.0(7) 2_655 . . . ? 
N1 Yb1 Si1 C1 -179.4(8) . . . . ? 
N1 Yb1 Si1 C1 54.5(6) 2_655 . . . ? 
N2 Yb1 Si1 C1 -133.5(9) . . . . ? 
N2 Yb1 Si1 C1 -84.5(6) 2_655 . . . ? 
C1 Yb1 Si1 C1 116.1(6) 2_655 . . . ? 
Si1 Yb1 Si1 C1 82.6(5) 2_655 . . . ? 
Si2 Yb1 Si1 C1 -178.5(5) . . . . ? 
Si2 Yb1 Si1 C1 29.0(5) 2_655 . . . ? 
N1 Yb1 Si1 C2 87.9(8) . . . . ? 
N1 Yb1 Si1 C2 -38.2(7) 2_655 . . . ? 
N2 Yb1 Si1 C2 133.8(10) . . . . ? 
N2 Yb1 Si1 C2 -177.2(7) 2_655 . . . ? 
C1 Yb1 Si1 C2 23.4(7) 2_655 . . . ? 
Si1 Yb1 Si1 C2 -10.1(6) 2_655 . . . ? 
Si2 Yb1 Si1 C2 88.8(7) . . . . ? 
Si2 Yb1 Si1 C2 -63.7(7) 2_655 . . . ? 
N1 Yb1 Si2 N1 77.7(9) 2_655 . . . ? 
N2 Yb1 Si2 N1 -164.4(6) . . . . ? 
N2 Yb1 Si2 N1 -92.7(6) 2_655 . . . ? 
C1 Yb1 Si2 N1 110.0(7) 2_655 . . . ? 
Si1 Yb1 Si2 N1 -1.0(6) . . . . ? 
Si1 Yb1 Si2 N1 93.9(6) 2_655 . . . ? 
Si2 Yb1 Si2 N1 52.8(6) 2_655 . . . ? 
N1 Yb1 Si2 C6 178.1(8) . . . . ? 
N1 Yb1 Si2 C6 -104.1(6) 2_655 . . . ? 
N2 Yb1 Si2 C6 13.8(6) . . . . ? 
N2 Yb1 Si2 C6 85.5(6) 2_655 . . . ? 
C1 Yb1 Si2 C6 -71.9(6) 2_655 . . . ? 
Si1 Yb1 Si2 C6 177.1(5) . . . . ? 
Si1 Yb1 Si2 C6 -88.0(5) 2_655 . . . ? 
Si2 Yb1 Si2 C6 -129.1(5) 2_655 . . . ? 
N1 Yb1 Si2 C4 78.6(9) . . . . ? 
N1 Yb1 Si2 C4 156.3(8) 2_655 . . . ? 
N2 Yb1 Si2 C4 -85.8(8) . . . . ? 
N2 Yb1 Si2 C4 -14.1(8) 2_655 . . . ? 
C1 Yb1 Si2 C4 -171.4(8) 2_655 . . . ? 
Si1 Yb1 Si2 C4 77.6(7) . . . . ? 
Si1 Yb1 Si2 C4 172.5(7) 2_655 . . . ? 
Si2 Yb1 Si2 C4 131.4(7) 2_655 . . . ? 
N1 Yb1 Si2 C5 -81.8(9) . . . . ? 
N1 Yb1 Si2 C5 -4.0(8) 2_655 . . . ? 
N2 Yb1 Si2 C5 113.9(7) . . . . ? 
N2 Yb1 Si2 C5 -174.4(7) 2_655 . . . ? 
C1 Yb1 Si2 C5 28.2(7) 2_655 . . . ? 
Si1 Yb1 Si2 C5 -82.8(7) . . . . ? 
Si1 Yb1 Si2 C5 12.1(7) 2_655 . . . ? 
Si2 Yb1 Si2 C5 -29.0(7) 2_655 . . . ? 
C3 Si1 N1 Si2 -57.8(10) . . . . ? 
C1 Si1 N1 Si2 -177.5(7) . . . . ? 
C2 Si1 N1 Si2 65.9(10) . . . . ? 
Yb1 Si1 N1 Si2 -178.1(11) . . . . ? 
C3 Si1 N1 Yb1 120.2(7) . . . . ? 
C1 Si1 N1 Yb1 0.6(7) . . . . ? 
C2 Si1 N1 Yb1 -116.0(8) . . . . ? 
C6 Si2 N1 Si1 176.0(8) . . . . ? 
C4 Si2 N1 Si1 55.9(10) . . . . ? 
C5 Si2 N1 Si1 -65.3(10) . . . . ? 
Yb1 Si2 N1 Si1 177.9(12) . . . . ? 
C6 Si2 N1 Yb1 -2.0(9) . . . . ? 
C4 Si2 N1 Yb1 -122.1(8) . . . . ? 
C5 Si2 N1 Yb1 116.8(7) . . . . ? 
N1 Yb1 N1 Si1 63.7(5) 2_655 . . . ? 
N2 Yb1 N1 Si1 -157.6(5) . . . . ? 
N2 Yb1 N1 Si1 -88.0(6) 2_655 . . . ? 
C1 Yb1 N1 Si1 115.9(6) 2_655 . . . ? 
Si1 Yb1 N1 Si1 89.0(5) 2_655 . . . ? 
Si2 Yb1 N1 Si1 -178.2(10) . . . . ? 
Si2 Yb1 N1 Si1 35.9(6) 2_655 . . . ? 
N1 Yb1 N1 Si2 -118.1(6) 2_655 . . . ? 
N2 Yb1 N1 Si2 20.6(8) . . . . ? 
N2 Yb1 N1 Si2 90.2(6) 2_655 . . . ? 
C1 Yb1 N1 Si2 -65.9(6) 2_655 . . . ? 
Si1 Yb1 N1 Si2 178.2(10) . . . . ? 
Si1 Yb1 N1 Si2 -92.8(6) 2_655 . . . ? 
Si2 Yb1 N1 Si2 -145.9(4) 2_655 . . . ? 
N1 Yb1 N2 C9 -176.5(7) . . . . ? 
N1 Yb1 N2 C9 -31.8(9) 2_655 . . . ? 
N2 Yb1 N2 C9 103.1(10) 2_655 . . . ? 
C1 Yb1 N2 C9 -92.6(8) 2_655 . . . ? 
Si1 Yb1 N2 C9 156.0(7) . . . . ? 
Si1 Yb1 N2 C9 -59.2(8) 2_655 . . . ? 
Si2 Yb1 N2 C9 -167.4(7) . . . . ? 
Si2 Yb1 N2 C9 -7.0(8) 2_655 . . . ? 
