# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2005

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Gardiner, M. G.'
_publ_contact_author_address     
;
School of Chemistry
University of Tasmania
Private Bag 75
Sandy Bay
Tasmania 6009
Australia
;
_publ_contact_author_email       michael.gardiner@utas.edu.au
_publ_contact_author_fax         (+61)_03_6226_2858
_publ_contact_author_phone       (+61)_03-6226_2404

_publ_section_title              
;
C-H Activation (g-deprotonation) of a Sm(III)
bis(trimethylsilyl)amide complex via macrocyclic stabilisation of the
sodium counter ion
;
loop_
_publ_author_name
'Michael Guy Gardiner'
'Jun Wang'

data_smnnono_b
_database_code_depnum_ccdc_archive 'CCDC 256898'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H66 N3 O2 Si2 Sm'
_chemical_formula_weight         851.51

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'
Sm Sm -0.1638 3.4418 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.17170(10)
_cell_length_b                   27.7942(3)
_cell_length_c                   13.62490(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.1423(5)
_cell_angle_gamma                90.00
_cell_volume                     4238.43(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prismatic
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.40
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1780
_exptl_absorpt_coefficient_mu    1.479
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_reflns_number            52474
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.40
_diffrn_reflns_theta_max         28.30
_reflns_number_total             10329
_reflns_number_gt                7552
_reflns_threshold_expression     >2sigma(I)

_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, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10329
_refine_ls_number_parameters     451
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0315
_refine_ls_wR_factor_ref         0.0718
_refine_ls_wR_factor_gt          0.0659
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_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
Sm1 Sm 0.939181(12) 0.111256(5) 0.207926(11) 0.01390(5) Uani 1 1 d . . .
N1 N 0.92084(19) 0.12508(8) 0.00944(17) 0.0158(5) Uani 1 1 d . . .
N2 N 1.09065(18) 0.03903(8) 0.28982(16) 0.0142(5) Uani 1 1 d . . .
O1 O 1.16266(15) 0.13763(6) 0.22979(13) 0.0152(4) Uani 1 1 d . . .
O2 O 0.82716(15) 0.03473(6) 0.08787(13) 0.0163(4) Uani 1 1 d . . .
C1 C 0.8021(2) 0.12561(10) -0.0040(2) 0.0165(6) Uani 1 1 d . . .
C2 C 0.7763(2) 0.16784(10) 0.0362(2) 0.0185(6) Uani 1 1 d . . .
H2 H 0.7035 0.1762 0.0387 0.022 Uiso 1 1 calc R . .
C3 C 0.8812(2) 0.19586(10) 0.0727(2) 0.0193(6) Uani 1 1 d . . .
H3 H 0.8914 0.2262 0.1038 0.023 Uiso 1 1 calc R . .
C4 C 0.9667(2) 0.16887(9) 0.0527(2) 0.0154(6) Uani 1 1 d . . .
C5 C 1.0912(2) 0.18269(9) 0.0620(2) 0.0157(6) Uani 1 1 d . . .
C6 C 1.1218(2) 0.23485(9) 0.1039(2) 0.0208(6) Uani 1 1 d . . .
H6A H 1.0667 0.2566 0.0520 0.025 Uiso 1 1 calc R . .
H6B H 1.1087 0.2379 0.1694 0.025 Uiso 1 1 calc R . .
C7 C 1.2488(2) 0.25090(10) 0.1256(2) 0.0275(7) Uani 1 1 d . . .
H7A H 1.2597 0.2835 0.1508 0.041 Uiso 1 1 calc R . .
H7B H 1.2624 0.2490 0.0609 0.041 Uiso 1 1 calc R . .
H7C H 1.3044 0.2304 0.1786 0.041 Uiso 1 1 calc R . .
C8 C 1.0963(2) 0.17717(10) -0.0497(2) 0.0204(6) Uani 1 1 d . . .
H8A H 1.1755 0.1863 -0.0441 0.024 Uiso 1 1 calc R . .
H8B H 1.0848 0.1435 -0.0701 0.024 Uiso 1 1 calc R . .
C9 C 1.0049(3) 0.20676(11) -0.1379(2) 0.0303(7) Uani 1 1 d . . .
H9A H 1.0141 0.2012 -0.2038 0.046 Uiso 1 1 calc R . .
H9B H 1.0170 0.2403 -0.1200 0.046 Uiso 1 1 calc R . .
H9C H 0.9259 0.1975 -0.1457 0.046 Uiso 1 1 calc R . .
C10 C 1.1798(2) 0.14841(9) 0.1362(2) 0.0146(6) Uani 1 1 d . . .
C11 C 1.2810(2) 0.12757(10) 0.1413(2) 0.0197(6) Uani 1 1 d . . .
H11 H 1.3127 0.1291 0.0895 0.024 Uiso 1 1 calc R . .
C12 C 1.3319(2) 0.10253(9) 0.2411(2) 0.0199(6) Uani 1 1 d . . .
H12 H 1.4023 0.0848 0.2655 0.024 Uiso 1 1 calc R . .
C13 C 1.2595(2) 0.10929(9) 0.2927(2) 0.0163(6) Uani 1 1 d . . .
C14 C 1.2557(2) 0.09331(10) 0.3963(2) 0.0167(6) Uani 1 1 d . . .
C15 C 1.2790(2) 0.13568(10) 0.4754(2) 0.0232(6) Uani 1 1 d . . .
H15A H 1.2102 0.1569 0.4499 0.028 Uiso 1 1 calc R . .
H15B H 1.2859 0.1230 0.5439 0.028 Uiso 1 1 calc R . .
C16 C 1.3903(3) 0.16522(12) 0.4918(2) 0.0359(8) Uani 1 1 d . . .
H16A H 1.3978 0.1907 0.5415 0.054 Uiso 1 1 calc R . .
H16B H 1.3838 0.1786 0.4248 0.054 Uiso 1 1 calc R . .
H16C H 1.4596 0.1449 0.5194 0.054 Uiso 1 1 calc R . .
C17 C 1.3514(2) 0.05321(10) 0.4419(2) 0.0218(6) Uani 1 1 d . . .
H17A H 1.3348 0.0279 0.3889 0.026 Uiso 1 1 calc R . .
H17B H 1.4290 0.0666 0.4531 0.026 Uiso 1 1 calc R . .
C18 C 1.3580(3) 0.03086(12) 0.5466(2) 0.0374(8) Uani 1 1 d . . .
H18A H 1.4192 0.0066 0.5691 0.056 Uiso 1 1 calc R . .
H18B H 1.2825 0.0165 0.5360 0.056 Uiso 1 1 calc R . .
H18C H 1.3766 0.0554 0.6003 0.056 Uiso 1 1 calc R . .
C19 C 1.1336(2) 0.07218(9) 0.3710(2) 0.0148(6) Uani 1 1 d . . .
C20 C 1.0563(2) 0.07692(10) 0.4237(2) 0.0178(6) Uani 1 1 d . . .
H20 H 1.0641 0.0980 0.4790 0.021 Uiso 1 1 calc R . .
C21 C 0.9645(2) 0.04337(9) 0.3759(2) 0.0164(6) Uani 1 1 d . . .
H21 H 0.8993 0.0378 0.3939 0.020 Uiso 1 1 calc R . .
C22 C 0.9892(2) 0.02002(9) 0.2966(2) 0.0145(6) Uani 1 1 d . . .
C23 C 0.9330(2) -0.02357(10) 0.2299(2) 0.0158(6) Uani 1 1 d . . .
C24 C 1.0324(2) -0.06117(10) 0.2476(2) 0.0189(6) Uani 1 1 d . . .
H24A H 0.9972 -0.0894 0.2049 0.023 Uiso 1 1 calc R . .
H24B H 1.0900 -0.0479 0.2221 0.023 Uiso 1 1 calc R . .
C25 C 1.0982(3) -0.07676(11) 0.3634(2) 0.0287(7) Uani 1 1 d . . .
H25A H 1.1579 -0.1002 0.3677 0.043 Uiso 1 1 calc R . .
H25B H 1.0424 -0.0906 0.3892 0.043 Uiso 1 1 calc R . .
H25C H 1.1357 -0.0493 0.4062 0.043 Uiso 1 1 calc R . .
C26 C 0.8316(2) -0.04410(10) 0.2606(2) 0.0203(6) Uani 1 1 d . . .
H26A H 0.8617 -0.0468 0.3377 0.024 Uiso 1 1 calc R . .
H26B H 0.7662 -0.0212 0.2387 0.024 Uiso 1 1 calc R . .
C27 C 0.7824(3) -0.09299(10) 0.2121(2) 0.0296(7) Uani 1 1 d . . .
H27A H 0.7208 -0.1027 0.2353 0.044 Uiso 1 1 calc R . .
H27B H 0.8456 -0.1163 0.2349 0.044 Uiso 1 1 calc R . .
