# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_compound3
_database_code_depnum_ccdc_archive 'CCDC 1048745'
_audit_update_record             
;
2015-02-11 deposited with the CCDC.
2015-03-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C55 H77 Ge N O4 Si'
_chemical_formula_weight         916.86

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'
O O 0.0106 0.0060 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 '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                   11.9476(4)
_cell_length_b                   13.7236(4)
_cell_length_c                   16.2518(5)
_cell_angle_alpha                81.454(3)
_cell_angle_beta                 83.839(2)
_cell_angle_gamma                80.731(3)
_cell_volume                     2591.21(14)
_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       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             984
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_T_max  0.943
_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  graphite
_diffrn_measurement_device_type  'Bruker Apex X8'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26342
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         25.50
_reflns_number_total             9642
_reflns_number_gt                8386
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
 A molecule of hexane of crystallisation was located in the asymmetric unit
 and its carbon atoms refined anisotropically.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0668P)²+4.5937P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9642
_refine_ls_number_parameters     574
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1344
_refine_ls_wR_factor_gt          0.1277
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.047
_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
Ge1 Ge 0.56721(2) 0.64816(2) 0.668229(17) 0.01767(10) Uani 1 1 d . . .
Si1 Si 0.67660(6) 0.81303(5) 0.75110(4) 0.01521(16) Uani 1 1 d . . .
O1 O 0.58881(16) 0.90240(14) 0.70717(12) 0.0215(4) Uani 1 1 d . . .
N1 N 0.68156(18) 0.70353(17) 0.70775(13) 0.0148(4) Uani 1 1 d . . .
C1 C 0.7870(2) 0.63440(19) 0.71059(15) 0.0127(5) Uani 1 1 d . . .
O2 O 0.80430(16) 0.84131(14) 0.73636(12) 0.0194(4) Uani 1 1 d . . .
C2 C 0.8080(2) 0.56290(19) 0.78067(15) 0.0137(5) Uani 1 1 d . . .
O3 O 0.63786(17) 0.79510(15) 0.85003(12) 0.0219(4) Uani 1 1 d . . .
C3 C 0.9121(2) 0.50023(19) 0.78260(15) 0.0146(5) Uani 1 1 d . . .
H3 H 0.9257 0.4525 0.8305 0.017 Uiso 1 1 calc R . .
O4 O 0.45306(17) 0.74800(16) 0.68365(15) 0.0319(5) Uani 1 1 d . . .
C4 C 0.9963(2) 0.50512(19) 0.71705(16) 0.0150(5) Uani 1 1 d . . .
C5 C 0.9727(2) 0.57371(19) 0.64649(15) 0.0141(5) Uani 1 1 d . . .
H5 H 1.0287 0.5775 0.6005 0.017 Uiso 1 1 calc R . .
C6 C 0.8692(2) 0.63675(19) 0.64161(15) 0.0130(5) Uani 1 1 d . . .
C7 C 0.8401(2) 0.70291(19) 0.56063(15) 0.0144(5) Uani 1 1 d . . .
H7 H 0.7959 0.7666 0.5766 0.017 Uiso 1 1 calc R . .
C8 C 0.7616(2) 0.6566(2) 0.51427(15) 0.0154(5) Uani 1 1 d . . .
C9 C 0.7621(2) 0.5546(2) 0.52191(17) 0.0211(6) Uani 1 1 d . . .
H9 H 0.8134 0.5112 0.5564 0.025 Uiso 1 1 calc R . .
C10 C 0.6885(3) 0.5152(2) 0.47958(18) 0.0275(7) Uani 1 1 d . . .
H10 H 0.6901 0.4450 0.4854 0.033 Uiso 1 1 calc R . .
C11 C 0.6131(3) 0.5769(3) 0.42919(19) 0.0302(7) Uani 1 1 d . . .
H11 H 0.5613 0.5500 0.4016 0.036 Uiso 1 1 calc R . .
C12 C 0.6141(3) 0.6786(3) 0.4196(2) 0.0311(7) Uani 1 1 d . . .
H12 H 0.5639 0.7218 0.3841 0.037 Uiso 1 1 calc R . .
C13 C 0.6877(2) 0.7180(2) 0.46135(18) 0.0232(6) Uani 1 1 d . . .
H13 H 0.6878 0.7880 0.4538 0.028 Uiso 1 1 calc R . .
C14 C 0.9428(2) 0.7307(2) 0.50308(16) 0.0166(5) Uani 1 1 d . . .
C15 C 0.9944(2) 0.6722(2) 0.44268(17) 0.0233(6) Uani 1 1 d . . .
H15 H 0.9673 0.6120 0.4381 0.028 Uiso 1 1 calc R . .
C16 C 1.0853(3) 0.7010(3) 0.38884(19) 0.0320(7) Uani 1 1 d . . .
H16 H 1.1199 0.6605 0.3478 0.038 Uiso 1 1 calc R . .
C17 C 1.1252(3) 0.7877(3) 0.3949(2) 0.0353(8) Uani 1 1 d . . .
H17 H 1.1867 0.8076 0.3577 0.042 Uiso 1 1 calc R . .
C18 C 1.0754(3) 0.8459(3) 0.4553(2) 0.0351(8) Uani 1 1 d . . .
H18 H 1.1035 0.9056 0.4601 0.042 Uiso 1 1 calc R . .
C19 C 0.9847(3) 0.8175(2) 0.50885(19) 0.0260(6) Uani 1 1 d . . .
H19 H 0.9509 0.8581 0.5501 0.031 Uiso 1 1 calc R . .
C20 C 0.7150(2) 0.5497(2) 0.85182(15) 0.0154(5) Uani 1 1 d . . .
H20 H 0.6707 0.6173 0.8564 0.019 Uiso 1 1 calc R . .
C21 C 0.6317(2) 0.4850(2) 0.83176(16) 0.0188(6) Uani 1 1 d . . .
C22 C 0.5199(3) 0.4975(3) 0.86810(19) 0.0287(7) Uani 1 1 d . . .
H22 H 0.4971 0.5457 0.9053 0.034 Uiso 1 1 calc R . .
C23 C 0.4419(3) 0.4407(3) 0.8508(2) 0.0382(8) Uani 1 1 d . . .
H23 H 0.3662 0.4504 0.8761 0.046 Uiso 1 1 calc R . .
C24 C 0.4728(3) 0.3705(3) 0.7975(2) 0.0375(8) Uani 1 1 d . . .
H24 H 0.4187 0.3321 0.7853 0.045 Uiso 1 1 calc R . .
C25 C 0.5828(3) 0.3563(3) 0.7618(2) 0.0381(8) Uani 1 1 d . . .
H25 H 0.6051 0.3072 0.7254 0.046 Uiso 1 1 calc R . .
C26 C 0.6616(3) 0.4134(2) 0.77871(19) 0.0287(7) Uani 1 1 d . . .
H26 H 0.7372 0.4031 0.7534 0.034 Uiso 1 1 calc R . .
C27 C 0.7641(2) 0.5127(2) 0.93585(15) 0.0165(5) Uani 1 1 d . . .
C28 C 0.7609(2) 0.4173(2) 0.97706(17) 0.0219(6) Uani 1 1 d . . .
H28 H 0.7242 0.3723 0.9541 0.026 Uiso 1 1 calc R . .
C29 C 0.8112(3) 0.3868(2) 1.05185(18) 0.0263(6) Uani 1 1 d . . .
H29 H 0.8088 0.3210 1.0796 0.032 Uiso 1 1 calc R . .
C30 C 0.8646(2) 0.4516(2) 1.08608(17) 0.0227(6) Uani 1 1 d . . .
H30 H 0.8994 0.4306 1.1369 0.027 Uiso 1 1 calc R . .
C31 C 0.8669(2) 0.5472(2) 1.04564(17) 0.0219(6) Uani 1 1 d . . .
H31 H 0.9032 0.5921 1.0688 0.026 Uiso 1 1 calc R . .
C32 C 0.8166(2) 0.5778(2) 0.97161(17) 0.0199(6) Uani 1 1 d . . .
H32 H 0.8178 0.6441 0.9448 0.024 Uiso 1 1 calc R . .
C33 C 1.1095(2) 0.4382(2) 0.72120(17) 0.0200(6) Uani 1 1 d . . .
H33A H 1.1569 0.4633 0.7566 0.030 Uiso 1 1 calc R . .
H33B H 1.1479 0.4375 0.6649 0.030 Uiso 1 1 calc R . .
H33C H 1.0972 0.3705 0.7449 0.030 Uiso 1 1 calc R . .
C34 C 0.5967(2) 0.9903(2) 0.64823(18) 0.0203(6) Uani 1 1 d . . .
C35 C 0.4808(2) 1.0186(2) 0.6144(2) 0.0264(6) Uani 1 1 d . . .
H35A H 0.4651 0.9648 0.5858 0.040 Uiso 1 1 calc R . .
H35B H 0.4801 1.0799 0.5748 0.040 Uiso 1 1 calc R . .
H35C H 0.4224 1.0293 0.6606 0.040 Uiso 1 1 calc R . .
C36 C 0.6878(3) 0.9695(2) 0.57784(19) 0.0274(7) Uani 1 1 d . . .
H36A H 0.7622 0.9509 0.6004 0.041 Uiso 1 1 calc R . .
H36B H 0.6887 1.0293 0.5367 0.041 Uiso 1 1 calc R . .
H36C H 0.6711 0.9147 0.5509 0.041 Uiso 1 1 calc R . .
C37 C 0.6220(3) 1.0724(2) 0.6931(2) 0.0337(7) Uani 1 1 d . . .
H37A H 0.5592 1.0883 0.7353 0.051 Uiso 1 1 calc R . .
H37B H 0.6305 1.1319 0.6528 0.051 Uiso 1 1 calc R . .
H37C H 0.6927 1.0502 0.7204 0.051 Uiso 1 1 calc R . .
C38 C 0.8961(2) 0.8577(2) 0.78131(18) 0.0219(6) Uani 1 1 d . . .
C39 C 0.9801(3) 0.7622(2) 0.7896(2) 0.0310(7) Uani 1 1 d . . .
H39A H 0.9431 0.7089 0.8231 0.047 Uiso 1 1 calc R . .
H39B H 1.0456 0.7724 0.8171 0.047 Uiso 1 1 calc R . .
H39C H 1.0058 0.7435 0.7340 0.047 Uiso 1 1 calc R . .
C40 C 0.8522(3) 0.8879(3) 0.8664(2) 0.0369(8) Uani 1 1 d . . .
H40A H 0.7941 0.9470 0.8596 0.055 Uiso 1 1 calc R . .
H40B H 0.9154 0.9030 0.8938 0.055 Uiso 1 1 calc R . .
H40C H 0.8188 0.8331 0.9007 0.055 Uiso 1 1 calc R . .
C41 C 0.9508(3) 0.9406(2) 0.7281(2) 0.0273(7) Uani 1 1 d . . .
H41A H 0.9770 0.9210 0.6729 0.041 Uiso 1 1 calc R . .
H41B H 1.0159 0.9529 0.7550 0.041 Uiso 1 1 calc R . .
H41C H 0.8951 1.0014 0.7221 0.041 Uiso 1 1 calc R . .
C42 C 0.5392(3) 0.8255(2) 0.90504(18) 0.0265(6) Uani 1 1 d . . .
C43 C 0.4338(4) 0.8035(5) 0.8722(3) 0.0684(14) Uani 1 1 d . . .
H43A H 0.4274 0.8376 0.8151 0.103 Uiso 1 1 calc R . .
H43B H 0.3666 0.8272 0.9080 0.103 Uiso 1 1 calc R . .
H43C H 0.4389 0.7315 0.8723 0.103 Uiso 1 1 calc R . .
C44 C 0.5609(4) 0.7735(5) 0.9891(2) 0.092(2) Uani 1 1 d . . .
H44A H 0.5767 0.7015 0.9874 0.139 Uiso 1 1 calc R . .
H44B H 0.4937 0.7887 1.0279 0.139 Uiso 1 1 calc R . .
H44C H 0.6265 0.7958 1.0080 0.139 Uiso 1 1 calc R . .
C45 C 0.5238(6) 0.9366(4) 0.9038(4) 0.091(2) Uani 1 1 d . . .
H45A H 0.5941 0.9561 0.9179 0.136 Uiso 1 1 calc R . .
H45B H 0.4612 0.9567 0.9448 0.136 Uiso 1 1 calc R . .
H45C H 0.5061 0.9695 0.8480 0.136 Uiso 1 1 calc R . .
C46 C 0.3422(2) 0.7452(2) 0.6562(2) 0.0317(7) Uani 1 1 d . . .
C47 C 0.3529(3) 0.7479(3) 0.5617(2) 0.0392(8) Uani 1 1 d . . .
H47A H 0.3832 0.8084 0.5353 0.059 Uiso 1 1 calc R . .
H47B H 0.2777 0.7480 0.5427 0.059 Uiso 1 1 calc R . .
H47C H 0.4045 0.6892 0.5463 0.059 Uiso 1 1 calc R . .
C48 C 0.2949(3) 0.6526(2) 0.6996(2) 0.0329(7) Uani 1 1 d . . .
H48A H 0.3432 0.5931 0.6822 0.049 Uiso 1 1 calc R . .
H48B H 0.2173 0.6545 0.6844 0.049 Uiso 1 1 calc R . .
H48C H 0.2937 0.6504 0.7603 0.049 Uiso 1 1 calc R . .
C49 C 0.2656(3) 0.8379(3) 0.6805(3) 0.0496(11) Uani 1 1 d . . .
H49A H 0.2602 0.8363 0.7412 0.074 Uiso 1 1 calc R . .
H49B H 0.1896 0.8400 0.6622 0.074 Uiso 1 1 calc R . .
H49C H 0.2977 0.8973 0.6536 0.074 Uiso 1 1 calc R . .
C50 C 0.7690(6) 1.1511(5) 0.9264(5) 0.117(2) Uani 1 1 d DU . .
H50A H 0.7876 1.0858 0.9595 0.176 Uiso 1 1 calc R . .
H50B H 0.7031 1.1509 0.8954 0.176 Uiso 1 1 calc R . .
H50C H 0.7509 1.2025 0.9637 0.176 Uiso 1 1 calc R . .
C51 C 0.8671(5) 1.1725(4) 0.8674(4) 0.091(2) Uani 1 1 d D . .
H51A H 0.8551 1.2437 0.8435 0.110 Uiso 1 1 calc R . .
H51B H 0.8724 1.1323 0.8210 0.110 Uiso 1 1 calc R . .
C52 C 0.9780(5) 1.1494(6) 0.9091(4) 0.112(2) Uani 1 1 d D . .
H52A H 0.9787 1.1969 0.9492 0.134 Uiso 1 1 calc R . .
H52B H 0.9856 1.0812 0.9400 0.134 Uiso 1 1 calc R . .
C53 C 1.0754(5) 1.1579(6) 0.8426(5) 0.108(2) Uani 1 1 d DU . .
H53A H 1.0787 1.1042 0.8076 0.129 Uiso 1 1 calc R . .
H53B H 1.0589 1.2222 0.8063 0.129 Uiso 1 1 calc R . .
C54 C 1.1882(5) 1.1522(6) 0.8733(4) 0.107(2) Uani 1 1 d D . .
H54A H 1.2014 1.0923 0.9153 0.128 Uiso 1 1 calc R . .
