data_2005src1636sq

_exptl_special_details
;
 The SQUEEZE program was used as there was a great deal of highly disordered
 solvent. It appears the majority was probably water molecules, but could easily
 contain some disordered choline.
;


 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. M. A. Beckett
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C35 H98 N7 O27 Si8'
_chemical_formula_weight          1273.92
 
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    C2/c
_symmetry_space_group_name_hall   '-C 2yc'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'
 
_cell_length_a                    31.7262(17)
_cell_length_b                    14.3868(7)
_cell_length_c                    23.1234(13)
_cell_angle_alpha                 90.00
_cell_angle_beta                  123.332(3)
_cell_angle_gamma                 90.00
_cell_volume                      8818.2(8)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     19296
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Slab
_exptl_crystal_colour             Colourless
_exptl_crystal_size_max           0.62
_exptl_crystal_size_mid           0.50
_exptl_crystal_size_min           0.16
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     0.960
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              2740
_exptl_absorpt_coefficient_mu     0.180
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8968
_exptl_absorpt_correction_T_max   0.9718
_exptl_absorpt_process_details       'SADABS V2.10 (Sheldrick, G.M., 2003)'

_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             75745
_diffrn_reflns_av_R_equivalents   0.0461
_diffrn_reflns_av_sigmaI/netI     0.0320
_diffrn_reflns_limit_h_min        -41
_diffrn_reflns_limit_h_max        41
_diffrn_reflns_limit_k_min        -18
_diffrn_reflns_limit_k_max        18
_diffrn_reflns_limit_l_min        -30
_diffrn_reflns_limit_l_max        30
_diffrn_reflns_theta_min          2.97
_diffrn_reflns_theta_max          27.48
_reflns_number_total              10096
_reflns_number_gt                 7730
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          10096
_refine_ls_number_parameters      383
_refine_ls_number_restraints      410
_refine_ls_R_factor_all           0.1126
_refine_ls_R_factor_gt            0.0961
_refine_ls_wR_factor_ref          0.3165
_refine_ls_wR_factor_gt           0.3016
_refine_ls_goodness_of_fit_ref    1.299
_refine_ls_restrained_S_all       1.324
_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