H27C H 0.7498 -0.0906 0.1357 0.044 Uiso 1 1 calc R . .
C28 C 0.8848(2) -0.01033(9) 0.1138(2) 0.0166(6) Uani 1 1 d . . .
C29 C 0.8817(2) -0.03115(10) 0.0241(2) 0.0196(6) Uani 1 1 d . . .
H29 H 0.9152 -0.0607 0.0194 0.023 Uiso 1 1 calc R . .
C30 C 0.8180(2) 0.00010(10) -0.0628(2) 0.0210(6) Uani 1 1 d . . .
H30 H 0.8020 -0.0056 -0.1344 0.025 Uiso 1 1 calc R . .
C31 C 0.7853(2) 0.03905(10) -0.0231(2) 0.0164(6) Uani 1 1 d . . .
C32 C 0.7207(2) 0.08517(10) -0.0658(2) 0.0173(6) Uani 1 1 d . . .
C33 C 0.6006(2) 0.08586(11) -0.0530(2) 0.0238(7) Uani 1 1 d . . .
H33A H 0.6164 0.0858 0.0226 0.029 Uiso 1 1 calc R . .
H33B H 0.5594 0.1156 -0.0829 0.029 Uiso 1 1 calc R . .
C34 C 0.5187(3) 0.04403(12) -0.1057(3) 0.0373(8) Uani 1 1 d . . .
H34A H 0.4464 0.0468 -0.0936 0.056 Uiso 1 1 calc R . .
H34B H 0.5579 0.0143 -0.0758 0.056 Uiso 1 1 calc R . .
H34C H 0.5000 0.0444 -0.1810 0.056 Uiso 1 1 calc R . .
C35 C 0.7025(2) 0.09011(11) -0.1850(2) 0.0231(6) Uani 1 1 d . . .
H35A H 0.7802 0.0900 -0.1893 0.028 Uiso 1 1 calc R . .
H35B H 0.6589 0.0622 -0.2237 0.028 Uiso 1 1 calc R . .
C36 C 0.6357(3) 0.13519(12) -0.2400(2) 0.0357(8) Uani 1 1 d . . .
H36A H 0.6292 0.1358 -0.3125 0.054 Uiso 1 1 calc R . .
H36B H 0.6784 0.1631 -0.2031 0.054 Uiso 1 1 calc R . .
H36C H 0.5572 0.1351 -0.2391 0.054 Uiso 1 1 calc R . .
N3 N 0.84240(19) 0.15566(8) 0.29364(17) 0.0175(5) Uani 1 1 d . . .
Si1 Si 0.69960(7) 0.14158(3) 0.27926(6) 0.01936(17) Uani 1 1 d . . .
C37 C 0.6631(2) 0.07656(10) 0.2402(2) 0.0251(7) Uani 1 1 d . . .
H37A H 0.6753 0.0701 0.1760 0.038 Uiso 1 1 calc R . .
H37B H 0.5812 0.0704 0.2282 0.038 Uiso 1 1 calc R . .
H37C H 0.7142 0.0562 0.2965 0.038 Uiso 1 1 calc R . .
C38 C 0.5814(2) 0.17875(10) 0.1761(2) 0.0273(7) Uani 1 1 d . . .
H38A H 0.5912 0.1769 0.1097 0.041 Uiso 1 1 calc R . .
H38B H 0.5887 0.2116 0.1994 0.041 Uiso 1 1 calc R . .
H38C H 0.5039 0.1668 0.1666 0.041 Uiso 1 1 calc R . .
C39 C 0.6709(3) 0.14815(11) 0.4044(2) 0.0278(7) Uani 1 1 d . . .
H39A H 0.7288 0.1298 0.4607 0.042 Uiso 1 1 calc R . .
H39B H 0.5921 0.1366 0.3918 0.042 Uiso 1 1 calc R . .
H39C H 0.6770 0.1814 0.4247 0.042 Uiso 1 1 calc R . .
Si2 Si 0.90920(7) 0.20544(3) 0.36831(6) 0.02064(18) Uani 1 1 d . . .
C40 C 1.0416(3) 0.22754(11) 0.3412(2) 0.0284(7) Uani 1 1 d . . .
H40A H 1.0172 0.2335 0.2662 0.043 Uiso 1 1 calc R . .
H40B H 1.1033 0.2035 0.3635 0.043 Uiso 1 1 calc R . .
H40C H 1.0715 0.2567 0.3802 0.043 Uiso 1 1 calc R . .
C41 C 0.9678(3) 0.19537(11) 0.5166(2) 0.0282(7) Uani 1 1 d . . .
H41A H 1.0201 0.1680 0.5352 0.042 Uiso 1 1 calc R . .
H41B H 0.9022 0.1897 0.5374 0.042 Uiso 1 1 calc R . .
H41C H 1.0112 0.2233 0.5530 0.042 Uiso 1 1 calc R . .
C42 C 0.8086(3) 0.25959(10) 0.3378(3) 0.0317(8) Uani 1 1 d . . .
H42A H 0.7770 0.2658 0.2624 0.048 Uiso 1 1 calc R . .
H42B H 0.8534 0.2870 0.3755 0.048 Uiso 1 1 calc R . .
H42C H 0.7441 0.2536 0.3599 0.048 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sm1 0.01345(8) 0.01272(7) 0.01671(8) 0.00083(6) 0.00720(6) 0.00149(6)
N1 0.0141(12) 0.0171(12) 0.0168(12) 0.0036(9) 0.0069(10) 0.0015(9)
N2 0.0118(11) 0.0133(12) 0.0174(12) 0.0008(9) 0.0056(10) 0.0012(9)
O1 0.0161(10) 0.0152(10) 0.0165(10) 0.0011(8) 0.0087(8) 0.0017(8)
O2 0.0160(10) 0.0162(10) 0.0167(10) 0.0009(8) 0.0065(8) 0.0017(8)
C1 0.0155(14) 0.0189(15) 0.0153(14) 0.0059(11) 0.0061(12) 0.0022(11)
C2 0.0144(14) 0.0196(15) 0.0225(15) 0.0056(12) 0.0083(12) 0.0042(12)
C3 0.0250(16) 0.0118(14) 0.0226(16) 0.0029(12) 0.0110(13) 0.0036(12)
C4 0.0177(14) 0.0140(14) 0.0154(14) 0.0033(11) 0.0073(12) -0.0008(12)
C5 0.0184(14) 0.0138(14) 0.0167(14) 0.0010(11) 0.0089(12) -0.0004(11)
C6 0.0256(16) 0.0146(15) 0.0255(16) -0.0015(12) 0.0135(14) -0.0011(12)
C7 0.0267(17) 0.0218(17) 0.0341(18) -0.0061(14) 0.0120(15) -0.0088(13)
C8 0.0213(15) 0.0198(16) 0.0222(15) 0.0003(12) 0.0107(13) -0.0021(12)
C9 0.0303(18) 0.037(2) 0.0276(18) 0.0112(15) 0.0158(15) 0.0050(15)
C10 0.0174(14) 0.0144(14) 0.0140(14) -0.0010(11) 0.0083(12) -0.0048(11)
C11 0.0188(15) 0.0225(15) 0.0222(16) -0.0006(12) 0.0128(13) -0.0024(12)
C12 0.0127(14) 0.0205(16) 0.0260(16) 0.0018(12) 0.0069(12) 0.0032(11)
C13 0.0138(13) 0.0126(13) 0.0196(14) -0.0005(12) 0.0033(11) -0.0017(12)
C14 0.0155(14) 0.0180(14) 0.0152(14) -0.0012(11) 0.0046(12) -0.0006(12)
C15 0.0259(16) 0.0219(16) 0.0204(16) -0.0035(13) 0.0076(13) -0.0037(13)
C16 0.0349(19) 0.035(2) 0.0363(19) -0.0158(16) 0.0125(16) -0.0180(16)
C17 0.0178(15) 0.0233(16) 0.0224(16) 0.0028(13) 0.0059(13) 0.0030(13)
C18 0.0346(19) 0.046(2) 0.0294(19) 0.0154(16) 0.0102(16) 0.0122(17)
C19 0.0145(14) 0.0153(14) 0.0137(14) 0.0028(11) 0.0045(11) 0.0033(11)
C20 0.0220(15) 0.0170(15) 0.0156(14) -0.0004(12) 0.0085(12) 0.0034(12)
C21 0.0158(14) 0.0175(15) 0.0186(15) 0.0038(11) 0.0097(12) 0.0040(12)
C22 0.0149(14) 0.0128(14) 0.0153(14) 0.0057(11) 0.0055(12) 0.0016(11)
C23 0.0182(14) 0.0141(14) 0.0165(15) 0.0017(11) 0.0083(12) 0.0001(11)
C24 0.0206(15) 0.0149(15) 0.0234(15) 0.0028(12) 0.0111(12) 0.0015(12)
C25 0.0307(18) 0.0257(18) 0.0313(18) 0.0060(14) 0.0138(15) 0.0093(14)
C26 0.0222(16) 0.0167(15) 0.0244(16) 0.0026(12) 0.0117(13) -0.0015(12)
C27 0.0288(17) 0.0210(16) 0.042(2) -0.0004(15) 0.0167(16) -0.0060(14)
C28 0.0136(14) 0.0123(14) 0.0226(15) 0.0022(11) 0.0055(12) -0.0003(11)
C29 0.0256(16) 0.0134(14) 0.0205(16) -0.0028(12) 0.0099(13) -0.0026(12)
C30 0.0232(16) 0.0206(16) 0.0188(15) -0.0021(12) 0.0079(13) -0.0051(13)
C31 0.0134(14) 0.0199(15) 0.0148(14) 0.0000(11) 0.0044(11) -0.0042(12)
C32 0.0133(14) 0.0198(16) 0.0180(15) 0.0027(12) 0.0054(12) 0.0009(12)
C33 0.0163(15) 0.0316(18) 0.0221(16) 0.0056(13) 0.0061(13) 0.0004(13)
C34 0.0190(17) 0.048(2) 0.043(2) 0.0033(17) 0.0104(16) -0.0057(15)
C35 0.0224(16) 0.0276(17) 0.0180(15) 0.0037(13) 0.0065(13) -0.0013(13)
C36 0.0346(19) 0.044(2) 0.0237(18) 0.0099(15) 0.0069(15) 0.0092(17)
N3 0.0179(12) 0.0161(13) 0.0195(12) 0.0011(10) 0.0084(10) 0.0032(10)
Si1 0.0177(4) 0.0201(4) 0.0223(4) 0.0005(3) 0.0100(4) 0.0035(3)
C37 0.0179(15) 0.0259(17) 0.0331(18) -0.0011(14) 0.0118(14) 0.0017(13)
C38 0.0179(15) 0.0287(18) 0.0379(19) 0.0054(14) 0.0137(14) 0.0061(13)
C39 0.0251(17) 0.0330(19) 0.0291(18) -0.0020(14) 0.0148(14) -0.0009(14)
Si2 0.0233(4) 0.0163(4) 0.0264(5) -0.0034(3) 0.0142(4) 0.0012(3)
C40 0.0293(17) 0.0268(18) 0.0317(18) -0.0084(14) 0.0147(15) -0.0049(14)
C41 0.0321(18) 0.0235(17) 0.0313(18) -0.0087(14) 0.0149(15) -0.0024(14)
C42 0.0345(18) 0.0183(17) 0.048(2) -0.0040(15) 0.0225(17) 0.0022(14)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 N3 2.314(2) . ?