H54B H 1.1893 1.2114 0.9012 0.128 Uiso 1 1 calc R . .
C55 C 1.2819(6) 1.1473(6) 0.8051(5) 0.123(3) Uani 1 1 d DU . .
H55A H 1.2720 1.0975 0.7701 0.184 Uiso 1 1 calc R . .
H55B H 1.3552 1.1285 0.8294 0.184 Uiso 1 1 calc R . .
H55C H 1.2802 1.2126 0.7710 0.184 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 O4 1.796(2) . ?
Ge1 N1 1.877(2) . ?
Si1 O1 1.613(2) . ?
Si1 O3 1.618(2) . ?
Si1 O2 1.6188(19) . ?
Si1 N1 1.742(2) . ?
O1 C34 1.433(3) . ?
N1 C1 1.450(3) . ?
C1 C2 1.405(4) . ?
C1 C6 1.409(4) . ?
O2 C38 1.445(3) . ?
C2 C3 1.393(4) . ?
C2 C20 1.527(3) . ?
O3 C42 1.445(3) . ?
C3 C4 1.387(4) . ?
O4 C46 1.450(4) . ?
C4 C5 1.394(4) . ?
C4 C33 1.509(4) . ?
C5 C6 1.392(4) . ?
C6 C7 1.523(3) . ?
C7 C14 1.524(4) . ?
C7 C8 1.528(4) . ?
C8 C9 1.386(4) . ?
C8 C13 1.391(4) . ?
C9 C10 1.391(4) . ?
C10 C11 1.381(5) . ?
C11 C12 1.383(5) . ?
C12 C13 1.385(4) . ?
C14 C19 1.384(4) . ?
C14 C15 1.390(4) . ?
C15 C16 1.391(4) . ?
C16 C17 1.370(5) . ?
C17 C18 1.383(5) . ?
C18 C19 1.385(4) . ?
C20 C21 1.525(4) . ?
C20 C27 1.529(3) . ?
C21 C26 1.381(4) . ?
C21 C22 1.396(4) . ?
C22 C23 1.381(5) . ?
C23 C24 1.371(5) . ?
C24 C25 1.374(5) . ?
C25 C26 1.391(4) . ?
C27 C28 1.384(4) . ?
C27 C32 1.393(4) . ?
C28 C29 1.392(4) . ?
C29 C30 1.384(4) . ?
C30 C31 1.380(4) . ?
C31 C32 1.382(4) . ?
C34 C37 1.516(4) . ?
C34 C35 1.516(4) . ?
C34 C36 1.517(4) . ?
C38 C39 1.515(4) . ?
C38 C41 1.515(4) . ?
C38 C40 1.517(4) . ?
C42 C44 1.472(5) . ?
C42 C45 1.504(6) . ?
C42 C43 1.508(5) . ?
C46 C49 1.520(5) . ?
C46 C48 1.520(4) . ?
C46 C47 1.523(5) . ?
C50 C51 1.471(6) . ?
C51 C52 1.519(6) . ?
C52 C53 1.507(6) . ?
C53 C54 1.473(6) . ?
C54 C55 1.489(6) . ?

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
O4 Ge1 N1 97.24(9) . . ?
O1 Si1 O3 108.78(11) . . ?
O1 Si1 O2 109.98(10) . . ?
O3 Si1 O2 110.08(10) . . ?
O1 Si1 N1 111.53(11) . . ?
O3 Si1 N1 110.10(11) . . ?
O2 Si1 N1 106.34(10) . . ?
C34 O1 Si1 136.50(18) . . ?
C1 N1 Si1 117.02(16) . . ?
C1 N1 Ge1 111.17(16) . . ?
Si1 N1 Ge1 131.31(12) . . ?
C2 C1 C6 118.9(2) . . ?
C2 C1 N1 121.0(2) . . ?
C6 C1 N1 120.0(2) . . ?
C38 O2 Si1 141.68(18) . . ?
C3 C2 C1 119.5(2) . . ?
C3 C2 C20 120.2(2) . . ?
C1 C2 C20 120.2(2) . . ?
C42 O3 Si1 137.17(18) . . ?
C4 C3 C2 122.3(2) . . ?
C46 O4 Ge1 119.81(18) . . ?
C3 C4 C5 117.7(2) . . ?
C3 C4 C33 121.5(2) . . ?
C5 C4 C33 120.9(2) . . ?
C6 C5 C4 121.8(2) . . ?
C5 C6 C1 119.7(2) . . ?
C5 C6 C7 120.9(2) . . ?
C1 C6 C7 119.3(2) . . ?
C6 C7 C14 114.7(2) . . ?
C6 C7 C8 110.7(2) . . ?
C14 C7 C8 110.9(2) . . ?
C9 C8 C13 118.1(2) . . ?
C9 C8 C7 122.3(2) . . ?
C13 C8 C7 119.5(2) . . ?
C8 C9 C10 120.8(3) . . ?
C11 C10 C9 120.6(3) . . ?
C10 C11 C12 118.9(3) . . ?
C11 C12 C13 120.5(3) . . ?
C12 C13 C8 121.0(3) . . ?
C19 C14 C15 118.4(3) . . ?
C19 C14 C7 119.8(2) . . ?
C15 C14 C7 121.7(2) . . ?
C14 C15 C16 120.6(3) . . ?
C17 C16 C15 120.2(3) . . ?
C16 C17 C18 119.8(3) . . ?
C17 C18 C19 120.1(3) . . ?
C14 C19 C18 120.8(3) . . ?
C21 C20 C2 111.4(2) . . ?
C21 C20 C27 112.8(2) . . ?
C2 C20 C27 112.1(2) . . ?
C26 C21 C22 117.7(3) . . ?
C26 C21 C20 122.9(2) . . ?
C22 C21 C20 119.4(3) . . ?
C23 C22 C21 120.9(3) . . ?
C24 C23 C22 120.6(3) . . ?
C23 C24 C25 119.3(3) . . ?
C24 C25 C26 120.4(3) . . ?
C21 C26 C25 121.0(3) . . ?
C28 C27 C32 118.6(2) . . ?
C28 C27 C20 123.1(2) . . ?
C32 C27 C20 118.2(2) . . ?
C27 C28 C29 120.4(3) . . ?
C30 C29 C28 120.4(3) . . ?
C31 C30 C29 119.3(3) . . ?
C30 C31 C32 120.4(3) . . ?
C31 C32 C27 120.8(3) . . ?
O1 C34 C37 109.1(2) . . ?
O1 C34 C35 105.6(2) . . ?
C37 C34 C35 110.1(2) . . ?
O1 C34 C36 110.8(2) . . ?
C37 C34 C36 110.9(3) . . ?
C35 C34 C36 110.1(2) . . ?
O2 C38 C39 107.7(2) . . ?
O2 C38 C41 106.2(2) . . ?
C39 C38 C41 110.3(2) . . ?
O2 C38 C40 111.3(2) . . ?
C39 C38 C40 111.0(3) . . ?
C41 C38 C40 110.2(3) . . ?
O3 C42 C44 106.8(3) . . ?
O3 C42 C45 109.3(3) . . ?
C44 C42 C45 111.0(4) . . ?
O3 C42 C43 109.5(3) . . ?
C44 C42 C43 114.2(4) . . ?
C45 C42 C43 106.0(4) . . ?
O4 C46 C49 106.4(3) . . ?
O4 C46 C48 110.3(3) . . ?
C49 C46 C48 109.9(3) . . ?
O4 C46 C47 109.2(3) . . ?
C49 C46 C47 109.8(3) . . ?
C48 C46 C47 111.2(3) . . ?
C50 C51 C52 112.0(6) . . ?
C53 C52 C51 108.7(5) . . ?
C54 C53 C52 115.6(6) . . ?
C53 C54 C55 112.6(6) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.393
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.077
####################################################################### 
# 
# 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_compound4
_database_code_depnum_ccdc_archive 'CCDC 1048746'
_audit_update_record             
;
2015-02-11 deposited with the CCDC.
2015-03-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H66 Ge N O3 Si'
_chemical_formula_weight         829.72

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 '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                   10.074(2)
_cell_length_b                   14.516(3)
_cell_length_c                   18.777(4)
_cell_angle_alpha                109.23(3)
_cell_angle_beta                 96.79(3)
_cell_angle_gamma                97.99(3)
_cell_volume                     2527.7(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             886
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.877
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_process_details   XDS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71090
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9771
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         26.00
_reflns_number_total             9771
_reflns_number_gt                9048
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
 A molecule of hexane of crystallisation in the asymmetric unit was refined
 with its atoms set at 50% occupancy, and its carbon atoms set as isotropic.
 The hydride ligand of the compound was located from difference maps and
 its atomic displacement and positional paramters freely refined with the 
 atom set as isotropic.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1058P)²+6.3706P] where P=(Fo²+2Fc²)/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         9771
_refine_ls_number_parameters     516
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0716
_refine_ls_wR_factor_ref         0.2099
_refine_ls_wR_factor_gt          0.2077
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.055
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.39713(4) 0.18068(3) 0.31775(3) 0.03964(17) Uani 1 1 d . . .
Si2 Si 0.71406(9) 0.26635(6) 0.37439(5) 0.0225(2) Uani 1 1 d . . .
N1 N 0.5816(3) 0.1800(2) 0.30875(16) 0.0229(5) Uani 1 1 d . . .
O2 O 0.7433(3) 0.23543(18) 0.44974(14) 0.0286(5) Uani 1 1 d . . .
O1 O 0.8435(2) 0.26712(18) 0.33198(14) 0.0281(5) Uani 1 1 d . . .
O3 O 0.6746(3) 0.37466(18) 0.40492(14) 0.0303(5) Uani 1 1 d . . .
C1 C 0.6145(3) 0.0965(2) 0.25114(18) 0.0217(6) Uani 1 1 d . . .
C4 C 0.6952(3) -0.0629(2) 0.14245(19) 0.0245(6) Uani 1 1 d . . .
C2 C 0.6332(3) 0.0108(2) 0.26776(18) 0.0227(6) Uani 1 1 d . . .
C11 C 0.6685(3) -0.0742(2) 0.36492(18) 0.0237(6) Uani 1 1 d . . .
C6 C 0.6277(3) 0.0994(2) 0.17837(19) 0.0228(6) Uani 1 1 d . . .
C10 C 0.5974(3) 0.0009(2) 0.34196(19) 0.0246(6) Uani 1 1 d . . .
H10 H 0.6319 0.0671 0.3834 0.029 Uiso 1 1 calc R . .
C3 C 0.6736(3) -0.0668(2) 0.21309(19) 0.0242(6) Uani 1 1 d . . .
H3 H 0.6867 -0.1242 0.2247 0.029 Uiso 1 1 calc R . .
C24 C 0.6642(3) 0.2087(3) 0.0976(2) 0.0269(7) Uani 1 1 d . . .
C23 C 0.5883(3) 0.1862(2) 0.15711(19) 0.0248(7) Uani 1 1 d . . .
H23 H 0.6152 0.2464 0.2048 0.030 Uiso 1 1 calc R . .
C17 C 0.4430(4) -0.0207(3) 0.3356(2) 0.0293(7) Uani 1 1 d . . .
C5 C 0.6691(3) 0.0212(2) 0.12567(18) 0.0248(6) Uani 1 1 d . . .
H5 H 0.6800 0.0245 0.0770 0.030 Uiso 1 1 calc R . .
C30 C 0.4334(3) 0.1706(3) 0.13436(19) 0.0278(7) Uani 1 1 d . . .
C16 C 0.8051(4) -0.0440(3) 0.3997(2) 0.0309(7) Uani 1 1 d . . .
H16 H 0.8492 0.0226 0.4110 0.037 Uiso 1 1 calc R . .
C14 C 0.8152(4) -0.2072(3) 0.4023(2) 0.0361(8) Uani 1 1 d . . .
H14 H 0.8649 -0.2527 0.4145 0.043 Uiso 1 1 calc R . .
C39 C 0.9741(4) 0.1504(3) 0.2663(2) 0.0368(8) Uani 1 1 d . . .
H39A H 0.9197 0.0944 0.2744 0.055 Uiso 1 1 calc R . .
H39B H 1.0667 0.1381 0.2623 0.055 Uiso 1 1 calc R . .
H39C H 0.9325 0.1573 0.2190 0.055 Uiso 1 1 calc R . .
C40 C 0.7428(4) 0.2823(3) 0.5308(2) 0.0328(8) Uani 1 1 d . . .
C38 C 1.0350(4) 0.2333(3) 0.4078(2) 0.0384(9) Uani 1 1 d . . .
H38A H 1.0342 0.2940 0.4506 0.058 Uiso 1 1 calc R . .
H38B H 1.1285 0.2218 0.4073 0.058 Uiso 1 1 calc R . .
H38C H 0.9780 0.1767 0.4138 0.058 Uiso 1 1 calc R . .
C12 C 0.6063(4) -0.1713(3) 0.3501(3) 0.0384(9) Uani 1 1 d . . .
H12 H 0.5128 -0.1930 0.3272 0.046 Uiso 1 1 calc R . .
C7 C 0.7508(4) -0.1425(3) 0.0862(2) 0.0309(7) Uani 1 1 d . . .
H7 H 0.7281 -0.1368 0.0347 0.037 Uiso 1 1 calc R . .
C25 C 0.7952(4) 0.2672(3) 0.1219(3) 0.0399(9) Uani 1 1 d . . .
H25 H 0.8348 0.2914 0.1747 0.048 Uiso 1 1 calc R . .
C37 C 1.0682(4) 0.3329(3) 0.3235(3) 0.0406(9) Uani 1 1 d . . .
H37A H 1.0313 0.3407 0.2756 0.061 Uiso 1 1 calc R . .
H37B H 1.1615 0.3210 0.3222 0.061 Uiso 1 1 calc R . .
H37C H 1.0686 0.3934 0.3667 0.061 Uiso 1 1 calc R . .
C22 C 0.3595(4) -0.0892(3) 0.2697(2) 0.0372(8) Uani 1 1 d . . .
H22 H 0.3997 -0.1265 0.2290 0.045 Uiso 1 1 calc R . .
C15 C 0.8776(4) -0.1103(3) 0.4182(2) 0.0354(8) Uani 1 1 d . . .
H15 H 0.9706 -0.0886 0.4419 0.042 Uiso 1 1 calc R . .
C36 C 0.9796(3) 0.2445(3) 0.3330(2) 0.0276(7) Uani 1 1 d . . .
C27 C 0.8112(5) 0.2555(4) -0.0074(3) 0.0510(12) Uani 1 1 d . . .
H27 H 0.8611 0.2714 -0.0431 0.061 Uiso 1 1 calc R . .
C18 C 0.3813(4) 0.0297(3) 0.3954(2) 0.0362(8) Uani 1 1 d . . .
H18 H 0.4359 0.0744 0.4420 0.043 Uiso 1 1 calc R . .
C41 C 0.6062(5) 0.3102(4) 0.5439(3) 0.0469(10) Uani 1 1 d . . .
H41A H 0.5912 0.3618 0.5226 0.070 Uiso 1 1 calc R . .
H41B H 0.6048 0.3353 0.5990 0.070 Uiso 1 1 calc R . .
H41C H 0.5339 0.2514 0.5187 0.070 Uiso 1 1 calc R . .
C43 C 0.7695(5) 0.2036(3) 0.5652(2) 0.0427(10) Uani 1 1 d . . .