N1 Yb1 N2 C8 -57.3(13) . . . . ? 
N1 Yb1 N2 C8 87.4(12) 2_655 . . . ? 
N2 Yb1 N2 C8 -137.7(14) 2_655 . . . ? 
C1 Yb1 N2 C8 26.6(12) 2_655 . . . ? 
Si1 Yb1 N2 C8 -84.8(13) . . . . ? 
Si1 Yb1 N2 C8 60.0(12) 2_655 . . . ? 
Si2 Yb1 N2 C8 -48.2(12) . . . . ? 
Si2 Yb1 N2 C8 112.2(11) 2_655 . . . ? 
N1 Yb1 N2 C7 66.0(12) . . . . ? 
N1 Yb1 N2 C7 -149.3(11) 2_655 . . . ? 
N2 Yb1 N2 C7 -14.4(9) 2_655 . . . ? 
C1 Yb1 N2 C7 149.8(11) 2_655 . . . ? 
Si1 Yb1 N2 C7 38.5(15) . . . . ? 
Si1 Yb1 N2 C7 -176.7(10) 2_655 . . . ? 
Si2 Yb1 N2 C7 75.1(11) . . . . ? 
Si2 Yb1 N2 C7 -124.6(10) 2_655 . . . ? 
C9 N2 C7 C7 -70.4(19) . . . 2_655 ? 
C8 N2 C7 C7 172.1(17) . . . 2_655 ? 
Yb1 N2 C7 C7 44(2) . . . 2_655 ? 
 
_diffrn_measured_fraction_theta_max    0.995 
_diffrn_reflns_theta_full              25.50 
_diffrn_measured_fraction_theta_full   0.995 
_refine_diff_density_max    3.747 
_refine_diff_density_min   -3.628 
_refine_diff_density_rms    0.280 

#==========================================================end
 
data_compound3
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety 
 'C40 H64 N2 O5 Yb'         
_chemical_formula_sum 
 'C40 H64 N2 O5 Yb' 
_chemical_formula_weight          825.97 
 
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' 
 'Yb'  'Yb'  -0.3850   5.5486 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_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                    12.5079(2) 
_cell_length_b                    14.1307(4) 
_cell_length_c                    14.1381(5) 
_cell_angle_alpha                 67.194(15) 
_cell_angle_beta                  64.666(14) 
_cell_angle_gamma                 64.700(15) 
_cell_volume                      1976.8(3) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     223(2) 
_cell_measurement_reflns_used     7805
_cell_measurement_theta_min       3.2
_cell_measurement_theta_max       27.6 
 
_exptl_crystal_description        'prism' 
_exptl_crystal_colour             'yellow'
_exptl_crystal_size_max           0.80 
_exptl_crystal_size_mid           0.15 
_exptl_crystal_size_min           0.15 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.388 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              856 
_exptl_absorpt_coefficient_mu     2.408 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.355
_exptl_absorpt_correction_T_max   0.697
_exptl_absorpt_process_details    
 'Jacobson, R. (1998) Private communication'
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       223(2) 
_diffrn_radiation_wavelength      0.71075 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Rigaku Saturn'
_diffrn_measurement_method        ω
_diffrn_detector_area_resol_mean  14.63
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             16579 
_diffrn_reflns_av_R_equivalents   0.0748 
_diffrn_reflns_av_sigmaI/netI     0.1028 
_diffrn_reflns_limit_h_min        -15 
_diffrn_reflns_limit_h_max        15 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        -15 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          3.22 
_diffrn_reflns_theta_max          25.50 
_reflns_number_total              7288 
_reflns_number_gt                 6233 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'CrystalClear'
_computing_cell_refinement        'CrystalClear'
_computing_data_reduction         'CrystalStructure'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0592P)²+0.0554P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          7288 
_refine_ls_number_parameters      405 
_refine_ls_number_restraints      22 
_refine_ls_R_factor_all           0.0804 
_refine_ls_R_factor_gt            0.0675 
_refine_ls_wR_factor_ref          0.1588 
_refine_ls_wR_factor_gt           0.1489 
_refine_ls_goodness_of_fit_ref    1.149 
_refine_ls_restrained_S_all       1.157 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Yb1 Yb 0.24999(3) 0.31255(3) 0.18745(3) 0.03821(15) Uani 1 1 d . . . 
O1 O 0.1820(5) 0.2266(4) 0.1233(5) 0.0428(14) Uani 1 1 d . . . 
O2 O 0.3185(5) 0.3757(4) 0.2739(5) 0.0427(14) Uani 1 1 d . . . 
O3 O 0.0404(5) 0.3735(6) 0.3191(5) 0.0641(19) Uani 1 1 d . . . 
O4 O 0.2501(7) 0.1495(5) 0.3507(6) 0.074(2) Uani 1 1 d D . . 
O5 O 0.4587(5) 0.1814(5) 0.1263(6) 0.0595(18) Uani 1 1 d . . . 
N1 N 0.2851(6) 0.3987(5) -0.0195(5) 0.0371(15) Uani 1 1 d . . . 
N2 N 0.2139(6) 0.5190(5) 0.1021(5) 0.0363(15) Uani 1 1 d . . . 
C1 C 0.1698(7) 0.2214(6) 0.0372(7) 0.0377(18) Uani 1 1 d . . . 
C2 C 0.0891(7) 0.1724(6) 0.0425(7) 0.0347(18) Uani 1 1 d . . . 
C3 C 0.0838(8) 0.1691(6) -0.0521(8) 0.047(2) Uani 1 1 d . . . 
H3 H 0.0311 0.1345 -0.0469 0.057 Uiso 1 1 calc R . . 
C4 C 0.1523(8) 0.2143(7) -0.1538(8) 0.046(2) Uani 1 1 d . . . 
C5 C 0.2276(8) 0.2654(7) -0.1587(8) 0.047(2) Uani 1 1 d . . . 
H5 H 0.2739 0.2979 -0.2270 0.056 Uiso 1 1 calc R . . 
C6 C 0.2382(7) 0.2712(6) -0.0681(7) 0.0414(19) Uani 1 1 d . . . 
C7 C 0.3299(7) 0.4633(7) 0.2779(7) 0.0394(18) Uani 1 1 d . . . 
C8 C 0.4108(7) 0.4562(7) 0.3293(6) 0.0382(18) Uani 1 1 d . . . 
C9 C 0.4160(7) 0.5524(6) 0.3301(6) 0.0410(19) Uani 1 1 d . . . 
H9 H 0.4698 0.5473 0.3635 0.049 Uiso 1 1 calc R . . 
C10 C 0.3484(8) 0.6544(7) 0.2857(7) 0.045(2) Uani 1 1 d . . . 