Sm1 N1 2.653(2) . ?
Sm1 N2 2.656(2) . ?
Sm1 O2 2.7029(17) . ?
Sm1 O1 2.7181(16) . ?
Sm1 C1 2.737(3) . ?
Sm1 C19 2.754(2) . ?
Sm1 C22 2.772(3) . ?
Sm1 C4 2.776(2) . ?
Sm1 C2 2.869(3) . ?
Sm1 C20 2.879(3) . ?
Sm1 C21 2.887(2) . ?
N1 C4 1.372(3) . ?
N1 C1 1.384(3) . ?
N2 C19 1.375(3) . ?
N2 C22 1.379(3) . ?
O1 C13 1.396(3) . ?
O1 C10 1.403(3) . ?
O2 C31 1.397(3) . ?
O2 C28 1.411(3) . ?
C1 C2 1.382(4) . ?
C1 C32 1.516(4) . ?
C2 C3 1.409(4) . ?
C3 C4 1.393(3) . ?
C4 C5 1.520(3) . ?
C5 C10 1.495(4) . ?
C5 C6 1.549(3) . ?
C5 C8 1.555(3) . ?
C6 C7 1.522(4) . ?
C8 C9 1.519(4) . ?
C10 C11 1.338(4) . ?
C11 C12 1.433(4) . ?
C12 C13 1.339(3) . ?
C13 C14 1.498(4) . ?
C14 C19 1.507(3) . ?
C14 C15 1.545(4) . ?
C14 C17 1.554(4) . ?
C15 C16 1.524(4) . ?
C17 C18 1.529(4) . ?
C19 C20 1.395(3) . ?
C20 C21 1.404(4) . ?
C21 C22 1.391(3) . ?
C22 C23 1.508(4) . ?
C23 C28 1.500(3) . ?
C23 C24 1.544(3) . ?
C23 C26 1.559(3) . ?
C24 C25 1.525(4) . ?
C26 C27 1.526(4) . ?
C28 C29 1.339(3) . ?
C29 C30 1.427(4) . ?
C30 C31 1.339(4) . ?
C31 C32 1.497(4) . ?
C32 C33 1.540(3) . ?
C32 C35 1.557(3) . ?
C33 C34 1.516(4) . ?
C35 C36 1.521(4) . ?
N3 Si1 1.716(2) . ?
N3 Si2 1.721(2) . ?
Si1 C38 1.877(3) . ?
Si1 C39 1.880(3) . ?
Si1 C37 1.887(3) . ?
Si2 C42 1.881(3) . ?
Si2 C41 1.881(3) . ?
Si2 C40 1.892(3) . ?

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
N3 Sm1 N1 125.57(7) . . ?
N3 Sm1 N2 126.72(7) . . ?
N1 Sm1 N2 107.70(6) . . ?
N3 Sm1 O2 119.29(6) . . ?
N1 Sm1 O2 71.14(6) . . ?
N2 Sm1 O2 76.19(6) . . ?
N3 Sm1 O1 119.13(7) . . ?
N1 Sm1 O1 75.66(6) . . ?
N2 Sm1 O1 70.02(6) . . ?
O2 Sm1 O1 121.58(5) . . ?
N3 Sm1 C1 103.55(8) . . ?
N1 Sm1 C1 29.70(7) . . ?
N2 Sm1 C1 126.01(7) . . ?
O2 Sm1 C1 61.51(7) . . ?
O1 Sm1 C1 104.20(6) . . ?
N3 Sm1 C19 104.45(7) . . ?
N1 Sm1 C19 125.53(7) . . ?
N2 Sm1 C19 29.38(7) . . ?
O2 Sm1 C19 104.30(7) . . ?
O1 Sm1 C19 60.82(6) . . ?
C1 Sm1 C19 151.99(7) . . ?
N3 Sm1 C22 109.64(7) . . ?
N1 Sm1 C22 119.54(7) . . ?
N2 Sm1 C22 29.33(7) . . ?
O2 Sm1 C22 61.06(7) . . ?
O1 Sm1 C22 99.20(6) . . ?
C1 Sm1 C22 122.12(8) . . ?
C19 Sm1 C22 46.80(8) . . ?
N3 Sm1 C4 108.33(8) . . ?
N1 Sm1 C4 29.16(7) . . ?
N2 Sm1 C4 118.98(7) . . ?
O2 Sm1 C4 100.14(6) . . ?
O1 Sm1 C4 60.85(6) . . ?
C1 Sm1 C4 47.02(7) . . ?
C19 Sm1 C4 121.32(7) . . ?
C22 Sm1 C4 142.03(7) . . ?
N3 Sm1 C2 78.09(7) . . ?
N1 Sm1 C2 48.31(7) . . ?
N2 Sm1 C2 154.13(7) . . ?
O2 Sm1 C2 85.15(7) . . ?
O1 Sm1 C2 106.40(6) . . ?
C1 Sm1 C2 28.43(7) . . ?
C19 Sm1 C2 166.75(7) . . ?
C22 Sm1 C2 145.09(8) . . ?
C4 Sm1 C2 46.68(7) . . ?
N3 Sm1 C20 78.91(7) . . ?
N1 Sm1 C20 153.93(7) . . ?
N2 Sm1 C20 48.48(7) . . ?
O2 Sm1 C20 106.66(7) . . ?
O1 Sm1 C20 84.53(6) . . ?
C1 Sm1 C20 167.74(8) . . ?
C19 Sm1 C20 28.56(7) . . ?
C22 Sm1 C20 46.83(8) . . ?
C4 Sm1 C20 144.04(7) . . ?
C2 Sm1 C20 157.00(7) . . ?
N3 Sm1 C21 82.27(7) . . ?
N1 Sm1 C21 147.42(7) . . ?
N2 Sm1 C21 48.17(6) . . ?
O2 Sm1 C21 80.60(6) . . ?
O1 Sm1 C21 107.39(6) . . ?
C1 Sm1 C21 139.65(8) . . ?
C19 Sm1 C21 46.57(7) . . ?
C22 Sm1 C21 28.35(7) . . ?
C4 Sm1 C21 166.79(7) . . ?
C2 Sm1 C21 145.98(7) . . ?
C20 Sm1 C21 28.18(7) . . ?
C4 N1 C1 105.9(2) . . ?
C4 N1 Sm1 80.40(14) . . ?