H43A H 0.6938 0.1466 0.5444 0.064 Uiso 1 1 calc R . .
H43B H 0.7776 0.2317 0.6210 0.064 Uiso 1 1 calc R . .
H43C H 0.8542 0.1819 0.5522 0.064 Uiso 1 1 calc R . .
C29 C 0.6089(4) 0.1749(3) 0.0203(2) 0.0361(8) Uani 1 1 d . . .
H29 H 0.5197 0.1358 0.0029 0.043 Uiso 1 1 calc R . .
C19 C 0.2388(5) 0.0149(4) 0.3873(3) 0.0471(11) Uani 1 1 d . . .
H19 H 0.1977 0.0506 0.4282 0.057 Uiso 1 1 calc R . .
C20 C 0.1582(4) -0.0507(4) 0.3208(3) 0.0503(12) Uani 1 1 d . . .
H20 H 0.0618 -0.0591 0.3153 0.060 Uiso 1 1 calc R . .
C46 C 0.5159(5) 0.4471(4) 0.3453(3) 0.0504(11) Uani 1 1 d . . .
H46A H 0.4909 0.3844 0.3016 0.076 Uiso 1 1 calc R . .
H46B H 0.5062 0.5025 0.3275 0.076 Uiso 1 1 calc R . .
H46C H 0.4560 0.4463 0.3827 0.076 Uiso 1 1 calc R . .
C42 C 0.8569(5) 0.3733(3) 0.5645(2) 0.0461(10) Uani 1 1 d . . .
H42A H 0.9444 0.3531 0.5561 0.069 Uiso 1 1 calc R . .
H42B H 0.8582 0.4038 0.6196 0.069 Uiso 1 1 calc R . .
H42C H 0.8417 0.4214 0.5395 0.069 Uiso 1 1 calc R . .
C45 C 0.7567(6) 0.4689(4) 0.3278(4) 0.0617(14) Uani 1 1 d . . .
H45A H 0.8513 0.4825 0.3539 0.093 Uiso 1 1 calc R . .
H45B H 0.7406 0.5235 0.3102 0.093 Uiso 1 1 calc R . .
H45C H 0.7396 0.4067 0.2837 0.093 Uiso 1 1 calc R . .
C44 C 0.6622(4) 0.4596(3) 0.3826(2) 0.0323(8) Uani 1 1 d . . .
C13 C 0.6797(4) -0.2376(3) 0.3684(3) 0.0455(10) Uani 1 1 d . . .
H13 H 0.6359 -0.3043 0.3575 0.055 Uiso 1 1 calc R . .
C21 C 0.2183(4) -0.1042(4) 0.2621(3) 0.0477(11) Uani 1 1 d . . .
H21 H 0.1633 -0.1512 0.2166 0.057 Uiso 1 1 calc R . .
C47 C 0.6943(6) 0.5472(3) 0.4562(3) 0.0499(11) Uani 1 1 d . . .
H47A H 0.6340 0.5360 0.4911 0.075 Uiso 1 1 calc R . .
H47B H 0.6806 0.6073 0.4456 0.075 Uiso 1 1 calc R . .
H47C H 0.7892 0.5555 0.4800 0.075 Uiso 1 1 calc R . .
C9 C 0.6890(6) -0.2478(3) 0.0793(3) 0.0515(12) Uani 1 1 d . . .
H9A H 0.7247 -0.2957 0.0395 0.077 Uiso 1 1 calc R . .
H9B H 0.5898 -0.2586 0.0654 0.077 Uiso 1 1 calc R . .
H9C H 0.7129 -0.2567 0.1284 0.077 Uiso 1 1 calc R . .
C28 C 0.6826(5) 0.1978(4) -0.0322(3) 0.0464(10) Uani 1 1 d . . .
H28 H 0.6439 0.1735 -0.0851 0.056 Uiso 1 1 calc R . .
C26 C 0.8675(4) 0.2902(4) 0.0699(3) 0.0515(12) Uani 1 1 d . . .
H26 H 0.9563 0.3300 0.0872 0.062 Uiso 1 1 calc R . .
C8 C 0.9057(5) -0.1216(4) 0.1077(3) 0.0571(13) Uani 1 1 d . . .
H8A H 0.9424 -0.0552 0.1084 0.086 Uiso 1 1 calc R . .
H8B H 0.9428 -0.1712 0.0700 0.086 Uiso 1 1 calc R . .
H8C H 0.9314 -0.1252 0.1586 0.086 Uiso 1 1 calc R . .
C35 C 0.3521(4) 0.0768(3) 0.1042(2) 0.0360(8) Uani 1 1 d . . .
H35 H 0.3932 0.0201 0.0965 0.043 Uiso 1 1 calc R . .
C31 C 0.3713(4) 0.2525(3) 0.1441(2) 0.0391(9) Uani 1 1 d . . .
H31 H 0.4254 0.3175 0.1630 0.047 Uiso 1 1 calc R . .
C33 C 0.1501(4) 0.1464(4) 0.0969(2) 0.0490(11) Uani 1 1 d . . .
H33 H 0.0539 0.1384 0.0851 0.059 Uiso 1 1 calc R . .
C34 C 0.2103(4) 0.0639(4) 0.0847(3) 0.0447(10) Uani 1 1 d . . .
H34 H 0.1562 -0.0010 0.0633 0.054 Uiso 1 1 calc R . .
C32 C 0.2297(4) 0.2403(4) 0.1262(2) 0.0498(11) Uani 1 1 d . . .
H32 H 0.1882 0.2969 0.1342 0.060 Uiso 1 1 calc R . .
C51 C 0.3801(4) 0.5477(4) 0.1664(2) 0.110(5) Uiso 0.50 1 d PRD . .
H51A H 0.4370 0.6066 0.2075 0.132 Uiso 0.50 1 calc PR . .
H51B H 0.3652 0.4932 0.1870 0.132 Uiso 0.50 1 calc PR . .
C52 C 0.4537(15) 0.517(2) 0.0992(6) 0.156(9) Uiso 0.50 1 d PD . .
H52A H 0.3981 0.4562 0.0590 0.187 Uiso 0.50 1 calc PR . .
H52B H 0.4649 0.5700 0.0773 0.187 Uiso 0.50 1 calc PR . .
C50 C 0.2438(11) 0.5723(17) 0.1427(7) 0.127(7) Uiso 0.50 1 d PD . .
H50A H 0.2594 0.6357 0.1330 0.153 Uiso 0.50 1 calc PR . .
H50B H 0.1955 0.5196 0.0944 0.153 Uiso 0.50 1 calc PR . .
C49 C 0.1560(13) 0.581(2) 0.2036(10) 0.149(8) Uiso 0.50 1 d PD . .
H49A H 0.2050 0.6334 0.2521 0.179 Uiso 0.50 1 calc PR . .
H49B H 0.1392 0.5177 0.2127 0.179 Uiso 0.50 1 calc PR . .
C48 C 0.0211(13) 0.608(2) 0.1806(13) 0.159(9) Uiso 0.50 1 d PD . .
H48A H 0.0360 0.6585 0.1572 0.238 Uiso 0.50 1 calc PR . .
H48B H -0.0204 0.6332 0.2261 0.238 Uiso 0.50 1 calc PR . .
H48C H -0.0398 0.5481 0.1437 0.238 Uiso 0.50 1 calc PR . .
H1 H 0.408(5) 0.257(3) 0.393(3) 0.043(12) Uiso 1 1 d . . .
C53 C 0.5921(13) 0.4956(18) 0.1223(10) 0.138(8) Uiso 0.50 1 d PD . .
H53A H 0.6284 0.5370 0.1759 0.207 Uiso 0.50 1 calc PR . .
H53B H 0.6540 0.5109 0.0895 0.207 Uiso 0.50 1 calc PR . .
H53C H 0.5834 0.4253 0.1165 0.207 Uiso 0.50 1 calc PR . .


_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
Ge1 N1 1.886(3) . ?
Si2 O1 1.607(2) . ?
Si2 O3 1.610(2) . ?
Si2 O2 1.627(2) . ?
Si2 N1 1.732(3) . ?
N1 C1 1.443(4) . ?
O2 C40 1.449(4) . ?
O1 C36 1.452(4) . ?
O3 C44 1.443(4) . ?
C1 C6 1.402(4) . ?
C1 C2 1.411(4) . ?
C4 C3 1.387(5) . ?
C4 C5 1.407(4) . ?
C4 C7 1.510(5) . ?
C2 C3 1.397(5) . ?
C2 C10 1.526(4) . ?
C11 C12 1.383(5) . ?
C11 C16 1.393(5) . ?
C11 C10 1.530(4) . ?
C6 C5 1.390(5) . ?
C6 C23 1.529(4) . ?
C10 C17 1.525(5) . ?
C24 C29 1.386(5) . ?
C24 C25 1.401(5) . ?
C24 C23 1.521(5) . ?
C23 C30 1.532(5) . ?
C17 C18 1.391(5) . ?
C17 C22 1.393(6) . ?
C30 C35 1.384(6) . ?
C30 C31 1.390(5) . ?
C16 C15 1.390(5) . ?
C14 C15 1.378(6) . ?
C14 C13 1.381(6) . ?
C39 C36 1.508(5) . ?
C40 C41 1.512(6) . ?
C40 C42 1.524(6) . ?
C40 C43 1.526(5) . ?
C38 C36 1.517(5) . ?
C12 C13 1.396(5) . ?
C7 C9 1.525(6) . ?
C7 C8 1.526(6) . ?
C25 C26 1.382(6) . ?
C37 C36 1.531(5) . ?
C22 C21 1.391(5) . ?
C27 C28 1.376(7) . ?
C27 C26 1.389(8) . ?
C18 C19 1.404(6) . ?
C29 C28 1.399(5) . ?
C19 C20 1.373(8) . ?
C20 C21 1.383(7) . ?
C46 C44 1.514(6) . ?
C45 C44 1.507(6) . ?
C44 C47 1.502(6) . ?
C35 C34 1.402(5) . ?
C31 C32 1.398(6) . ?
C33 C32 1.379(7) . ?
C33 C34 1.381(7) . ?
C51 C52 1.513(5) . ?
C51 C50 1.519(5) . ?
C52 C53 1.511(5) . ?
C50 C49 1.510(5) . ?
C49 C48 1.515(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
O1 Si2 O3 111.72(14) . . ?
O1 Si2 O2 112.02(13) . . ?
O3 Si2 O2 105.54(13) . . ?
O1 Si2 N1 106.78(14) . . ?
O3 Si2 N1 111.39(14) . . ?
O2 Si2 N1 109.44(14) . . ?
C1 N1 Si2 118.2(2) . . ?
C1 N1 Ge1 118.5(2) . . ?
Si2 N1 Ge1 122.73(16) . . ?
C40 O2 Si2 135.2(2) . . ?
C36 O1 Si2 143.1(2) . . ?
C44 O3 Si2 141.4(2) . . ?
C6 C1 C2 119.4(3) . . ?
C6 C1 N1 120.7(3) . . ?
C2 C1 N1 119.9(3) . . ?
C3 C4 C5 117.5(3) . . ?
C3 C4 C7 122.3(3) . . ?
C5 C4 C7 120.2(3) . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 C10 121.3(3) . . ?
C1 C2 C10 119.4(3) . . ?
C12 C11 C16 118.4(3) . . ?
C12 C11 C10 123.5(3) . . ?
C16 C11 C10 118.1(3) . . ?
C5 C6 C1 119.7(3) . . ?
C5 C6 C23 121.3(3) . . ?
C1 C6 C23 119.0(3) . . ?
C17 C10 C2 109.6(3) . . ?
C17 C10 C11 113.7(3) . . ?
C2 C10 C11 112.1(3) . . ?
C4 C3 C2 122.3(3) . . ?
C29 C24 C25 118.4(3) . . ?
C29 C24 C23 122.9(3) . . ?
C25 C24 C23 118.7(3) . . ?
C24 C23 C6 113.5(3) . . ?
C24 C23 C30 112.7(3) . . ?
C6 C23 C30 110.4(3) . . ?
C18 C17 C22 117.9(3) . . ?
C18 C17 C10 120.5(4) . . ?
C22 C17 C10 121.5(3) . . ?
C6 C5 C4 121.8(3) . . ?
C35 C30 C31 118.3(3) . . ?
C35 C30 C23 122.2(3) . . ?
C31 C30 C23 119.5(3) . . ?
C15 C16 C11 120.9(3) . . ?
C15 C14 C13 119.3(3) . . ?
O2 C40 C41 110.8(3) . . ?
O2 C40 C42 109.5(3) . . ?
C41 C40 C42 111.0(4) . . ?
O2 C40 C43 104.6(3) . . ?
C41 C40 C43 110.3(3) . . ?
C42 C40 C43 110.3(3) . . ?
C11 C12 C13 120.5(4) . . ?
C4 C7 C9 113.6(3) . . ?
C4 C7 C8 109.0(3) . . ?
C9 C7 C8 111.6(4) . . ?
C26 C25 C24 120.7(4) . . ?
C21 C22 C17 121.4(4) . . ?
C14 C15 C16 120.3(3) . . ?
O1 C36 C39 108.2(3) . . ?
O1 C36 C38 112.0(3) . . ?
C39 C36 C38 110.6(3) . . ?
O1 C36 C37 105.5(3) . . ?
C39 C36 C37 110.8(3) . . ?
C38 C36 C37 109.6(3) . . ?
C28 C27 C26 119.6(4) . . ?
C17 C18 C19 120.4(4) . . ?
C24 C29 C28 120.8(4) . . ?
C20 C19 C18 120.6(4) . . ?
C19 C20 C21 119.5(4) . . ?
O3 C44 C47 105.1(3) . . ?
O3 C44 C45 111.2(3) . . ?
C47 C44 C45 112.4(4) . . ?
O3 C44 C46 108.1(3) . . ?
C47 C44 C46 109.6(4) . . ?
C45 C44 C46 110.2(4) . . ?
C14 C13 C12 120.6(4) . . ?
C20 C21 C22 120.0(5) . . ?
C27 C28 C29 120.1(4) . . ?
C25 C26 C27 120.4(4) . . ?
C30 C35 C34 121.4(4) . . ?
C30 C31 C32 120.6(4) . . ?
C32 C33 C34 120.0(4) . . ?
C33 C34 C35 119.4(4) . . ?
C33 C32 C31 120.3(4) . . ?
C52 C51 C50 111.0(5) . . ?
C53 C52 C51 111.8(5) . . ?
C49 C50 C51 111.6(5) . . ?
C50 C49 C48 111.7(5) . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.567
_refine_diff_density_min         -1.222
_refine_diff_density_rms         0.090
####################################################################### 
# 
# 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_compound5
_database_code_depnum_ccdc_archive 'CCDC 1048747'
_audit_update_record             
;
2015-02-11 deposited with the CCDC.
2015-03-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H55 Ge N O3 Si'
_chemical_formula_weight         758.58

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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                   10.7047(5)
_cell_length_b                   21.7462(9)
_cell_length_c                   17.0790(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.615(2)
_cell_angle_gamma                90.00
_cell_volume                     3971.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1608
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_process_details   'Sortav (Blessing)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex X8'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            52358
_diffrn_reflns_av_R_equivalents  0.1433
_diffrn_reflns_av_sigmaI/netI    0.1453
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         26.00
_reflns_number_total             7760
_reflns_number_gt                3947
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
 All atoms of the three tert-butoxy groups of the compound were found to be
 disordered over two sites. This disorder was modelled and the C and O
 atoms of the major set refined anisotropically, while those of the minor
 set were refined isotropically (Level A cifcheck alert)
 The hydride ligand of the compound could not be located from difference
 maps. It was not included in a calculated position during refinement.