C11 C 0.2719(7) 0.6601(6) 0.2340(7) 0.0416(19) Uani 1 1 d . . . 
H11 H 0.2262 0.7283 0.2007 0.050 Uiso 1 1 calc R . . 
C12 C 0.2613(7) 0.5696(6) 0.2303(7) 0.0402(19) Uani 1 1 d . . . 
C13 C 0.3323(8) 0.3221(6) -0.0864(7) 0.0414(19) Uani 1 1 d . . . 
H13A H 0.4064 0.2647 -0.0707 0.050 Uiso 1 1 calc R . . 
H13B H 0.3577 0.3604 -0.1628 0.050 Uiso 1 1 calc R . . 
C14 C 0.1648(8) 0.4777(7) -0.0251(7) 0.049(2) Uani 1 1 d . . . 
H14A H 0.1026 0.4409 0.0020 0.059 Uiso 1 1 calc R . . 
H14B H 0.1706 0.5181 -0.1003 0.059 Uiso 1 1 calc R . . 
C15 C 0.1254(9) 0.5554(7) 0.0433(8) 0.055(2) Uani 1 1 d . . . 
H15A H 0.1227 0.6283 -0.0034 0.066 Uiso 1 1 calc R . . 
H15B H 0.0418 0.5583 0.0948 0.066 Uiso 1 1 calc R . . 
C16 C 0.3734(8) 0.4582(8) -0.0540(7) 0.056(2) Uani 1 1 d . . . 
H16A H 0.3768 0.5054 -0.1268 0.067 Uiso 1 1 calc R . . 
H16B H 0.4570 0.4067 -0.0567 0.067 Uiso 1 1 calc R . . 
C17 C 0.3342(8) 0.5246(7) 0.0226(7) 0.047(2) Uani 1 1 d . . . 
H17A H 0.3965 0.4975 0.0594 0.056 Uiso 1 1 calc R . . 
H17B H 0.3283 0.6000 -0.0174 0.056 Uiso 1 1 calc R . . 
C18 C 0.1687(7) 0.5865(6) 0.1776(7) 0.0424(19) Uani 1 1 d . . . 
H18A H 0.0938 0.5721 0.2348 0.051 Uiso 1 1 calc R . . 
H18B H 0.1443 0.6626 0.1383 0.051 Uiso 1 1 calc R . . 
C19 C 0.0142(8) 0.1159(7) 0.1534(7) 0.045(2) Uani 1 1 d . . . 
C20 C -0.0770(10) 0.0765(9) 0.1440(9) 0.070(3) Uani 1 1 d . . . 
H20A H -0.0311 0.0256 0.0991 0.105 Uiso 1 1 calc R . . 
H20B H -0.1361 0.1378 0.1116 0.105 Uiso 1 1 calc R . . 
H20C H -0.1214 0.0414 0.2154 0.105 Uiso 1 1 calc R . . 
C21 C -0.0640(8) 0.1959(7) 0.2253(7) 0.050(2) Uani 1 1 d . . . 
H21A H -0.1072 0.1591 0.2963 0.075 Uiso 1 1 calc R . . 
H21B H -0.1244 0.2552 0.1928 0.075 Uiso 1 1 calc R . . 
H21C H -0.0099 0.2239 0.2322 0.075 Uiso 1 1 calc R . . 
C22 C 0.1032(9) 0.0193(7) 0.2058(8) 0.066(3) Uani 1 1 d . . . 
H22A H 0.1465 -0.0334 0.1628 0.100 Uiso 1 1 calc R . . 
H22B H 0.0571 -0.0131 0.2779 0.100 Uiso 1 1 calc R . . 
H22C H 0.1633 0.0421 0.2106 0.100 Uiso 1 1 calc R . . 
C23 C 0.1462(9) 0.2042(8) -0.2559(8) 0.062(3) Uani 1 1 d . . . 
H23A H 0.1428 0.2725 -0.3101 0.093 Uiso 1 1 calc R . . 
H23B H 0.0723 0.1857 -0.2378 0.093 Uiso 1 1 calc R . . 
H23C H 0.2197 0.1481 -0.2840 0.093 Uiso 1 1 calc R . . 
C24 C 0.4862(8) 0.3457(7) 0.3836(7) 0.047(2) Uani 1 1 d . . . 
C25 C 0.5776(9) 0.3560(8) 0.4232(9) 0.070(3) Uani 1 1 d . . . 
H25A H 0.6239 0.2847 0.4566 0.106 Uiso 1 1 calc R . . 
H25B H 0.5312 0.3994 0.4755 0.106 Uiso 1 1 calc R . . 
H25C H 0.6352 0.3904 0.3622 0.106 Uiso 1 1 calc R . . 
C26 C 0.3967(9) 0.2934(8) 0.4813(8) 0.065(3) Uani 1 1 d . . . 
H26A H 0.3318 0.2945 0.4603 0.097 Uiso 1 1 calc R . . 
H26B H 0.3596 0.3330 0.5364 0.097 Uiso 1 1 calc R . . 
H26C H 0.4416 0.2191 0.5099 0.097 Uiso 1 1 calc R . . 
C27 C 0.5647(8) 0.2733(7) 0.3048(7) 0.050(2) Uani 1 1 d . . . 
H27A H 0.6094 0.2033 0.3417 0.075 Uiso 1 1 calc R . . 
H27B H 0.6238 0.3065 0.2445 0.075 Uiso 1 1 calc R . . 
H27C H 0.5107 0.2642 0.2783 0.075 Uiso 1 1 calc R . . 
C28 C 0.3553(10) 0.7563(7) 0.2944(9) 0.070(3) Uani 1 1 d . . . 
H28A H 0.2783 0.7892 0.3450 0.105 Uiso 1 1 calc R . . 
H28B H 0.3675 0.8072 0.2239 0.105 Uiso 1 1 calc R . . 
H28C H 0.4245 0.7370 0.3198 0.105 Uiso 1 1 calc R . . 
C29 C 0.0337(10) 0.3814(8) 0.4236(9) 0.073(3) Uiso 1 1 d D . . 
C30 C -0.0924(16) 0.4683(16) 0.4511(19) 0.071(4) Uiso 0.50 1 d PD . . 
C30' C -0.0986(15) 0.4114(18) 0.4886(17) 0.071(4) Uiso 0.50 1 d PD . . 
C31 C -0.1757(16) 0.4654(17) 0.4004(15) 0.062(5) Uiso 0.50 1 d PD . . 
C31' C -0.1666(19) 0.402(2) 0.4270(14) 0.078(7) Uiso 0.50 1 d PD . . 
