# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_li0003
_audit_block_doi                 10.5517/ccdc.csd.cc1lfl1n
_database_code_depnum_ccdc_archive 'CCDC 1472811'
_audit_update_record             
;
2016-04-07 deposited with the CCDC.
2016-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C90 H154 B2 N20 S4 Yb2, 2(C5 H12)'
_chemical_formula_sum            'C100 H178 B2 N20 S4 Yb2'
_chemical_formula_weight         2156.55

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'
B B 0.0013 0.0007 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   21.7535(5)
_cell_length_b                   17.0849(5)
_cell_length_c                   16.4796(4)
_cell_angle_alpha                90
_cell_angle_beta                 112.597(2)
_cell_angle_gamma                90
_cell_volume                     5654.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    19624
_cell_measurement_theta_min      1.954
_cell_measurement_theta_max      26.138

_exptl_crystal_description       rod
_exptl_crystal_colour            rose
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_F_000             2264
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    1.768
_shelx_estimated_absorpt_T_min   0.843
_shelx_estimated_absorpt_T_max   0.843
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6344
_exptl_absorpt_correction_T_max  0.8078
_exptl_absorpt_process_details   'X-Area and X-Red (STOE & Cie, 1999)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19624
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.954
_diffrn_reflns_theta_max         26.138
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             11252
_reflns_number_gt                10767
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.929
_reflns_Friedel_fraction_max     0.994
_reflns_Friedel_fraction_full    0.997

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'X-Area (STOE & Cie, 1999)'
_computing_cell_refinement       'X-Area (STOE & Cie, 1999)'
_computing_data_reduction        'X-Area and X-Red (STOE & Cie, 1999)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond (Brandenburg, 1997)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1169P)²+4.2180P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.011(14)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         11252
_refine_ls_number_parameters     614
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0352
_refine_ls_wR_factor_ref         0.1398
_refine_ls_wR_factor_gt          0.1153
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.064
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8353(5) 0.5178(6) 0.2258(6) 0.037(2) Uani 1 1 d . . . . .
C2 C 0.8066(5) 0.5700(6) 0.1555(6) 0.039(2) Uani 1 1 d . . . . .
H2 H 0.8087 0.6256 0.1575 0.046 Uiso 1 1 calc R U . . .
C3 C 0.7747(5) 0.5239(5) 0.0834(6) 0.0323(18) Uani 1 1 d . . . . .
C4 C 0.7296(5) 0.5489(5) -0.0079(6) 0.0360(19) Uani 1 1 d . . . . .
H3 H 0.7354 0.5112 -0.0509 0.043 Uiso 1 1 calc R U . . .
C5 C 0.6579(5) 0.5449(7) -0.0164(7) 0.047(2) Uani 1 1 d . . . . .
H6 H 0.6286 0.5611 -0.0758 0.057 Uiso 1 1 calc R U . . .
H4 H 0.6472 0.4912 -0.0059 0.057 Uiso 1 1 calc R U . . .
H5 H 0.6516 0.5800 0.0268 0.057 Uiso 1 1 calc R U . . .
C6 C 0.7481(6) 0.6303(6) -0.0285(7) 0.045(2) Uani 1 1 d . . . . .
H8 H 0.7183 0.6454 -0.0880 0.053 Uiso 1 1 calc R U . . .
H9 H 0.7438 0.6678 0.0140 0.053 Uiso 1 1 calc R U . . .
H7 H 0.7942 0.6300 -0.0247 0.053 Uiso 1 1 calc R U . . .
C7 C 0.8767(6) 0.5413(7) 0.3185(7) 0.043(3) Uani 1 1 d . . . . .
H10 H 0.8900 0.4923 0.3543 0.052 Uiso 1 1 calc R U . . .
C8 C 0.9388(7) 0.5823(8) 0.3246(9) 0.063(4) Uani 1 1 d . . . . .
H11 H 0.9646 0.5968 0.3859 0.076 Uiso 1 1 calc R U . . .
H12 H 0.9654 0.5475 0.3038 0.076 Uiso 1 1 calc R U . . .
H13 H 0.9273 0.6296 0.2882 0.076 Uiso 1 1 calc R U . . .
C9 C 0.8366(8) 0.5918(7) 0.3582(8) 0.060(3) Uani 1 1 d . . . . .
H15 H 0.7960 0.5639 0.3535 0.072 Uiso 1 1 calc R U . . .
H16 H 0.8637 0.6023 0.4202 0.072 Uiso 1 1 calc R U . . .
H14 H 0.8246 0.6415 0.3261 0.072 Uiso 1 1 calc R U . . .
C10 C 0.6735(4) 0.2510(4) 0.1530(5) 0.0262(16) Uani 1 1 d . . . . .
C11 C 0.6227(4) 0.2595(5) 0.0701(5) 0.0299(17) Uani 1 1 d . . . . .
H17 H 0.5796 0.2365 0.0507 0.036 Uiso 1 1 calc R U . . .
C12 C 0.6464(4) 0.3070(7) 0.0222(5) 0.0312(19) Uani 1 1 d . . . . .
C13 C 0.6729(5) 0.2011(6) 0.2283(6) 0.0330(19) Uani 1 1 d . . . . .
H18 H 0.7067 0.2233 0.2837 0.040 Uiso 1 1 calc R U . . .
C14 C 0.6053(5) 0.2042(7) 0.2364(7) 0.045(2) Uani 1 1 d . . . . .
H21 H 0.6065 0.1713 0.2857 0.054 Uiso 1 1 calc R U . . .
H19 H 0.5953 0.2583 0.2466 0.054 Uiso 1 1 calc R U . . .
H20 H 0.5708 0.1848 0.1819 0.054 Uiso 1 1 calc R U . . .
C15 C 0.6932(5) 0.1177(7) 0.2200(8) 0.043(2) Uani 1 1 d . . . . .
H23 H 0.6924 0.0867 0.2697 0.052 Uiso 1 1 calc R U . . .
H22 H 0.6621 0.0951 0.1649 0.052 Uiso 1 1 calc R U . . .
H24 H 0.7383 0.1173 0.2201 0.052 Uiso 1 1 calc R U . . .
C16 C 0.6117(4) 0.3335(5) -0.0711(6) 0.034(2) Uani 1 1 d . . . . .
H25 H 0.6382 0.3773 -0.0816 0.041 Uiso 1 1 calc R U . . .
C17 C 0.6085(7) 0.2694(8) -0.1337(7) 0.057(3) Uani 1 1 d . . . . .
H26 H 0.5856 0.2882 -0.1941 0.068 Uiso 1 1 calc R U . . .
H28 H 0.6538 0.2529 -0.1250 0.068 Uiso 1 1 calc R U . . .
H27 H 0.5840 0.2249 -0.1233 0.068 Uiso 1 1 calc R U . . .
C18 C 0.5420(5) 0.3648(9) -0.0868(8) 0.059(3) Uani 1 1 d . . . . .
H31 H 0.5455 0.4069 -0.0448 0.070 Uiso 1 1 calc R U . . .
H29 H 0.5214 0.3852 -0.1468 0.070 Uiso 1 1 calc R U . . .
H30 H 0.5145 0.3224 -0.0788 0.070 Uiso 1 1 calc R U . . .
C19 C 0.9149(4) 0.2604(6) 0.1255(5) 0.0310(17) Uani 1 1 d . . . . .
C20 C 0.9024(4) 0.2617(6) 0.0365(6) 0.0340(18) Uani 1 1 d . . . . .
H32 H 0.9302 0.2415 0.0088 0.041 Uiso 1 1 calc R U . . .
C21 C 0.8422(4) 0.2981(5) -0.0036(5) 0.030(2) Uani 1 1 d . . . . .
C22 C 0.9768(4) 0.2293(6) 0.1985(5) 0.0340(19) Uani 1 1 d . . . . .
H33 H 0.9661 0.2186 0.2513 0.041 Uiso 1 1 calc R U . . .
C23 C 1.0303(5) 0.2932(6) 0.2217(7) 0.041(2) Uani 1 1 d . . . . .
H36 H 1.0130 0.3414 0.2372 0.050 Uiso 1 1 calc R U . . .
H35 H 1.0698 0.2760 0.2718 0.050 Uiso 1 1 calc R U . . .
H34 H 1.0423 0.3029 0.1710 0.050 Uiso 1 1 calc R U . . .
C24 C 1.0042(5) 0.1562(7) 0.1751(7) 0.042(2) Uani 1 1 d . . . . .
H39 H 1.0440 0.1397 0.2251 0.050 Uiso 1 1 calc R U . . .
H37 H 0.9706 0.1147 0.1604 0.050 Uiso 1 1 calc R U . . .
H38 H 1.0160 0.1663 0.1243 0.050 Uiso 1 1 calc R U . . .
C25 C 0.8049(4) 0.3193(11) -0.0992(5) 0.043(2) Uani 1 1 d . . . . .
H40 H 0.7564 0.3219 -0.1103 0.052 Uiso 1 1 calc R U . . .
C26 C 0.8144(6) 0.2561(9) -0.1582(8) 0.053(3) Uani 1 1 d . . . . .
H41 H 0.8006 0.2055 -0.1430 0.064 Uiso 1 1 calc R U . . .
H43 H 0.7872 0.2685 -0.2197 0.064 Uiso 1 1 calc R U . . .
H42 H 0.8614 0.2537 -0.1501 0.064 Uiso 1 1 calc R U . . .
C27 C 0.8257(7) 0.3986(8) -0.1208(8) 0.051(3) Uani 1 1 d . . . . .
H45 H 0.8006 0.4104 -0.1830 0.062 Uiso 1 1 calc R U . . .
H46 H 0.8165 0.4387 -0.0844 0.062 Uiso 1 1 calc R U . . .
H44 H 0.8734 0.3980 -0.1088 0.062 Uiso 1 1 calc R U . . .
C28 C 0.8408(4) 0.1750(5) 0.4312(5) 0.0301(17) Uani 1 1 d . . . . .
C29 C 0.8643(5) 0.1039(6) 0.4144(6) 0.0362(19) Uani 1 1 d . . . . .
H47 H 0.8723 0.0579 0.4493 0.043 Uiso 1 1 calc R U . . .
C30 C 0.8736(5) 0.1131(6) 0.3367(6) 0.0306(19) Uani 1 1 d . . . . .
C31 C 0.8218(6) 0.2008(7) 0.5056(8) 0.037(2) Uani 1 1 d . . . . .
H48 H 0.8442 0.2522 0.5267 0.045 Uiso 1 1 calc R U . . .
C32 C 0.7471(6) 0.2150(11) 0.4753(8) 0.058(4) Uani 1 1 d . . . . .
H51 H 0.7366 0.2317 0.5254 0.070 Uiso 1 1 calc R U . . .
H49 H 0.7336 0.2560 0.4302 0.070 Uiso 1 1 calc R U . . .
H50 H 0.7230 0.1666 0.4507 0.070 Uiso 1 1 calc R U . . .
C33 C 0.8473(8) 0.1449(9) 0.5828(8) 0.057(3) Uani 1 1 d . . . . .
H53 H 0.8339 0.1636 0.6298 0.069 Uiso 1 1 calc R U . . .
H52 H 0.8285 0.0927 0.5639 0.069 Uiso 1 1 calc R U . . .
H54 H 0.8960 0.1422 0.6045 0.069 Uiso 1 1 calc R U . . .
C34 C 0.8995(6) 0.0560(6) 0.2876(7) 0.041(2) Uani 1 1 d . . . . .
H55 H 0.9013 0.0833 0.2349 0.049 Uiso 1 1 calc R U . . .
C35 C 0.9709(7) 0.0309(11) 0.3467(13) 0.080(5) Uani 1 1 d . . . . .
H58 H 0.9991 0.0774 0.3663 0.096 Uiso 1 1 calc R U . . .
H56 H 0.9700 0.0026 0.3980 0.096 Uiso 1 1 calc R U . . .
H57 H 0.9888 -0.0033 0.3134 0.096 Uiso 1 1 calc R U . . .
C36 C 0.8554(7) -0.0144(7) 0.2568(9) 0.056(3) Uani 1 1 d . . . . .
H61 H 0.8740 -0.0499 0.2254 0.067 Uiso 1 1 calc R U . . .
H60 H 0.8526 -0.0416 0.3077 0.067 Uiso 1 1 calc R U . . .
H59 H 0.8108 0.0022 0.2174 0.067 Uiso 1 1 calc R U . . .
C37 C 0.8146(6) 0.4226(6) 0.4996(7) 0.032(2) Uani 1 1 d . . . . .
C38 C 0.7485(5) 0.4373(7) 0.4509(7) 0.041(2) Uani 1 1 d . . . . .
H63 H 0.7170 0.4578 0.4723 0.049 Uiso 1 1 calc R U . . .
C39 C 0.7362(5) 0.4163(5) 0.3640(6) 0.0341(18) Uani 1 1 d . . . . .
C40 C 0.8585(5) 0.4345(7) 0.5944(6) 0.042(2) Uani 1 1 d . . . . .
H64 H 0.8970 0.3977 0.6088 0.051 Uiso 1 1 calc R U . . .
C41 C 0.8217(8) 0.4142(12) 0.6537(8) 0.072(4) Uani 1 1 d . . . . .
H65 H 0.8044 0.3607 0.6413 0.087 Uiso 1 1 calc R U . . .
H67 H 0.8524 0.4181 0.7153 0.087 Uiso 1 1 calc R U . . .
H66 H 0.7847 0.4508 0.6427 0.087 Uiso 1 1 calc R U . . .
C42 C 0.8856(9) 0.5150(10) 0.6110(10) 0.072(4) Uani 1 1 d . . . . .
H69 H 0.9141 0.5207 0.6734 0.087 Uiso 1 1 calc R U . . .
H70 H 0.9119 0.5250 0.5753 0.087 Uiso 1 1 calc R U . . .
H68 H 0.8488 0.5526 0.5953 0.087 Uiso 1 1 calc R U . . .
C43 C 0.6728(5) 0.4209(8) 0.2842(7) 0.051(3) Uani 1 1 d . . . . .
H71 H 0.6698 0.3737 0.2470 0.061 Uiso 1 1 calc R U . . .
C44 C 0.6135(6) 0.4197(10) 0.3135(9) 0.065(4) Uani 1 1 d . . . . .
H72 H 0.5718 0.4227 0.2617 0.078 Uiso 1 1 calc R U . . .
H73 H 0.6144 0.3711 0.3455 0.078 Uiso 1 1 calc R U . . .
H74 H 0.6166 0.4646 0.3519 0.078 Uiso 1 1 calc R U . . .
C45 C 0.6684(7) 0.4936(12) 0.2291(8) 0.065(5) Uani 1 1 d . . . . .
H75 H 0.6260 0.4934 0.1781 0.079 Uiso 1 1 calc R U . . .
H76 H 0.6708 0.5404 0.2647 0.079 Uiso 1 1 calc R U . . .
H77 H 0.7054 0.4939 0.2091 0.079 Uiso 1 1 calc R U . . .
C46 C 0.9514(17) 0.512(2) 0.113(2) 0.072(8) Uani 0.5 1 d D U P A 1
H78 H 0.9533 0.4688 0.1523 0.087 Uiso 0.5 1 calc R U P A 1
H80 H 0.9660 0.5606 0.1472 0.087 Uiso 0.5 1 calc R U P A 1
H79 H 0.9056 0.5189 0.0702 0.087 Uiso 0.5 1 calc R U P A 1
C50 C 1.0369(17) 0.4725(16) -0.1006(19) 0.063(7) Uani 0.5 1 d D U P B 2
H89 H 1.0703 0.4701 -0.1268 0.075 Uiso 0.5 1 calc R U P B 2
H87 H 1.0409 0.4262 -0.0637 0.075 Uiso 0.5 1 calc R U P B 2
H88 H 0.9923 0.4740 -0.1473 0.075 Uiso 0.5 1 calc R U P B 2
C47 C 0.9974(12) 0.4951(13) 0.0639(16) 0.055(5) Uani 0.5 1 d D U P A 1
H82 H 1.0431 0.4870 0.1080 0.066 Uiso 0.5 1 calc R U P A 1
H81 H 0.9829 0.4454 0.0312 0.066 Uiso 0.5 1 calc R U P A 1
C49 C 1.0478(12) 0.5458(14) -0.0446(16) 0.055(5) Uani 0.5 1 d D U P B 2
H86 H 1.0935 0.5442 0.0009 0.065 Uiso 0.5 1 calc R U P B 2
H85 H 1.0450 0.5918 -0.0824 0.065 Uiso 0.5 1 calc R U P B 2
C48 C 1.0000 0.5576(10) 0.0000 0.056(4) Uani 1 2 d DS TU P . .
H84 H 1.0405 0.5905 0.0229 0.067 Uiso 0.5 1 calc R U P A 1
H83 H 0.9595 0.5905 -0.0229 0.067 Uiso 0.5 1 calc R U P A 1
B B 0.7618(5) 0.3734(5) 0.0518(5) 0.0261(17) Uani 1 1 d . . . . .
H1 H 0.7404 0.3909 -0.0107 0.031 Uiso 1 1 calc R U . . .
N11 N 0.7842(3) 0.4471(4) 0.1099(5) 0.0268(13) Uani 1 1 d . . . . .
N12 N 0.8221(4) 0.4436(4) 0.1984(5) 0.0283(14) Uani 1 1 d . . . . .
N21 N 0.7098(3) 0.3265(5) 0.0741(4) 0.0260(16) Uani 1 1 d . . . . .
N22 N 0.7270(3) 0.2921(4) 0.1558(4) 0.0229(13) Uani 1 1 d . . . . .
N31 N 0.8217(3) 0.3229(6) 0.0605(4) 0.0272(14) Uani 1 1 d . . . . .
N32 N 0.8662(3) 0.2968(4) 0.1409(4) 0.0248(15) Uani 1 1 d . . . . .
N41 N 0.8572(4) 0.1860(4) 0.3066(5) 0.0285(14) Uani 1 1 d . . . . .
N42 N 0.8362(4) 0.2252(4) 0.3648(4) 0.0273(14) Uani 1 1 d . . . . .
N52 N 0.7932(4) 0.3904(4) 0.3586(5) 0.0293(14) Uani 1 1 d . . . . .
N51 N 0.8397(4) 0.3943(5) 0.4427(5) 0.0299(15) Uani 1 1 d . . . . .
H62 H 0.8815 0.3798 0.4578 0.036 Uiso 1 1 calc R U . . .
S1 S 0.95920(11) 0.36827(13) 0.37025(13) 0.0318(4) Uani 1 1 d . . . . .
S2 S 1.00921(11) 0.27289(14) 0.44368(15) 0.0344(5) Uani 1 1 d . . . . .
Yb Yb 0.83707(2) 0.31555(3) 0.26640(2) 0.02267(13) Uani 1 1 d . . . . .
C51 C 0.617(4) 0.314(3) 0.556(4) 0.158(14) Uani 0.5 1 d D U P C .
H92 H 0.6600 0.3039 0.5512 0.189 Uiso 0.5 1 calc R U P . .
H91 H 0.6078 0.3701 0.5501 0.189 Uiso 0.5 1 calc R U P . .
H90 H 0.6188 0.2955 0.6129 0.189 Uiso 0.5 1 calc R U P . .
C53A C 0.5000 0.293(4) 0.5000 0.27(2) Uani 0.5 2 d DS TU P C 3
H95A H 0.4930 0.2493 0.5354 0.324 Uiso 0.25 1 calc R U P C 3
H96A H 0.5133 0.3386 0.5395 0.324 Uiso 0.25 1 calc R U P C 3
C53B C 0.5000 0.293(4) 0.5000 0.27(2) Uani 0.5 2 d DS TU P D 4
H95B H 0.5070 0.2493 0.4646 0.324 Uiso 0.25 1 calc R U P D 4
H96B H 0.4867 0.3386 0.4605 0.324 Uiso 0.25 1 calc R U P D 4
C52 C 0.562(3) 0.270(4) 0.482(6) 0.26(3) Uani 0.5 1 d D U P . .
H93 H 0.5582 0.2880 0.4231 0.312 Uiso 0.5 1 calc R U P C 3
H94 H 0.5693 0.2127 0.4864 0.312 Uiso 0.5 1 calc R U P C 3
C55 C 0.399(6) 0.351(4) 0.489(8) 0.27(3) Uani 0.5 1 d D U P C .
H100 H 0.3537 0.3669 0.4533 0.328 Uiso 0.5 1 calc R U P . .
H99 H 0.3985 0.3134 0.5341 0.328 Uiso 0.5 1 calc R U P . .
H101 H 0.4255 0.3969 0.5183 0.328 Uiso 0.5 1 calc R U P . .
C54 C 0.431(3) 0.312(6) 0.431(5) 0.27(3) Uani 0.5 1 d D U P . .
H98 H 0.4066 0.2645 0.4019 0.329 Uiso 0.5 1 calc R U P C 3
H97 H 0.4337 0.3488 0.3860 0.329 Uiso 0.5 1 calc R U P C 3