 The empirical formula and F(000) value were adjusted accordingly in the 
 final refinement of the compound.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0915P)²+5.4960P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7760
_refine_ls_number_parameters     540
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.1783
_refine_ls_R_factor_gt           0.0772
_refine_ls_wR_factor_ref         0.2110
_refine_ls_wR_factor_gt          0.1675
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.028
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.15318(6) 0.14662(3) 0.28325(4) 0.0426(3) Uani 1 1 d . . .
Si1 Si -0.00345(15) 0.25653(7) 0.21207(9) 0.0333(4) Uani 1 1 d D . .
O1 O -0.0470(8) 0.3008(3) 0.2805(3) 0.032(2) Uani 0.487(6) 1 d PD A 1
N1 N 0.0117(4) 0.17826(18) 0.2281(2) 0.0218(10) Uani 1 1 d . A .
C1 C -0.0734(5) 0.1376(2) 0.1876(3) 0.0181(11) Uani 1 1 d . . .
O2 O -0.0961(5) 0.2696(3) 0.1366(2) 0.019(2) Uani 0.487(6) 1 d PD A 1
C2 C -0.0587(5) 0.1227(2) 0.1081(3) 0.0191(12) Uani 1 1 d . A .
O3 O 0.0826(9) 0.2819(4) 0.1448(4) 0.052(3) Uani 0.487(6) 1 d PDU A 1
C3 C -0.1502(5) 0.0895(2) 0.0670(3) 0.0239(13) Uani 1 1 d . . .
H3 H -0.1408 0.0814 0.0130 0.029 Uiso 1 1 calc R A .
C4 C -0.2554(5) 0.0675(2) 0.1025(3) 0.0230(12) Uani 1 1 d . A .
C5 C -0.2624(5) 0.0767(2) 0.1829(3) 0.0226(12) Uani 1 1 d . . .
H5 H -0.3301 0.0589 0.2090 0.027 Uiso 1 1 calc R A .
C6 C -0.1741(5) 0.1107(2) 0.2263(3) 0.0182(12) Uani 1 1 d . A .
C7 C -0.3572(5) 0.0345(3) 0.0555(3) 0.0339(14) Uani 1 1 d . . .
H7A H -0.4167 0.0646 0.0329 0.051 Uiso 1 1 calc R A .
H7B H -0.4009 0.0064 0.0898 0.051 Uiso 1 1 calc R . .
H7C H -0.3203 0.0111 0.0133 0.051 Uiso 1 1 calc R . .
C8 C 0.0637(5) 0.1404(2) 0.0702(3) 0.0227(12) Uani 1 1 d . . .
H8 H 0.0801 0.1846 0.0830 0.027 Uiso 1 1 calc R A .
C9 C 0.0568(5) 0.1349(2) -0.0182(3) 0.0246(13) Uani 1 1 d . A .
C10 C 0.1002(5) 0.0842(3) -0.0579(3) 0.0326(14) Uani 1 1 d . . .
H10 H 0.1389 0.0514 -0.0291 0.039 Uiso 1 1 calc R A .
C11 C 0.0883(6) 0.0805(3) -0.1388(3) 0.0370(15) Uani 1 1 d . A .
H11 H 0.1182 0.0452 -0.1648 0.044 Uiso 1 1 calc R . .
C12 C 0.0342(6) 0.1267(3) -0.1810(3) 0.0430(17) Uani 1 1 d . . .
H12 H 0.0271 0.1241 -0.2365 0.052 Uiso 1 1 calc R A .
C13 C -0.0105(7) 0.1777(3) -0.1432(3) 0.054(2) Uani 1 1 d . A .
H13 H -0.0504 0.2097 -0.1727 0.064 Uiso 1 1 calc R . .
C14 C 0.0027(6) 0.1821(3) -0.0628(3) 0.0439(17) Uani 1 1 d . . .
H14 H -0.0256 0.2181 -0.0374 0.053 Uiso 1 1 calc R A .
C15 C 0.1708(5) 0.1034(2) 0.1082(3) 0.0263(13) Uani 1 1 d . A .
C16 C 0.2832(5) 0.1318(3) 0.1303(3) 0.0361(15) Uani 1 1 d . . .
H16 H 0.2939 0.1742 0.1192 0.043 Uiso 1 1 calc R A .
C17 C 0.3796(6) 0.0999(3) 0.1677(4) 0.0442(17) Uani 1 1 d . A .
H17 H 0.4553 0.1204 0.1828 0.053 Uiso 1 1 calc R . .
C18 C 0.3659(6) 0.0384(3) 0.1832(4) 0.0468(17) Uani 1 1 d . . .
H18 H 0.4317 0.0163 0.2097 0.056 Uiso 1 1 calc R A .
C19 C 0.2557(6) 0.0084(3) 0.1600(4) 0.0394(16) Uani 1 1 d . A .
H19 H 0.2469 -0.0344 0.1691 0.047 Uiso 1 1 calc R . .
C20 C 0.1588(5) 0.0414(2) 0.1234(3) 0.0313(14) Uani 1 1 d . . .
H20 H 0.0829 0.0209 0.1086 0.038 Uiso 1 1 calc R A .
C21 C -0.1790(5) 0.1176(2) 0.3149(3) 0.0201(12) Uani 1 1 d . . .
H21 H -0.1592 0.1616 0.3271 0.024 Uiso 1 1 calc R A .
C22 C -0.3072(5) 0.1051(2) 0.3466(3) 0.0218(12) Uani 1 1 d . A .
C23 C -0.3964(5) 0.1512(3) 0.3444(3) 0.0328(14) Uani 1 1 d . . .
H23 H -0.3753 0.1903 0.3239 0.039 Uiso 1 1 calc R A .
C24 C -0.5131(6) 0.1426(3) 0.3707(4) 0.0442(17) Uani 1 1 d . A .
H24 H -0.5716 0.1755 0.3690 0.053 Uiso 1 1 calc R . .
C25 C -0.5468(6) 0.0862(3) 0.3996(4) 0.0469(17) Uani 1 1 d . . .
H25 H -0.6287 0.0798 0.4172 0.056 Uiso 1 1 calc R A .
C26 C -0.4610(6) 0.0394(3) 0.4028(4) 0.0464(17) Uani 1 1 d . A .
H26 H -0.4829 0.0006 0.4237 0.056 Uiso 1 1 calc R . .
C27 C -0.3416(6) 0.0486(3) 0.3756(3) 0.0358(15) Uani 1 1 d . . .
H27 H -0.2833 0.0156 0.3769 0.043 Uiso 1 1 calc R A .
C28 C -0.0768(5) 0.0797(2) 0.3560(3) 0.0241(13) Uani 1 1 d . A .
C29 C -0.0090(6) 0.1016(3) 0.4214(3) 0.0338(15) Uani 1 1 d . . .
H29 H -0.0300 0.1405 0.4424 0.041 Uiso 1 1 calc R A .
C30 C 0.0875(6) 0.0687(3) 0.4565(3) 0.0404(16) Uani 1 1 d . A .
H30 H 0.1344 0.0857 0.4997 0.048 Uiso 1 1 calc R . .
C31 C 0.1168(6) 0.0111(3) 0.4295(3) 0.0370(15) Uani 1 1 d . . .
H31 H 0.1837 -0.0117 0.4535 0.044 Uiso 1 1 calc R A .
C32 C 0.0480(6) -0.0124(3) 0.3676(4) 0.0405(16) Uani 1 1 d . A .
H32 H 0.0651 -0.0528 0.3497 0.049 Uiso 1 1 calc R . .
C33 C -0.0462(6) 0.0214(3) 0.3306(3) 0.0353(15) Uani 1 1 d . . .
H33 H -0.0913 0.0042 0.2866 0.042 Uiso 1 1 calc R A .
C34 C 0.1744(8) 0.3304(4) 0.1391(6) 0.040(6) Uani 0.487(6) 1 d PDU A 1
C35 C 0.2785(13) 0.3204(6) 0.2001(8) 0.077(5) Uani 0.487(6) 1 d PD A 1
H35D H 0.2544 0.3377 0.2502 0.115 Uiso 0.487(6) 1 calc PR A 1
H35E H 0.3545 0.3409 0.1835 0.115 Uiso 0.487(6) 1 calc PR A 1
H35F H 0.2943 0.2763 0.2062 0.115 Uiso 0.487(6) 1 calc PR A 1
C36 C 0.2128(14) 0.3170(6) 0.0574(6) 0.068(5) Uani 0.487(6) 1 d PD A 1
H36D H 0.2480 0.2755 0.0553 0.102 Uiso 0.487(6) 1 calc PR A 1
H36E H 0.2759 0.3470 0.0425 0.102 Uiso 0.487(6) 1 calc PR A 1
H36F H 0.1397 0.3199 0.0209 0.102 Uiso 0.487(6) 1 calc PR A 1
C37 C 0.1106(13) 0.3914(5) 0.1463(8) 0.045(4) Uani 0.487(6) 1 d PDU A 1
H37A H 0.0355 0.3924 0.1113 0.067 Uiso 0.487(6) 1 calc PR A 1
H37B H 0.1677 0.4243 0.1317 0.067 Uiso 0.487(6) 1 calc PR A 1
H37C H 0.0870 0.3975 0.2005 0.067 Uiso 0.487(6) 1 calc PR A 1
C38 C -0.2237(5) 0.2917(4) 0.1266(5) 0.032(5) Uani 0.487(6) 1 d PD A 1
C39 C -0.2745(12) 0.2766(5) 0.0442(5) 0.038(3) Uani 0.487(6) 1 d PD A 1
H39A H -0.2285 0.3002 0.0060 0.057 Uiso 0.487(6) 1 calc PR A 1
H39B H -0.3634 0.2874 0.0393 0.057 Uiso 0.487(6) 1 calc PR A 1
H39C H -0.2645 0.2326 0.0343 0.057 Uiso 0.487(6) 1 calc PR A 1
C40 C -0.2231(14) 0.3609(4) 0.1401(8) 0.040(4) Uani 0.487(6) 1 d PD A 1
H40A H -0.1834 0.3700 0.1916 0.060 Uiso 0.487(6) 1 calc PR A 1
H40B H -0.3093 0.3762 0.1379 0.060 Uiso 0.487(6) 1 calc PR A 1
H40C H -0.1762 0.3810 0.0993 0.060 Uiso 0.487(6) 1 calc PR A 1
C41 C -0.3018(10) 0.2599(4) 0.1870(6) 0.031(3) Uani 0.487(6) 1 d PD A 1
H41A H -0.3026 0.2155 0.1772 0.047 Uiso 0.487(6) 1 calc PR A 1
H41B H -0.3876 0.2757 0.1828 0.047 Uiso 0.487(6) 1 calc PR A 1
H41C H -0.2656 0.2680 0.2397 0.047 Uiso 0.487(6) 1 calc PR A 1
C42 C -0.0039(10) 0.3214(4) 0.3578(4) 0.036(5) Uani 0.487(6) 1 d PDU A 1
C43 C -0.0596(15) 0.3854(5) 0.3574(12) 0.059(7) Uani 0.487(6) 1 d PDU A 1
H43A H -0.0219 0.4102 0.3167 0.089 Uiso 0.487(6) 1 calc PR A 1
H43B H -0.0427 0.4047 0.4086 0.089 Uiso 0.487(6) 1 calc PR A 1
H43C H -0.1501 0.3828 0.3465 0.089 Uiso 0.487(6) 1 calc PR A 1
C44 C 0.1367(9) 0.3229(6) 0.3708(7) 0.050(4) Uani 0.487(6) 1 d PD A 1
H44A H 0.1704 0.2813 0.3658 0.074 Uiso 0.487(6) 1 calc PR A 1
H44B H 0.1582 0.3388 0.4234 0.074 Uiso 0.487(6) 1 calc PR A 1
H44C H 0.1728 0.3498 0.3316 0.074 Uiso 0.487(6) 1 calc PR A 1
C45 C -0.0643(12) 0.2802(6) 0.4166(7) 0.070(5) Uani 0.487(6) 1 d PD A 1
H45A H -0.1542 0.2774 0.4037 0.105 Uiso 0.487(6) 1 calc PR A 1
H45B H -0.0507 0.2975 0.4693 0.105 Uiso 0.487(6) 1 calc PR A 1
H45C H -0.0270 0.2391 0.4149 0.105 Uiso 0.487(6) 1 calc PR A 1
O1A O 0.0236(9) 0.2929(4) 0.2934(3) 0.040(3) Uiso 0.513(6) 1 d PD A 2
O2A O -0.1529(3) 0.2637(4) 0.1989(5) 0.049(3) Uiso 0.513(6) 1 d PD A 2
O3A O 0.1303(4) 0.2749(3) 0.1784(5) 0.025(2) Uiso 0.513(6) 1 d PD A 2
C34A C 0.1841(8) 0.3222(4) 0.1302(5) 0.038(5) Uiso 0.513(6) 1 d PD A 2
C35A C 0.3268(8) 0.3164(5) 0.1341(7) 0.042(3) Uiso 0.513(6) 1 d PD A 2
H35A H 0.3574 0.3146 0.1890 0.063 Uiso 0.513(6) 1 calc PR A 2
H35B H 0.3634 0.3522 0.1087 0.063 Uiso 0.513(6) 1 calc PR A 2
H35C H 0.3511 0.2789 0.1070 0.063 Uiso 0.513(6) 1 calc PR A 2
C36A C 0.1362(11) 0.3190(7) 0.0446(6) 0.058(5) Uiso 0.513(6) 1 d PD A 2
H36A H 0.1616 0.2799 0.0218 0.086 Uiso 0.513(6) 1 calc PR A 2
H36B H 0.1715 0.3532 0.0154 0.086 Uiso 0.513(6) 1 calc PR A 2
H36C H 0.0448 0.3220 0.0419 0.086 Uiso 0.513(6) 1 calc PR A 2
C37A C 0.1477(12) 0.3843(6) 0.1647(8) 0.047(5) Uiso 0.513(6) 1 d PD A 2
H37D H 0.0564 0.3872 0.1655 0.071 Uiso 0.513(6) 1 calc PR A 2
H37E H 0.1796 0.4176 0.1324 0.071 Uiso 0.513(6) 1 calc PR A 2
H37F H 0.1838 0.3880 0.2182 0.071 Uiso 0.513(6) 1 calc PR A 2
C38A C -0.2401(8) 0.2917(4) 0.1420(5) 0.029(4) Uiso 0.513(6) 1 d PD A 2
C39A C -0.1980(12) 0.2830(6) 0.0587(7) 0.052(4) Uiso 0.513(6) 1 d PD A 2
H39D H -0.1083 0.2918 0.0572 0.078 Uiso 0.513(6) 1 calc PR A 2
H39E H -0.2446 0.3111 0.0234 0.078 Uiso 0.513(6) 1 calc PR A 2
H39F H -0.2139 0.2405 0.0420 0.078 Uiso 0.513(6) 1 calc PR A 2
C40A C -0.2458(16) 0.3598(5) 0.1618(10) 0.046(6) Uiso 0.513(6) 1 d PD A 2
H40D H -0.2622 0.3648 0.2175 0.068 Uiso 0.513(6) 1 calc PR A 2
H40E H -0.3130 0.3794 0.1299 0.068 Uiso 0.513(6) 1 calc PR A 2
H40F H -0.1658 0.3793 0.1509 0.068 Uiso 0.513(6) 1 calc PR A 2
C41A C -0.3669(11) 0.2617(6) 0.1511(8) 0.062(5) Uiso 0.513(6) 1 d PD A 2
H41D H -0.3615 0.2178 0.1385 0.093 Uiso 0.513(6) 1 calc PR A 2
H41E H -0.4290 0.2814 0.1154 0.093 Uiso 0.513(6) 1 calc PR A 2
H41F H -0.3918 0.2666 0.2052 0.093 Uiso 0.513(6) 1 calc PR A 2
C42A C -0.0184(10) 0.3153(6) 0.3677(4) 0.055(7) Uiso 0.513(6) 1 d PD A 2
C43A C -0.0314(18) 0.3847(7) 0.3568(14) 0.083(9) Uiso 0.513(6) 1 d PD A 2
H43D H 0.0499 0.4022 0.3447 0.124 Uiso 0.513(6) 1 calc PR A 2
H43E H -0.0601 0.4032 0.4050 0.124 Uiso 0.513(6) 1 calc PR A 2
H43F H -0.0922 0.3932 0.3135 0.124 Uiso 0.513(6) 1 calc PR A 2
C44A C 0.0838(13) 0.3014(9) 0.4304(11) 0.127(8) Uiso 0.513(6) 1 d PD A 2
H44D H 0.0854 0.2572 0.4413 0.191 Uiso 0.513(6) 1 calc PR A 2
H44E H 0.0666 0.3239 0.4785 0.191 Uiso 0.513(6) 1 calc PR A 2
H44F H 0.1649 0.3143 0.4117 0.191 Uiso 0.513(6) 1 calc PR A 2
C45A C -0.1421(11) 0.2880(7) 0.3912(9) 0.068(5) Uiso 0.513(6) 1 d PD A 2
H45D H -0.2092 0.3017 0.3543 0.102 Uiso 0.513(6) 1 calc PR A 2
H45E H -0.1600 0.3017 0.4442 0.102 Uiso 0.513(6) 1 calc PR A 2
H45F H -0.1368 0.2430 0.3902 0.102 Uiso 0.513(6) 1 calc PR A 2


_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
Ge1 N1 1.877(4) . ?