C32 C -0.0844(10) 0.4174(9) 0.3101(9) 0.074(3) Uiso 1 1 d D . . 
C33 C 0.3587(19) 0.090(2) 0.3859(19) 0.094(3) Uiso 0.50 1 d PD . . 
C33' C 0.327(2) 0.1076(19) 0.418(2) 0.094(3) Uiso 0.50 1 d PD . . 
C34 C 0.289(3) 0.040(2) 0.501(2) 0.094(3) Uiso 0.50 1 d PD . . 
C34' C 0.329(2) -0.0101(19) 0.467(2) 0.094(3) Uiso 0.50 1 d PD . . 
C35 C 0.220(3) -0.012(2) 0.473(2) 0.094(3) Uiso 0.50 1 d PD . . 
C35' C 0.188(2) 0.042(2) 0.509(2) 0.094(3) Uiso 0.50 1 d PD . . 
C36 C 0.175(2) 0.0813(19) 0.390(2) 0.094(3) Uiso 0.50 1 d PD . . 
C36' C 0.143(2) 0.113(2) 0.413(2) 0.094(3) Uiso 0.50 1 d PD . . 
C37 C 0.4675(10) 0.0769(9) 0.1185(9) 0.073(3) Uiso 1 1 d D . . 
C38 C 0.6026(16) 0.0171(17) 0.080(2) 0.082(5) Uiso 0.50 1 d PD . . 
C38' C 0.5978(17) 0.047(2) 0.0352(18) 0.082(5) Uiso 0.50 1 d PD . . 
C39 C 0.6740(18) 0.1002(15) 0.0333(19) 0.073(4) Uiso 0.50 1 d PD . . 
C39' C 0.6638(19) 0.0738(14) 0.089(2) 0.073(4) Uiso 0.50 1 d PD . . 
C40 C 0.5833(10) 0.1907(8) 0.0826(9) 0.071(3) Uiso 1 1 d D . . 
 
 
_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 2.327(5) . ? 
Yb1 O2 2.328(5) . ? 
Yb1 O5 2.484(6) . ? 
Yb1 O3 2.493(6) . ? 
Yb1 O4 2.552(6) . ? 
Yb1 N2 2.604(6) . ? 
Yb1 N1 2.614(7) . ? 
O1 C1 1.322(9) . ? 
O2 C7 1.331(9) . ? 
O3 C32 1.455(12) . ? 
O3 C29 1.488(12) . ? 
O4 C36 1.421(17) . ? 
O4 C33' 1.423(17) . ? 
O4 C36' 1.442(17) . ? 
O4 C33 1.442(17) . ? 
O5 C40 1.454(12) . ? 
O5 C37 1.477(11) . ? 
N1 C14 1.455(10) . ? 
N1 C16 1.476(9) . ? 
N1 C13 1.478(9) . ? 
N2 C17 1.456(10) . ? 
N2 C15 1.466(9) . ? 
N2 C18 1.477(9) . ? 
C1 C2 1.414(10) . ? 
C1 C6 1.434(11) . ? 
C2 C3 1.387(11) . ? 
C2 C19 1.544(11) . ? 
C3 C4 1.383(12) . ? 
C3 H3 0.9400 . ? 
C4 C5 1.379(11) . ? 
C4 C23 1.539(12) . ? 
C5 C6 1.378(11) . ? 
C5 H5 0.9400 . ? 
C6 C13 1.512(10) . ? 
C7 C8 1.431(10) . ? 
C7 C12 1.433(11) . ? 
C8 C9 1.393(11) . ? 
C8 C24 1.532(12) . ? 
C9 C10 1.378(11) . ? 
C9 H9 0.9400 . ? 
C10 C11 1.395(11) . ? 
C10 C28 1.532(11) . ? 
C11 C12 1.363(10) . ? 
C11 H11 0.9400 . ? 
C12 C18 1.522(10) . ? 
C13 H13A 0.9800 . ? 
C13 H13B 0.9800 . ? 
C14 C15 1.529(12) . ? 
C14 H14A 0.9800 . ? 
C14 H14B 0.9800 . ? 
C15 H15A 0.9800 . ? 
C15 H15B 0.9800 . ? 
C16 C17 1.496(12) . ? 
C16 H16A 0.9800 . ? 
C16 H16B 0.9800 . ? 
C17 H17A 0.9800 . ? 
C17 H17B 0.9800 . ? 
C18 H18A 0.9800 . ? 
C18 H18B 0.9800 . ? 
C19 C22 1.508(12) . ? 
C19 C20 1.535(11) . ? 
C19 C21 1.537(11) . ? 
C20 H20A 0.9700 . ? 
C20 H20B 0.9700 . ? 
C20 H20C 0.9700 . ? 
C21 H21A 0.9700 . ? 
C21 H21B 0.9700 . ? 
C21 H21C 0.9700 . ? 
C22 H22A 0.9700 . ? 
C22 H22B 0.9700 . ? 
C22 H22C 0.9700 . ? 
C23 H23A 0.9700 . ? 
C23 H23B 0.9700 . ? 
C23 H23C 0.9700 . ? 
C24 C26 1.516(12) . ? 
C24 C27 1.529(12) . ? 
C24 C25 1.549(11) . ? 
C25 H25A 0.9700 . ? 
C25 H25B 0.9700 . ? 
C25 H25C 0.9700 . ? 
C26 H26A 0.9700 . ? 
C26 H26B 0.9700 . ? 
C26 H26C 0.9700 . ? 
C27 H27A 0.9700 . ? 
C27 H27B 0.9700 . ? 
C27 H27C 0.9700 . ? 
C28 H28A 0.9700 . ? 
C28 H28B 0.9700 . ? 
C28 H28C 0.9700 . ? 
C29 C30' 1.471(16) . ? 
C29 C30 1.529(16) . ? 
C30 C31 1.516(17) . ? 
C30' C31' 1.522(17) . ? 
C31 C32 1.467(15) . ? 
C31' C32 1.514(16) . ? 
C33 C34 1.526(18) . ? 
C33' C34' 1.526(18) . ? 
C34 C35 1.590(18) . ? 
C34' C35' 1.525(18) . ? 
C35 C36 1.461(18) . ? 
C35' C36' 1.514(18) . ? 
C37 C38 1.488(17) . ? 
C37 C38' 1.541(17) . ? 
C38 C39 1.550(17) . ? 
C38' C39' 1.555(18) . ? 
C39 C40 1.478(16) . ? 
C39' C40 1.515(16) . ? 
 
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 O2 171.31(19) . . ? 
O1 Yb1 O5 85.10(19) . . ? 
O2 Yb1 O5 92.83(19) . . ? 