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N12 1.339(12) . ?
C1 C2 1.404(13) . ?
C1 C7 1.499(14) . ?
C2 C3 1.372(14) . ?
C3 N11 1.374(11) . ?
C3 C4 1.508(12) . ?
C4 C5 1.512(15) . ?
C4 C6 1.522(13) . ?
C7 C8 1.491(19) . ?
C7 C9 1.540(19) . ?
C10 N22 1.346(11) . ?
C10 C11 1.396(12) . ?
C10 C13 1.510(11) . ?
C11 C12 1.365(13) . ?
C12 N21 1.355(11) . ?
C12 C16 1.499(12) . ?
C13 C15 1.514(16) . ?
C13 C14 1.527(13) . ?
C16 C17 1.488(15) . ?
C16 C18 1.534(14) . ?
C19 N32 1.334(11) . ?
C19 C20 1.387(12) . ?
C19 C22 1.516(11) . ?
C20 C21 1.368(12) . ?
C21 N31 1.362(10) . ?
C21 C25 1.513(12) . ?
C22 C24 1.496(14) . ?
C22 C23 1.533(14) . ?
C25 C27 1.51(2) . ?
C25 C26 1.520(18) . ?
C28 N42 1.364(11) . ?
C28 C29 1.388(13) . ?
C28 C31 1.503(14) . ?
C29 C30 1.380(14) . ?
C30 N41 1.336(12) . ?
C30 C34 1.508(13) . ?
C31 C33 1.515(17) . ?
C31 C32 1.524(17) . ?
C34 C36 1.501(17) . ?
C34 C35 1.543(18) . ?
C37 N51 1.345(12) . ?
C37 C38 1.373(15) . ?
C37 C40 1.499(15) . ?
C38 C39 1.398(13) . ?
C39 N52 1.352(12) . ?
C39 C43 1.499(14) . ?
C40 C42 1.48(2) . ?
C40 C41 1.523(17) . ?
C43 C45 1.52(2) . ?
C43 C44 1.540(17) . ?
C46 C47 1.54(2) . ?
C50 C49 1.52(2) . ?
C47 C48 1.52(2) . ?
C49 C48 1.501(19) . ?
C48 C49 1.501(19) 2_755 ?
C48 C47 1.52(2) 2_755 ?
B N31 1.524(12) . ?
B N21 1.541(11) . ?
B N11 1.543(11) . ?
N11 N12 1.373(10) . ?
N12 Yb 2.423(7) . ?
N21 N22 1.382(9) . ?
N22 Yb 2.421(7) . ?
N31 N32 1.380(9) . ?
N32 Yb 2.406(6) . ?
N41 N42 1.383(10) . ?
N41 Yb 2.304(7) . ?
N42 Yb 2.244(7) . ?
N52 N51 1.367(11) . ?
N52 Yb 2.443(7) . ?
S1 S2 2.072(3) . ?
S1 Yb 2.703(2) . ?
S2 S2 2.044(5) 2_756 ?
C51 C52 1.54(3) . ?
C53A C54 1.53(2) . ?
C53A C52 1.53(2) . ?
C53B C54 1.53(2) 2_656 ?
C53B C52 1.53(2) 2_656 ?
C55 C54 1.53(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
N12 C1 C2 110.7(8) . . ?
N12 C1 C7 124.3(9) . . ?
C2 C1 C7 125.0(9) . . ?
C3 C2 C1 105.5(8) . . ?
C2 C3 N11 108.0(8) . . ?
C2 C3 C4 128.4(8) . . ?
N11 C3 C4 123.2(8) . . ?
C3 C4 C5 109.5(8) . . ?
C3 C4 C6 110.7(8) . . ?
C5 C4 C6 111.8(8) . . ?
C8 C7 C1 111.6(11) . . ?
C8 C7 C9 110.7(11) . . ?
C1 C7 C9 111.5(10) . . ?
N22 C10 C11 109.2(7) . . ?
N22 C10 C13 123.1(8) . . ?
C11 C10 C13 127.6(8) . . ?
C12 C11 C10 107.1(7) . . ?
N21 C12 C11 107.5(8) . . ?
N21 C12 C16 124.2(8) . . ?
C11 C12 C16 128.2(8) . . ?
C10 C13 C15 111.2(8) . . ?
C10 C13 C14 111.4(8) . . ?
C15 C13 C14 111.3(9) . . ?
C17 C16 C12 111.1(8) . . ?
C17 C16 C18 111.1(10) . . ?
C12 C16 C18 110.7(8) . . ?
N32 C19 C20 110.2(7) . . ?
N32 C19 C22 122.8(7) . . ?
C20 C19 C22 126.7(8) . . ?
C21 C20 C19 106.2(7) . . ?
N31 C21 C20 107.8(7) . . ?
N31 C21 C25 121.9(8) . . ?
C20 C21 C25 130.0(7) . . ?
C24 C22 C19 114.1(8) . . ?
C24 C22 C23 108.6(7) . . ?
C19 C22 C23 107.9(8) . . ?
C27 C25 C21 111.7(10) . . ?
C27 C25 C26 111.0(9) . . ?
C21 C25 C26 110.2(12) . . ?
N42 C28 C29 108.0(8) . . ?
N42 C28 C31 120.9(9) . . ?
C29 C28 C31 131.2(9) . . ?
C30 C29 C28 106.4(8) . . ?
N41 C30 C29 109.8(8) . . ?
N41 C30 C34 120.3(8) . . ?
C29 C30 C34 129.9(9) . . ?
C28 C31 C33 111.9(10) . . ?
C28 C31 C32 111.8(9) . . ?
C33 C31 C32 112.1(11) . . ?
C36 C34 C30 112.2(9) . . ?
C36 C34 C35 110.3(11) . . ?
C30 C34 C35 109.5(10) . . ?
N51 C37 C38 105.8(9) . . ?
N51 C37 C40 120.5(9) . . ?
C38 C37 C40 133.7(10) . . ?
C37 C38 C39 107.3(8) . . ?
N52 C39 C38 109.4(8) . . ?
N52 C39 C43 121.2(8) . . ?
C38 C39 C43 129.4(9) . . ?
C42 C40 C37 111.6(10) . . ?
C42 C40 C41 111.2(12) . . ?
C37 C40 C41 110.8(11) . . ?
C39 C43 C45 113.1(11) . . ?
C39 C43 C44 108.9(10) . . ?
C45 C43 C44 109.2(11) . . ?
C48 C47 C46 116(2) . . ?
C48 C49 C50 116(2) . . ?
C49 C48 C49 165(2) 2_755 . ?
C47 C48 C47 90(2) . 2_755 ?
N31 B N21 111.3(7) . . ?
N31 B N11 110.4(7) . . ?
N21 B N11 111.3(7) . . ?
N12 N11 C3 109.6(7) . . ?
N12 N11 B 122.8(6) . . ?
C3 N11 B 127.5(7) . . ?
C1 N12 N11 106.3(7) . . ?
C1 N12 Yb 136.5(6) . . ?
N11 N12 Yb 116.7(5) . . ?
C12 N21 N22 109.9(7) . . ?
C12 N21 B 129.8(7) . . ?
N22 N21 B 120.2(6) . . ?
C10 N22 N21 106.3(6) . . ?
C10 N22 Yb 134.8(5) . . ?
N21 N22 Yb 118.9(5) . . ?
C21 N31 N32 109.0(7) . . ?
C21 N31 B 128.8(7) . . ?
N32 N31 B 122.1(6) . . ?
C19 N32 N31 106.5(6) . . ?
C19 N32 Yb 135.7(5) . . ?
N31 N32 Yb 117.6(5) . . ?
C30 N41 N42 107.8(7) . . ?
C30 N41 Yb 174.6(7) . . ?
N42 N41 Yb 69.9(4) . . ?
C28 N42 N41 108.1(7) . . ?
C28 N42 Yb 173.8(6) . . ?
N41 N42 Yb 74.7(4) . . ?
C39 N52 N51 104.9(7) . . ?
C39 N52 Yb 143.1(6) . . ?
N51 N52 Yb 110.0(5) . . ?
C37 N51 N52 112.6(8) . . ?
S2 S1 Yb 105.99(11) . . ?
S2 S2 S1 106.75(12) 2_756 . ?
N42 Yb N41 35.4(3) . . ?
N42 Yb N32 127.4(2) . . ?
N41 Yb N32 92.0(2) . . ?
N42 Yb N22 98.6(2) . . ?
N41 Yb N22 94.7(2) . . ?
N32 Yb N22 80.9(2) . . ?
N42 Yb N12 156.7(3) . . ?
N41 Yb N12 167.9(3) . . ?
N32 Yb N12 75.8(2) . . ?
N22 Yb N12 83.3(2) . . ?
N42 Yb N52 78.3(3) . . ?
N41 Yb N52 113.6(2) . . ?
N32 Yb N52 154.0(2) . . ?
N22 Yb N52 92.6(2) . . ?
N12 Yb N52 78.5(2) . . ?
N42 Yb S1 92.9(2) . . ?
N41 Yb S1 96.08(19) . . ?
N32 Yb S1 93.97(16) . . ?
N22 Yb S1 168.23(16) . . ?
N12 Yb S1 85.22(18) . . ?
N52 Yb S1 87.45(19) . . ?
C54 C53A C52 126(6) . . ?
C54 C53B C52 126(6) 2_656 2_656 ?
C53A C52 C51 102(5) . . ?
C53A C54 C55 100(6) . . ?