Si1 O1 1.601(2) . ?
Si1 O3 1.602(2) . ?
Si1 O1A 1.613(2) . ?
Si1 O2A 1.613(2) . ?
Si1 O2 1.614(2) . ?
Si1 O3A 1.618(2) . ?
Si1 N1 1.730(4) . ?
O1 C42 1.448(2) . ?
N1 C1 1.427(6) . ?
C1 C2 1.411(7) . ?
C1 C6 1.415(7) . ?
O2 C38 1.451(2) . ?
C2 C3 1.383(7) . ?
C2 C8 1.536(7) . ?
O3 C34 1.447(2) . ?
C3 C4 1.387(7) . ?
C4 C5 1.393(7) . ?
C4 C7 1.505(7) . ?
C5 C6 1.388(7) . ?
C6 C21 1.524(6) . ?
C8 C9 1.513(7) . ?
C8 C15 1.522(7) . ?
C9 C10 1.387(7) . ?
C9 C14 1.389(8) . ?
C10 C11 1.383(8) . ?
C11 C12 1.351(8) . ?
C12 C13 1.379(9) . ?
C13 C14 1.378(8) . ?
C15 C20 1.380(7) . ?
C15 C16 1.389(8) . ?
C16 C17 1.375(8) . ?
C17 C18 1.373(9) . ?
C18 C19 1.390(8) . ?
C19 C20 1.386(8) . ?
C21 C28 1.516(7) . ?
C21 C22 1.523(7) . ?
C22 C27 1.381(7) . ?
C22 C23 1.384(7) . ?
C23 C24 1.360(8) . ?
C24 C25 1.375(9) . ?
C25 C26 1.370(9) . ?
C26 C27 1.394(8) . ?
C28 C33 1.384(7) . ?
C28 C29 1.388(7) . ?
C29 C30 1.373(8) . ?
C30 C31 1.375(8) . ?
C31 C32 1.360(8) . ?
C32 C33 1.378(8) . ?
C34 C37 1.501(5) . ?
C34 C36 1.502(5) . ?
C34 C35 1.505(5) . ?
C38 C39 1.521(5) . ?
C38 C40 1.522(5) . ?
C38 C41 1.523(5) . ?
C42 C45 1.512(5) . ?
C42 C44 1.512(5) . ?
C42 C43 1.515(5) . ?
O1A C42A 1.451(2) . ?
O2A C38A 1.451(2) . ?
O3A C34A 1.452(2) . ?
C34A C36A 1.528(5) . ?
C34A C37A 1.531(5) . ?
C34A C35A 1.531(5) . ?
C38A C41A 1.520(5) . ?
C38A C40A 1.522(5) . ?
C38A C39A 1.523(5) . ?
C42A C45A 1.522(5) . ?
C42A C44A 1.525(5) . ?
C42A C43A 1.526(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
O1 Si1 O3 120.8(4) . . ?
O1 Si1 O1A 28.7(3) . . ?
O3 Si1 O1A 111.2(4) . . ?
O1 Si1 O2A 73.9(4) . . ?
O3 Si1 O2A 117.8(5) . . ?
O1A Si1 O2A 102.1(5) . . ?
O1 Si1 O2 106.7(4) . . ?
O3 Si1 O2 73.7(5) . . ?
O1A Si1 O2 132.9(4) . . ?
O2A Si1 O2 45.8(3) . . ?
O1 Si1 O3A 113.8(4) . . ?
O3 Si1 O3A 27.5(4) . . ?
O1A Si1 O3A 93.3(4) . . ?
O2A Si1 O3A 144.6(4) . . ?
O2 Si1 O3A 101.2(4) . . ?
O1 Si1 N1 120.3(3) . . ?
O3 Si1 N1 113.5(4) . . ?
O1A Si1 N1 109.5(4) . . ?
O2A Si1 N1 101.7(3) . . ?
O2 Si1 N1 110.4(3) . . ?
O3A Si1 N1 102.8(3) . . ?
C42 O1 Si1 139.4(7) . . ?
C1 N1 Si1 118.7(3) . . ?
C1 N1 Ge1 119.9(3) . . ?
Si1 N1 Ge1 120.5(2) . . ?
C2 C1 C6 118.4(4) . . ?
C2 C1 N1 120.8(4) . . ?
C6 C1 N1 120.8(4) . . ?
C38 O2 Si1 133.9(5) . . ?
C3 C2 C1 120.0(5) . . ?
C3 C2 C8 121.0(4) . . ?
C1 C2 C8 118.9(4) . . ?
C34 O3 Si1 135.5(7) . . ?
C2 C3 C4 122.0(5) . . ?
C3 C4 C5 117.5(5) . . ?
C3 C4 C7 121.0(5) . . ?
C5 C4 C7 121.6(5) . . ?
C6 C5 C4 122.5(5) . . ?
C5 C6 C1 119.0(4) . . ?
C5 C6 C21 122.0(4) . . ?
C1 C6 C21 119.0(4) . . ?
C9 C8 C15 112.7(4) . . ?
C9 C8 C2 113.4(4) . . ?
C15 C8 C2 109.2(4) . . ?
C10 C9 C14 117.4(5) . . ?
C10 C9 C8 123.3(5) . . ?
C14 C9 C8 119.3(5) . . ?
C11 C10 C9 121.1(5) . . ?
C12 C11 C10 120.5(5) . . ?
C11 C12 C13 119.8(6) . . ?
C14 C13 C12 120.0(6) . . ?
C13 C14 C9 121.1(6) . . ?
C20 C15 C16 118.0(5) . . ?
C20 C15 C8 121.5(5) . . ?
C16 C15 C8 120.5(5) . . ?
C17 C16 C15 121.6(6) . . ?
C18 C17 C16 119.7(6) . . ?
C17 C18 C19 119.9(6) . . ?
C20 C19 C18 119.7(6) . . ?
C15 C20 C19 121.0(6) . . ?
C28 C21 C22 112.4(4) . . ?
C28 C21 C6 110.5(4) . . ?
C22 C21 C6 114.1(4) . . ?
C27 C22 C23 117.3(5) . . ?
C27 C22 C21 123.1(5) . . ?
C23 C22 C21 119.6(5) . . ?
C24 C23 C22 122.3(6) . . ?
C23 C24 C25 120.1(6) . . ?
C26 C25 C24 119.4(6) . . ?
C25 C26 C27 120.2(6) . . ?
C22 C27 C26 120.7(6) . . ?
C33 C28 C29 116.4(5) . . ?
C33 C28 C21 121.9(5) . . ?
C29 C28 C21 121.6(5) . . ?
C30 C29 C28 121.8(5) . . ?
C29 C30 C31 120.5(5) . . ?
C32 C31 C30 118.6(6) . . ?
C31 C32 C33 121.0(6) . . ?
C32 C33 C28 121.5(5) . . ?
O3 C34 C37 109.0(9) . . ?
O3 C34 C36 97.9(7) . . ?
C37 C34 C36 113.1(5) . . ?
O3 C34 C35 109.4(9) . . ?
C37 C34 C35 113.3(5) . . ?
C36 C34 C35 112.9(5) . . ?
O2 C38 C39 109.4(7) . . ?
O2 C38 C40 108.2(8) . . ?
C39 C38 C40 110.6(4) . . ?
O2 C38 C41 108.2(7) . . ?
C39 C38 C41 110.1(4) . . ?
C40 C38 C41 110.3(4) . . ?
O1 C42 C45 107.2(8) . . ?
O1 C42 C44 114.5(9) . . ?
C45 C42 C44 111.6(4) . . ?
O1 C42 C43 99.8(9) . . ?
C45 C42 C43 111.6(5) . . ?
C44 C42 C43 111.6(5) . . ?
C42A O1A Si1 150.2(8) . . ?
C38A O2A Si1 137.5(7) . . ?
C34A O3A Si1 139.2(6) . . ?
O3A C34A C36A 112.7(9) . . ?
O3A C34A C37A 107.0(9) . . ?
C36A C34A C37A 109.1(4) . . ?
O3A C34A C35A 109.7(7) . . ?
C36A C34A C35A 109.1(4) . . ?
C37A C34A C35A 109.1(4) . . ?
O2A C38A C41A 107.5(9) . . ?
O2A C38A C40A 106.8(10) . . ?
C41A C38A C40A 110.5(5) . . ?
O2A C38A C39A 111.4(10) . . ?
C41A C38A C39A 110.3(5) . . ?
C40A C38A C39A 110.2(4) . . ?
O1A C42A C45A 114.0(11) . . ?
O1A C42A C44A 107.8(11) . . ?
C45A C42A C44A 110.0(5) . . ?
O1A C42A C43A 104.8(14) . . ?
C45A C42A C43A 110.1(5) . . ?
C44A C42A C43A 109.9(5) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.091
####################################################################### 
# 
# 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_LH
_database_code_depnum_ccdc_archive 'CCDC 1048748'
_audit_update_record             
;
2015-02-11 deposited with the CCDC.
2015-03-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H55 N O3 Si'
_chemical_formula_weight         685.99

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'
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   P2(1)/n

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                   12.369(3)
_cell_length_b                   21.768(4)
_cell_length_c                   14.724(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.32(3)
_cell_angle_gamma                90.00
_cell_volume                     3940.3(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1480
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.979
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_process_details   XDS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71090
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27068
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         25.50
_reflns_number_total             6763
_reflns_number_gt                6609
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 The methyl groups of one tert-butyl substituent were found to be disordered
 over two sites. This disorder was modelled and both sets of C atoms refined
 anisotropically. 
 The low value (92.4%) for completeness of data to theta = 25.5 deg. arises 
 from hardware constraints associated with the diffractometer used at the 
 Australian Synchrotron and is on that instrument. 
 Its minimum crystal to detector distance is 72 mm and its
 goniometer only rotates about the phi axis.(level A cifcheck alert)
  
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0522P)²+2.4930P] where P=(Fo²+2Fc²)/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         6763
_refine_ls_number_parameters     496
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0530
_refine_ls_wR_factor_ref         0.1350
_refine_ls_wR_factor_gt          0.1345
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.059
_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
Si1 Si 0.17185(3) 0.616978(18) 0.78906(3) 0.01372(14) Uani 1 1 d . . .
O1 O 0.21878(8) 0.63239(5) 0.89371(7) 0.0181(2) Uani 1 1 d . . .
N1 N 0.28426(10) 0.61170(6) 0.73116(9) 0.0153(3) Uani 1 1 d . . .
C1 C 0.37057(11) 0.56777(6) 0.73676(10) 0.0138(3) Uani 1 1 d . . .
H1 H 0.2790(18) 0.6309(10) 0.6778(17) 0.033(5) Uiso 1 1 d . . .
O2 O 0.09202(8) 0.66870(5) 0.73994(7) 0.0194(3) Uani 1 1 d . A .
C2 C 0.37182(11) 0.52231(7) 0.66861(10) 0.0146(3) Uani 1 1 d . . .
O3 O 0.10137(8) 0.55403(5) 0.78868(8) 0.0200(3) Uani 1 1 d . . .
C3 C 0.45540(12) 0.47930(7) 0.67369(10) 0.0156(3) Uani 1 1 d . . .
H3 H 0.4548 0.4484 0.6280 0.019 Uiso 1 1 calc R . .
C4 C 0.54011(12) 0.48055(7) 0.74447(10) 0.0163(3) Uani 1 1 d . . .
C5 C 0.54170(12) 0.52805(7) 0.80770(10) 0.0162(3) Uani 1 1 d . . .
H5 H 0.6008 0.5305 0.8546 0.019 Uiso 1 1 calc R . .
C6 C 0.45975(11) 0.57218(6) 0.80482(10) 0.0142(3) Uani 1 1 d . . .
C7 C 0.28571(11) 0.52522(7) 0.58573(10) 0.0162(3) Uani 1 1 d . . .
H7 H 0.2138 0.5303 0.6100 0.019 Uiso 1 1 calc R . .
C8 C 0.27870(11) 0.46636(7) 0.52928(10) 0.0172(3) Uani 1 1 d . . .
C9 C 0.31624(12) 0.46309(7) 0.44385(10) 0.0193(3) Uani 1 1 d . . .
H9 H 0.3471 0.4985 0.4191 0.023 Uiso 1 1 calc R . .
C10 C 0.30926(13) 0.40868(8) 0.39409(11) 0.0223(3) Uani 1 1 d . . .
H10 H 0.3350 0.4073 0.3356 0.027 Uiso 1 1 calc R . .
C11 C 0.26538(13) 0.35668(8) 0.42886(12) 0.0257(4) Uani 1 1 d . . .
H11 H 0.2608 0.3195 0.3947 0.031 Uiso 1 1 calc R . .
C12 C 0.22792(14) 0.35911(8) 0.51425(12) 0.0279(4) Uani 1 1 d . . .
H12 H 0.1978 0.3234 0.5389 0.034 Uiso 1 1 calc R . .