O1 Yb1 O3 92.9(2) . . ? 
O2 Yb1 O3 85.3(2) . . ? 
O5 Yb1 O3 154.4(2) . . ? 
O1 Yb1 O4 85.9(2) . . ? 
O2 Yb1 O4 85.4(2) . . ? 
O5 Yb1 O4 77.3(2) . . ? 
O3 Yb1 O4 77.2(2) . . ? 
O1 Yb1 N2 116.79(19) . . ? 
O2 Yb1 N2 71.51(19) . . ? 
O5 Yb1 N2 119.9(2) . . ? 
O3 Yb1 N2 83.7(2) . . ? 
O4 Yb1 N2 151.1(2) . . ? 
O1 Yb1 N1 71.04(19) . . ? 
O2 Yb1 N1 117.19(19) . . ? 
O5 Yb1 N1 83.9(2) . . ? 
O3 Yb1 N1 119.6(2) . . ? 
O4 Yb1 N1 151.4(2) . . ? 
N2 Yb1 N1 57.51(19) . . ? 
C1 O1 Yb1 145.3(5) . . ? 
C7 O2 Yb1 144.0(5) . . ? 
C32 O3 C29 109.3(7) . . ? 
C32 O3 Yb1 131.9(6) . . ? 
C29 O3 Yb1 118.3(5) . . ? 
C36 O4 C33' 106.7(15) . . ? 
C36 O4 C36' 22.3(16) . . ? 
C33' O4 C36' 106.8(16) . . ? 
C36 O4 C33 108.5(16) . . ? 
C33' O4 C33 21.0(16) . . ? 
C36' O4 C33 116.6(15) . . ? 
C36 O4 Yb1 126.3(12) . . ? 
C33' O4 Yb1 126.9(11) . . ? 
C36' O4 Yb1 122.4(11) . . ? 
C33 O4 Yb1 120.9(11) . . ? 
C40 O5 C37 108.6(7) . . ? 
C40 O5 Yb1 131.7(5) . . ? 
C37 O5 Yb1 119.3(5) . . ? 
C14 N1 C16 107.9(6) . . ? 
C14 N1 C13 112.7(6) . . ? 
C16 N1 C13 110.6(6) . . ? 
C14 N1 Yb1 104.0(5) . . ? 
C16 N1 Yb1 105.2(5) . . ? 
C13 N1 Yb1 115.8(4) . . ? 
C17 N2 C15 107.8(7) . . ? 
C17 N2 C18 111.9(6) . . ? 
C15 N2 C18 110.1(6) . . ? 
C17 N2 Yb1 103.8(5) . . ? 
C15 N2 Yb1 106.4(5) . . ? 
C18 N2 Yb1 116.4(5) . . ? 
O1 C1 C2 123.7(7) . . ? 
O1 C1 C6 119.0(7) . . ? 
C2 C1 C6 117.3(7) . . ? 
C3 C2 C1 119.7(7) . . ? 
C3 C2 C19 120.3(7) . . ? 
C1 C2 C19 119.8(7) . . ? 
C4 C3 C2 123.1(7) . . ? 
C4 C3 H3 118.5 . . ? 
C2 C3 H3 118.5 . . ? 
C5 C4 C3 117.0(8) . . ? 
C5 C4 C23 122.4(8) . . ? 
C3 C4 C23 120.6(8) . . ? 
C6 C5 C4 123.1(8) . . ? 
C6 C5 H5 118.4 . . ? 
C4 C5 H5 118.4 . . ? 
C5 C6 C1 119.7(7) . . ? 
C5 C6 C13 116.9(7) . . ? 
C1 C6 C13 123.1(7) . . ? 
O2 C7 C8 121.9(7) . . ? 
O2 C7 C12 121.0(7) . . ? 
C8 C7 C12 117.1(7) . . ? 
C9 C8 C7 117.8(7) . . ? 
C9 C8 C24 121.8(7) . . ? 
C7 C8 C24 120.4(7) . . ? 
C10 C9 C8 124.9(8) . . ? 
C10 C9 H9 117.5 . . ? 
C8 C9 H9 117.5 . . ? 
C9 C10 C11 116.6(7) . . ? 
C9 C10 C28 121.7(8) . . ? 
C11 C10 C28 121.8(8) . . ? 
C12 C11 C10 121.9(8) . . ? 
C12 C11 H11 119.0 . . ? 
C10 C11 H11 119.0 . . ? 
C11 C12 C7 121.7(7) . . ? 
C11 C12 C18 116.9(7) . . ? 
C7 C12 C18 121.4(7) . . ? 
N1 C13 C6 113.7(6) . . ? 
N1 C13 H13A 108.8 . . ? 
C6 C13 H13A 108.8 . . ? 
N1 C13 H13B 108.8 . . ? 
C6 C13 H13B 108.8 . . ? 
H13A C13 H13B 107.7 . . ? 
N1 C14 C15 109.1(7) . . ? 
N1 C14 H14A 109.9 . . ? 
C15 C14 H14A 109.9 . . ? 
N1 C14 H14B 109.9 . . ? 
C15 C14 H14B 109.9 . . ? 
H14A C14 H14B 108.3 . . ? 
N2 C15 C14 109.9(7) . . ? 
N2 C15 H15A 109.7 . . ? 
C14 C15 H15A 109.7 . . ? 
N2 C15 H15B 109.7 . . ? 
C14 C15 H15B 109.7 . . ? 
H15A C15 H15B 108.2 . . ? 
N1 C16 C17 110.6(7) . . ? 
N1 C16 H16A 109.5 . . ? 
C17 C16 H16A 109.5 . . ? 
N1 C16 H16B 109.5 . . ? 
C17 C16 H16B 109.5 . . ? 
H16A C16 H16B 108.1 . . ? 
N2 C17 C16 109.7(6) . . ? 
N2 C17 H17A 109.7 . . ? 
C16 C17 H17A 109.7 . . ? 
N2 C17 H17B 109.7 . . ? 
C16 C17 H17B 109.7 . . ? 
H17A C17 H17B 108.2 . . ? 
N2 C18 C12 115.5(6) . . ? 
N2 C18 H18A 108.4 . . ? 
C12 C18 H18A 108.4 . . ? 
N2 C18 H18B 108.4 . . ? 
C12 C18 H18B 108.4 . . ? 
H18A C18 H18B 107.5 . . ? 
C22 C19 C20 108.2(7) . . ? 
C22 C19 C21 110.5(8) . . ? 
C20 C19 C21 106.8(7) . . ? 
C22 C19 C2 109.3(7) . . ? 
C20 C19 C2 112.4(7) . . ? 
C21 C19 C2 109.7(6) . . ? 