C1 N1 Sm1 78.54(13) . . ?
C19 N2 C22 105.65(19) . . ?
C19 N2 Sm1 79.25(14) . . ?
C22 N2 Sm1 79.98(14) . . ?
C13 O1 C10 106.68(18) . . ?
C13 O1 Sm1 118.83(14) . . ?
C10 O1 Sm1 117.24(14) . . ?
C31 O2 C28 106.34(19) . . ?
C31 O2 Sm1 118.00(14) . . ?
C28 O2 Sm1 117.65(14) . . ?
C2 C1 N1 110.1(2) . . ?
C2 C1 C32 130.5(2) . . ?
N1 C1 C32 119.1(2) . . ?
C2 C1 Sm1 81.09(16) . . ?
N1 C1 Sm1 71.76(14) . . ?
C32 C1 Sm1 118.18(16) . . ?
C1 C2 C3 107.1(2) . . ?
C1 C2 Sm1 70.49(15) . . ?
C3 C2 Sm1 77.02(15) . . ?
C4 C3 C2 106.0(2) . . ?
C4 C3 Sm1 70.95(14) . . ?
C2 C3 Sm1 74.72(15) . . ?
N1 C4 C3 110.7(2) . . ?
N1 C4 C5 118.9(2) . . ?
C3 C4 C5 130.1(2) . . ?
N1 C4 Sm1 70.44(13) . . ?
C3 C4 Sm1 80.73(14) . . ?
C5 C4 Sm1 119.82(16) . . ?
C10 C5 C4 109.0(2) . . ?
C10 C5 C6 110.0(2) . . ?
C4 C5 C6 110.8(2) . . ?
C10 C5 C8 107.7(2) . . ?
C4 C5 C8 108.4(2) . . ?
C6 C5 C8 110.9(2) . . ?
C7 C6 C5 115.1(2) . . ?
C9 C8 C5 115.0(2) . . ?
C11 C10 O1 108.8(2) . . ?
C11 C10 C5 135.7(2) . . ?
O1 C10 C5 115.2(2) . . ?
C10 C11 C12 107.8(2) . . ?
C13 C12 C11 107.6(2) . . ?
C12 C13 O1 109.1(2) . . ?
C12 C13 C14 136.4(3) . . ?
O1 C13 C14 114.5(2) . . ?
C13 C14 C19 107.0(2) . . ?
C13 C14 C15 111.5(2) . . ?
C19 C14 C15 110.5(2) . . ?
C13 C14 C17 107.1(2) . . ?
C19 C14 C17 109.2(2) . . ?
C15 C14 C17 111.4(2) . . ?
C16 C15 C14 114.9(2) . . ?
C18 C17 C14 114.9(2) . . ?
N2 C19 C20 110.9(2) . . ?
N2 C19 C14 118.3(2) . . ?
C20 C19 C14 130.5(2) . . ?
N2 C19 Sm1 71.37(13) . . ?
C20 C19 Sm1 80.71(15) . . ?
C14 C19 Sm1 119.22(16) . . ?
C19 C20 C21 105.9(2) . . ?
C19 C20 Sm1 70.73(14) . . ?
C21 C20 Sm1 76.24(15) . . ?
C22 C21 C20 107.1(2) . . ?
C22 C21 Sm1 71.20(14) . . ?
C20 C21 Sm1 75.58(15) . . ?
N2 C22 C21 110.3(2) . . ?
N2 C22 C23 118.3(2) . . ?
C21 C22 C23 131.1(2) . . ?
N2 C22 Sm1 70.69(13) . . ?
C21 C22 Sm1 80.45(15) . . ?
C23 C22 Sm1 120.14(16) . . ?
C28 C23 C22 109.6(2) . . ?
C28 C23 C24 106.8(2) . . ?
C22 C23 C24 107.9(2) . . ?
C28 C23 C26 110.5(2) . . ?
C22 C23 C26 110.6(2) . . ?
C24 C23 C26 111.4(2) . . ?
C25 C24 C23 114.5(2) . . ?
C27 C26 C23 115.3(2) . . ?
C29 C28 O2 108.8(2) . . ?
C29 C28 C23 135.6(3) . . ?
O2 C28 C23 115.6(2) . . ?
C28 C29 C30 107.8(2) . . ?
C31 C30 C29 107.9(2) . . ?
C30 C31 O2 109.1(2) . . ?
C30 C31 C32 136.8(3) . . ?
O2 C31 C32 114.0(2) . . ?
C31 C32 C1 106.9(2) . . ?
C31 C32 C33 110.1(2) . . ?
C1 C32 C33 111.7(2) . . ?
C31 C32 C35 108.6(2) . . ?
C1 C32 C35 108.0(2) . . ?
C33 C32 C35 111.4(2) . . ?
C34 C33 C32 114.4(2) . . ?
C36 C35 C32 114.6(2) . . ?
Si1 N3 Si2 118.22(12) . . ?
Si1 N3 Sm1 120.95(11) . . ?
Si2 N3 Sm1 120.75(10) . . ?
N3 Si1 C38 113.81(12) . . ?
N3 Si1 C39 114.55(12) . . ?
C38 Si1 C39 105.35(13) . . ?
N3 Si1 C37 111.47(11) . . ?
C38 Si1 C37 106.86(13) . . ?
C39 Si1 C37 104.00(13) . . ?
N3 Si2 C42 113.42(13) . . ?
N3 Si2 C41 114.03(12) . . ?
C42 Si2 C41 107.21(13) . . ?
N3 Si2 C40 112.74(11) . . ?
C42 Si2 C40 103.15(13) . . ?
C41 Si2 C40 105.38(13) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        28.30
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.095

data_smnnono
_database_code_depnum_ccdc_archive 'CCDC 256899'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52.50 H77 N3 Na O2 Si2 Sm'
_chemical_formula_weight         1011.69

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'
Sm Sm -0.1638 3.4418 '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'
Na Na 0.0362 0.0249 '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

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.87350(10)
_cell_length_b                   12.4181(2)
_cell_length_c                   18.6506(2)
_cell_angle_alpha                88.0740(6)
_cell_angle_beta                 89.2062(6)
_cell_angle_gamma                70.8546(4)
_cell_volume                     2596.38(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prismatic
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.40
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1060
_exptl_absorpt_coefficient_mu    1.226
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_reflns_number            52007
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_sigmaI/netI    0.0871
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         28.30
_reflns_number_total             12644
_reflns_number_gt                9343
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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 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^)+(0.0525P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12644
_refine_ls_number_parameters     569
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0424
_refine_ls_wR_factor_ref         0.1002
_refine_ls_wR_factor_gt          0.0915
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.583759(16) 0.641642(14) 0.744529(8) 0.01867(7) Uani 1 1 d . . .
Na1 Na 0.77775(10) 0.81552(10) 0.81218(5) 0.0159(3) Uani 1 1 d . . .
O1 O 0.8330(2) 0.6214(2) 0.69772(12) 0.0320(6) Uani 1 1 d . . .
O2 O 0.5097(2) 0.82588(18) 0.85594(11) 0.0218(5) Uani 1 1 d . . .
N1 N 0.6119(3) 0.8508(2) 0.70256(13) 0.0248(7) Uani 1 1 d . . .
N2 N 0.7471(3) 0.6117(2) 0.85960(14) 0.0260(7) Uani 1 1 d . . .
C1 C 0.4905(3) 0.8791(3) 0.71076(16) 0.0204(7) Uani 1 1 d . . .
C2 C 0.4437(3) 0.8309(3) 0.65802(17) 0.0252(8) Uani 1 1 d . . .
H2 H 0.3645 0.8350 0.6534 0.030 Uiso 1 1 calc R . .
C3 C 0.5393(3) 0.7743(3) 0.61255(17) 0.0290(9) Uani 1 1 d . . .
H3 H 0.5354 0.7341 0.5720 0.035 Uiso 1 1 calc R . .
C4 C 0.6396(3) 0.7903(3) 0.63996(16) 0.0262(8) Uani 1 1 d . . .
C5 C 0.7597(4) 0.7725(3) 0.60583(18) 0.0376(10) Uani 1 1 d . . .
C6 C 0.7736(4) 0.8905(4) 0.5882(2) 0.0447(11) Uani 1 1 d . . .
H6A H 0.7681 0.9307 0.6325 0.054 Uiso 1 1 calc R . .
H6B H 0.8524 0.8787 0.5682 0.054 Uiso 1 1 calc R . .
C7 C 0.6814(5) 0.9651(4) 0.5359(2) 0.0578(14) Uani 1 1 d . . .
H7A H 0.6959 1.0361 0.5273 0.087 Uiso 1 1 calc R . .
H7B H 0.6031 0.9795 0.5559 0.087 Uiso 1 1 calc R . .
H7C H 0.6870 0.9267 0.4915 0.087 Uiso 1 1 calc R . .
C8 C 0.7732(4) 0.7002(4) 0.5380(2) 0.0504(12) Uani 1 1 d . . .