O1 O 0.84891(8) 0.74457(18) 0.06946(12) 0.0337(5) Uani 1 1 d U . .
O2 O 0.79529(9) 0.58900(17) 0.02817(12) 0.0352(6) Uani 1 1 d U . .
O3 O 0.75505(10) 0.66249(16) -0.09527(12) 0.0341(6) Uani 1 1 d U . .
O4 O 0.79628(9) 0.82717(17) -0.05165(11) 0.0333(5) Uani 1 1 d U . .
O5 O 0.88274(8) 0.89993(17) 0.04813(12) 0.0335(5) Uani 1 1 d U . .
O6 O 0.88107(8) 0.59660(17) 0.15034(11) 0.0325(5) Uani 1 1 d U . .
O7 O 0.74942(10) 0.48170(17) -0.08291(12) 0.0357(6) Uani 1 1 d U . .
O8 O 0.75061(8) 0.78434(17) -0.18370(11) 0.0317(5) Uani 1 1 d U . .
O9 O 0.80333(9) 0.90290(17) 0.05714(12) 0.0325(5) Uani 1 1 d U . .
O10 O 0.80221(8) 0.68839(19) 0.12871(11) 0.0335(5) Uani 1 1 d U . .
Si1 Si 0.83398(3) 0.84523(6) 0.03122(4) 0.0257(3) Uani 1 1 d U . .
Si2 Si 0.83202(3) 0.65446(6) 0.09400(4) 0.0261(3) Uani 1 1 d U . .
Si3 Si 0.74911(3) 0.57988(6) -0.05256(4) 0.0250(3) Uani 1 1 d U . .
Si4 Si 0.75015(3) 0.77167(6) -0.11595(4) 0.0244(2) Uani 1 1 d U . .
C11 C 0.9990(2) 0.8760(7) 0.1092(3) 0.153(4) Uani 1 1 d DU . .
H11A H 0.9765 0.9226 0.0741 0.184 Uiso 1 1 calc R . .
H11B H 1.0053 0.8276 0.0845 0.184 Uiso 1 1 calc R . .
C12 C 1.0460(2) 0.9212(6) 0.1551(4) 0.112(3) Uani 1 1 d DU . .
H12A H 1.0382 0.9800 0.1695 0.134 Uiso 1 1 calc R . .
H12B H 1.0598 0.9385 0.1273 0.134 Uiso 1 1 calc R . .
C13 C 1.1331(3) 0.9251(9) 0.2529(5) 0.170(5) Uani 1 1 d DU . .
H13A H 1.1580 0.8900 0.2941 0.255 Uiso 1 1 calc R . .
H13B H 1.1283 0.9865 0.2667 0.255 Uiso 1 1 calc R . .
H13C H 1.1451 0.9324 0.2221 0.255 Uiso 1 1 calc R . .
C14 C 1.0729(2) 0.8521(7) 0.2684(3) 0.128(4) Uani 1 1 d DU . .
H14A H 1.0409 0.8178 0.2445 0.192 Uiso 1 1 calc R . .
H14B H 1.0691 0.9091 0.2884 0.192 Uiso 1 1 calc R . .
H14C H 1.0994 0.8134 0.3054 0.192 Uiso 1 1 calc R . .
C15 C 1.1034(6) 0.7870(8) 0.2042(7) 0.223(7) Uani 1 1 d DU . .
H15A H 1.0745 0.7447 0.1797 0.334 Uiso 1 1 calc R . .
H15B H 1.1295 0.7589 0.2483 0.334 Uiso 1 1 calc R . .
H15C H 1.1170 0.7985 0.1758 0.334 Uiso 1 1 calc R . .
N11 N 1.08679(13) 0.8767(3) 0.21787(17) 0.0555(9) Uani 1 1 d DU . .
O11 O 0.97137(10) 0.8339(3) 0.13267(16) 0.0646(10) Uani 1 1 d DU . .
H11 H 0.9431 0.8174 0.0986 0.097 Uiso 1 1 calc R . .
C21 C 0.7104(3) 0.3299(7) 0.1741(4) 0.124(3) Uani 1 1 d DU . .
H21A H 0.6893 0.3855 0.1512 0.149 Uiso 1 1 calc R . .
H21B H 0.6881 0.2801 0.1720 0.149 Uiso 1 1 calc R . .
C22 C 0.7328(3) 0.2988(4) 0.1344(3) 0.098(2) Uani 1 1 d DU . .
H22A H 0.7616 0.2570 0.1643 0.118 Uiso 1 1 calc R . .
H22B H 0.7071 0.2621 0.0939 0.118 Uiso 1 1 calc R . .
C23 C 0.7196(5) 0.4522(6) 0.0762(5) 0.168(5) Uani 1 1 d DU . .