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
N12 C1 C2 C3 0.2(12) . . . . ?
C7 C1 C2 C3 178.7(11) . . . . ?
C1 C2 C3 N11 0.0(11) . . . . ?
C1 C2 C3 C4 172.9(10) . . . . ?
C2 C3 C4 C5 -94.5(12) . . . . ?
N11 C3 C4 C5 77.4(11) . . . . ?
C2 C3 C4 C6 29.2(15) . . . . ?
N11 C3 C4 C6 -158.8(9) . . . . ?
N12 C1 C7 C8 115.6(12) . . . . ?
C2 C1 C7 C8 -62.8(15) . . . . ?
N12 C1 C7 C9 -120.0(12) . . . . ?
C2 C1 C7 C9 61.7(15) . . . . ?
N22 C10 C11 C12 -0.1(11) . . . . ?
C13 C10 C11 C12 -177.0(9) . . . . ?
C10 C11 C12 N21 0.3(11) . . . . ?
C10 C11 C12 C16 179.2(9) . . . . ?
N22 C10 C13 C15 -91.3(10) . . . . ?
C11 C10 C13 C15 85.1(11) . . . . ?
N22 C10 C13 C14 143.8(9) . . . . ?
C11 C10 C13 C14 -39.7(14) . . . . ?
N21 C12 C16 C17 103.5(12) . . . . ?
C11 C12 C16 C17 -75.2(13) . . . . ?
N21 C12 C16 C18 -132.5(11) . . . . ?
C11 C12 C16 C18 48.9(14) . . . . ?
N32 C19 C20 C21 -2.4(11) . . . . ?
C22 C19 C20 C21 -177.2(9) . . . . ?
C19 C20 C21 N31 4.3(11) . . . . ?
C19 C20 C21 C25 177.0(12) . . . . ?
N32 C19 C22 C24 146.7(9) . . . . ?
C20 C19 C22 C24 -39.1(14) . . . . ?
N32 C19 C22 C23 -92.6(10) . . . . ?
C20 C19 C22 C23 81.7(12) . . . . ?
N31 C21 C25 C27 84.6(10) . . . . ?
C20 C21 C25 C27 -87.2(14) . . . . ?
N31 C21 C25 C26 -151.5(9) . . . . ?
C20 C21 C25 C26 36.8(16) . . . . ?
N42 C28 C29 C30 0.1(10) . . . . ?
C31 C28 C29 C30 -179.9(9) . . . . ?
C28 C29 C30 N41 0.3(11) . . . . ?
C28 C29 C30 C34 178.7(10) . . . . ?
N42 C28 C31 C33 -164.9(10) . . . . ?
C29 C28 C31 C33 15.2(16) . . . . ?
N42 C28 C31 C32 68.3(14) . . . . ?
C29 C28 C31 C32 -111.6(13) . . . . ?
N41 C30 C34 C36 -118.9(11) . . . . ?
C29 C30 C34 C36 62.9(15) . . . . ?
N41 C30 C34 C35 118.2(12) . . . . ?
C29 C30 C34 C35 -60.0(16) . . . . ?
N51 C37 C38 C39 0.1(13) . . . . ?
C40 C37 C38 C39 177.7(12) . . . . ?
C37 C38 C39 N52 -0.8(13) . . . . ?
C37 C38 C39 C43 -179.6(12) . . . . ?
N51 C37 C40 C42 92.7(13) . . . . ?
C38 C37 C40 C42 -84.7(17) . . . . ?
N51 C37 C40 C41 -142.8(12) . . . . ?
C38 C37 C40 C41 39.9(19) . . . . ?
N52 C39 C43 C45 -80.8(13) . . . . ?
C38 C39 C43 C45 97.9(15) . . . . ?
N52 C39 C43 C44 157.6(11) . . . . ?
C38 C39 C43 C44 -23.7(18) . . . . ?
C50 C49 C48 C49 31(2) . . . 2_755 ?
C46 C47 C48 C47 -141(3) . . . 2_755 ?
C2 C3 N11 N12 -0.2(10) . . . . ?
C4 C3 N11 N12 -173.6(8) . . . . ?
C2 C3 N11 B -176.0(8) . . . . ?
C4 C3 N11 B 10.6(14) . . . . ?
N31 B N11 N12 -54.8(9) . . . . ?
N21 B N11 N12 69.3(10) . . . . ?
N31 B N11 C3 120.5(9) . . . . ?
N21 B N11 C3 -115.4(9) . . . . ?
C2 C1 N12 N11 -0.3(11) . . . . ?
C7 C1 N12 N11 -178.9(10) . . . . ?
C2 C1 N12 Yb -171.7(7) . . . . ?
C7 C1 N12 Yb 9.7(16) . . . . ?
C3 N11 N12 C1 0.3(10) . . . . ?
B N11 N12 C1 176.3(8) . . . . ?
C3 N11 N12 Yb 173.7(6) . . . . ?
B N11 N12 Yb -10.2(9) . . . . ?
C11 C12 N21 N22 -0.4(11) . . . . ?
C16 C12 N21 N22 -179.3(8) . . . . ?
C11 C12 N21 B 174.8(8) . . . . ?
C16 C12 N21 B -4.1(17) . . . . ?
N31 B N21 C12 -116.0(11) . . . . ?
N11 B N21 C12 120.4(10) . . . . ?
N31 B N21 N22 58.8(9) . . . . ?
N11 B N21 N22 -64.8(10) . . . . ?
C11 C10 N22 N21 -0.1(9) . . . . ?
C13 C10 N22 N21 176.9(8) . . . . ?
C11 C10 N22 Yb 179.5(6) . . . . ?
C13 C10 N22 Yb -3.5(12) . . . . ?
C12 N21 N22 C10 0.3(9) . . . . ?
B N21 N22 C10 -175.4(7) . . . . ?
C12 N21 N22 Yb -179.4(6) . . . . ?
B N21 N22 Yb 4.9(9) . . . . ?
C20 C21 N31 N32 -4.8(10) . . . . ?
C25 C21 N31 N32 -178.1(10) . . . . ?
C20 C21 N31 B 173.3(9) . . . . ?
C25 C21 N31 B -0.1(16) . . . . ?
N21 B N31 C21 113.1(10) . . . . ?
N11 B N31 C21 -122.8(9) . . . . ?
N21 B N31 N32 -69.1(10) . . . . ?
N11 B N31 N32 55.0(10) . . . . ?
C20 C19 N32 N31 -0.5(10) . . . . ?
C22 C19 N32 N31 174.6(9) . . . . ?
C20 C19 N32 Yb 173.4(6) . . . . ?
C22 C19 N32 Yb -11.5(14) . . . . ?
C21 N31 N32 C19 3.3(10) . . . . ?
B N31 N32 C19 -174.9(8) . . . . ?
C21 N31 N32 Yb -172.0(5) . . . . ?
B N31 N32 Yb 9.8(10) . . . . ?
C29 C30 N41 N42 -0.6(11) . . . . ?
C34 C30 N41 N42 -179.1(8) . . . . ?
C29 C28 N42 N41 -0.5(10) . . . . ?
C31 C28 N42 N41 179.6(8) . . . . ?
C30 N41 N42 C28 0.6(10) . . . . ?
Yb N41 N42 C28 -174.2(7) . . . . ?
C30 N41 N42 Yb 174.9(7) . . . . ?
C38 C39 N52 N51 1.1(11) . . . . ?
C43 C39 N52 N51 -180.0(10) . . . . ?
C38 C39 N52 Yb 162.1(8) . . . . ?
C43 C39 N52 Yb -19.0(17) . . . . ?
C38 C37 N51 N52 0.6(12) . . . . ?
C40 C37 N51 N52 -177.4(9) . . . . ?
C39 N52 N51 C37 -1.0(11) . . . . ?
Yb N52 N51 C37 -169.0(7) . . . . ?
C54 C53A C52 C51 140(7) . . . . ?
C52 C53A C54 C55 -165(7) . . . . ?