H8A H 0.7612 0.6287 0.5517 0.061 Uiso 1 1 calc R . .
H8B H 0.7108 0.7404 0.5043 0.061 Uiso 1 1 calc R . .
C9 C 0.8935(6) 0.6739(5) 0.4999(3) 0.090(2) Uani 1 1 d . . .
H9A H 0.8940 0.6304 0.4583 0.134 Uiso 1 1 calc R . .
H9B H 0.9559 0.6309 0.5319 0.134 Uiso 1 1 calc R . .
H9C H 0.9062 0.7441 0.4856 0.134 Uiso 1 1 calc R . .
C10 C 0.8538(4) 0.7104(4) 0.6597(2) 0.0399(10) Uani 1 1 d . . .
C11 C 0.9573(4) 0.7216(4) 0.6814(3) 0.0534(12) Uani 1 1 d . . .
H11 H 0.9913 0.7752 0.6644 0.064 Uiso 1 1 calc R . .
C12 C 1.0045(4) 0.6347(4) 0.7358(3) 0.0611(14) Uani 1 1 d . . .
H12 H 1.0758 0.6209 0.7603 0.073 Uiso 1 1 calc R . .
C13 C 0.9271(3) 0.5765(4) 0.7450(2) 0.0399(10) Uani 1 1 d . . .
C14 C 0.9164(3) 0.4790(3) 0.7917(2) 0.0399(10) Uani 1 1 d . . .
C15 C 0.9442(4) 0.3691(3) 0.7482(2) 0.0472(12) Uani 1 1 d . . .
H15A H 0.9413 0.3072 0.7806 0.057 Uiso 1 1 calc R . .
H15B H 0.8819 0.3805 0.7128 0.057 Uiso 1 1 calc R . .
C16 C 1.0638(4) 0.3330(4) 0.7099(3) 0.0699(16) Uani 1 1 d . . .
H16A H 1.0735 0.2645 0.6846 0.105 Uiso 1 1 calc R . .
H16B H 1.1266 0.3192 0.7445 0.105 Uiso 1 1 calc R . .
H16C H 1.0671 0.3925 0.6766 0.105 Uiso 1 1 calc R . .
C17 C 1.0072(4) 0.4596(4) 0.8545(2) 0.0588(14) Uani 1 1 d . . .
H17A H 1.0869 0.4404 0.8345 0.071 Uiso 1 1 calc R . .
H17B H 0.9910 0.5307 0.8792 0.071 Uiso 1 1 calc R . .
C18 C 1.0046(5) 0.3691(5) 0.9077(3) 0.0775(18) Uani 1 1 d . . .
H18A H 1.0619 0.3634 0.9447 0.116 Uiso 1 1 calc R . .
H18B H 1.0238 0.2976 0.8843 0.116 Uiso 1 1 calc R . .
H18C H 0.9264 0.3878 0.9285 0.116 Uiso 1 1 calc R . .
C19 C 0.7930(3) 0.5110(3) 0.82313(18) 0.0285(8) Uani 1 1 d . . .
C20 C 0.7185(3) 0.4462(3) 0.83083(18) 0.0299(9) Uani 1 1 d . . .
H20 H 0.7286 0.3764 0.8103 0.036 Uiso 1 1 calc R . .
C21 C 0.6240(3) 0.5065(3) 0.87592(16) 0.0256(8) Uani 1 1 d . . .
H21 H 0.5592 0.4849 0.8906 0.031 Uiso 1 1 calc R . .
C22 C 0.6475(3) 0.6041(3) 0.89377(16) 0.0226(8) Uani 1 1 d . . .
C23 C 0.5886(3) 0.6897(3) 0.95120(16) 0.0250(8) Uani 1 1 d . . .
C24 C 0.6760(4) 0.6677(3) 1.01549(17) 0.0326(9) Uani 1 1 d . . .
H24A H 0.7491 0.6794 0.9991 0.039 Uiso 1 1 calc R . .
H24B H 0.6408 0.7232 1.0517 0.039 Uiso 1 1 calc R . .
C25 C 0.7064(4) 0.5494(4) 1.0495(2) 0.0467(12) Uani 1 1 d . . .
H25A H 0.7608 0.5417 1.0885 0.070 Uiso 1 1 calc R . .
H25B H 0.7428 0.4937 1.0143 0.070 Uiso 1 1 calc R . .
H25C H 0.6349 0.5377 1.0673 0.070 Uiso 1 1 calc R . .
C26 C 0.4684(3) 0.6769(3) 0.97379(17) 0.0287(8) Uani 1 1 d . . .
H26A H 0.4180 0.6903 0.9317 0.034 Uiso 1 1 calc R . .
H26B H 0.4826 0.5986 0.9903 0.034 Uiso 1 1 calc R . .
C27 C 0.4003(4) 0.7557(3) 1.03232(19) 0.0422(11) Uani 1 1 d . . .
H27A H 0.3272 0.7411 1.0427 0.063 Uiso 1 1 calc R . .
H27B H 0.3828 0.8337 1.0161 0.063 Uiso 1 1 calc R . .
H27C H 0.4481 0.7421 1.0749 0.063 Uiso 1 1 calc R . .
C28 C 0.5683(3) 0.8063(3) 0.92090(16) 0.0250(8) Uani 1 1 d . . .
C29 C 0.5898(4) 0.9017(3) 0.93906(18) 0.0327(9) Uani 1 1 d . . .
H29 H 0.6285 0.9115 0.9801 0.039 Uiso 1 1 calc R . .
C30 C 0.5412(4) 0.9856(3) 0.88252(18) 0.0326(9) Uani 1 1 d . . .
H30 H 0.5420 1.0603 0.8805 0.039 Uiso 1 1 calc R . .
C31 C 0.4946(3) 0.9362(3) 0.83361(17) 0.0253(8) Uani 1 1 d . . .
C32 C 0.4286(3) 0.9685(3) 0.76434(18) 0.0263(8) Uani 1 1 d . . .
C33 C 0.4363(4) 1.0853(3) 0.7367(2) 0.0381(10) Uani 1 1 d . . .
H33A H 0.3978 1.1427 0.7712 0.046 Uiso 1 1 calc R . .
H33B H 0.5195 1.0802 0.7336 0.046 Uiso 1 1 calc R . .
C34 C 0.3783(4) 1.1232(3) 0.6635(2) 0.0486(12) Uani 1 1 d . . .
H34A H 0.3853 1.1958 0.6494 0.073 Uiso 1 1 calc R . .
H34B H 0.2955 1.1296 0.6662 0.073 Uiso 1 1 calc R . .
H34C H 0.4175 1.0679 0.6286 0.073 Uiso 1 1 calc R . .
C35 C 0.2974(3) 0.9734(3) 0.7772(2) 0.0375(10) Uani 1 1 d . . .
H35A H 0.2544 0.9953 0.7323 0.045 Uiso 1 1 calc R . .
H35B H 0.2971 0.8975 0.7909 0.045 Uiso 1 1 calc R . .
C36 C 0.2309(4) 1.0549(4) 0.8340(3) 0.0668(15) Uani 1 1 d . . .
H36A H 0.1512 1.0522 0.8385 0.100 Uiso 1 1 calc R . .
H36B H 0.2281 1.1310 0.8204 0.100 Uiso 1 1 calc R . .
H36C H 0.2713 1.0331 0.8791 0.100 Uiso 1 1 calc R . .
N3 N 0.5488(2) 0.5011(2) 0.68087(13) 0.0218(6) Uani 1 1 d . . .
Si1 Si 0.40202(9) 0.52919(8) 0.70806(5) 0.0237(2) Uani 1 1 d . . .
C37 C 0.3794(3) 0.6434(3) 0.77138(17) 0.0246(8) Uani 1 1 d . . .
H37A H 0.3678 0.6212 0.8206 0.030 Uiso 1 1 calc R . .
H37B H 0.3180 0.7139 0.7571 0.030 Uiso 1 1 calc R . .
C38 C 0.3791(4) 0.3987(3) 0.7516(2) 0.0437(10) Uani 1 1 d . . .
H38A H 0.3921 0.3406 0.7168 0.066 Uiso 1 1 calc R . .
H38B H 0.2990 0.4181 0.7698 0.066 Uiso 1 1 calc R . .
H38C H 0.4344 0.3710 0.7904 0.066 Uiso 1 1 calc R . .
C39 C 0.2953(3) 0.5743(4) 0.63031(19) 0.0437(11) Uani 1 1 d . . .
H39A H 0.3102 0.5125 0.5981 0.065 Uiso 1 1 calc R . .
H39B H 0.3065 0.6390 0.6054 0.065 Uiso 1 1 calc R . .
H39C H 0.2149 0.5944 0.6479 0.065 Uiso 1 1 calc R . .
Si2 Si 0.62500(9) 0.38782(8) 0.63059(5) 0.0273(2) Uani 1 1 d . . .