C13 C 0.23425(13) 0.41358(8) 0.56391(11) 0.0233(3) Uani 1 1 d . . .
H13 H 0.2080 0.4148 0.6221 0.028 Uiso 1 1 calc R . .
C14 C 0.30246(13) 0.58219(7) 0.52829(10) 0.0181(3) Uani 1 1 d . . .
C15 C 0.21392(15) 0.61188(9) 0.48037(12) 0.0293(4) Uani 1 1 d . . .
H15 H 0.1427 0.5959 0.4822 0.035 Uiso 1 1 calc R . .
C16 C 0.22888(18) 0.66454(10) 0.42991(13) 0.0399(5) Uani 1 1 d . . .
H16 H 0.1678 0.6843 0.3977 0.048 Uiso 1 1 calc R . .
C17 C 0.33189(19) 0.68844(8) 0.42609(13) 0.0362(5) Uani 1 1 d . . .
H17 H 0.3417 0.7249 0.3924 0.043 Uiso 1 1 calc R . .
C18 C 0.42034(16) 0.65876(8) 0.47180(12) 0.0296(4) Uani 1 1 d . . .
H18 H 0.4915 0.6744 0.4687 0.035 Uiso 1 1 calc R . .
C19 C 0.40578(14) 0.60624(8) 0.52226(11) 0.0221(3) Uani 1 1 d . . .
H19 H 0.4674 0.5863 0.5533 0.027 Uiso 1 1 calc R . .
C20 C 0.47000(12) 0.62711(7) 0.87008(10) 0.0154(3) Uani 1 1 d . . .
H20 H 0.4020 0.6284 0.9010 0.018 Uiso 1 1 calc R . .
C21 C 0.56524(12) 0.61977(7) 0.94502(10) 0.0162(3) Uani 1 1 d . . .
C22 C 0.55230(12) 0.58523(7) 1.02245(11) 0.0198(3) Uani 1 1 d . . .
H22 H 0.4830 0.5683 1.0299 0.024 Uiso 1 1 calc R . .
C23 C 0.63928(14) 0.57497(8) 1.08933(11) 0.0263(4) Uani 1 1 d . . .
H23 H 0.6291 0.5514 1.1420 0.032 Uiso 1 1 calc R . .
C24 C 0.74057(14) 0.59932(9) 1.07878(12) 0.0299(4) Uani 1 1 d . . .
H24 H 0.8003 0.5921 1.1238 0.036 Uiso 1 1 calc R . .
C25 C 0.75432(14) 0.63422(9) 1.00224(13) 0.0304(4) Uani 1 1 d . . .
H25 H 0.8236 0.6513 0.9952 0.037 Uiso 1 1 calc R . .
C26 C 0.66745(13) 0.64447(8) 0.93567(11) 0.0234(3) Uani 1 1 d . . .
H26 H 0.6778 0.6685 0.8834 0.028 Uiso 1 1 calc R . .
C27 C 0.47704(12) 0.68799(7) 0.81950(10) 0.0173(3) Uani 1 1 d . . .
C28 C 0.45359(14) 0.74230(8) 0.86329(12) 0.0244(4) Uani 1 1 d . . .
H28 H 0.4325 0.7407 0.9234 0.029 Uiso 1 1 calc R . .
C29 C 0.46048(15) 0.79863(8) 0.82066(13) 0.0301(4) Uani 1 1 d . . .
H29 H 0.4443 0.8352 0.8517 0.036 Uiso 1 1 calc R . .
C30 C 0.49091(15) 0.80197(8) 0.73275(13) 0.0284(4) Uani 1 1 d . . .
H30 H 0.4951 0.8406 0.7032 0.034 Uiso 1 1 calc R . .
C31 C 0.51497(16) 0.74830(8) 0.68888(12) 0.0294(4) Uani 1 1 d . . .
H31 H 0.5366 0.7500 0.6290 0.035 Uiso 1 1 calc R . .
C32 C 0.50774(14) 0.69202(7) 0.73185(12) 0.0247(4) Uani 1 1 d . . .
H32 H 0.5241 0.6555 0.7007 0.030 Uiso 1 1 calc R . .
C33 C 0.62835(13) 0.43249(7) 0.75107(11) 0.0229(3) Uani 1 1 d . . .
H33A H 0.6970 0.4508 0.7778 0.034 Uiso 1 1 calc R . .
H33B H 0.6370 0.4168 0.6899 0.034 Uiso 1 1 calc R . .
H33C H 0.6085 0.3986 0.7898 0.034 Uiso 1 1 calc R . .
C34 C -0.00222(12) 0.53357(7) 0.74304(11) 0.0195(3) Uani 1 1 d . . .
C35 C -0.01202(13) 0.54700(8) 0.64086(11) 0.0244(4) Uani 1 1 d . . .
H35A H -0.0039 0.5912 0.6312 0.037 Uiso 1 1 calc R . .
H35B H -0.0835 0.5336 0.6125 0.037 Uiso 1 1 calc R . .
H35C H 0.0451 0.5248 0.6132 0.037 Uiso 1 1 calc R . .
C36 C -0.09445(13) 0.56415(8) 0.78711(12) 0.0246(4) Uani 1 1 d . . .
H36A H -0.0873 0.5545 0.8525 0.037 Uiso 1 1 calc R . .
H36B H -0.1644 0.5489 0.7582 0.037 Uiso 1 1 calc R . .
H36C H -0.0908 0.6088 0.7789 0.037 Uiso 1 1 calc R . .
C37 C -0.00410(14) 0.46462(8) 0.75945(13) 0.0278(4) Uani 1 1 d . . .
H37A H 0.0560 0.4453 0.7320 0.042 Uiso 1 1 calc R . .
H37B H -0.0733 0.4477 0.7316 0.042 Uiso 1 1 calc R . .
H37C H 0.0038 0.4565 0.8253 0.042 Uiso 1 1 calc R . .
C38 C 0.09790(13) 0.73271(7) 0.71512(11) 0.0234(4) Uani 1 1 d D . .
C39 C -0.0087(5) 0.7489(2) 0.6626(6) 0.099(3) Uani 0.685(8) 1 d PD A 1
H39A H -0.0670 0.7439 0.7020 0.148 Uiso 0.685(8) 1 calc PR A 1
H39B H -0.0222 0.7217 0.6096 0.148 Uiso 0.685(8) 1 calc PR A 1
H39C H -0.0067 0.7916 0.6419 0.148 Uiso 0.685(8) 1 calc PR A 1
C40 C 0.1206(6) 0.77208(15) 0.7999(2) 0.0563(14) Uani 0.685(8) 1 d PD A 1
H40A H 0.1887 0.7587 0.8346 0.085 Uiso 0.685(8) 1 calc PR A 1
H40B H 0.0608 0.7678 0.8379 0.085 Uiso 0.685(8) 1 calc PR A 1
H40C H 0.1270 0.8152 0.7820 0.085 Uiso 0.685(8) 1 calc PR A 1
C41 C 0.1918(5) 0.74321(17) 0.6575(4) 0.078(2) Uani 0.685(8) 1 d PD A 1
H41A H 0.1943 0.7867 0.6405 0.117 Uiso 0.685(8) 1 calc PR A 1
H41B H 0.1807 0.7180 0.6021 0.117 Uiso 0.685(8) 1 calc PR A 1
H41C H 0.2605 0.7317 0.6929 0.117 Uiso 0.685(8) 1 calc PR A 1
C42 C 0.17811(13) 0.62626(7) 0.98146(10) 0.0198(3) Uani 1 1 d . . .
C43 C 0.06217(14) 0.65023(11) 0.97714(12) 0.0347(4) Uani 1 1 d . . .
H43A H 0.0604 0.6935 0.9587 0.052 Uiso 1 1 calc R . .
H43B H 0.0363 0.6464 1.0374 0.052 Uiso 1 1 calc R . .
H43C H 0.0151 0.6262 0.9325 0.052 Uiso 1 1 calc R . .
C44 C 0.25252(14) 0.66591(8) 1.04646(11) 0.0241(4) Uani 1 1 d . . .
H44A H 0.3275 0.6511 1.0480 0.036 Uiso 1 1 calc R . .
H44B H 0.2293 0.6636 1.1079 0.036 Uiso 1 1 calc R . .
H44C H 0.2486 0.7086 1.0253 0.036 Uiso 1 1 calc R . .
C45 C 0.18532(17) 0.55928(9) 1.00980(12) 0.0324(4) Uani 1 1 d . . .
H45A H 0.1361 0.5348 0.9674 0.049 Uiso 1 1 calc R . .
H45B H 0.1644 0.5550 1.0718 0.049 Uiso 1 1 calc R . .
H45C H 0.2601 0.5447 1.0086 0.049 Uiso 1 1 calc R . .
C39A C -0.0134(7) 0.7555(4) 0.7368(13) 0.088(5) Uani 0.315(8) 1 d PD A 2
H39D H -0.0186 0.7512 0.8024 0.133 Uiso 0.315(8) 1 calc PR A 2
H39E H -0.0707 0.7311 0.7025 0.133 Uiso 0.315(8) 1 calc PR A 2
H39F H -0.0222 0.7988 0.7193 0.133 Uiso 0.315(8) 1 calc PR A 2
C40A C 0.1909(9) 0.7641(3) 0.7679(8) 0.062(4) Uani 0.315(8) 1 d PD A 2
H40D H 0.1836 0.7610 0.8334 0.092 Uiso 0.315(8) 1 calc PR A 2
H40E H 0.1916 0.8075 0.7502 0.092 Uiso 0.315(8) 1 calc PR A 2
H40F H 0.2590 0.7446 0.7551 0.092 Uiso 0.315(8) 1 calc PR A 2
C41A C 0.0991(13) 0.7333(4) 0.6128(3) 0.068(4) Uani 0.315(8) 1 d PD A 2
H41D H 0.0992 0.7759 0.5912 0.103 Uiso 0.315(8) 1 calc PR A 2
H41E H 0.0343 0.7122 0.5838 0.103 Uiso 0.315(8) 1 calc PR A 2
H41F H 0.1645 0.7123 0.5969 0.103 Uiso 0.315(8) 1 calc PR A 2


_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
Si1 O2 1.6152(11) . ?
Si1 O1 1.6208(11) . ?
Si1 O3 1.6238(11) . ?
Si1 N1 1.7129(14) . ?
O1 C42 1.4433(19) . ?
N1 C1 1.4288(18) . ?
N1 H1 0.89(2) . ?
C1 C6 1.410(2) . ?
C1 C2 1.411(2) . ?
O2 C38 1.4443(19) . ?
C2 C3 1.391(2) . ?
C2 C7 1.530(2) . ?
O3 C34 1.4498(18) . ?
C3 C4 1.394(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.390(2) . ?
C4 C33 1.507(2) . ?
C5 C6 1.394(2) . ?
C5 H5 0.9500 . ?
C6 C20 1.530(2) . ?
C7 C8 1.524(2) . ?
C7 C14 1.528(2) . ?
C7 H7 1.0000 . ?
C8 C9 1.390(2) . ?
C8 C13 1.394(2) . ?
C9 C10 1.390(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.378(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.388(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.391(2) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C19 1.393(2) . ?
C14 C15 1.395(2) . ?
C15 C16 1.389(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.383(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.380(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.386(2) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C27 1.527(2) . ?
C20 C21 1.531(2) . ?
C20 H20 1.0000 . ?
C21 C22 1.390(2) . ?
C21 C26 1.394(2) . ?
C22 C23 1.394(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.385(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.385(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.390(2) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C32 1.388(2) . ?
C27 C28 1.392(2) . ?
C28 C29 1.384(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.389(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.383(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.386(2) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C37 1.521(2) . ?
C34 C35 1.524(2) . ?
C34 C36 1.526(2) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C40A 1.482(4) . ?
C38 C39 1.495(3) . ?
C38 C41A 1.509(4) . ?
C38 C40 1.514(3) . ?
C38 C41 1.529(3) . ?
C38 C39A 1.529(5) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C45 1.516(2) . ?
C42 C43 1.521(2) . ?
C42 C44 1.521(2) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C39A H39D 0.9800 . ?
C39A H39E 0.9800 . ?
C39A H39F 0.9800 . ?
C40A H40D 0.9800 . ?
C40A H40E 0.9800 . ?
C40A H40F 0.9800 . ?
C41A H41D 0.9800 . ?
C41A H41E 0.9800 . ?
C41A H41F 0.9800 . ?

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
O2 Si1 O1 114.76(6) . . ?
O2 Si1 O3 106.57(6) . . ?
O1 Si1 O3 108.30(6) . . ?
O2 Si1 N1 108.28(6) . . ?
O1 Si1 N1 105.16(6) . . ?
O3 Si1 N1 113.99(6) . . ?
C42 O1 Si1 135.09(10) . . ?
C1 N1 Si1 131.18(10) . . ?
C1 N1 H1 110.4(15) . . ?
Si1 N1 H1 115.2(15) . . ?
C6 C1 C2 118.98(13) . . ?
C6 C1 N1 121.11(13) . . ?
C2 C1 N1 119.68(13) . . ?
C38 O2 Si1 137.77(10) . . ?
C3 C2 C1 120.02(13) . . ?
C3 C2 C7 121.25(13) . . ?
C1 C2 C7 118.50(13) . . ?
C34 O3 Si1 135.03(10) . . ?
C2 C3 C4 121.34(13) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C5 C4 C3 117.97(13) . . ?
C5 C4 C33 121.09(13) . . ?
C3 C4 C33 120.93(13) . . ?
C4 C5 C6 122.39(13) . . ?
C4 C5 H5 118.8 . . ?
C6 C5 H5 118.8 . . ?
C5 C6 C1 118.97(13) . . ?
C5 C6 C20 120.64(13) . . ?
C1 C6 C20 120.25(13) . . ?
C8 C7 C14 112.54(12) . . ?
C8 C7 C2 113.14(12) . . ?
C14 C7 C2 110.49(12) . . ?
C8 C7 H7 106.7 . . ?
C14 C7 H7 106.7 . . ?
C2 C7 H7 106.7 . . ?
C9 C8 C13 118.25(14) . . ?
C9 C8 C7 122.14(14) . . ?
C13 C8 C7 119.61(14) . . ?
C8 C9 C10 120.87(15) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 H9 119.6 . . ?
C11 C10 C9 120.54(15) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C10 C11 C12 119.31(15) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C11 C12 C13 120.25(16) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C12 C13 C8 120.79(16) . . ?
C12 C13 H13 119.6 . . ?
C8 C13 H13 119.6 . . ?
C19 C14 C15 117.94(15) . . ?
C19 C14 C7 121.44(13) . . ?
C15 C14 C7 120.63(15) . . ?
C16 C15 C14 120.63(18) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C17 C16 C15 120.64(17) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C18 C17 C16 119.23(17) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C17 C18 C19 120.31(18) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C18 C19 C14 121.23(16) . . ?
C18 C19 H19 119.4 . . ?
C14 C19 H19 119.4 . . ?
C27 C20 C6 112.15(12) . . ?
C27 C20 C21 111.17(12) . . ?
C6 C20 C21 112.02(12) . . ?
C27 C20 H20 107.0 . . ?
C6 C20 H20 107.0 . . ?
C21 C20 H20 107.0 . . ?
C22 C21 C26 118.50(14) . . ?
C22 C21 C20 119.92(13) . . ?