_refine_diff_density_max         0.839
_refine_diff_density_min         -1.991
_refine_diff_density_rms         0.138


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_tak1422
_database_code_depnum_ccdc_archive 'CCDC 1472923'
_audit_update_record             
;
2016-04-07 deposited with the CCDC.
2016-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C63 H107 B2 N14 Sm, C5 H12'
_chemical_formula_sum            'C68 H119 B2 N14 Sm'
_chemical_formula_weight         1304.73

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'
B B 0.0013 0.0007 '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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_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                   21.5176(10)
_cell_length_b                   17.2726(8)
_cell_length_c                   19.2117(9)
_cell_angle_alpha                90
_cell_angle_beta                 93.2336(6)
_cell_angle_gamma                90
_cell_volume                     7128.9(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    9915
_cell_measurement_theta_min      2.12
_cell_measurement_theta_max      21.80

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_F_000             2788
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.247
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.872
_shelx_estimated_absorpt_T_min   0.813
_shelx_estimated_absorpt_T_max   0.880
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8463
_exptl_absorpt_correction_T_max  0.9263
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32295
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.513
_diffrn_reflns_theta_max         28.274
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8673
_reflns_number_gt                7570
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0561P)²+1.2805P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8673
_refine_ls_number_parameters     378
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0364
_refine_ls_wR_factor_ref         0.0968
_refine_ls_wR_factor_gt          0.0927
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm Sm 0.0000 0.26981(2) 0.2500 0.02578(7) Uani 1 2 d S T P . .
N1 N 0.02537(9) 0.13915(11) 0.22940(11) 0.0312(4) Uani 1 1 d . . . . .
N11 N 0.15318(9) 0.26560(11) 0.33100(11) 0.0296(4) Uani 1 1 d . . . . .
N12 N 0.09819(9) 0.22907(11) 0.34536(11) 0.0298(4) Uani 1 1 d . . . . .
N21 N 0.14569(9) 0.33283(11) 0.21296(10) 0.0283(4) Uani 1 1 d . . . . .
N22 N 0.09459(9) 0.29448(12) 0.18308(11) 0.0309(4) Uani 1 1 d . . . . .
N31 N 0.10865(8) 0.40157(11) 0.32383(10) 0.0283(4) Uani 1 1 d . . . . .
N32 N 0.04451(8) 0.39408(11) 0.31541(10) 0.0273(4) Uani 1 1 d . . . . .
C1 C 0.04141(13) 0.06422(16) 0.21754(15) 0.0416(6) Uani 1 1 d . . . . .
C2 C 0.0000 0.0158(2) 0.2500 0.0497(10) Uani 1 2 d S T P . .
H2 H 0.0000 -0.0392 0.2500 0.060 Uiso 1 2 calc R U P . .
C3 C 0.09594(15) 0.04560(18) 0.17461(17) 0.0521(7) Uani 1 1 d . . . . .
H3 H 0.0833 0.0571 0.1248 0.063 Uiso 1 1 calc R U . . .
C4 C 0.15172(14) 0.0966(2) 0.19544(19) 0.0586(8) Uani 1 1 d . . . . .
H4A H 0.1865 0.0834 0.1668 0.070 Uiso 1 1 calc R U . . .
H4B H 0.1405 0.1511 0.1881 0.070 Uiso 1 1 calc R U . . .
H4C H 0.1640 0.0881 0.2447 0.070 Uiso 1 1 calc R U . . .
C5 C 0.11300(18) -0.0405(2) 0.1795(2) 0.0718(10) Uani 1 1 d . . . . .
H5A H 0.1485 -0.0508 0.1512 0.086 Uiso 1 1 calc R U . . .
H5B H 0.1240 -0.0539 0.2282 0.086 Uiso 1 1 calc R U . . .
H5C H 0.0773 -0.0717 0.1624 0.086 Uiso 1 1 calc R U . . .
C13 C 0.11527(11) 0.16702(14) 0.38413(13) 0.0326(5) Uani 1 1 d . . . . .
C14 C 0.17998(12) 0.16376(16) 0.39459(14) 0.0387(6) Uani 1 1 d . . . . .
H14 H 0.2034 0.1260 0.4206 0.046 Uiso 1 1 calc R U . . .
C15 C 0.20280(12) 0.22573(14) 0.35999(14) 0.0348(6) Uani 1 1 d . . . . .
C16 C 0.26988(12) 0.24566(18) 0.34852(17) 0.0436(7) Uani 1 1 d . . . . .
H16 H 0.2740 0.3032 0.3454 0.052 Uiso 1 1 calc R U . . .
C16A C 0.28842(15) 0.2097(2) 0.28023(19) 0.0585(9) Uani 1 1 d . . . . .
H16A H 0.3319 0.2225 0.2727 0.070 Uiso 1 1 calc R U . . .
H16B H 0.2837 0.1533 0.2825 0.070 Uiso 1 1 calc R U . . .
H16C H 0.2616 0.2301 0.2416 0.070 Uiso 1 1 calc R U . . .
C16B C 0.31294(15) 0.2163(2) 0.4086(2) 0.0646(10) Uani 1 1 d . . . . .
H16D H 0.3561 0.2299 0.4000 0.078 Uiso 1 1 calc R U . . .
H16E H 0.3013 0.2403 0.4523 0.078 Uiso 1 1 calc R U . . .
H16F H 0.3091 0.1599 0.4122 0.078 Uiso 1 1 calc R U . . .
C17 C 0.07138(12) 0.11076(16) 0.41548(14) 0.0393(6) Uani 1 1 d . . . . .
H17 H 0.0283 0.1201 0.3950 0.047 Uiso 1 1 calc R U . . .
C17A C 0.08999(15) 0.02738(18) 0.40078(19) 0.0562(8) Uani 1 1 d . . . . .
H17A H 0.0608 -0.0081 0.4217 0.067 Uiso 1 1 calc R U . . .
H17B H 0.0890 0.0189 0.3503 0.067 Uiso 1 1 calc R U . . .
H17C H 0.1321 0.0178 0.4209 0.067 Uiso 1 1 calc R U . . .
C17B C 0.07192(15) 0.1212(2) 0.49400(17) 0.0604(9) Uani 1 1 d . . . . .
H17D H 0.0431 0.0841 0.5135 0.072 Uiso 1 1 calc R U . . .
H17E H 0.1141 0.1121 0.5144 0.072 Uiso 1 1 calc R U . . .
H17F H 0.0589 0.1740 0.5047 0.072 Uiso 1 1 calc R U . . .
C23 C 0.10472(13) 0.28527(15) 0.11559(14) 0.0360(6) Uani 1 1 d . . . . .
C24 C 0.16226(12) 0.31700(17) 0.10146(14) 0.0408(6) Uani 1 1 d . . . . .
H24 H 0.1806 0.3183 0.0576 0.049 Uiso 1 1 calc R U . . .
C25 C 0.18713(11) 0.34600(15) 0.16366(13) 0.0346(5) Uani 1 1 d . . . . .
C26 C 0.24781(12) 0.38832(16) 0.17636(15) 0.0397(6) Uani 1 1 d . . . . .
H26 H 0.2656 0.3741 0.2238 0.048 Uiso 1 1 calc R U . . .
C26A C 0.29427(14) 0.3638(2) 0.12272(19) 0.0595(9) Uani 1 1 d . . . . .
H26A H 0.3335 0.3918 0.1317 0.071 Uiso 1 1 calc R U . . .
H26B H 0.3019 0.3080 0.1266 0.071 Uiso 1 1 calc R U . . .
H26C H 0.2770 0.3760 0.0757 0.071 Uiso 1 1 calc R U . . .
C26B C 0.23745(14) 0.47502(17) 0.17454(18) 0.0516(7) Uani 1 1 d . . . . .
H26D H 0.2774 0.5016 0.1829 0.062 Uiso 1 1 calc R U . . .
H26E H 0.2189 0.4900 0.1288 0.062 Uiso 1 1 calc R U . . .
H26F H 0.2094 0.4896 0.2108 0.062 Uiso 1 1 calc R U . . .
C27 C 0.05902(15) 0.24532(19) 0.06550(16) 0.0460(7) Uani 1 1 d . . . . .
H27 H 0.0298 0.2144 0.0932 0.055 Uiso 1 1 calc R U . . .
C27A C 0.09321(17) 0.1899(2) 0.01943(17) 0.0630(9) Uani 1 1 d . . . . .
H27A H 0.0632 0.1641 -0.0130 0.076 Uiso 1 1 calc R U . . .
H27B H 0.1232 0.2189 -0.0069 0.076 Uiso 1 1 calc R U . . .
H27C H 0.1153 0.1510 0.0486 0.076 Uiso 1 1 calc R U . . .
C27B C 0.02082(17) 0.3034(2) 0.02118(19) 0.0637(9) Uani 1 1 d . . . . .
H27D H -0.0084 0.2756 -0.0108 0.076 Uiso 1 1 calc R U . . .
H27E H -0.0024 0.3370 0.0516 0.076 Uiso 1 1 calc R U . . .
H27F H 0.0487 0.3350 -0.0057 0.076 Uiso 1 1 calc R U . . .
C33 C 0.02088(11) 0.45474(14) 0.34983(12) 0.0292(5) Uani 1 1 d . . . . .
C34 C 0.06932(11) 0.49887(15) 0.38068(13) 0.0347(5) Uani 1 1 d . . . . .
H34 H 0.0654 0.5440 0.4083 0.042 Uiso 1 1 calc R U . . .
C35 C 0.12376(11) 0.46440(14) 0.36333(12) 0.0310(5) Uani 1 1 d . . . . .
C36 C 0.18929(12) 0.48851(17) 0.38572(14) 0.0400(6) Uani 1 1 d . . . . .
H36 H 0.2159 0.4818 0.3451 0.048 Uiso 1 1 calc R U . . .
C36A C 0.21549(14) 0.4370(2) 0.44541(16) 0.0602(9) Uani 1 1 d . . . . .
H36A H 0.2580 0.4534 0.4593 0.072 Uiso 1 1 calc R U . . .
H36B H 0.1893 0.4417 0.4853 0.072 Uiso 1 1 calc R U . . .
H36C H 0.2160 0.3830 0.4298 0.072 Uiso 1 1 calc R U . . .
C36B C 0.19154(14) 0.5733(2) 0.40722(19) 0.0609(9) Uani 1 1 d . . . . .
H36D H 0.2345 0.5876 0.4215 0.073 Uiso 1 1 calc R U . . .
H36E H 0.1768 0.6056 0.3677 0.073 Uiso 1 1 calc R U . . .
H36F H 0.1648 0.5814 0.4463 0.073 Uiso 1 1 calc R U . . .
C37 C -0.04711(11) 0.47526(15) 0.35204(13) 0.0349(5) Uani 1 1 d . . . . .
H37 H -0.0726 0.4296 0.3357 0.042 Uiso 1 1 calc R U . . .
C37A C -0.06431(13) 0.4963(2) 0.42554(15) 0.0498(7) Uani 1 1 d . . . . .
H37A H -0.1087 0.5092 0.4251 0.060 Uiso 1 1 calc R U . . .
H37B H -0.0557 0.4521 0.4567 0.060 Uiso 1 1 calc R U . . .
H37C H -0.0396 0.5409 0.4421 0.060 Uiso 1 1 calc R U . . .
C37B C -0.06386(13) 0.54379(17) 0.30505(16) 0.0474(7) Uani 1 1 d . . . . .
H37D H -0.1082 0.5557 0.3076 0.057 Uiso 1 1 calc R U . . .
H37E H -0.0391 0.5889 0.3204 0.057 Uiso 1 1 calc R U . . .
H37F H -0.0551 0.5310 0.2569 0.057 Uiso 1 1 calc R U . . .
B B 0.15481(12) 0.34405(16) 0.29324(14) 0.0294(5) Uani 1 1 d . . . . .
H1B H 0.1975 0.3659 0.3027 0.035 Uiso 1 1 calc R U . . .
C1S C 0.4367(10) 0.2213(13) 0.1782(14) 0.187(4) Uiso 0.5 1 d D U P A -1
H1SA H 0.3982 0.2280 0.1490 0.224 Uiso 0.5 1 calc R U P A -1
H1SB H 0.4623 0.1811 0.1580 0.224 Uiso 0.5 1 calc R U P A -1
H1SC H 0.4264 0.2058 0.2253 0.224 Uiso 0.5 1 calc R U P A -1
C2S C 0.4723(8) 0.2968(9) 0.1816(8) 0.187(4) Uiso 0.5 1 d D U P A -1
H2SA H 0.4469 0.3379 0.2020 0.224 Uiso 0.5 1 calc R U P A -1
H2SB H 0.4829 0.3131 0.1344 0.224 Uiso 0.5 1 calc R U P A -1
C3S C 0.5324(6) 0.2823(10) 0.2283(8) 0.187(4) Uiso 0.5 1 d D U P A -1
H3SA H 0.5577 0.2406 0.2086 0.224 Uiso 0.5 1 calc R U P A -1
H3SB H 0.5580 0.3300 0.2324 0.224 Uiso 0.5 1 calc R U P A -1
C4S C 0.5099(8) 0.2584(12) 0.3000(8) 0.187(4) Uiso 0.5 1 d D U P A -1
H4SA H 0.4938 0.3040 0.3244 0.224 Uiso 0.5 1 calc R U P A -1
H4SB H 0.4761 0.2196 0.2941 0.224 Uiso 0.5 1 calc R U P A -1
C5S C 0.5657(11) 0.2238(14) 0.3419(10) 0.187(4) Uiso 0.5 1 d D U P A -1
H5SA H 0.5530 0.2079 0.3879 0.224 Uiso 0.5 1 calc R U P A -1
H5SB H 0.5812 0.1787 0.3172 0.224 Uiso 0.5 1 calc R U P A -1
H5SC H 0.5988 0.2627 0.3474 0.224 Uiso 0.5 1 calc R U P A -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm N1 2.3606(19) . ?
Sm N1 2.361(2) 2 ?
Sm N22 2.5044(19) 2 ?
Sm N22 2.5045(19) . ?
Sm N32 2.6397(19) . ?
Sm N32 2.6397(19) 2 ?
Sm N12 2.807(2) 2 ?
Sm N12 2.807(2) . ?
N1 C1 1.362(3) . ?
N1 N1 1.384(4) 2 ?
N11 C15 1.363(3) . ?
N11 N12 1.382(3) . ?
N11 B 1.538(3) . ?
N12 C13 1.345(3) . ?
N21 C25 1.356(3) . ?
N21 N22 1.380(3) . ?
N21 B 1.556(3) . ?
N22 C23 1.336(3) . ?
N31 C35 1.353(3) . ?
N31 N32 1.387(2) . ?
N31 B 1.544(3) . ?
N32 C33 1.353(3) . ?
C1 C2 1.395(4) . ?
C1 C3 1.506(4) . ?
C2 C1 1.395(4) 2 ?
C3 C4 1.524(4) . ?
C3 C5 1.533(5) . ?
C13 C14 1.397(3) . ?
C13 C17 1.504(3) . ?
C14 C15 1.366(4) . ?
C15 C16 1.512(4) . ?
C16 C16A 1.525(5) . ?
C16 C16B 1.526(4) . ?
C17 C17B 1.519(4) . ?
C17 C17A 1.525(4) . ?
C23 C24 1.395(3) . ?
C23 C27 1.504(4) . ?
C24 C25 1.376(4) . ?
C25 C26 1.504(3) . ?
C26 C26B 1.514(4) . ?
C26 C26A 1.535(4) . ?
C27 C27A 1.522(4) . ?
C27 C27B 1.526(5) . ?
C33 C34 1.396(3) . ?
C33 C37 1.508(3) . ?
C34 C35 1.372(3) . ?
C35 C36 1.509(3) . ?
C36 C36B 1.522(4) . ?
C36 C36A 1.533(4) . ?
C37 C37B 1.520(4) . ?
C37 C37A 1.524(4) . ?
C1S C2S 1.512(9) . ?
C2S C3S 1.553(9) . ?
C3S C4S 1.541(9) . ?
C4S C5S 1.528(9) . ?