C40 C 0.6912(4) 0.2519(3) 0.6857(2) 0.0381(10) Uani 1 1 d . . .
H40A H 0.6292 0.2352 0.7127 0.057 Uiso 1 1 calc R . .
H40B H 0.7495 0.2610 0.7179 0.057 Uiso 1 1 calc R . .
H40C H 0.7285 0.1903 0.6544 0.057 Uiso 1 1 calc R . .
C41 C 0.5342(4) 0.3476(3) 0.56102(19) 0.0384(10) Uani 1 1 d . . .
H41A H 0.4680 0.3320 0.5838 0.058 Uiso 1 1 calc R . .
H41B H 0.5831 0.2809 0.5373 0.058 Uiso 1 1 calc R . .
H41C H 0.5053 0.4095 0.5265 0.058 Uiso 1 1 calc R . .
C42 C 0.7508(4) 0.4139(3) 0.5789(2) 0.0377(10) Uani 1 1 d . . .
H42A H 0.8015 0.4354 0.6112 0.056 Uiso 1 1 calc R . .
H42B H 0.7192 0.4741 0.5437 0.056 Uiso 1 1 calc R . .
H42C H 0.7962 0.3455 0.5554 0.056 Uiso 1 1 calc R . .
C43 C 1.1269(7) 0.7573(6) 0.9054(4) 0.117(3) Uani 1 1 d . . .
H43A H 1.1098 0.7275 0.9509 0.175 Uiso 1 1 calc R . .
H43B H 1.1971 0.7789 0.9094 0.175 Uiso 1 1 calc R . .
H43C H 1.1399 0.7001 0.8700 0.175 Uiso 1 1 calc R . .
C44 C 1.0298(5) 0.8537(5) 0.8846(4) 0.0766(18) Uani 1 1 d . . .
C45 C 0.9442(6) 0.9072(5) 0.9392(3) 0.0792(17) Uani 1 1 d . . .
H45 H 0.9506 0.8787 0.9862 0.095 Uiso 1 1 calc R . .
C46 C 0.8564(6) 0.9990(6) 0.9182(4) 0.097(2) Uani 1 1 d . . .
H46 H 0.7996 1.0347 0.9522 0.116 Uiso 1 1 calc R . .
C47 C 0.8421(6) 1.0475(6) 0.8471(4) 0.097(2) Uani 1 1 d . . .
H47 H 0.7802 1.1146 0.8366 0.116 Uiso 1 1 calc R . .
C48 C 0.9171(6) 0.9966(6) 0.7968(4) 0.0871(19) Uani 1 1 d . . .
H48 H 0.9063 1.0233 0.7494 0.104 Uiso 1 1 calc R . .
C49 C 1.0170(5) 0.8979(5) 0.8173(3) 0.0689(15) Uani 1 1 d . . .
H49 H 1.0740 0.8640 0.7829 0.083 Uiso 1 1 calc R . .
C65 C 1.0836(8) 0.9804(9) 0.6052(4) 0.114(3) Uani 1 1 d . . .
C66 C 1.0337(10) 0.9927(9) 0.5342(6) 0.061(3) Uani 0.50 1 d P . .
C63 C 0.9378(5) 1.0896(4) 0.5163(4) 0.0623(14) Uani 1 1 d . . .
C67 C 0.8849(8) 1.1140(11) 0.4537(8) 0.084(4) Uani 0.50 1 d P . .
C68 C 0.9821(12) 1.0830(12) 0.5772(7) 0.079(4) Uani 0.50 1 d P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sm1 0.02193(11) 0.01681(10) 0.01783(9) -0.00183(6) -0.00205(6) -0.00691(7)
Na1 0.0146(7) 0.0220(7) 0.0105(5) -0.0027(5) 0.0052(5) -0.0053(5)
O1 0.0258(15) 0.0396(15) 0.0353(14) -0.0134(11) 0.0054(11) -0.0162(13)
O2 0.0307(15) 0.0178(12) 0.0201(11) -0.0023(9) 0.0003(10) -0.0121(11)
N1 0.037(2) 0.0268(16) 0.0186(14) 0.0010(11) -0.0010(12) -0.0212(14)
N2 0.0255(18) 0.0273(16) 0.0267(15) -0.0020(12) -0.0110(13) -0.0098(14)
C1 0.024(2) 0.0168(17) 0.0242(17) 0.0091(13) -0.0041(14) -0.0131(15)
C2 0.029(2) 0.0223(18) 0.0273(18) 0.0075(14) -0.0105(15) -0.0133(16)
C3 0.050(3) 0.031(2) 0.0156(16) 0.0033(14) -0.0064(16) -0.0270(19)
C4 0.038(2) 0.034(2) 0.0158(16) -0.0014(14) 0.0026(15) -0.0234(18)
C5 0.050(3) 0.049(2) 0.0261(19) -0.0125(17) 0.0143(18) -0.032(2)
C6 0.060(3) 0.058(3) 0.035(2) -0.0111(19) 0.021(2) -0.044(3)
C7 0.088(4) 0.063(3) 0.041(2) 0.006(2) 0.003(2) -0.052(3)
C8 0.080(4) 0.056(3) 0.031(2) -0.0183(19) 0.023(2) -0.043(3)
C9 0.124(6) 0.097(5) 0.071(4) -0.052(3) 0.065(4) -0.064(4)
C10 0.037(3) 0.047(3) 0.046(2) -0.0195(19) 0.0230(19) -0.027(2)
C11 0.033(3) 0.060(3) 0.075(3) -0.015(3) 0.011(2) -0.025(2)
C12 0.021(3) 0.072(4) 0.096(4) -0.034(3) 0.002(2) -0.019(3)
C13 0.018(2) 0.047(3) 0.053(2) -0.022(2) 0.0022(18) -0.0070(19)
C14 0.022(2) 0.044(2) 0.048(2) -0.0177(19) -0.0122(18) 0.0002(19)
C15 0.038(3) 0.036(2) 0.056(3) -0.016(2) -0.019(2) 0.006(2)
C16 0.039(3) 0.072(4) 0.082(4) -0.044(3) -0.004(3) 0.010(3)
C17 0.026(3) 0.076(4) 0.060(3) -0.026(3) -0.023(2) 0.007(2)
C18 0.066(4) 0.079(4) 0.064(3) -0.011(3) -0.043(3) 0.012(3)
C19 0.023(2) 0.0252(19) 0.0336(19) -0.0052(15) -0.0134(15) -0.0028(17)
C20 0.039(2) 0.0179(18) 0.0297(19) 0.0032(14) -0.0169(17) -0.0045(17)
C21 0.037(2) 0.0208(18) 0.0209(17) 0.0070(14) -0.0094(15) -0.0118(17)
C22 0.029(2) 0.0239(18) 0.0171(16) 0.0053(13) -0.0091(14) -0.0124(16)
C23 0.038(2) 0.0296(19) 0.0154(16) -0.0003(13) -0.0035(14) -0.0211(18)
C24 0.045(3) 0.042(2) 0.0204(17) -0.0012(15) -0.0083(16) -0.026(2)
C25 0.066(3) 0.059(3) 0.029(2) 0.0168(19) -0.027(2) -0.040(3)
C26 0.042(2) 0.031(2) 0.0202(17) -0.0011(14) -0.0013(15) -0.0213(18)
C27 0.062(3) 0.046(2) 0.029(2) -0.0116(17) 0.0126(19) -0.031(2)
C28 0.033(2) 0.0295(19) 0.0169(16) -0.0057(14) 0.0030(14) -0.0152(17)
C29 0.051(3) 0.032(2) 0.0228(18) -0.0073(15) 0.0011(16) -0.0222(19)
C30 0.051(3) 0.0221(19) 0.033(2) -0.0091(15) 0.0080(17) -0.0216(19)
C31 0.030(2) 0.0175(17) 0.0305(18) -0.0048(14) 0.0087(15) -0.0101(16)
C32 0.032(2) 0.0154(17) 0.0323(19) 0.0017(14) -0.0027(15) -0.0085(16)
C33 0.057(3) 0.0166(19) 0.044(2) 0.0038(16) -0.0063(19) -0.0172(19)
C34 0.074(4) 0.023(2) 0.050(2) 0.0145(18) -0.018(2) -0.019(2)
C35 0.033(2) 0.023(2) 0.055(2) -0.0036(17) -0.0056(19) -0.0066(18)
C36 0.039(3) 0.046(3) 0.113(4) -0.041(3) 0.018(3) -0.007(2)
N3 0.0227(17) 0.0197(15) 0.0230(14) -0.0036(11) -0.0061(12) -0.0063(13)
Si1 0.0262(6) 0.0248(5) 0.0240(5) -0.0039(4) -0.0044(4) -0.0131(4)
C37 0.032(2) 0.0204(18) 0.0222(17) 0.0021(13) -0.0037(15) -0.0104(16)
C38 0.056(3) 0.036(2) 0.050(2) -0.0052(18) 0.006(2) -0.030(2)
C39 0.023(2) 0.070(3) 0.033(2) -0.011(2) -0.0042(16) -0.006(2)
Si2 0.0323(6) 0.0192(5) 0.0286(5) -0.0074(4) -0.0063(4) -0.0051(4)
C40 0.046(3) 0.022(2) 0.042(2) -0.0085(16) -0.0082(19) -0.0049(19)
C41 0.051(3) 0.033(2) 0.033(2) -0.0095(16) -0.0089(18) -0.013(2)
C42 0.040(3) 0.031(2) 0.038(2) -0.0106(17) -0.0002(18) -0.0048(19)
C43 0.129(7) 0.109(6) 0.114(6) -0.006(5) -0.015(5) -0.040(6)
C44 0.064(4) 0.056(3) 0.115(5) 0.017(3) -0.047(4) -0.027(3)
C45 0.067(4) 0.082(4) 0.084(4) -0.019(3) 0.006(3) -0.018(4)
C46 0.070(5) 0.085(5) 0.117(5) 0.015(4) -0.018(4) -0.001(4)
C47 0.071(5) 0.066(4) 0.142(7) 0.013(4) -0.027(5) -0.006(4)
C48 0.081(5) 0.082(5) 0.098(5) -0.008(4) -0.010(4) -0.026(4)
C49 0.061(4) 0.066(4) 0.086(4) -0.013(3) 0.000(3) -0.028(3)
C65 0.100(6) 0.191(9) 0.084(5) 0.034(5) -0.010(4) -0.097(6)
C66 0.052(7) 0.052(6) 0.090(8) -0.005(6) 0.032(6) -0.032(6)
C63 0.048(4) 0.044(3) 0.100(4) -0.007(3) 0.030(3) -0.022(3)
C67 0.015(5) 0.087(9) 0.144(12) 0.077(9) -0.004(6) -0.015(6)
C68 0.076(9) 0.118(11) 0.075(8) -0.034(8) 0.028(7) -0.073(9)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 N3 2.292(2) . ?