C26 C21 C20 121.51(14) . . ?
C21 C22 C23 121.10(15) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 H22 119.5 . . ?
C24 C23 C22 119.79(16) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C23 C24 C25 119.66(15) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
C24 C25 C26 120.47(16) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C21 120.48(16) . . ?
C25 C26 H26 119.8 . . ?
C21 C26 H26 119.8 . . ?
C32 C27 C28 117.99(14) . . ?
C32 C27 C20 122.98(13) . . ?
C28 C27 C20 119.02(14) . . ?
C29 C28 C27 121.05(16) . . ?
C29 C28 H28 119.5 . . ?
C27 C28 H28 119.5 . . ?
C28 C29 C30 120.35(16) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C31 C30 C29 119.02(16) . . ?
C31 C30 H30 120.5 . . ?
C29 C30 H30 120.5 . . ?
C30 C31 C32 120.36(16) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C31 C32 C27 121.22(15) . . ?
C31 C32 H32 119.4 . . ?
C27 C32 H32 119.4 . . ?
C4 C33 H33A 109.5 . . ?
C4 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C4 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O3 C34 C37 104.93(12) . . ?
O3 C34 C35 111.64(13) . . ?
C37 C34 C35 110.19(14) . . ?
O3 C34 C36 109.44(12) . . ?
C37 C34 C36 109.73(14) . . ?
C35 C34 C36 110.74(13) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O2 C38 C40A 111.7(3) . . ?
O2 C38 C39 107.0(2) . . ?
C40A C38 C39 138.8(4) . . ?
O2 C38 C41A 105.5(3) . . ?
C40A C38 C41A 115.3(7) . . ?
C39 C38 C41A 65.6(6) . . ?
O2 C38 C40 110.32(18) . . ?
C40A C38 C40 40.9(5) . . ?
C39 C38 C40 111.5(4) . . ?
C41A C38 C40 142.8(4) . . ?
O2 C38 C41 110.31(17) . . ?
C40A C38 C41 68.2(6) . . ?
C39 C38 C41 111.0(4) . . ?
C41A C38 C41 49.7(5) . . ?
C40 C38 C41 106.8(3) . . ?
O2 C38 C39A 100.9(4) . . ?
C40A C38 C39A 113.9(8) . . ?
C39 C38 C39A 43.0(6) . . ?
C41A C38 C39A 108.3(8) . . ?
C40 C38 C39A 74.6(7) . . ?
C41 C38 C39A 145.4(5) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
O1 C42 C45 108.62(13) . . ?
O1 C42 C43 110.54(13) . . ?
C45 C42 C43 111.59(16) . . ?
O1 C42 C44 105.34(13) . . ?
C45 C42 C44 111.05(14) . . ?
C43 C42 C44 109.52(14) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C38 C39A H39D 109.5 . . ?
C38 C39A H39E 109.5 . . ?
H39D C39A H39E 109.5 . . ?
C38 C39A H39F 109.5 . . ?
H39D C39A H39F 109.5 . . ?
H39E C39A H39F 109.5 . . ?
C38 C40A H40D 109.5 . . ?
C38 C40A H40E 109.5 . . ?
H40D C40A H40E 109.5 . . ?
C38 C40A H40F 109.5 . . ?
H40D C40A H40F 109.5 . . ?
H40E C40A H40F 109.5 . . ?
C38 C41A H41D 109.5 . . ?
C38 C41A H41E 109.5 . . ?
H41D C41A H41E 109.5 . . ?
C38 C41A H41F 109.5 . . ?
H41D C41A H41F 109.5 . . ?
H41E C41A H41F 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.924
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.924
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.047
####################################################################### 
# 
# 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_LLi(THF)
_database_code_depnum_ccdc_archive 'CCDC 1048749'
_audit_update_record             
;
2015-02-11 deposited with the CCDC.
2015-03-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C53 H70 Li N O5 Si'
_chemical_formula_weight         836.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   11.531(2)
_cell_length_b                   24.287(5)
_cell_length_c                   17.056(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.37(3)
_cell_angle_gamma                90.00
_cell_volume                     4725.7(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1808
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.990
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_process_details   XDS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71090
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            35498
_diffrn_reflns_av_R_equivalents  0.0932
_diffrn_reflns_av_sigmaI/netI    0.0627
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.94
_diffrn_reflns_theta_max         26.00
_reflns_number_total             8997
_reflns_number_gt                6824
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
 one molecule of THF of crystallisation was located in the asymmetric unit.
 One CH2 fragment of this was found to be disordered over two sites. The 
 disorder was modelled and all non-hydrogen atoms of the molecule refined
 anisotropically.(level A cifcheck alert)
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0957P)²+3.3771P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.050(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8997
_refine_ls_number_parameters     570
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0654
_refine_ls_wR_factor_ref         0.1841
_refine_ls_wR_factor_gt          0.1684
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.056
_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
Si1 Si 0.26234(6) 0.67684(3) 0.30056(4) 0.02082(19) Uani 1 1 d . . .
O1 O 0.17337(14) 0.68106(7) 0.36643(10) 0.0233(4) Uani 1 1 d . . .
N1 N 0.24914(17) 0.62319(8) 0.24001(12) 0.0206(4) Uani 1 1 d . . .
C1 C 0.16089(19) 0.58382(9) 0.23082(14) 0.0191(5) Uani 1 1 d . . .
Li1 Li 0.4168(4) 0.60154(18) 0.2816(3) 0.0273(9) Uani 1 1 d . . .
O2 O 0.26119(16) 0.73868(7) 0.26299(11) 0.0287(4) Uani 1 1 d . . .
C2 C 0.0819(2) 0.57851(9) 0.15913(13) 0.0194(5) Uani 1 1 d . . .
O3 O 0.39640(15) 0.66530(7) 0.35061(10) 0.0248(4) Uani 1 1 d . . .
C3 C -0.0060(2) 0.53890(10) 0.15097(14) 0.0225(5) Uani 1 1 d . . .
H3 H -0.0580 0.5368 0.1024 0.027 Uiso 1 1 calc R . .
O4 O 0.54840(15) 0.59563(8) 0.22841(11) 0.0284(4) Uani 1 1 d . . .
C4 C -0.0205(2) 0.50213(10) 0.21153(14) 0.0225(5) Uani 1 1 d . . .
O5 O 0.2285(4) 0.31756(18) 0.4065(2) 0.1015(12) Uani 1 1 d . . .
C5 C 0.0600(2) 0.50531(10) 0.28059(14) 0.0206(5) Uani 1 1 d . . .
H5 H 0.0538 0.4799 0.3221 0.025 Uiso 1 1 calc R . .
C6 C 0.1491(2) 0.54435(10) 0.29102(13) 0.0189(5) Uani 1 1 d . . .
C7 C 0.1032(2) 0.61448(10) 0.08929(14) 0.0208(5) Uani 1 1 d . . .
H7 H 0.1351 0.6502 0.1124 0.025 Uiso 1 1 calc R . .
C8 C -0.1167(2) 0.45957(12) 0.20215(16) 0.0298(6) Uani 1 1 d . . .
H8A H -0.0835 0.4234 0.2179 0.045 Uiso 1 1 calc R . .
H8B H -0.1535 0.4583 0.1467 0.045 Uiso 1 1 calc R . .
H8C H -0.1756 0.4694 0.2358 0.045 Uiso 1 1 calc R . .
C9 C 0.2457(2) 0.54086(10) 0.36208(14) 0.0201(5) Uani 1 1 d . . .
H9 H 0.2695 0.5796 0.3760 0.024 Uiso 1 1 calc R . .
C10 C 0.1973(2) 0.59037(10) 0.04507(14) 0.0215(5) Uani 1 1 d . . .
C11 C 0.2591(2) 0.62486(10) 0.00031(15) 0.0250(5) Uani 1 1 d . . .
H11 H 0.2423 0.6632 -0.0017 0.030 Uiso 1 1 calc R . .
C12 C 0.3444(2) 0.60440(12) -0.04120(16) 0.0291(6) Uani 1 1 d . . .
H12 H 0.3850 0.6286 -0.0715 0.035 Uiso 1 1 calc R . .
C13 C 0.3706(2) 0.54864(11) -0.03862(16) 0.0300(6) Uani 1 1 d . . .
H13 H 0.4294 0.5345 -0.0667 0.036 Uiso 1 1 calc R . .
C14 C 0.3100(2) 0.51397(11) 0.00526(16) 0.0295(6) Uani 1 1 d . . .
H14 H 0.3273 0.4757 0.0072 0.035 Uiso 1 1 calc R . .
C15 C 0.2242(2) 0.53443(10) 0.04642(15) 0.0251(5) Uani 1 1 d . . .
H15 H 0.1831 0.5099 0.0760 0.030 Uiso 1 1 calc R . .
C16 C -0.0086(2) 0.62851(10) 0.03391(14) 0.0236(5) Uani 1 1 d . . .
C17 C -0.0754(2) 0.67335(12) 0.05106(16) 0.0321(6) Uani 1 1 d . . .
H17 H -0.0496 0.6949 0.0967 0.039 Uiso 1 1 calc R . .
C18 C -0.1792(3) 0.68742(14) 0.00294(18) 0.0415(8) Uani 1 1 d . . .
H18 H -0.2236 0.7182 0.0158 0.050 Uiso 1 1 calc R . .
C19 C -0.2172(3) 0.65629(14) -0.0635(2) 0.0430(8) Uani 1 1 d . . .
H19 H -0.2882 0.6654 -0.0965 0.052 Uiso 1 1 calc R . .
C20 C -0.1518(3) 0.61194(13) -0.08172(18) 0.0399(7) Uani 1 1 d . . .
H20 H -0.1781 0.5906 -0.1275 0.048 Uiso 1 1 calc R . .
C21 C -0.0476(2) 0.59797(11) -0.03377(16) 0.0310(6) Uani 1 1 d . . .
H21 H -0.0029 0.5675 -0.0474 0.037 Uiso 1 1 calc R . .
C22 C 0.3545(2) 0.51236(10) 0.33877(14) 0.0207(5) Uani 1 1 d . . .
C23 C 0.3542(2) 0.48550(10) 0.26677(15) 0.0263(5) Uani 1 1 d . . .
H23 H 0.2844 0.4844 0.2296 0.032 Uiso 1 1 calc R . .
C24 C 0.4557(2) 0.46002(11) 0.24844(17) 0.0313(6) Uani 1 1 d . . .
H24 H 0.4544 0.4419 0.1990 0.038 Uiso 1 1 calc R . .
C25 C 0.5576(2) 0.46108(11) 0.30199(18) 0.0330(6) Uani 1 1 d . . .
H25 H 0.6265 0.4437 0.2895 0.040 Uiso 1 1 calc R . .
C26 C 0.5592(2) 0.48750(11) 0.37398(17) 0.0309(6) Uani 1 1 d . . .
H26 H 0.6292 0.4882 0.4111 0.037 Uiso 1 1 calc R . .
C27 C 0.4590(2) 0.51297(11) 0.39198(16) 0.0268(5) Uani 1 1 d . . .
H27 H 0.4612 0.5312 0.4414 0.032 Uiso 1 1 calc R . .
C28 C 0.2087(2) 0.51584(10) 0.43607(14) 0.0211(5) Uani 1 1 d . . .
C29 C 0.2177(2) 0.45970(11) 0.45329(15) 0.0250(5) Uani 1 1 d . . .
H29 H 0.2492 0.4355 0.4180 0.030 Uiso 1 1 calc R . .
C30 C 0.1811(2) 0.43876(11) 0.52139(16) 0.0290(6) Uani 1 1 d . . .
H30 H 0.1872 0.4004 0.5322 0.035 Uiso 1 1 calc R . .
C31 C 0.1357(2) 0.47367(12) 0.57377(15) 0.0295(6) Uani 1 1 d . . .
H31 H 0.1103 0.4594 0.6202 0.035 Uiso 1 1 calc R . .
C32 C 0.1278(2) 0.52930(12) 0.55773(15) 0.0287(6) Uani 1 1 d . . .
H32 H 0.0971 0.5534 0.5935 0.034 Uiso 1 1 calc R . .
C33 C 0.1644(2) 0.55038(11) 0.48957(14) 0.0240(5) Uani 1 1 d . . .
H33 H 0.1590 0.5888 0.4795 0.029 Uiso 1 1 calc R . .
C34 C 0.0584(2) 0.70631(10) 0.36041(16) 0.0258(5) Uani 1 1 d . . .
C35 C -0.0064(3) 0.67624(12) 0.4188(2) 0.0382(7) Uani 1 1 d . . .
H35A H -0.0170 0.6376 0.4028 0.057 Uiso 1 1 calc R . .
H35B H -0.0832 0.6934 0.4193 0.057 Uiso 1 1 calc R . .
H35C H 0.0392 0.6783 0.4719 0.057 Uiso 1 1 calc R . .
C36 C 0.0736(3) 0.76641(11) 0.38397(18) 0.0346(6) Uani 1 1 d . . .
H36A H 0.1141 0.7690 0.4385 0.052 Uiso 1 1 calc R . .
H36B H -0.0035 0.7840 0.3804 0.052 Uiso 1 1 calc R . .
H36C H 0.1200 0.7851 0.3482 0.052 Uiso 1 1 calc R . .
C37 C -0.0067(3) 0.70019(13) 0.27668(18) 0.0380(7) Uani 1 1 d . . .
H37A H 0.0347 0.7207 0.2398 0.057 Uiso 1 1 calc R . .
H37B H -0.0864 0.7147 0.2744 0.057 Uiso 1 1 calc R . .
H37C H -0.0104 0.6612 0.2619 0.057 Uiso 1 1 calc R . .
C38 C 0.3057(3) 0.76346(11) 0.19672(17) 0.0330(6) Uani 1 1 d . . .
C39 C 0.3618(4) 0.81776(13) 0.2257(2) 0.0504(9) Uani 1 1 d . . .
H39A H 0.3062 0.8392 0.2517 0.076 Uiso 1 1 calc R . .
H39B H 0.3827 0.8385 0.1805 0.076 Uiso 1 1 calc R . .
H39C H 0.4326 0.8106 0.2635 0.076 Uiso 1 1 calc R . .
C40 C 0.2015(3) 0.77468(15) 0.1331(2) 0.0516(9) Uani 1 1 d . . .
H40A H 0.1619 0.7399 0.1169 0.077 Uiso 1 1 calc R . .
H40B H 0.2289 0.7919 0.0871 0.077 Uiso 1 1 calc R . .
H40C H 0.1465 0.7995 0.1542 0.077 Uiso 1 1 calc R . .
C41 C 0.3936(3) 0.72623(13) 0.1653(2) 0.0449(8) Uani 1 1 d . . .
H41A H 0.4605 0.7200 0.2068 0.067 Uiso 1 1 calc R . .
H41B H 0.4209 0.7437 0.1195 0.067 Uiso 1 1 calc R . .
H41C H 0.3564 0.6909 0.1492 0.067 Uiso 1 1 calc R . .
C42 C 0.4602(2) 0.68895(12) 0.42201(17) 0.0313(6) Uani 1 1 d . . .
C43 C 0.5877(3) 0.6789(2) 0.4176(3) 0.0647(12) Uani 1 1 d . . .
H43A H 0.5998 0.6398 0.4070 0.097 Uiso 1 1 calc R . .