C19 C20 H20A 109.5 . . ? 
C19 C20 H20B 109.5 . . ? 
H20A C20 H20B 109.5 . . ? 
C19 C20 H20C 109.5 . . ? 
H20A C20 H20C 109.5 . . ? 
H20B C20 H20C 109.5 . . ? 
C19 C21 H21A 109.5 . . ? 
C19 C21 H21B 109.5 . . ? 
H21A C21 H21B 109.5 . . ? 
C19 C21 H21C 109.5 . . ? 
H21A C21 H21C 109.5 . . ? 
H21B C21 H21C 109.5 . . ? 
C19 C22 H22A 109.5 . . ? 
C19 C22 H22B 109.5 . . ? 
H22A C22 H22B 109.5 . . ? 
C19 C22 H22C 109.5 . . ? 
H22A C22 H22C 109.5 . . ? 
H22B C22 H22C 109.5 . . ? 
C4 C23 H23A 109.5 . . ? 
C4 C23 H23B 109.5 . . ? 
H23A C23 H23B 109.5 . . ? 
C4 C23 H23C 109.5 . . ? 
H23A C23 H23C 109.5 . . ? 
H23B C23 H23C 109.5 . . ? 
C26 C24 C27 110.7(8) . . ? 
C26 C24 C8 108.7(7) . . ? 
C27 C24 C8 111.1(7) . . ? 
C26 C24 C25 107.8(8) . . ? 
C27 C24 C25 106.7(7) . . ? 
C8 C24 C25 111.8(7) . . ? 
C24 C25 H25A 109.5 . . ? 
C24 C25 H25B 109.5 . . ? 
H25A C25 H25B 109.5 . . ? 
C24 C25 H25C 109.5 . . ? 
H25A C25 H25C 109.5 . . ? 
H25B C25 H25C 109.5 . . ? 
C24 C26 H26A 109.5 . . ? 
C24 C26 H26B 109.5 . . ? 
H26A C26 H26B 109.5 . . ? 
C24 C26 H26C 109.5 . . ? 
H26A C26 H26C 109.5 . . ? 
H26B C26 H26C 109.5 . . ? 
C24 C27 H27A 109.5 . . ? 
C24 C27 H27B 109.5 . . ? 
H27A C27 H27B 109.5 . . ? 
C24 C27 H27C 109.5 . . ? 
H27A C27 H27C 109.5 . . ? 
H27B C27 H27C 109.5 . . ? 
C10 C28 H28A 109.5 . . ? 
C10 C28 H28B 109.5 . . ? 
H28A C28 H28B 109.5 . . ? 
C10 C28 H28C 109.5 . . ? 
H28A C28 H28C 109.5 . . ? 
H28B C28 H28C 109.5 . . ? 
C30' C29 O3 107.4(11) . . ? 
C30' C29 C30 30.4(11) . . ? 
O3 C29 C30 101.0(11) . . ? 
C31 C30 C29 109.1(14) . . ? 
C29 C30' C31' 105.0(15) . . ? 
C32 C31 C30 102.0(14) . . ? 
C32 C31' C30' 105.9(15) . . ? 
O3 C32 C31 111.1(11) . . ? 
O3 C32 C31' 103.0(11) . . ? 
C31 C32 C31' 31.1(10) . . ? 
O4 C33 C34 95.6(17) . . ? 
O4 C33' C34' 103.4(18) . . ? 
C33 C34 C35 98.4(19) . . ? 
C35' C34' C33' 82.8(19) . . ? 
C36 C35 C34 97.8(19) . . ? 
C36' C35' C34' 108(2) . . ? 
O4 C36 C35 108.3(19) . . ? 
O4 C36' C35' 95.8(17) . . ? 
O5 C37 C38 106.8(11) . . ? 
O5 C37 C38' 101.2(11) . . ? 
C38 C37 C38' 23.5(14) . . ? 
C37 C38 C39 107.2(15) . . ? 
C37 C38' C39' 95.5(14) . . ? 
C40 C39 C38 103.3(15) . . ? 
C40 C39' C38' 96.3(15) . . ? 
O5 C40 C39 110.4(11) . . ? 
O5 C40 C39' 101.7(11) . . ? 
C39 C40 C39' 27.3(12) . . ? 
 
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
O2 Yb1 O1 C1 -160.5(11) . . . . ? 
O5 Yb1 O1 C1 -84.0(9) . . . . ? 
O3 Yb1 O1 C1 121.5(9) . . . . ? 
O4 Yb1 O1 C1 -161.6(9) . . . . ? 
N2 Yb1 O1 C1 37.1(9) . . . . ? 
N1 Yb1 O1 C1 1.2(8) . . . . ? 
O1 Yb1 O2 C7 -162.5(11) . . . . ? 
O5 Yb1 O2 C7 121.6(8) . . . . ? 
O3 Yb1 O2 C7 -84.0(8) . . . . ? 
O4 Yb1 O2 C7 -161.5(9) . . . . ? 
N2 Yb1 O2 C7 1.0(8) . . . . ? 
N1 Yb1 O2 C7 37.0(9) . . . . ? 
O1 Yb1 O3 C32 -41.6(8) . . . . ? 
O2 Yb1 O3 C32 147.0(8) . . . . ? 
O5 Yb1 O3 C32 -126.4(8) . . . . ? 
O4 Yb1 O3 C32 -126.7(9) . . . . ? 
N2 Yb1 O3 C32 75.1(8) . . . . ? 
N1 Yb1 O3 C32 28.3(9) . . . . ? 
O1 Yb1 O3 C29 147.1(6) . . . . ? 
O2 Yb1 O3 C29 -24.4(6) . . . . ? 
O5 Yb1 O3 C29 62.3(9) . . . . ? 
O4 Yb1 O3 C29 62.0(6) . . . . ? 
N2 Yb1 O3 C29 -96.2(6) . . . . ? 
N1 Yb1 O3 C29 -143.1(6) . . . . ? 
O1 Yb1 O4 C36 -26.1(15) . . . . ? 
O2 Yb1 O4 C36 154.0(15) . . . . ? 
O5 Yb1 O4 C36 -112.0(15) . . . . ? 
O3 Yb1 O4 C36 67.9(15) . . . . ? 
N2 Yb1 O4 C36 117.7(15) . . . . ? 
N1 Yb1 O4 C36 -62.0(16) . . . . ? 
O1 Yb1 O4 C33' 152.1(16) . . . . ? 
O2 Yb1 O4 C33' -27.8(16) . . . . ? 
O5 Yb1 O4 C33' 66.2(15) . . . . ? 
O3 Yb1 O4 C33' -113.9(16) . . . . ? 