Sm1 C37 2.464(4) . ?
Sm1 N1 2.810(3) . ?
Sm1 C1 2.841(3) . ?
Sm1 N2 2.845(3) . ?
Sm1 C2 2.855(3) . ?
Sm1 C4 2.859(3) . ?
Sm1 C3 2.871(3) . ?
Sm1 C19 2.873(3) . ?
Sm1 C22 2.877(3) . ?
Sm1 C21 2.878(3) . ?
Sm1 C20 2.882(3) . ?
Na1 N1 2.782(3) . ?
Na1 N2 2.787(3) . ?
O1 C10 1.381(5) . ?
O1 C13 1.386(5) . ?
O2 C31 1.374(4) . ?
O2 C28 1.380(4) . ?
N1 C1 1.374(4) . ?
N1 C4 1.387(4) . ?
N2 C22 1.365(4) . ?
N2 C19 1.387(4) . ?
C1 C2 1.382(4) . ?
C1 C32 1.514(5) . ?
C2 C3 1.412(5) . ?
C3 C4 1.377(5) . ?
C4 C5 1.505(5) . ?
C5 C10 1.506(6) . ?
C5 C6 1.551(5) . ?
C5 C8 1.553(5) . ?
C6 C7 1.520(6) . ?
C8 C9 1.527(6) . ?
C10 C11 1.350(6) . ?
C11 C12 1.433(7) . ?
C12 C13 1.348(6) . ?
C13 C14 1.506(6) . ?
C14 C19 1.502(5) . ?
C14 C15 1.550(5) . ?
C14 C17 1.561(5) . ?
C15 C16 1.518(6) . ?
C17 C18 1.481(7) . ?
C19 C20 1.381(5) . ?
C20 C21 1.411(5) . ?
C21 C22 1.382(5) . ?
C22 C23 1.527(5) . ?
C23 C28 1.482(5) . ?
C23 C26 1.538(5) . ?
C23 C24 1.554(4) . ?
C24 C25 1.512(5) . ?
C26 C27 1.527(5) . ?
C28 C29 1.345(5) . ?
C29 C30 1.442(5) . ?
C30 C31 1.337(5) . ?
C31 C32 1.494(5) . ?
C32 C33 1.552(5) . ?
C32 C35 1.555(5) . ?
C33 C34 1.528(5) . ?
C35 C36 1.514(5) . ?
N3 Si2 1.705(3) . ?
N3 Si1 1.734(3) . ?
Si1 C37 1.825(3) . ?
Si1 C39 1.885(4) . ?
Si1 C38 1.885(4) . ?
Si2 C42 1.877(4) . ?
Si2 C41 1.879(4) . ?
Si2 C40 1.886(4) . ?
C43 C44 1.410(8) . ?
C44 C49 1.344(7) . ?
C44 C45 1.443(8) . ?
C45 C46 1.321(8) . ?
C46 C47 1.425(9) . ?
C47 C48 1.312(8) . ?
C48 C49 1.442(8) . ?
C65 C66 1.441(12) . ?
C65 C68 1.521(16) . ?
C65 C67 1.583(17) 2_776 ?
C66 C68 1.368(15) . ?
C66 C63 1.368(11) 2_776 ?
C66 C67 1.374(15) 2_776 ?
C66 C63 1.393(12) . ?
C66 C66 1.49(2) 2_776 ?
C63 C68 1.247(13) . ?
C63 C67 1.311(13) . ?
C63 C66 1.368(11) 2_776 ?
C67 C66 1.374(15) 2_776 ?
C67 C65 1.583(17) 2_776 ?

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
N3 Sm1 C37 71.77(10) . . ?
N3 Sm1 N1 132.42(8) . . ?
C37 Sm1 N1 116.95(10) . . ?
N3 Sm1 C1 125.32(9) . . ?
C37 Sm1 C1 88.83(10) . . ?
N1 Sm1 C1 28.14(9) . . ?
N3 Sm1 N2 126.93(9) . . ?
C37 Sm1 N2 118.95(10) . . ?
N1 Sm1 N2 91.44(8) . . ?
C1 Sm1 N2 107.37(8) . . ?
N3 Sm1 C2 97.25(9) . . ?
C37 Sm1 C2 77.87(11) . . ?
N1 Sm1 C2 47.09(9) . . ?
C1 Sm1 C2 28.07(9) . . ?
N2 Sm1 C2 135.25(9) . . ?
N3 Sm1 C4 105.67(9) . . ?
C37 Sm1 C4 123.71(11) . . ?
N1 Sm1 C4 28.30(8) . . ?
C1 Sm1 C4 45.44(10) . . ?
N2 Sm1 C4 106.92(9) . . ?
C2 Sm1 C4 46.08(11) . . ?
N3 Sm1 C3 86.12(9) . . ?
C37 Sm1 C3 99.17(11) . . ?
N1 Sm1 C3 47.05(8) . . ?
C1 Sm1 C3 46.18(9) . . ?
N2 Sm1 C3 134.62(9) . . ?
C2 Sm1 C3 28.55(10) . . ?
C4 Sm1 C3 27.81(10) . . ?
N3 Sm1 C19 100.60(9) . . ?
C37 Sm1 C19 125.19(11) . . ?
N1 Sm1 C19 107.62(9) . . ?
C1 Sm1 C19 130.79(10) . . ?
N2 Sm1 C19 28.08(8) . . ?
C2 Sm1 C19 154.43(11) . . ?
C4 Sm1 C19 110.76(11) . . ?
C3 Sm1 C19 135.16(11) . . ?
N3 Sm1 C22 120.51(9) . . ?
C37 Sm1 C22 91.37(10) . . ?
N1 Sm1 C22 106.40(8) . . ?
C1 Sm1 C22 110.24(9) . . ?
N2 Sm1 C22 27.59(9) . . ?
C2 Sm1 C22 135.35(9) . . ?
C4 Sm1 C22 129.41(9) . . ?
C3 Sm1 C22 153.33(9) . . ?
C19 Sm1 C22 44.74(10) . . ?
N3 Sm1 C21 92.80(9) . . ?
C37 Sm1 C21 79.72(11) . . ?
N1 Sm1 C21 134.14(8) . . ?
C1 Sm1 C21 134.35(9) . . ?
N2 Sm1 C21 46.73(9) . . ?
C2 Sm1 C21 151.11(11) . . ?
C4 Sm1 C21 153.52(10) . . ?
C3 Sm1 C21 178.65(10) . . ?
C19 Sm1 C21 45.84(11) . . ?
C22 Sm1 C21 27.80(9) . . ?
N3 Sm1 C20 80.92(9) . . ?
C37 Sm1 C20 100.28(11) . . ?
N1 Sm1 C20 135.14(10) . . ?
C1 Sm1 C20 153.74(9) . . ?
N2 Sm1 C20 46.76(9) . . ?
C2 Sm1 C20 177.76(10) . . ?