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 Sm N1 34.10(9) . 2 ?
N1 Sm N22 116.82(7) . 2 ?
N1 Sm N22 82.78(7) 2 2 ?
N1 Sm N22 82.78(7) . . ?
N1 Sm N22 116.81(7) 2 . ?
N22 Sm N22 160.40(9) 2 . ?
N1 Sm N32 140.91(6) . . ?
N1 Sm N32 141.15(6) 2 . ?
N22 Sm N32 84.31(6) 2 . ?
N22 Sm N32 79.77(6) . . ?
N1 Sm N32 141.14(6) . 2 ?
N1 Sm N32 140.90(6) 2 2 ?
N22 Sm N32 79.77(6) 2 2 ?
N22 Sm N32 84.31(6) . 2 ?
N32 Sm N32 71.19(8) . 2 ?
N1 Sm N12 79.84(6) . 2 ?
N1 Sm N12 72.37(6) 2 2 ?
N22 Sm N12 76.95(6) 2 2 ?
N22 Sm N12 108.13(6) . 2 ?
N32 Sm N12 138.94(6) . 2 ?
N32 Sm N12 69.73(6) 2 2 ?
N1 Sm N12 72.37(6) . . ?
N1 Sm N12 79.84(6) 2 . ?
N22 Sm N12 108.13(6) 2 . ?
N22 Sm N12 76.94(6) . . ?
N32 Sm N12 69.73(6) . . ?
N32 Sm N12 138.95(6) 2 . ?
N12 Sm N12 150.96(8) 2 . ?
C1 N1 N1 108.12(15) . 2 ?
C1 N1 Sm 178.69(18) . . ?
N1 N1 Sm 72.95(5) 2 . ?
C15 N11 N12 110.34(19) . . ?
C15 N11 B 126.8(2) . . ?
N12 N11 B 122.60(19) . . ?
C13 N12 N11 105.31(19) . . ?
C13 N12 Sm 137.19(16) . . ?
N11 N12 Sm 112.12(14) . . ?
C25 N21 N22 109.25(19) . . ?
C25 N21 B 128.3(2) . . ?
N22 N21 B 121.66(18) . . ?
C23 N22 N21 106.91(19) . . ?
C23 N22 Sm 131.26(17) . . ?
N21 N22 Sm 121.30(14) . . ?
C35 N31 N32 110.26(18) . . ?
C35 N31 B 126.15(19) . . ?
N32 N31 B 123.57(18) . . ?
C33 N32 N31 105.65(18) . . ?
C33 N32 Sm 136.55(15) . . ?
N31 N32 Sm 117.61(13) . . ?
N1 C1 C2 108.7(2) . . ?
N1 C1 C3 120.5(3) . . ?
C2 C1 C3 130.8(3) . . ?
C1 C2 C1 106.3(3) 2 . ?
C1 C3 C4 111.0(3) . . ?
C1 C3 C5 111.4(3) . . ?
C4 C3 C5 111.2(3) . . ?
N12 C13 C14 110.5(2) . . ?
N12 C13 C17 125.4(2) . . ?
C14 C13 C17 124.0(2) . . ?
C15 C14 C13 106.3(2) . . ?
N11 C15 C14 107.5(2) . . ?
N11 C15 C16 123.9(2) . . ?
C14 C15 C16 128.4(2) . . ?
C15 C16 C16A 109.3(3) . . ?
C15 C16 C16B 111.0(3) . . ?
C16A C16 C16B 109.8(3) . . ?
C13 C17 C17B 110.6(2) . . ?
C13 C17 C17A 111.0(2) . . ?
C17B C17 C17A 108.0(3) . . ?
N22 C23 C24 109.7(2) . . ?
N22 C23 C27 122.6(2) . . ?
C24 C23 C27 127.7(2) . . ?
C25 C24 C23 106.3(2) . . ?
N21 C25 C24 107.9(2) . . ?
N21 C25 C26 124.5(2) . . ?
C24 C25 C26 127.5(2) . . ?
C25 C26 C26B 110.6(2) . . ?
C25 C26 C26A 110.4(2) . . ?
C26B C26 C26A 111.0(2) . . ?
C23 C27 C27A 109.9(3) . . ?
C23 C27 C27B 111.6(3) . . ?
C27A C27 C27B 110.6(3) . . ?
N32 C33 C34 109.8(2) . . ?
N32 C33 C37 126.0(2) . . ?
C34 C33 C37 124.2(2) . . ?
C35 C34 C33 106.7(2) . . ?
N31 C35 C34 107.6(2) . . ?
N31 C35 C36 124.9(2) . . ?
C34 C35 C36 127.4(2) . . ?
C35 C36 C36B 111.0(2) . . ?
C35 C36 C36A 110.6(2) . . ?
C36B C36 C36A 110.5(3) . . ?
C33 C37 C37B 111.4(2) . . ?
C33 C37 C37A 111.6(2) . . ?
C37B C37 C37A 107.6(2) . . ?
N11 B N31 110.78(19) . . ?
N11 B N21 110.7(2) . . ?
N31 B N21 114.17(19) . . ?
C1S C2S C3S 106.9(8) . . ?
C4S C3S C2S 105.4(8) . . ?
C5S C4S C3S 107.3(9) . . ?

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
N22 Sm N1 N1 -3.8(2) 2 . . 2 ?
N22 Sm N1 N1 176.55(18) . . . 2 ?
N32 Sm N1 N1 112.64(16) . . . 2 ?
N32 Sm N1 N1 -111.91(17) 2 . . 2 ?
N12 Sm N1 N1 -73.49(17) 2 . . 2 ?
N12 Sm N1 N1 98.01(17) . . . 2 ?
C15 N11 N12 C13 0.7(3) . . . . ?
B N11 N12 C13 -174.2(2) . . . . ?
C15 N11 N12 Sm -158.11(16) . . . . ?
B N11 N12 Sm 27.0(3) . . . . ?
N1 Sm N12 C13 -38.7(2) . . . . ?
N1 Sm N12 C13 -4.4(2) 2 . . . ?
N22 Sm N12 C13 74.5(2) 2 . . . ?
N22 Sm N12 C13 -125.1(2) . . . . ?
N32 Sm N12 C13 151.1(2) . . . . ?
N32 Sm N12 C13 169.8(2) 2 . . . ?
N12 Sm N12 C13 -21.2(2) 2 . . . ?
N1 Sm N12 N11 110.44(15) . . . . ?
N1 Sm N12 N11 144.78(15) 2 . . . ?
N22 Sm N12 N11 -136.35(14) 2 . . . ?
N22 Sm N12 N11 23.98(14) . . . . ?
N32 Sm N12 N11 -59.78(14) . . . . ?
N32 Sm N12 N11 -41.10(18) 2 . . . ?
N12 Sm N12 N11 127.89(14) 2 . . . ?
C25 N21 N22 C23 -0.7(3) . . . . ?
B N21 N22 C23 -171.6(2) . . . . ?
C25 N21 N22 Sm -173.28(15) . . . . ?
B N21 N22 Sm 15.9(3) . . . . ?
N1 Sm N22 C23 70.8(2) . . . . ?
N1 Sm N22 C23 72.9(2) 2 . . . ?
N22 Sm N22 C23 -108.2(2) 2 . . . ?
N32 Sm N22 C23 -144.4(2) . . . . ?
N32 Sm N22 C23 -72.5(2) 2 . . . ?
N12 Sm N22 C23 -6.0(2) 2 . . . ?
N12 Sm N22 C23 144.3(2) . . . . ?
N1 Sm N22 N21 -118.72(17) . . . . ?
N1 Sm N22 N21 -116.56(16) 2 . . . ?
N22 Sm N22 N21 62.30(16) 2 . . . ?
N32 Sm N22 N21 26.14(16) . . . . ?
N32 Sm N22 N21 98.00(17) 2 . . . ?
N12 Sm N22 N21 164.49(15) 2 . . . ?
N12 Sm N22 N21 -45.23(16) . . . . ?
C35 N31 N32 C33 1.0(2) . . . . ?
B N31 N32 C33 179.6(2) . . . . ?
C35 N31 N32 Sm -174.71(15) . . . . ?
B N31 N32 Sm 3.9(3) . . . . ?
N1 Sm N32 C33 -145.0(2) . . . . ?
N1 Sm N32 C33 -89.5(2) 2 . . . ?
N22 Sm N32 C33 -18.4(2) 2 . . . ?
N22 Sm N32 C33 150.1(2) . . . . ?
N32 Sm N32 C33 62.7(2) 2 . . . ?
N12 Sm N32 C33 44.2(3) 2 . . . ?
N12 Sm N32 C33 -130.2(2) . . . . ?
N1 Sm N32 N31 28.94(19) . . . . ?
N1 Sm N32 N31 84.51(17) 2 . . . ?
N22 Sm N32 N31 155.54(15) 2 . . . ?
N22 Sm N32 N31 -35.93(14) . . . . ?
N32 Sm N32 N31 -123.36(17) 2 . . . ?
N12 Sm N32 N31 -141.86(13) 2 . . . ?
N12 Sm N32 N31 43.81(14) . . . . ?
N1 N1 C1 C2 1.3(3) 2 . . . ?
N1 N1 C1 C3 -179.3(3) 2 . . . ?
N1 C1 C2 C1 -0.48(12) . . . 2 ?
C3 C1 C2 C1 -179.9(4) . . . 2 ?
N1 C1 C3 C4 44.7(4) . . . . ?
C2 C1 C3 C4 -136.0(3) . . . . ?
N1 C1 C3 C5 169.2(3) . . . . ?
C2 C1 C3 C5 -11.5(4) . . . . ?
N11 N12 C13 C14 0.1(3) . . . . ?
Sm N12 C13 C14 150.55(19) . . . . ?
N11 N12 C13 C17 177.1(2) . . . . ?
Sm N12 C13 C17 -32.5(4) . . . . ?
N12 C13 C14 C15 -0.8(3) . . . . ?
C17 C13 C14 C15 -177.8(2) . . . . ?
N12 N11 C15 C14 -1.2(3) . . . . ?
B N11 C15 C14 173.4(2) . . . . ?
N12 N11 C15 C16 174.0(2) . . . . ?
B N11 C15 C16 -11.4(4) . . . . ?
C13 C14 C15 N11 1.2(3) . . . . ?
C13 C14 C15 C16 -173.7(3) . . . . ?
N11 C15 C16 C16A -83.2(3) . . . . ?
C14 C15 C16 C16A 91.0(4) . . . . ?
N11 C15 C16 C16B 155.6(3) . . . . ?
C14 C15 C16 C16B -30.3(4) . . . . ?
N12 C13 C17 C17B -108.2(3) . . . . ?
C14 C13 C17 C17B 68.3(3) . . . . ?
N12 C13 C17 C17A 131.9(3) . . . . ?
C14 C13 C17 C17A -51.5(4) . . . . ?
N21 N22 C23 C24 0.3(3) . . . . ?
Sm N22 C23 C24 171.86(18) . . . . ?
N21 N22 C23 C27 179.8(3) . . . . ?
Sm N22 C23 C27 -8.7(4) . . . . ?
N22 C23 C24 C25 0.2(3) . . . . ?
C27 C23 C24 C25 -179.2(3) . . . . ?
N22 N21 C25 C24 0.8(3) . . . . ?
B N21 C25 C24 170.9(2) . . . . ?
N22 N21 C25 C26 178.4(2) . . . . ?
B N21 C25 C26 -11.6(4) . . . . ?
C23 C24 C25 N21 -0.6(3) . . . . ?
C23 C24 C25 C26 -178.0(3) . . . . ?
N21 C25 C26 C26B -81.1(3) . . . . ?
C24 C25 C26 C26B 95.9(3) . . . . ?
N21 C25 C26 C26A 155.7(3) . . . . ?
C24 C25 C26 C26A -27.3(4) . . . . ?
N22 C23 C27 C27A -135.7(3) . . . . ?
C24 C23 C27 C27A 43.7(4) . . . . ?
N22 C23 C27 C27B 101.3(3) . . . . ?
C24 C23 C27 C27B -79.4(4) . . . . ?
N31 N32 C33 C34 -1.2(3) . . . . ?
Sm N32 C33 C34 173.26(17) . . . . ?
N31 N32 C33 C37 175.7(2) . . . . ?
Sm N32 C33 C37 -9.8(4) . . . . ?
N32 C33 C34 C35 1.0(3) . . . . ?
C37 C33 C34 C35 -176.0(2) . . . . ?
N32 N31 C35 C34 -0.4(3) . . . . ?
B N31 C35 C34 -178.9(2) . . . . ?
N32 N31 C35 C36 177.3(2) . . . . ?
B N31 C35 C36 -1.2(4) . . . . ?
C33 C34 C35 N31 -0.3(3) . . . . ?
C33 C34 C35 C36 -178.0(2) . . . . ?
N31 C35 C36 C36B 160.6(3) . . . . ?
C34 C35 C36 C36B -22.2(4) . . . . ?
N31 C35 C36 C36A -76.4(3) . . . . ?
C34 C35 C36 C36A 100.8(3) . . . . ?
N32 C33 C37 C37B -104.0(3) . . . . ?
C34 C33 C37 C37B 72.5(3) . . . . ?
N32 C33 C37 C37A 135.7(3) . . . . ?
C34 C33 C37 C37A -47.8(3) . . . . ?
C15 N11 B N31 -128.2(2) . . . . ?
N12 N11 B N31 45.8(3) . . . . ?
C15 N11 B N21 104.1(3) . . . . ?
N12 N11 B N21 -81.9(3) . . . . ?
C35 N31 B N11 108.8(3) . . . . ?
N32 N31 B N11 -69.5(3) . . . . ?
C35 N31 B N21 -125.4(2) . . . . ?
N32 N31 B N21 56.2(3) . . . . ?
C25 N21 B N11 -113.4(3) . . . . ?
N22 N21 B N11 55.5(3) . . . . ?
C25 N21 B N31 120.8(3) . . . . ?
N22 N21 B N31 -70.3(3) . . . . ?
C1S C2S C3S C4S -61(2) . . . . ?
C2S C3S C4S C5S 165.8(14) . . . . ?