N2 Yb1 O4 C33' -64.1(17) . . . . ? 
N1 Yb1 O4 C33' 116.2(15) . . . . ? 
O1 Yb1 O4 C36' -52.8(14) . . . . ? 
O2 Yb1 O4 C36' 127.3(14) . . . . ? 
O5 Yb1 O4 C36' -138.7(14) . . . . ? 
O3 Yb1 O4 C36' 41.2(14) . . . . ? 
N2 Yb1 O4 C36' 91.0(15) . . . . ? 
N1 Yb1 O4 C36' -88.7(15) . . . . ? 
O1 Yb1 O4 C33 127.8(14) . . . . ? 
O2 Yb1 O4 C33 -52.0(14) . . . . ? 
O5 Yb1 O4 C33 41.9(14) . . . . ? 
O3 Yb1 O4 C33 -138.2(14) . . . . ? 
N2 Yb1 O4 C33 -88.4(15) . . . . ? 
N1 Yb1 O4 C33 91.9(15) . . . . ? 
O1 Yb1 O5 C40 146.8(8) . . . . ? 
O2 Yb1 O5 C40 -41.6(8) . . . . ? 
O3 Yb1 O5 C40 -126.6(8) . . . . ? 
O4 Yb1 O5 C40 -126.3(8) . . . . ? 
N2 Yb1 O5 C40 28.6(9) . . . . ? 
N1 Yb1 O5 C40 75.4(8) . . . . ? 
O1 Yb1 O5 C37 -25.2(7) . . . . ? 
O2 Yb1 O5 C37 146.4(7) . . . . ? 
O3 Yb1 O5 C37 61.4(9) . . . . ? 
O4 Yb1 O5 C37 61.8(7) . . . . ? 
N2 Yb1 O5 C37 -143.4(6) . . . . ? 
N1 Yb1 O5 C37 -96.6(7) . . . . ? 
O1 Yb1 N1 C14 83.3(5) . . . . ? 
O2 Yb1 N1 C14 -99.7(4) . . . . ? 
O5 Yb1 N1 C14 170.2(5) . . . . ? 
O3 Yb1 N1 C14 1.0(5) . . . . ? 
O4 Yb1 N1 C14 121.5(5) . . . . ? 
N2 Yb1 N1 C14 -58.3(4) . . . . ? 
O1 Yb1 N1 C16 -163.4(5) . . . . ? 
O2 Yb1 N1 C16 13.6(6) . . . . ? 
O5 Yb1 N1 C16 -76.5(5) . . . . ? 
O3 Yb1 N1 C16 114.2(5) . . . . ? 
O4 Yb1 N1 C16 -125.2(6) . . . . ? 
N2 Yb1 N1 C16 55.0(5) . . . . ? 
O1 Yb1 N1 C13 -40.9(5) . . . . ? 
O2 Yb1 N1 C13 136.0(5) . . . . ? 
O5 Yb1 N1 C13 46.0(5) . . . . ? 
O3 Yb1 N1 C13 -123.3(5) . . . . ? 
O4 Yb1 N1 C13 -2.8(7) . . . . ? 
N2 Yb1 N1 C13 177.4(5) . . . . ? 
O1 Yb1 N2 C17 -99.4(5) . . . . ? 
O2 Yb1 N2 C17 83.4(5) . . . . ? 
O5 Yb1 N2 C17 1.0(5) . . . . ? 
O3 Yb1 N2 C17 170.5(5) . . . . ? 
O4 Yb1 N2 C17 122.0(6) . . . . ? 
N1 Yb1 N2 C17 -58.2(5) . . . . ? 
O1 Yb1 N2 C15 14.2(6) . . . . ? 
O2 Yb1 N2 C15 -163.1(6) . . . . ? 
O5 Yb1 N2 C15 114.5(5) . . . . ? 
O3 Yb1 N2 C15 -76.0(5) . . . . ? 
O4 Yb1 N2 C15 -124.5(6) . . . . ? 
N1 Yb1 N2 C15 55.3(5) . . . . ? 
O1 Yb1 N2 C18 137.2(5) . . . . ? 
O2 Yb1 N2 C18 -40.0(5) . . . . ? 
O5 Yb1 N2 C18 -122.4(5) . . . . ? 
O3 Yb1 N2 C18 47.1(5) . . . . ? 
O4 Yb1 N2 C18 -1.4(7) . . . . ? 
N1 Yb1 N2 C18 178.4(5) . . . . ? 
Yb1 O1 C1 C2 -161.8(6) . . . . ? 
Yb1 O1 C1 C6 15.9(13) . . . . ? 
O1 C1 C2 C3 -179.0(7) . . . . ? 
C6 C1 C2 C3 3.3(11) . . . . ? 
O1 C1 C2 C19 -3.2(11) . . . . ? 
C6 C1 C2 C19 179.1(7) . . . . ? 
C1 C2 C3 C4 -1.6(12) . . . . ? 
C19 C2 C3 C4 -177.3(8) . . . . ? 
C2 C3 C4 C5 -0.7(13) . . . . ? 
C2 C3 C4 C23 177.7(8) . . . . ? 
C3 C4 C5 C6 1.2(13) . . . . ? 
C23 C4 C5 C6 -177.2(8) . . . . ? 
C4 C5 C6 C1 0.7(13) . . . . ? 
C4 C5 C6 C13 175.2(8) . . . . ? 
O1 C1 C6 C5 179.3(7) . . . . ? 
C2 C1 C6 C5 -2.9(11) . . . . ? 
O1 C1 C6 C13 5.1(12) . . . . ? 
C2 C1 C6 C13 -177.1(7) . . . . ? 
Yb1 O2 C7 C8 -163.0(6) . . . . ? 
Yb1 O2 C7 C12 16.8(13) . . . . ? 
O2 C7 C8 C9 -179.5(7) . . . . ? 
C12 C7 C8 C9 0.6(11) . . . . ? 
O2 C7 C8 C24 -1.0(12) . . . . ? 
C12 C7 C8 C24 179.2(7) . . . . ? 
C7 C8 C9 C10 0.4(12) . . . . ? 
C24 C8 C9 C10 -178.1(8) . . . . ? 
C8 C9 C10 C11 -1.7(13) . . . . ? 
C8 C9 C10 C28 177.3(8) . . . . ? 
C9 C10 C11 C12 2.0(13) . . . . ? 
C28 C10 C11 C12 -177.0(9) . . . . ? 
C10 C11 C12 C7 -1.0(13) . . . . ? 
C10 C11 C12 C18 176.3(8) . . . . ? 
O2 C7 C12 C11 179.8(8) . . . . ? 
C8 C7 C12 C11 -0.3(12) . . . . ? 