C4 Sm1 C20 135.61(11) . . ?
C3 Sm1 C20 151.87(11) . . ?
C19 Sm1 C20 27.77(10) . . ?
C22 Sm1 C20 45.59(10) . . ?
C21 Sm1 C20 28.36(10) . . ?
N1 Na1 N2 93.30(8) . . ?
N1 Na1 Sm1 46.31(6) . . ?
N2 Na1 Sm1 47.03(5) . . ?
C10 O1 C13 107.2(3) . . ?
C10 O1 Sm1 119.8(2) . . ?
C13 O1 Sm1 119.9(2) . . ?
C31 O2 C28 107.9(2) . . ?
C31 O2 Sm1 117.96(17) . . ?
C28 O2 Sm1 118.78(18) . . ?
C1 N1 C4 105.8(3) . . ?
C1 N1 Na1 126.25(19) . . ?
C4 N1 Na1 121.2(2) . . ?
C1 N1 Sm1 77.19(17) . . ?
C4 N1 Sm1 77.81(18) . . ?
Na1 N1 Sm1 87.99(8) . . ?
C22 N2 C19 105.3(3) . . ?
C22 N2 Na1 124.4(2) . . ?
C19 N2 Na1 122.8(2) . . ?
C22 N2 Sm1 77.50(17) . . ?
C19 N2 Sm1 77.07(17) . . ?
Na1 N2 Sm1 87.20(8) . . ?
N1 C1 C2 110.5(3) . . ?
N1 C1 C32 118.4(3) . . ?
C2 C1 C32 130.3(3) . . ?
N1 C1 Sm1 74.67(17) . . ?
C2 C1 Sm1 76.52(18) . . ?
C32 C1 Sm1 124.1(2) . . ?
C1 C2 C3 106.7(3) . . ?
C1 C2 Sm1 75.41(18) . . ?
C3 C2 Sm1 76.37(19) . . ?
C4 C3 C2 106.6(3) . . ?
C4 C3 Sm1 75.60(19) . . ?
C2 C3 Sm1 75.08(18) . . ?
C3 C4 N1 110.3(3) . . ?
C3 C4 C5 129.8(3) . . ?
N1 C4 C5 118.7(3) . . ?
C3 C4 Sm1 76.59(19) . . ?
N1 C4 Sm1 73.89(17) . . ?
C5 C4 Sm1 126.0(2) . . ?
C4 C5 C10 108.0(3) . . ?
C4 C5 C6 109.0(3) . . ?
C10 C5 C6 108.1(3) . . ?
C4 C5 C8 110.1(3) . . ?
C10 C5 C8 109.6(4) . . ?
C6 C5 C8 112.0(3) . . ?
C7 C6 C5 114.2(3) . . ?
C9 C8 C5 114.7(4) . . ?
C11 C10 O1 109.7(4) . . ?
C11 C10 C5 134.7(4) . . ?
O1 C10 C5 115.6(3) . . ?
C10 C11 C12 106.5(4) . . ?
C13 C12 C11 107.7(4) . . ?
C12 C13 O1 108.8(4) . . ?
C12 C13 C14 137.5(4) . . ?
O1 C13 C14 113.7(3) . . ?
C19 C14 C13 109.4(3) . . ?
C19 C14 C15 110.6(3) . . ?
C13 C14 C15 110.8(3) . . ?
C19 C14 C17 108.3(3) . . ?
C13 C14 C17 107.7(4) . . ?
C15 C14 C17 110.0(3) . . ?
C16 C15 C14 115.2(4) . . ?
C18 C17 C14 114.7(4) . . ?
C20 C19 N2 110.4(3) . . ?
C20 C19 C14 129.1(3) . . ?
N2 C19 C14 119.8(3) . . ?
C20 C19 Sm1 76.46(19) . . ?
N2 C19 Sm1 74.86(18) . . ?
C14 C19 Sm1 122.9(2) . . ?
C19 C20 C21 106.7(3) . . ?
C19 C20 Sm1 75.77(19) . . ?
C21 C20 Sm1 75.67(18) . . ?
C22 C21 C20 106.0(3) . . ?
C22 C21 Sm1 76.07(18) . . ?
C20 C21 Sm1 75.97(18) . . ?
N2 C22 C21 111.4(3) . . ?
N2 C22 C23 119.1(3) . . ?
C21 C22 C23 128.9(3) . . ?
N2 C22 Sm1 74.91(16) . . ?
C21 C22 Sm1 76.13(17) . . ?
C23 C22 Sm1 123.0(2) . . ?
C28 C23 C22 108.5(3) . . ?
C28 C23 C26 109.4(3) . . ?
C22 C23 C26 110.0(3) . . ?
C28 C23 C24 109.2(3) . . ?
C22 C23 C24 107.9(3) . . ?
C26 C23 C24 111.8(3) . . ?
C25 C24 C23 114.0(3) . . ?
C27 C26 C23 115.8(3) . . ?
C29 C28 O2 109.0(3) . . ?
C29 C28 C23 138.0(3) . . ?
O2 C28 C23 113.0(3) . . ?
C28 C29 C30 106.7(3) . . ?
C31 C30 C29 107.3(3) . . ?
C30 C31 O2 109.1(3) . . ?
C30 C31 C32 138.0(3) . . ?
O2 C31 C32 112.8(3) . . ?
C31 C32 C1 107.6(3) . . ?
C31 C32 C33 108.8(3) . . ?
C1 C32 C33 108.5(3) . . ?
C31 C32 C35 108.6(3) . . ?
C1 C32 C35 111.4(3) . . ?
C33 C32 C35 111.8(3) . . ?
C34 C33 C32 113.3(3) . . ?
C36 C35 C32 115.1(3) . . ?
Si2 N3 Si1 123.72(16) . . ?
Si2 N3 Sm1 139.41(16) . . ?
Si1 N3 Sm1 96.43(11) . . ?
N3 Si1 C37 103.30(15) . . ?
N3 Si1 C39 111.96(15) . . ?
C37 Si1 C39 111.82(17) . . ?
N3 Si1 C38 111.12(17) . . ?
C37 Si1 C38 111.88(16) . . ?
C39 Si1 C38 106.9(2) . . ?
N3 Si1 Sm1 48.86(8) . . ?
C37 Si1 Sm1 54.52(11) . . ?
C39 Si1 Sm1 124.54(15) . . ?
C38 Si1 Sm1 128.46(14) . . ?
Si1 C37 Sm1 88.38(14) . . ?
N3 Si2 C42 112.23(15) . . ?
N3 Si2 C41 115.28(16) . . ?
C42 Si2 C41 104.63(18) . . ?
N3 Si2 C40 113.19(15) . . ?
C42 Si2 C40 106.91(18) . . ?
C41 Si2 C40 103.75(17) . . ?
C49 C44 C43 122.4(7) . . ?
C49 C44 C45 120.0(6) . . ?
C43 C44 C45 117.6(6) . . ?
C46 C45 C44 115.9(6) . . ?
C45 C46 C47 124.8(7) . . ?
C48 C47 C46 119.4(6) . . ?
C47 C48 C49 118.0(6) . . ?
C44 C49 C48 121.8(6) . . ?
C66 C65 C68 54.9(6) . . ?
C66 C65 C67 53.8(6) . 2_776 ?
C68 C65 C67 108.4(7) . 2_776 ?
C68 C66 C63 167.6(12) . 2_776 ?
C68 C66 C67 133.5(13) . 2_776 ?
C63 C66 C67 57.1(8) 2_776 2_776 ?
C68 C66 C63 53.7(8) . . ?
C63 C66 C63 114.8(9) 2_776 . ?
C67 C66 C63 168.9(11) 2_776 . ?
C68 C66 C65 65.5(8) . . ?
C63 C66 C65 125.5(10) 2_776 . ?
C67 C66 C65 68.4(9) 2_776 . ?
C63 C66 C65 119.2(9) . . ?
C68 C66 C66 110.1(14) . 2_776 ?
C63 C66 C66 58.2(7) 2_776 2_776 ?
C67 C66 C66 114.8(13) 2_776 2_776 ?
C63 C66 C66 56.6(8) . 2_776 ?
C65 C66 C66 172.1(12) . 2_776 ?
C68 C63 C67 170.9(10) . . ?
C68 C63 C66 127.2(10) . 2_776 ?
C67 C63 C66 61.6(8) . 2_776 ?
C68 C63 C66 62.2(8) . . ?
C67 C63 C66 126.2(9) . . ?
C66 C63 C66 65.2(9) 2_776 . ?
C63 C67 C66 61.2(7) . 2_776 ?
C63 C67 C65 119.0(9) . 2_776 ?
C66 C67 C65 57.8(8) 2_776 2_776 ?
C63 C68 C66 64.1(7) . . ?
C63 C68 C65 123.6(10) . . ?
C66 C68 C65 59.5(8) . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        28.30
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         1.665
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.112