_refine_diff_density_max         0.976
_refine_diff_density_min         -1.028
_refine_diff_density_rms         0.077


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method pentane
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_tak1506
_database_code_depnum_ccdc_archive 'CCDC 1472924'
_audit_update_record             
;
2016-04-07 deposited with the CCDC.
2016-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H62 B N8 S5 Sm, C4 H8 O'
_chemical_formula_sum            'C40 H70 B N8 O S5 Sm'
_chemical_formula_weight         1000.50

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'
B B 0.0013 0.0007 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.8065(4)
_cell_length_b                   12.8567(4)
_cell_length_c                   18.9856(6)
_cell_angle_alpha                91.7130(4)
_cell_angle_beta                 101.7977(4)
_cell_angle_gamma                116.9095(3)
_cell_volume                     2490.68(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9584
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      27.10

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_F_000             1042
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.124
_exptl_absorpt_coefficient_mu    1.426
_shelx_estimated_absorpt_T_min   0.668
_shelx_estimated_absorpt_T_max   0.843
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7483
_exptl_absorpt_correction_T_max  0.8740
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21641
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_av_R_equivalents  0.0171
_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       24
_diffrn_reflns_theta_min         1.794
_diffrn_reflns_theta_max         27.106
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10973
_reflns_number_gt                10149
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0346P)²+1.4156P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10973
_refine_ls_number_parameters     505
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0260
_refine_ls_wR_factor_ref         0.0661
_refine_ls_wR_factor_gt          0.0641
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm Sm 0.25284(2) 0.14496(2) 0.22699(2) 0.02028(4) Uani 1 1 d . . . . .
S1 S 0.30869(6) 0.14263(6) 0.09315(3) 0.03191(13) Uani 1 1 d . . . . .
S2 S 0.41317(7) 0.07620(7) 0.15529(4) 0.04321(16) Uani 1 1 d . . . . .
S3 S 0.59675(7) 0.21768(9) 0.20208(4) 0.0599(2) Uani 1 1 d . . . . .
S4 S 0.54772(7) 0.32224(7) 0.26026(4) 0.04920(18) Uani 1 1 d . . . . .
S5 S 0.47591(6) 0.23772(7) 0.34233(3) 0.04217(16) Uani 1 1 d . . . . .
N11 N 0.01368(16) 0.16973(15) 0.29290(9) 0.0192(3) Uani 1 1 d . . . . .
N12 N 0.12093(16) 0.15037(15) 0.31548(9) 0.0210(3) Uani 1 1 d . . . . .
N21 N 0.05431(16) 0.27552(15) 0.18228(9) 0.0199(3) Uani 1 1 d . . . . .
N22 N 0.17970(16) 0.29417(15) 0.18372(9) 0.0215(3) Uani 1 1 d . . . . .
N31 N -0.07706(16) 0.05155(14) 0.16611(9) 0.0192(3) Uani 1 1 d . . . . .
N32 N 0.01876(16) 0.02149(14) 0.15811(9) 0.0197(3) Uani 1 1 d . . . . .
N41 N 0.17336(18) -0.05652(16) 0.27678(10) 0.0260(4) Uani 1 1 d . . . . .
N42 N 0.04501(18) -0.10969(16) 0.27937(10) 0.0275(4) Uani 1 1 d . . . . .
H42N H -0.0081 -0.0794 0.2655 0.033 Uiso 1 1 calc R U . . .
C13 C 0.1380(2) 0.14950(18) 0.38782(11) 0.0232(4) Uani 1 1 d . . . . .
C14 C 0.0449(2) 0.1696(2) 0.41149(12) 0.0267(4) Uani 1 1 d . . . . .
H14 H 0.0361 0.1738 0.4600 0.032 Uiso 1 1 calc R U . . .
C15 C -0.0321(2) 0.18220(18) 0.35068(11) 0.0225(4) Uani 1 1 d . . . . .
C16 C -0.1517(2) 0.1992(2) 0.34518(12) 0.0313(5) Uani 1 1 d . . . . .
H16 H -0.1637 0.2365 0.3007 0.038 Uiso 1 1 calc R U . . .
C16A C -0.2723(3) 0.0793(3) 0.33686(16) 0.0478(7) Uani 1 1 d . . . . .
H16A H -0.3501 0.0903 0.3333 0.057 Uiso 1 1 calc R U . . .
H16B H -0.2834 0.0306 0.2927 0.057 Uiso 1 1 calc R U . . .
H16C H -0.2608 0.0401 0.3792 0.057 Uiso 1 1 calc R U . . .
C16B C -0.1358(3) 0.2799(4) 0.41088(17) 0.0656(10) Uani 1 1 d . . . . .
H16D H -0.2149 0.2892 0.4058 0.079 Uiso 1 1 calc R U . . .
H16E H -0.1224 0.2453 0.4551 0.079 Uiso 1 1 calc R U . . .
H16F H -0.0600 0.3571 0.4140 0.079 Uiso 1 1 calc R U . . .
C17 C 0.2404(2) 0.1234(2) 0.43303(12) 0.0292(5) Uani 1 1 d . . . . .
H17 H 0.2889 0.1079 0.4001 0.035 Uiso 1 1 calc R U . . .
C17A C 0.1760(3) 0.0131(2) 0.46883(14) 0.0389(6) Uani 1 1 d . . . . .
H17A H 0.2439 -0.0026 0.4980 0.047 Uiso 1 1 calc R U . . .
H17B H 0.1258 0.0257 0.5003 0.047 Uiso 1 1 calc R U . . .
H17C H 0.1172 -0.0543 0.4312 0.047 Uiso 1 1 calc R U . . .
C17B C 0.3390(3) 0.2272(2) 0.49101(14) 0.0415(6) Uani 1 1 d . . . . .
H17D H 0.4039 0.2072 0.5193 0.050 Uiso 1 1 calc R U . . .
H17E H 0.3833 0.2964 0.4676 0.050 Uiso 1 1 calc R U . . .
H17F H 0.2930 0.2447 0.5234 0.050 Uiso 1 1 calc R U . . .
C23 C 0.2363(2) 0.39342(18) 0.15387(12) 0.0251(4) Uani 1 1 d . . . . .
C24 C 0.1481(2) 0.4379(2) 0.13355(13) 0.0294(5) Uani 1 1 d . . . . .
H24 H 0.1633 0.5066 0.1113 0.035 Uiso 1 1 calc R U . . .
C25 C 0.0345(2) 0.36225(18) 0.15220(11) 0.0244(4) Uani 1 1 d . . . . .
C26 C -0.0886(2) 0.3739(2) 0.14514(13) 0.0295(5) Uani 1 1 d . . . . .
H26 H -0.1600 0.2966 0.1513 0.035 Uiso 1 1 calc R U . . .
C26A C -0.0684(3) 0.4668(2) 0.20478(15) 0.0419(6) Uani 1 1 d . . . . .
H26A H -0.1491 0.4736 0.1996 0.050 Uiso 1 1 calc R U . . .
H26B H -0.0465 0.4438 0.2524 0.050 Uiso 1 1 calc R U . . .
H26C H 0.0032 0.5429 0.2007 0.050 Uiso 1 1 calc R U . . .
C26B C -0.1313(3) 0.4033(2) 0.06960(15) 0.0415(6) Uani 1 1 d . . . . .
H26D H -0.2113 0.4104 0.0664 0.050 Uiso 1 1 calc R U . . .
H26E H -0.0616 0.4779 0.0620 0.050 Uiso 1 1 calc R U . . .
H26F H -0.1481 0.3403 0.0323 0.050 Uiso 1 1 calc R U . . .
C27 C 0.3748(2) 0.4451(2) 0.14646(13) 0.0312(5) Uani 1 1 d . . . . .
H27 H 0.4046 0.3838 0.1536 0.037 Uiso 1 1 calc R U . . .
C27A C 0.4646(3) 0.5510(3) 0.20512(18) 0.0513(7) Uani 1 1 d . . . . .
H27A H 0.5547 0.5839 0.1997 0.062 Uiso 1 1 calc R U . . .
H27B H 0.4353 0.6112 0.2001 0.062 Uiso 1 1 calc R U . . .
H27C H 0.4614 0.5259 0.2532 0.062 Uiso 1 1 calc R U . . .
C27B C 0.3844(3) 0.4801(3) 0.07094(18) 0.0595(9) Uani 1 1 d . . . . .
H27D H 0.4757 0.5135 0.0677 0.071 Uiso 1 1 calc R U . . .
H27E H 0.3299 0.4104 0.0342 0.071 Uiso 1 1 calc R U . . .
H27F H 0.3537 0.5389 0.0624 0.071 Uiso 1 1 calc R U . . .
C33 C -0.0435(2) -0.08358(17) 0.11488(11) 0.0219(4) Uani 1 1 d . . . . .
C34 C -0.1779(2) -0.12132(18) 0.09612(11) 0.0247(4) Uani 1 1 d . . . . .
H34 H -0.2438 -0.1929 0.0670 0.030 Uiso 1 1 calc R U . . .
C35 C -0.1966(2) -0.03413(18) 0.12819(11) 0.0228(4) Uani 1 1 d . . . . .
C36 C -0.3215(2) -0.0253(2) 0.11939(13) 0.0295(5) Uani 1 1 d . . . . .
H36 H -0.3206 0.0120 0.1666 0.035 Uiso 1 1 calc R U . . .
C36A C -0.3299(2) 0.0523(2) 0.06111(13) 0.0343(5) Uani 1 1 d . . . . .
H36A H -0.4114 0.0576 0.0557 0.041 Uiso 1 1 calc R U . . .
H36B H -0.2549 0.1313 0.0755 0.041 Uiso 1 1 calc R U . . .
H36C H -0.3287 0.0177 0.0147 0.041 Uiso 1 1 calc R U . . .
C36B C -0.4414(2) -0.1472(3) 0.09925(19) 0.0500(7) Uani 1 1 d . . . . .
H36D H -0.5212 -0.1390 0.0939 0.060 Uiso 1 1 calc R U . . .
H36E H -0.4430 -0.1853 0.0533 0.060 Uiso 1 1 calc R U . . .
H36F H -0.4368 -0.1954 0.1377 0.060 Uiso 1 1 calc R U . . .
C37 C 0.0285(2) -0.14360(19) 0.09103(12) 0.0272(5) Uani 1 1 d . . . . .
H37 H 0.1231 -0.0976 0.1169 0.033 Uiso 1 1 calc R U . . .
C37A C 0.0174(3) -0.1453(2) 0.00903(13) 0.0345(5) Uani 1 1 d . . . . .
H37A H 0.0648 -0.1847 -0.0059 0.041 Uiso 1 1 calc R U . . .
H37B H -0.0750 -0.1880 -0.0172 0.041 Uiso 1 1 calc R U . . .
H37C H 0.0555 -0.0643 -0.0022 0.041 Uiso 1 1 calc R U . . .
C37B C -0.0228(3) -0.2692(2) 0.10977(15) 0.0416(6) Uani 1 1 d . . . . .
H37D H 0.0262 -0.3056 0.0935 0.050 Uiso 1 1 calc R U . . .
H37E H -0.0116 -0.2671 0.1625 0.050 Uiso 1 1 calc R U . . .
H37F H -0.1159 -0.3153 0.0854 0.050 Uiso 1 1 calc R U . . .
C43 C 0.0079(2) -0.21358(19) 0.30543(12) 0.0285(5) Uani 1 1 d . . . . .
C44 C 0.1181(2) -0.2289(2) 0.32156(13) 0.0328(5) Uani 1 1 d . . . . .
H44 H 0.1250 -0.2935 0.3412 0.039 Uiso 1 1 calc R U . . .
C45 C 0.2181(2) -0.1302(2) 0.30316(13) 0.0297(5) Uani 1 1 d . . . . .
C46 C 0.3576(3) -0.1039(3) 0.31105(17) 0.0438(7) Uani 1 1 d . . . . .
H46 H 0.4059 -0.0239 0.2971 0.053 Uiso 1 1 calc R U . . .
C46A C 0.3656(4) -0.1919(3) 0.2601(3) 0.0974(17) Uani 1 1 d . . . . .
H46A H 0.4575 -0.1734 0.2660 0.117 Uiso 1 1 calc R U . . .
H46B H 0.3162 -0.2715 0.2716 0.117 Uiso 1 1 calc R U . . .
H46C H 0.3284 -0.1877 0.2098 0.117 Uiso 1 1 calc R U . . .
C46B C 0.4203(3) -0.1008(4) 0.3902(2) 0.0970(17) Uani 1 1 d . . . . .
H46D H 0.5116 -0.0836 0.3951 0.116 Uiso 1 1 calc R U . . .
H46E H 0.4176 -0.0395 0.4206 0.116 Uiso 1 1 calc R U . . .
H46F H 0.3721 -0.1775 0.4057 0.116 Uiso 1 1 calc R U . . .
C47 C -0.1310(2) -0.2889(2) 0.31092(13) 0.0353(5) Uani 1 1 d . . . . .
H47 H -0.1797 -0.3429 0.2639 0.042 Uiso 1 1 calc R U . . .
C47A C -0.1346(3) -0.3658(3) 0.37058(18) 0.0581(8) Uani 1 1 d . . . . .
H47A H -0.2254 -0.4139 0.3733 0.070 Uiso 1 1 calc R U . . .
H47B H -0.0977 -0.4172 0.3597 0.070 Uiso 1 1 calc R U . . .
H47C H -0.0829 -0.3157 0.4172 0.070 Uiso 1 1 calc R U . . .
C47B C -0.1999(3) -0.2160(3) 0.31986(19) 0.0534(8) Uani 1 1 d . . . . .
H47D H -0.2895 -0.2680 0.3232 0.064 Uiso 1 1 calc R U . . .
H47E H -0.1522 -0.1590 0.3643 0.064 Uiso 1 1 calc R U . . .
H47F H -0.2024 -0.1739 0.2779 0.064 Uiso 1 1 calc R U . . .
B B -0.0427(2) 0.16881(19) 0.21146(12) 0.0192(4) Uani 1 1 d . . . . .
H1B H -0.1252 0.1751 0.2070 0.023 Uiso 1 1 calc R U . . .
O1S O 0.1752(3) 0.5506(2) 0.38338(13) 0.0731(7) Uani 1 1 d . . . . .
C1S C 0.2285(3) 0.4925(3) 0.34739(15) 0.0478(7) Uani 1 1 d . . . . .
H1SA H 0.2501 0.5277 0.3032 0.057 Uiso 1 1 calc R U . . .
H1SB H 0.1651 0.4078 0.3330 0.057 Uiso 1 1 calc R U . . .
C2S C 0.3493(3) 0.5073(4) 0.39975(17) 0.0623(9) Uani 1 1 d . . . . .
H2SA H 0.4259 0.5832 0.3987 0.075 Uiso 1 1 calc R U . . .
H2SB H 0.3689 0.4419 0.3899 0.075 Uiso 1 1 calc R U . . .
C3S C 0.3106(3) 0.5047(3) 0.47129(17) 0.0621(9) Uani 1 1 d . . . . .
H3SA H 0.2582 0.4229 0.4800 0.075 Uiso 1 1 calc R U . . .
H3SB H 0.3886 0.5461 0.5125 0.075 Uiso 1 1 calc R U . . .
C4S C 0.2305(4) 0.5686(3) 0.46023(18) 0.0706(11) Uani 1 1 d . . . . .
H4SA H 0.1603 0.5366 0.4866 0.085 Uiso 1 1 calc R U . . .
H4SB H 0.2863 0.6536 0.4782 0.085 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm N32 2.5090(17) . ?
Sm N22 2.5308(17) . ?
Sm N12 2.5326(17) . ?
Sm N41 2.6063(18) . ?
Sm S1 2.7551(6) . ?
Sm S5 2.7921(6) . ?
Sm S2 2.9519(6) . ?
Sm S4 3.0897(7) . ?
S1 S2 2.0154(9) . ?
S2 S3 2.0839(12) . ?
S3 S4 2.0591(13) . ?
S4 S5 2.0334(10) . ?
N11 C15 1.354(3) . ?
N11 N12 1.385(2) . ?
N11 B 1.551(3) . ?
N12 C13 1.348(3) . ?
N21 C25 1.358(3) . ?
N21 N22 1.383(2) . ?
N21 B 1.544(3) . ?
N22 C23 1.350(3) . ?
N31 C35 1.361(3) . ?
N31 N32 1.384(2) . ?
N31 B 1.551(3) . ?
N32 C33 1.352(3) . ?
N41 C45 1.342(3) . ?
N41 N42 1.364(3) . ?
N42 C43 1.349(3) . ?
C13 C14 1.389(3) . ?
C13 C17 1.507(3) . ?
C14 C15 1.379(3) . ?
C15 C16 1.507(3) . ?
C16 C16B 1.523(4) . ?
C16 C16A 1.528(4) . ?
C17 C17B 1.527(3) . ?
C17 C17A 1.531(3) . ?
C23 C24 1.395(3) . ?
C23 C27 1.501(3) . ?
C24 C25 1.380(3) . ?
C25 C26 1.507(3) . ?
C26 C26A 1.522(3) . ?
C26 C26B 1.537(3) . ?
C27 C27B 1.526(4) . ?
C27 C27A 1.529(4) . ?
C33 C34 1.394(3) . ?
C33 C37 1.501(3) . ?
C34 C35 1.383(3) . ?
C35 C36 1.506(3) . ?
C36 C36A 1.530(3) . ?
C36 C36B 1.530(3) . ?
C37 C37B 1.529(3) . ?
C37 C37A 1.534(3) . ?
C43 C44 1.378(3) . ?
C43 C47 1.509(3) . ?
C44 C45 1.402(3) . ?
C45 C46 1.497(3) . ?
C46 C46A 1.514(5) . ?
C46 C46B 1.524(5) . ?
C47 C47B 1.518(4) . ?
C47 C47A 1.520(4) . ?
O1S C1S 1.412(4) . ?
O1S C4S 1.436(4) . ?
C1S C2S 1.490(4) . ?
C2S C3S 1.516(5) . ?
C3S C4S 1.498(5) . ?