H43B H 0.6346 0.6891 0.4682 0.097 Uiso 1 1 calc R . .
H43C H 0.6119 0.7012 0.3750 0.097 Uiso 1 1 calc R . .
C44 C 0.4218(4) 0.65795(15) 0.49230(19) 0.0530(9) Uani 1 1 d . . .
H44A H 0.3385 0.6649 0.4939 0.079 Uiso 1 1 calc R . .
H44B H 0.4680 0.6708 0.5417 0.079 Uiso 1 1 calc R . .
H44C H 0.4345 0.6184 0.4862 0.079 Uiso 1 1 calc R . .
C45 C 0.4326(3) 0.74907(13) 0.4295(2) 0.0464(8) Uani 1 1 d . . .
H45A H 0.4512 0.7689 0.3829 0.070 Uiso 1 1 calc R . .
H45B H 0.4794 0.7640 0.4773 0.070 Uiso 1 1 calc R . .
H45C H 0.3491 0.7534 0.4333 0.070 Uiso 1 1 calc R . .
C46 C 0.5218(2) 0.58791(12) 0.14400(15) 0.0317(6) Uani 1 1 d . . .
H46A H 0.4417 0.6011 0.1240 0.038 Uiso 1 1 calc R . .
H46B H 0.5276 0.5485 0.1300 0.038 Uiso 1 1 calc R . .
C47 C 0.6124(3) 0.62154(13) 0.10990(17) 0.0371(7) Uani 1 1 d . . .
H47A H 0.6294 0.6059 0.0592 0.044 Uiso 1 1 calc R . .
H47B H 0.5870 0.6603 0.1014 0.044 Uiso 1 1 calc R . .
C48 C 0.7168(3) 0.6169(3) 0.1739(3) 0.0847(17) Uani 1 1 d . . .
H48A H 0.7739 0.5901 0.1581 0.102 Uiso 1 1 calc R . .
H48B H 0.7561 0.6531 0.1829 0.102 Uiso 1 1 calc R . .
C49 C 0.6743(2) 0.59837(16) 0.24630(19) 0.0441(8) Uani 1 1 d . . .
H49A H 0.7070 0.5617 0.2623 0.053 Uiso 1 1 calc R . .
H49B H 0.6979 0.6246 0.2901 0.053 Uiso 1 1 calc R . .
C50 C 0.1192(4) 0.3291(2) 0.3609(3) 0.0721(12) Uani 1 1 d . B .
H50A H 0.0763 0.3575 0.3871 0.087 Uiso 1 1 calc R . .
H50B H 0.0704 0.2955 0.3531 0.087 Uiso 1 1 calc R . .
C51 C 0.1479(4) 0.34964(19) 0.2844(3) 0.0734(12) Uani 1 1 d . . .
H51A H 0.1584 0.3901 0.2857 0.088 Uiso 1 1 calc R B .
H51B H 0.0852 0.3401 0.2405 0.088 Uiso 1 1 calc R . .
C52 C 0.2603(5) 0.3211(2) 0.2749(3) 0.0872(15) Uani 1 1 d . B .
H52A H 0.3245 0.3480 0.2739 0.105 Uiso 1 1 calc R A 1
H52B H 0.2513 0.2992 0.2254 0.105 Uiso 1 1 calc R A 1
C53 C 0.2851(9) 0.2829(4) 0.3489(6) 0.075(3) Uani 0.50 1 d PU B 1
H53A H 0.2468 0.2466 0.3396 0.090 Uiso 0.50 1 calc PR B 1
H53B H 0.3702 0.2779 0.3664 0.090 Uiso 0.50 1 calc PR B 1
C53A C 0.3211(10) 0.3211(6) 0.3522(7) 0.094(3) Uani 0.50 1 d PU B 2
H53C H 0.3676 0.3553 0.3624 0.113 Uiso 0.50 1 calc PR B 2
H53D H 0.3748 0.2891 0.3604 0.113 Uiso 0.50 1 calc PR B 2


_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
Si1 O1 1.6312(18) . ?
Si1 O2 1.6321(18) . ?
Si1 N1 1.656(2) . ?
Si1 O3 1.6771(19) . ?
Si1 Li1 2.606(4) . ?
O1 C34 1.451(3) . ?
N1 C1 1.389(3) . ?
N1 Li1 2.029(5) . ?
C1 C2 1.420(3) . ?
C1 C6 1.426(3) . ?
Li1 O4 1.883(5) . ?
Li1 O3 1.980(5) . ?
Li1 C22 2.523(5) . ?
O2 C38 1.440(3) . ?
C2 C3 1.390(3) . ?
C2 C7 1.525(3) . ?
O3 C42 1.447(3) . ?
C3 C4 1.394(3) . ?
C3 H3 0.9500 . ?
O4 C49 1.440(3) . ?
O4 C46 1.440(3) . ?
C4 C5 1.391(3) . ?
C4 C8 1.508(3) . ?
O5 C50 1.411(6) . ?
O5 C53A 1.514(12) . ?
O5 C53 1.512(11) . ?
C5 C6 1.391(3) . ?
C5 H5 0.9500 . ?
C6 C9 1.524(3) . ?
C7 C16 1.521(3) . ?
C7 C10 1.525(3) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C28 1.517(3) . ?
C9 C22 1.535(3) . ?
C9 H9 1.0000 . ?
C10 C15 1.393(3) . ?
C10 C11 1.397(3) . ?
C11 C12 1.385(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.387(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.382(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.386(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.390(4) . ?
C16 C21 1.391(4) . ?
C17 C18 1.392(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.379(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.376(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.394(4) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.390(4) . ?
C22 C27 1.399(4) . ?
C23 C24 1.398(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.380(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.383(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.385(4) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C33 1.390(3) . ?
C28 C29 1.395(3) . ?
C29 C30 1.389(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.388(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.379(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.391(3) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 C35 1.516(4) . ?
C34 C36 1.517(4) . ?
C34 C37 1.521(4) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C41 1.514(4) . ?
C38 C39 1.519(4) . ?
C38 C40 1.522(5) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.503(4) . ?
C42 C45 1.504(4) . ?
C42 C44 1.535(4) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C47 1.508(4) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.507(5) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.464(5) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C51 1.478(6) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.500(7) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C53A 1.401(13) . ?
C52 C53 1.558(11) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53A H53C 0.9900 . ?
C53A H53D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Si1 O2 104.04(9) . . ?
O1 Si1 N1 117.98(10) . . ?
O2 Si1 N1 118.98(10) . . ?
O1 Si1 O3 106.59(9) . . ?
O2 Si1 O3 107.92(10) . . ?
N1 Si1 O3 100.38(10) . . ?
O1 Si1 Li1 129.76(12) . . ?
O2 Si1 Li1 124.30(12) . . ?
N1 Si1 Li1 51.14(12) . . ?
O3 Si1 Li1 49.45(11) . . ?
C34 O1 Si1 129.63(16) . . ?
C1 N1 Si1 127.70(16) . . ?
C1 N1 Li1 120.4(2) . . ?
Si1 N1 Li1 89.41(15) . . ?
N1 C1 C2 121.8(2) . . ?
N1 C1 C6 121.8(2) . . ?
C2 C1 C6 116.3(2) . . ?
O4 Li1 O3 121.3(2) . . ?
O4 Li1 N1 130.2(2) . . ?
O3 Li1 N1 79.35(17) . . ?
O4 Li1 C22 114.6(2) . . ?
O3 Li1 C22 112.1(2) . . ?
N1 Li1 C22 92.68(17) . . ?
O4 Li1 Si1 136.6(2) . . ?
O3 Li1 Si1 40.05(10) . . ?
N1 Li1 Si1 39.45(10) . . ?
C22 Li1 Si1 108.42(16) . . ?
C38 O2 Si1 135.19(16) . . ?
C3 C2 C1 121.1(2) . . ?
C3 C2 C7 121.1(2) . . ?
C1 C2 C7 117.7(2) . . ?
C42 O3 Si1 132.86(16) . . ?
C42 O3 Li1 136.1(2) . . ?
Si1 O3 Li1 90.50(15) . . ?
C2 C3 C4 122.2(2) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 H3 118.9 . . ?
C49 O4 C46 106.2(2) . . ?
C49 O4 Li1 138.8(2) . . ?
C46 O4 Li1 115.0(2) . . ?
C5 C4 C3 117.1(2) . . ?
C5 C4 C8 121.2(2) . . ?
C3 C4 C8 121.8(2) . . ?
C50 O5 C53A 107.7(6) . . ?
C50 O5 C53 100.9(4) . . ?
C53A O5 C53 39.1(6) . . ?
C6 C5 C4 122.4(2) . . ?
C6 C5 H5 118.8 . . ?
C4 C5 H5 118.8 . . ?
C5 C6 C1 120.8(2) . . ?
C5 C6 C9 120.3(2) . . ?
C1 C6 C9 118.4(2) . . ?
C16 C7 C2 113.29(19) . . ?
C16 C7 C10 112.21(19) . . ?
C2 C7 C10 111.89(19) . . ?
C16 C7 H7 106.3 . . ?
C2 C7 H7 106.3 . . ?
C10 C7 H7 106.3 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C28 C9 C6 115.00(19) . . ?
C28 C9 C22 111.98(19) . . ?
C6 C9 C22 110.43(19) . . ?
C28 C9 H9 106.3 . . ?
C6 C9 H9 106.3 . . ?
C22 C9 H9 106.3 . . ?
C15 C10 C11 117.6(2) . . ?
C15 C10 C7 122.6(2) . . ?
C11 C10 C7 119.8(2) . . ?
C12 C11 C10 121.4(2) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C11 C12 C13 120.1(2) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C14 C13 C12 119.2(2) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C13 C14 C15 120.7(2) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C14 C15 C10 121.0(2) . . ?
C14 C15 H15 119.5 . . ?
C10 C15 H15 119.5 . . ?
C17 C16 C21 118.1(2) . . ?
C17 C16 C7 119.4(2) . . ?
C21 C16 C7 122.6(2) . . ?
C16 C17 C18 121.6(3) . . ?
C16 C17 H17 119.2 . . ?
C18 C17 H17 119.2 . . ?
C19 C18 C17 119.5(3) . . ?
C19 C18 H18 120.2 . . ?
C17 C18 H18 120.2 . . ?
C20 C19 C18 119.8(3) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C21 120.8(3) . . ?
C19 C20 H20 119.6 . . ?
C21 C20 H20 119.6 . . ?
C16 C21 C20 120.3(3) . . ?
C16 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C23 C22 C27 118.0(2) . . ?
C23 C22 C9 122.9(2) . . ?
C27 C22 C9 119.1(2) . . ?
C23 C22 Li1 91.45(18) . . ?
C27 C22 Li1 88.55(18) . . ?
C9 C22 Li1 90.16(17) . . ?
C22 C23 C24 120.7(2) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 H23 119.6 . . ?
C25 C24 C23 120.2(3) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C24 C25 C26 119.7(2) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C25 C26 C27 120.0(3) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C26 C27 C22 121.3(3) . . ?
C26 C27 H27 119.3 . . ?
C22 C27 H27 119.3 . . ?
C33 C28 C29 118.3(2) . . ?
C33 C28 C9 118.6(2) . . ?
C29 C28 C9 123.0(2) . . ?
C30 C29 C28 120.8(2) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C31 C30 C29 120.2(3) . . ?
C31 C30 H30 119.9 . . ?
C29 C30 H30 119.9 . . ?
C32 C31 C30 119.4(2) . . ?
C32 C31 H31 120.3 . . ?
C30 C31 H31 120.3 . . ?
C31 C32 C33 120.5(3) . . ?
C31 C32 H32 119.8 . . ?
C33 C32 H32 119.8 . . ?
C32 C33 C28 120.8(2) . . ?
C32 C33 H33 119.6 . . ?
C28 C33 H33 119.6 . . ?
O1 C34 C35 106.4(2) . . ?
O1 C34 C36 108.6(2) . . ?
C35 C34 C36 109.8(2) . . ?
O1 C34 C37 110.2(2) . . ?
C35 C34 C37 110.3(2) . . ?
C36 C34 C37 111.4(2) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O2 C38 C41 111.2(2) . . ?
O2 C38 C39 106.9(2) . . ?
C41 C38 C39 111.0(3) . . ?
O2 C38 C40 107.5(2) . . ?
C41 C38 C40 110.7(3) . . ?
C39 C38 C40 109.3(3) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O3 C42 C43 106.0(2) . . ?
O3 C42 C45 111.7(2) . . ?
C43 C42 C45 112.5(3) . . ?
O3 C42 C44 107.1(2) . . ?
C43 C42 C44 110.8(3) . . ?
C45 C42 C44 108.7(3) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
O4 C46 C47 104.9(2) . . ?
O4 C46 H46A 110.8 . . ?
C47 C46 H46A 110.8 . . ?
O4 C46 H46B 110.8 . . ?
C47 C46 H46B 110.8 . . ?
H46A C46 H46B 108.9 . . ?
C48 C47 C46 101.8(2) . . ?
C48 C47 H47A 111.4 . . ?
C46 C47 H47A 111.4 . . ?
C48 C47 H47B 111.4 . . ?
C46 C47 H47B 111.4 . . ?
H47A C47 H47B 109.3 . . ?
C49 C48 C47 107.7(3) . . ?
C49 C48 H48A 110.2 . . ?
C47 C48 H48A 110.2 . . ?
C49 C48 H48B 110.2 . . ?
C47 C48 H48B 110.2 . . ?
H48A C48 H48B 108.5 . . ?
O4 C49 C48 106.6(3) . . ?
O4 C49 H49A 110.4 . . ?
C48 C49 H49A 110.4 . . ?
O4 C49 H49B 110.4 . . ?
C48 C49 H49B 110.4 . . ?
H49A C49 H49B 108.6 . . ?
O5 C50 C51 104.9(4) . . ?
O5 C50 H50A 110.8 . . ?
C51 C50 H50A 110.8 . . ?
O5 C50 H50B 110.8 . . ?
C51 C50 H50B 110.8 . . ?
H50A C50 H50B 108.8 . . ?
C50 C51 C52 104.3(4) . . ?
C50 C51 H51A 110.9 . . ?
C52 C51 H51A 110.9 . . ?
C50 C51 H51B 110.9 . . ?
C52 C51 H51B 110.9 . . ?
H51A C51 H51B 108.9 . . ?
C53A C52 C51 102.7(6) . . ?
C53A C52 C53 39.6(6) . . ?
C51 C52 C53 104.3(5) . . ?
C53A C52 H52A 75.1 . . ?
C51 C52 H52A 110.9 . . ?
C53 C52 H52A 110.9 . . ?
C53A C52 H52B 141.2 . . ?
C51 C52 H52B 110.9 . . ?
C53 C52 H52B 110.9 . . ?
H52A C52 H52B 108.9 . . ?
O5 C53 C52 98.6(6) . . ?
O5 C53 H53A 112.0 . . ?
C52 C53 H53A 112.0 . . ?
O5 C53 H53B 112.0 . . ?
C52 C53 H53B 112.0 . . ?
H53A C53 H53B 109.7 . . ?
C52 C53A O5 106.0(8) . . ?
C52 C53A H53C 110.5 . . ?
O5 C53A H53C 110.5 . . ?
C52 C53A H53D 110.5 . . ?
O5 C53A H53D 110.5 . . ?
H53C C53A H53D 108.7 . . ?

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.090