O2 C7 C12 C18 2.7(12) . . . . ? 
C8 C7 C12 C18 -177.5(7) . . . . ? 
C14 N1 C13 C6 -49.9(9) . . . . ? 
C16 N1 C13 C6 -170.8(7) . . . . ? 
Yb1 N1 C13 C6 69.7(8) . . . . ? 
C5 C6 C13 N1 135.6(8) . . . . ? 
C1 C6 C13 N1 -50.0(11) . . . . ? 
C16 N1 C14 C15 -55.8(9) . . . . ? 
C13 N1 C14 C15 -178.2(7) . . . . ? 
Yb1 N1 C14 C15 55.6(7) . . . . ? 
C17 N2 C15 C14 64.1(9) . . . . ? 
C18 N2 C15 C14 -173.6(7) . . . . ? 
Yb1 N2 C15 C14 -46.7(8) . . . . ? 
N1 C14 C15 N2 -6.1(10) . . . . ? 
C14 N1 C16 C17 63.8(9) . . . . ? 
C13 N1 C16 C17 -172.5(7) . . . . ? 
Yb1 N1 C16 C17 -46.8(8) . . . . ? 
C15 N2 C17 C16 -56.8(9) . . . . ? 
C18 N2 C17 C16 -178.0(7) . . . . ? 
Yb1 N2 C17 C16 55.8(7) . . . . ? 
N1 C16 C17 N2 -5.7(10) . . . . ? 
C17 N2 C18 C12 -50.6(9) . . . . ? 
C15 N2 C18 C12 -170.4(7) . . . . ? 
Yb1 N2 C18 C12 68.5(8) . . . . ? 
C11 C12 C18 N2 135.3(8) . . . . ? 
C7 C12 C18 N2 -47.5(11) . . . . ? 
C3 C2 C19 C22 110.6(9) . . . . ? 
C1 C2 C19 C22 -65.1(9) . . . . ? 
C3 C2 C19 C20 -9.5(11) . . . . ? 
C1 C2 C19 C20 174.8(7) . . . . ? 
C3 C2 C19 C21 -128.2(8) . . . . ? 
C1 C2 C19 C21 56.1(9) . . . . ? 
C9 C8 C24 C26 111.3(9) . . . . ? 
C7 C8 C24 C26 -67.2(10) . . . . ? 
C9 C8 C24 C27 -126.7(8) . . . . ? 
C7 C8 C24 C27 54.8(10) . . . . ? 
C9 C8 C24 C25 -7.6(11) . . . . ? 
C7 C8 C24 C25 173.9(8) . . . . ? 
C32 O3 C29 C30' 10.7(14) . . . . ? 
Yb1 O3 C29 C30' -176.2(10) . . . . ? 
C32 O3 C29 C30 -20.0(13) . . . . ? 
Yb1 O3 C29 C30 153.2(10) . . . . ? 
C30' C29 C30 C31 -78(2) . . . . ? 
O3 C29 C30 C31 27.8(18) . . . . ? 
O3 C29 C30' C31' 9.2(19) . . . . ? 
C30 C29 C30' C31' 91(3) . . . . ? 
C29 C30 C31 C32 -25(2) . . . . ? 
C29 C30' C31' C32 -25(2) . . . . ? 
C29 O3 C32 C31 5.7(14) . . . . ? 
Yb1 O3 C32 C31 -166.2(10) . . . . ? 
C29 O3 C32 C31' -25.7(13) . . . . ? 
Yb1 O3 C32 C31' 162.4(10) . . . . ? 
C30 C31 C32 O3 11.6(18) . . . . ? 
C30 C31 C32 C31' 91(3) . . . . ? 
C30' C31' C32 O3 31.0(19) . . . . ? 
C30' C31' C32 C31 -79(2) . . . . ? 
C36 O4 C33 C34 -43(2) . . . . ? 
C33' O4 C33 C34 46(4) . . . . ? 
C36' O4 C33 C34 -20(3) . . . . ? 
Yb1 O4 C33 C34 159.0(12) . . . . ? 
C36 O4 C33' C34' 22(2) . . . . ? 
C36' O4 C33' C34' 45(2) . . . . ? 
C33 O4 C33' C34' -76(5) . . . . ? 
Yb1 O4 C33' C34' -156.5(13) . . . . ? 
O4 C33 C34 C35 54(2) . . . . ? 
O4 C33' C34' C35' -59(2) . . . . ? 
C33 C34 C35 C36 -46(2) . . . . ? 
C33' C34' C35' C36' 58(2) . . . . ? 
C33' O4 C36 C35 -8(3) . . . . ? 
C36' O4 C36 C35 -102(5) . . . . ? 
C33 O4 C36 C35 14(3) . . . . ? 
Yb1 O4 C36 C35 170.3(14) . . . . ? 
C34 C35 C36 O4 21(3) . . . . ? 
C36 O4 C36' C35' 88(5) . . . . ? 
C33' O4 C36' C35' -5(2) . . . . ? 
C33 O4 C36' C35' 15(3) . . . . ? 
Yb1 O4 C36' C35' -164.7(12) . . . . ? 
C34' C35' C36' O4 -37(3) . . . . ? 
C40 O5 C37 C38 6.0(15) . . . . ? 
Yb1 O5 C37 C38 179.6(12) . . . . ? 
C40 O5 C37 C38' -17.5(14) . . . . ? 
Yb1 O5 C37 C38' 156.2(10) . . . . ? 
O5 C37 C38 C39 -16(2) . . . . ? 
C38' C37 C38 C39 63(3) . . . . ? 
O5 C37 C38' C39' 46.5(16) . . . . ? 
C38 C37 C38' C39' -60(3) . . . . ? 
C37 C38 C39 C40 19(2) . . . . ? 
C37 C38' C39' C40 -58.2(18) . . . . ? 
C37 O5 C40 C39 6.9(15) . . . . ? 
Yb1 O5 C40 C39 -165.7(11) . . . . ? 
C37 O5 C40 C39' -20.1(14) . . . . ? 
Yb1 O5 C40 C39' 167.3(10) . . . . ? 
C38 C39 C40 O5 -16(2) . . . . ? 
C38 C39 C40 C39' 60(3) . . . . ? 
C38' C39' C40 O5 48.8(16) . . . . ? 
C38' C39' C40 C39 -63(3) . . . . ? 
 
_diffrn_measured_fraction_theta_max    0.992 
_diffrn_reflns_theta_full              25.50 
_diffrn_measured_fraction_theta_full   0.992 
_refine_diff_density_max    1.753 
_refine_diff_density_min   -1.549 
_refine_diff_density_rms    0.139 