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
N32 Sm N22 76.00(5) . . ?
N32 Sm N12 75.60(5) . . ?
N22 Sm N12 77.22(5) . . ?
N32 Sm N41 74.19(5) . . ?
N22 Sm N41 142.63(6) . . ?
N12 Sm N41 73.95(6) . . ?
N32 Sm S1 84.99(4) . . ?
N22 Sm S1 84.37(4) . . ?
N12 Sm S1 155.88(4) . . ?
N41 Sm S1 114.64(4) . . ?
N32 Sm S5 159.45(4) . . ?
N22 Sm S5 113.99(4) . . ?
N12 Sm S5 88.81(4) . . ?
N41 Sm S5 88.82(4) . . ?
S1 Sm S5 113.101(19) . . ?
N32 Sm S2 106.92(4) . . ?
N22 Sm S2 122.99(4) . . ?
N12 Sm S2 159.79(4) . . ?
N41 Sm S2 87.29(4) . . ?
S1 Sm S2 41.178(19) . . ?
S5 Sm S2 83.21(2) . . ?
N32 Sm S4 160.48(4) . . ?
N22 Sm S4 94.17(4) . . ?
N12 Sm S4 119.19(4) . . ?
N41 Sm S4 120.54(4) . . ?
S1 Sm S4 77.20(2) . . ?
S5 Sm S4 40.05(2) . . ?
S2 Sm S4 64.06(2) . . ?
S2 S1 Sm 74.66(3) . . ?
S1 S2 S3 106.63(5) . . ?
S1 S2 Sm 64.17(2) . . ?
S3 S2 Sm 98.90(3) . . ?
S4 S3 S2 101.42(4) . . ?
S5 S4 S3 108.54(5) . . ?
S5 S4 Sm 62.07(2) . . ?
S3 S4 Sm 95.29(3) . . ?
S4 S5 Sm 77.88(3) . . ?
C15 N11 N12 109.88(16) . . ?
C15 N11 B 128.50(17) . . ?
N12 N11 B 121.53(16) . . ?
C13 N12 N11 105.97(16) . . ?
C13 N12 Sm 133.35(14) . . ?
N11 N12 Sm 120.33(12) . . ?
C25 N21 N22 109.89(16) . . ?
C25 N21 B 128.15(17) . . ?
N22 N21 B 121.96(16) . . ?
C23 N22 N21 106.28(16) . . ?
C23 N22 Sm 133.03(14) . . ?
N21 N22 Sm 120.47(12) . . ?
C35 N31 N32 109.70(16) . . ?
C35 N31 B 128.67(17) . . ?
N32 N31 B 121.62(15) . . ?
C33 N32 N31 106.47(16) . . ?
C33 N32 Sm 132.21(13) . . ?
N31 N32 Sm 121.05(11) . . ?
C45 N41 N42 104.35(18) . . ?
C45 N41 Sm 140.74(15) . . ?
N42 N41 Sm 114.91(13) . . ?
C43 N42 N41 113.00(18) . . ?
N12 C13 C14 110.08(18) . . ?
N12 C13 C17 122.90(19) . . ?
C14 C13 C17 126.95(19) . . ?
C15 C14 C13 106.39(19) . . ?
N11 C15 C14 107.67(18) . . ?
N11 C15 C16 123.91(19) . . ?
C14 C15 C16 128.32(19) . . ?
C15 C16 C16B 111.3(2) . . ?
C15 C16 C16A 109.4(2) . . ?
C16B C16 C16A 110.9(2) . . ?
C13 C17 C17B 111.7(2) . . ?
C13 C17 C17A 110.56(19) . . ?
C17B C17 C17A 109.9(2) . . ?
N22 C23 C24 109.78(19) . . ?
N22 C23 C27 122.9(2) . . ?
C24 C23 C27 127.3(2) . . ?
C25 C24 C23 106.47(19) . . ?
N21 C25 C24 107.59(19) . . ?
N21 C25 C26 124.65(19) . . ?
C24 C25 C26 127.69(19) . . ?
C25 C26 C26A 110.22(19) . . ?
C25 C26 C26B 111.0(2) . . ?
C26A C26 C26B 110.9(2) . . ?
C23 C27 C27B 111.3(2) . . ?
C23 C27 C27A 110.3(2) . . ?
C27B C27 C27A 110.6(2) . . ?
N32 C33 C34 109.72(18) . . ?
N32 C33 C37 122.51(19) . . ?
C34 C33 C37 127.74(19) . . ?
C35 C34 C33 106.51(18) . . ?
N31 C35 C34 107.58(18) . . ?
N31 C35 C36 123.98(19) . . ?
C34 C35 C36 128.23(19) . . ?
C35 C36 C36A 109.95(18) . . ?
C35 C36 C36B 111.1(2) . . ?
C36A C36 C36B 110.0(2) . . ?
C33 C37 C37B 111.7(2) . . ?
C33 C37 C37A 110.23(18) . . ?
C37B C37 C37A 109.91(19) . . ?
N42 C43 C44 105.7(2) . . ?
N42 C43 C47 121.8(2) . . ?
C44 C43 C47 132.5(2) . . ?
C43 C44 C45 106.3(2) . . ?
N41 C45 C44 110.6(2) . . ?
N41 C45 C46 122.0(2) . . ?
C44 C45 C46 127.4(2) . . ?
C45 C46 C46A 110.5(3) . . ?
C45 C46 C46B 109.7(2) . . ?
C46A C46 C46B 112.4(3) . . ?
C43 C47 C47B 112.0(2) . . ?
C43 C47 C47A 110.6(2) . . ?
C47B C47 C47A 112.5(3) . . ?
N21 B N31 110.97(16) . . ?
N21 B N11 110.73(16) . . ?
N31 B N11 110.64(16) . . ?
C1S O1S C4S 109.1(2) . . ?
O1S C1S C2S 106.6(2) . . ?
C1S C2S C3S 101.3(3) . . ?
C4S C3S C2S 102.3(3) . . ?
O1S C4S C3S 106.3(3) . . ?

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
N32 Sm S1 S2 -122.96(5) . . . . ?
N22 Sm S1 S2 160.66(5) . . . . ?
N12 Sm S1 S2 -159.18(10) . . . . ?
N41 Sm S1 S2 -52.90(5) . . . . ?
S5 Sm S1 S2 46.94(4) . . . . ?
S4 Sm S1 S2 65.07(3) . . . . ?
Sm S1 S2 S3 -91.99(3) . . . . ?
N32 Sm S2 S1 60.89(5) . . . . ?
N22 Sm S2 S1 -23.14(6) . . . . ?
N12 Sm S2 S1 155.14(11) . . . . ?
N41 Sm S2 S1 133.47(5) . . . . ?
S5 Sm S2 S1 -137.40(3) . . . . ?
S4 Sm S2 S1 -100.47(3) . . . . ?
N32 Sm S2 S3 165.14(5) . . . . ?
N22 Sm S2 S3 81.10(6) . . . . ?
N12 Sm S2 S3 -100.61(12) . . . . ?
N41 Sm S2 S3 -122.29(5) . . . . ?
S1 Sm S2 S3 104.24(4) . . . . ?
S5 Sm S2 S3 -33.16(3) . . . . ?
S4 Sm S2 S3 3.77(3) . . . . ?
S1 S2 S3 S4 60.37(5) . . . . ?
Sm S2 S3 S4 -5.20(4) . . . . ?
S2 S3 S4 S5 67.21(5) . . . . ?
S2 S3 S4 Sm 4.93(4) . . . . ?
N32 Sm S4 S5 -178.20(12) . . . . ?
N22 Sm S4 S5 123.15(5) . . . . ?
N12 Sm S4 S5 45.47(6) . . . . ?
N41 Sm S4 S5 -42.35(6) . . . . ?
S1 Sm S4 S5 -153.59(4) . . . . ?
S2 Sm S4 S5 -111.99(4) . . . . ?
N32 Sm S4 S3 -70.00(13) . . . . ?
N22 Sm S4 S3 -128.65(5) . . . . ?
N12 Sm S4 S3 153.67(5) . . . . ?
N41 Sm S4 S3 65.85(6) . . . . ?
S1 Sm S4 S3 -45.39(3) . . . . ?
S5 Sm S4 S3 108.20(5) . . . . ?
S2 Sm S4 S3 -3.79(3) . . . . ?
S3 S4 S5 Sm -86.12(4) . . . . ?
N32 Sm S5 S4 178.29(11) . . . . ?
N22 Sm S5 S4 -66.06(5) . . . . ?
N12 Sm S5 S4 -141.50(5) . . . . ?
N41 Sm S5 S4 144.53(5) . . . . ?
S1 Sm S5 S4 28.13(4) . . . . ?
S2 Sm S5 S4 57.11(3) . . . . ?
C15 N11 N12 C13 0.9(2) . . . . ?
B N11 N12 C13 -176.07(17) . . . . ?
C15 N11 N12 Sm -173.12(13) . . . . ?
B N11 N12 Sm 9.9(2) . . . . ?
N32 Sm N12 C13 142.44(19) . . . . ?
N22 Sm N12 C13 -138.97(19) . . . . ?
N41 Sm N12 C13 65.08(19) . . . . ?
S1 Sm N12 C13 179.87(14) . . . . ?
S5 Sm N12 C13 -24.03(18) . . . . ?
S2 Sm N12 C13 42.5(3) . . . . ?
S4 Sm N12 C13 -51.3(2) . . . . ?
N32 Sm N12 N11 -45.44(13) . . . . ?
N22 Sm N12 N11 33.15(13) . . . . ?
N41 Sm N12 N11 -122.79(14) . . . . ?
S1 Sm N12 N11 -8.0(2) . . . . ?
S5 Sm N12 N11 148.09(13) . . . . ?
S2 Sm N12 N11 -145.37(11) . . . . ?
S4 Sm N12 N11 120.79(13) . . . . ?
C25 N21 N22 C23 -0.2(2) . . . . ?
B N21 N22 C23 179.51(17) . . . . ?
C25 N21 N22 Sm -175.46(13) . . . . ?
B N21 N22 Sm 4.2(2) . . . . ?
N32 Sm N22 C23 -136.15(19) . . . . ?
N12 Sm N22 C23 145.75(19) . . . . ?
N41 Sm N22 C23 -174.06(16) . . . . ?
S1 Sm N22 C23 -49.93(18) . . . . ?
S5 Sm N22 C23 62.88(19) . . . . ?
S2 Sm N22 C23 -34.9(2) . . . . ?
S4 Sm N22 C23 26.75(19) . . . . ?
N32 Sm N22 N21 37.65(13) . . . . ?
N12 Sm N22 N21 -40.45(13) . . . . ?
N41 Sm N22 N21 -0.26(19) . . . . ?
S1 Sm N22 N21 123.88(13) . . . . ?
S5 Sm N22 N21 -123.31(13) . . . . ?
S2 Sm N22 N21 138.95(12) . . . . ?
S4 Sm N22 N21 -159.45(13) . . . . ?
C35 N31 N32 C33 0.0(2) . . . . ?
B N31 N32 C33 -178.89(17) . . . . ?
C35 N31 N32 Sm -174.76(13) . . . . ?
B N31 N32 Sm 6.4(2) . . . . ?
N22 Sm N32 C33 143.79(18) . . . . ?
N12 Sm N32 C33 -136.08(18) . . . . ?
N41 Sm N32 C33 -59.02(18) . . . . ?
S1 Sm N32 C33 58.35(17) . . . . ?
S5 Sm N32 C33 -94.3(2) . . . . ?
S2 Sm N32 C33 23.08(18) . . . . ?
S4 Sm N32 C33 82.4(2) . . . . ?
N22 Sm N32 N31 -43.05(13) . . . . ?
N12 Sm N32 N31 37.08(13) . . . . ?
N41 Sm N32 N31 114.15(14) . . . . ?
S1 Sm N32 N31 -128.48(13) . . . . ?
S5 Sm N32 N31 78.87(18) . . . . ?
S2 Sm N32 N31 -163.76(12) . . . . ?
S4 Sm N32 N31 -104.42(16) . . . . ?
N32 Sm N41 C45 146.8(2) . . . . ?
N22 Sm N41 C45 -174.9(2) . . . . ?
N12 Sm N41 C45 -134.0(2) . . . . ?
S1 Sm N41 C45 70.1(2) . . . . ?
S5 Sm N41 C45 -44.9(2) . . . . ?
S2 Sm N41 C45 38.4(2) . . . . ?
S4 Sm N41 C45 -19.2(3) . . . . ?
N32 Sm N41 N42 -34.19(14) . . . . ?
N22 Sm N41 N42 4.10(19) . . . . ?
N12 Sm N41 N42 45.00(14) . . . . ?
S1 Sm N41 N42 -110.91(14) . . . . ?
S5 Sm N41 N42 134.11(14) . . . . ?
S2 Sm N41 N42 -142.63(14) . . . . ?
S4 Sm N41 N42 159.80(12) . . . . ?
C45 N41 N42 C43 -0.7(2) . . . . ?
Sm N41 N42 C43 -179.99(14) . . . . ?
N11 N12 C13 C14 -0.9(2) . . . . ?
Sm N12 C13 C14 172.08(14) . . . . ?
N11 N12 C13 C17 176.10(19) . . . . ?
Sm N12 C13 C17 -11.0(3) . . . . ?
N12 C13 C14 C15 0.5(3) . . . . ?
C17 C13 C14 C15 -176.3(2) . . . . ?
N12 N11 C15 C14 -0.7(2) . . . . ?
B N11 C15 C14 176.08(19) . . . . ?
N12 N11 C15 C16 -177.27(19) . . . . ?
B N11 C15 C16 -0.5(3) . . . . ?
C13 C14 C15 N11 0.1(2) . . . . ?
C13 C14 C15 C16 176.5(2) . . . . ?
N11 C15 C16 C16B -145.4(3) . . . . ?
C14 C15 C16 C16B 38.7(4) . . . . ?
N11 C15 C16 C16A 91.6(3) . . . . ?
C14 C15 C16 C16A -84.3(3) . . . . ?
N12 C13 C17 C17B 118.9(2) . . . . ?
C14 C13 C17 C17B -64.7(3) . . . . ?
N12 C13 C17 C17A -118.4(2) . . . . ?
C14 C13 C17 C17A 58.0(3) . . . . ?
N21 N22 C23 C24 0.0(2) . . . . ?
Sm N22 C23 C24 174.45(15) . . . . ?
N21 N22 C23 C27 178.97(19) . . . . ?
Sm N22 C23 C27 -6.6(3) . . . . ?
N22 C23 C24 C25 0.2(3) . . . . ?
C27 C23 C24 C25 -178.7(2) . . . . ?
N22 N21 C25 C24 0.3(2) . . . . ?
B N21 C25 C24 -179.39(19) . . . . ?
N22 N21 C25 C26 -176.83(19) . . . . ?
B N21 C25 C26 3.5(3) . . . . ?
C23 C24 C25 N21 -0.3(3) . . . . ?
C23 C24 C25 C26 176.7(2) . . . . ?
N21 C25 C26 C26A 100.6(2) . . . . ?
C24 C25 C26 C26A -75.9(3) . . . . ?
N21 C25 C26 C26B -136.0(2) . . . . ?
C24 C25 C26 C26B 47.4(3) . . . . ?
N22 C23 C27 C27B 134.3(3) . . . . ?
C24 C23 C27 C27B -46.9(3) . . . . ?
N22 C23 C27 C27A -102.6(3) . . . . ?
C24 C23 C27 C27A 76.2(3) . . . . ?
N31 N32 C33 C34 -0.8(2) . . . . ?
Sm N32 C33 C34 173.13(14) . . . . ?
N31 N32 C33 C37 177.53(18) . . . . ?
Sm N32 C33 C37 -8.6(3) . . . . ?
N32 C33 C34 C35 1.3(2) . . . . ?
C37 C33 C34 C35 -176.9(2) . . . . ?
N32 N31 C35 C34 0.8(2) . . . . ?
B N31 C35 C34 179.57(19) . . . . ?
N32 N31 C35 C36 -174.36(19) . . . . ?
B N31 C35 C36 4.4(3) . . . . ?
C33 C34 C35 N31 -1.2(2) . . . . ?
C33 C34 C35 C36 173.7(2) . . . . ?
N31 C35 C36 C36A 78.6(3) . . . . ?
C34 C35 C36 C36A -95.5(3) . . . . ?
N31 C35 C36 C36B -159.4(2) . . . . ?
C34 C35 C36 C36B 26.5(3) . . . . ?
N32 C33 C37 C37B 125.6(2) . . . . ?
C34 C33 C37 C37B -56.4(3) . . . . ?
N32 C33 C37 C37A -111.9(2) . . . . ?
C34 C33 C37 C37A 66.1(3) . . . . ?
N41 N42 C43 C44 0.7(3) . . . . ?
N41 N42 C43 C47 -178.2(2) . . . . ?
N42 C43 C44 C45 -0.4(3) . . . . ?
C47 C43 C44 C45 178.3(2) . . . . ?
N42 N41 C45 C44 0.4(3) . . . . ?
Sm N41 C45 C44 179.43(17) . . . . ?
N42 N41 C45 C46 -178.9(2) . . . . ?
Sm N41 C45 C46 0.1(4) . . . . ?
C43 C44 C45 N41 0.0(3) . . . . ?
C43 C44 C45 C46 179.3(2) . . . . ?
N41 C45 C46 C46A -114.0(3) . . . . ?
C44 C45 C46 C46A 66.8(4) . . . . ?
N41 C45 C46 C46B 121.5(3) . . . . ?
C44 C45 C46 C46B -57.8(4) . . . . ?
N42 C43 C47 C47B -27.4(3) . . . . ?
C44 C43 C47 C47B 154.1(3) . . . . ?
N42 C43 C47 C47A -153.8(2) . . . . ?
C44 C43 C47 C47A 27.7(4) . . . . ?
C25 N21 B N31 115.6(2) . . . . ?
N22 N21 B N31 -64.0(2) . . . . ?
C25 N21 B N11 -121.1(2) . . . . ?
N22 N21 B N11 59.3(2) . . . . ?
C35 N31 B N21 -121.1(2) . . . . ?
N32 N31 B N21 57.5(2) . . . . ?
C35 N31 B N11 115.6(2) . . . . ?
N32 N31 B N11 -65.8(2) . . . . ?
C15 N11 B N21 115.3(2) . . . . ?
N12 N11 B N21 -68.3(2) . . . . ?
C15 N11 B N31 -121.2(2) . . . . ?
N12 N11 B N31 55.2(2) . . . . ?
C4S O1S C1S C2S -17.6(4) . . . . ?
O1S C1S C2S C3S 34.1(4) . . . . ?
C1S C2S C3S C4S -36.8(4) . . . . ?
C1S O1S C4S C3S -6.7(4) . . . . ?
C2S C3S C4S O1S 27.5(4) . . . . ?

_refine_diff_density_max         1.219
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.070


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method THF