H23A H 0.7368 0.4954 0.0629 0.252 Uiso 1 1 calc R . .
H23B H 0.7126 0.4835 0.1077 0.252 Uiso 1 1 calc R . .
H23C H 0.6878 0.4319 0.0347 0.252 Uiso 1 1 calc R . .
C24 C 0.7679(5) 0.3384(7) 0.0649(6) 0.164(5) Uani 1 1 d DU . .
H24A H 0.7900 0.2847 0.0875 0.245 Uiso 1 1 calc R . .
H24B H 0.7864 0.3873 0.0584 0.245 Uiso 1 1 calc R . .
H24C H 0.7385 0.3197 0.0198 0.245 Uiso 1 1 calc R . .
C25 C 0.7956(4) 0.4201(7) 0.1709(5) 0.134(3) Uani 1 1 d DU . .
H25A H 0.8211 0.3728 0.1990 0.201 Uiso 1 1 calc R . .
H25B H 0.7853 0.4513 0.1989 0.201 Uiso 1 1 calc R . .
H25C H 0.8099 0.4659 0.1549 0.201 Uiso 1 1 calc R . .
N21 N 0.7506(2) 0.3746(3) 0.1095(2) 0.0699(13) Uani 1 1 d DU . .
O21 O 0.7473(2) 0.3519(3) 0.2459(2) 0.0916(15) Uani 1 1 d DU . .
H21 H 0.7513 0.3057 0.2707 0.137 Uiso 1 1 calc R . .
C31 C 1.0024(5) 0.6242(9) 0.0478(9) 0.387(13) Uani 1 1 d DU . .
H31A H 1.0328 0.6306 0.0463 0.465 Uiso 1 1 calc R . .
H31B H 0.9967 0.6860 0.0612 0.465 Uiso 1 1 calc R . .
C32 C 0.9598(3) 0.6105(12) -0.0252(8) 0.247(7) Uani 1 1 d DU . .
H32A H 0.9658 0.6553 -0.0526 0.297 Uiso 1 1 calc R . .
H32B H 0.9650 0.5480 -0.0382 0.297 Uiso 1 1 calc R . .
C33 C 0.8979(3) 0.6970(8) -0.0247(6) 0.202(6) Uani 1 1 d DU . .
H33A H 0.8619 0.7031 -0.0429 0.304 Uiso 1 1 calc R . .
H33B H 0.9093 0.7521 -0.0374 0.304 Uiso 1 1 calc R . .
H33C H 0.9171 0.6913 0.0258 0.304 Uiso 1 1 calc R . .
C34 C 0.8666(6) 0.6215(10) -0.1311(5) 0.233(7) Uani 1 1 d DU . .
H34A H 0.8706 0.5680 -0.1539 0.350 Uiso 1 1 calc R . .
H34B H 0.8713 0.6790 -0.1495 0.350 Uiso 1 1 calc R . .
H34C H 0.8327 0.6207 -0.1398 0.350 Uiso 1 1 calc R . .
C35 C 0.8873(8) 0.5451(10) -0.0257(11) 0.384(14) Uani 1 1 d DU . .
H35A H 0.8901 0.4833 -0.0411 0.575 Uiso 1 1 calc R . .
H35B H 0.8519 0.5576 -0.0428 0.575 Uiso 1 1 calc R . .
H35C H 0.9077 0.5475 0.0250 0.575 Uiso 1 1 calc R . .
N31 N 0.90568(14) 0.6163(3) -0.0534(2) 0.0615(10) Uani 1 1 d DU . .
O31 O 1.0172(3) 0.5640(10) 0.1063(7) 0.356(10) Uani 1 1 d DU . .
H31 H 0.9937 0.5265 0.0958 0.533 Uiso 1 1 calc R . .
C41 C 0.9155(5) 0.3771(10) 0.1806(7) 0.096(4) Uani 0.50 1 d PDU . .
H41A H 0.8884 0.3381 0.1771 0.115 Uiso 0.50 1 calc PR . .
H41B H 0.9262 0.4213 0.2191 0.115 Uiso 0.50 1 calc PR . .
C42 C 0.9587(6) 0.3158(14) 0.2006(10) 0.151(7) Uani 0.50 1 d PDU . .
H42A H 0.9735 0.2962 0.2491 0.181 Uiso 0.50 1 calc PR . .
H42B H 0.9456 0.2592 0.1715 0.181 Uiso 0.50 1 calc PR . .
C43 C 0.9807(7) 0.362(2) 0.1225(11) 0.277(16) Uani 0.50 1 d PDU . .
H43A H 1.0080 0.3842 0.1179 0.416 Uiso 0.50 1 calc PR . .
H43B H 0.9530 0.4073 0.1010 0.416 Uiso 0.50 1 calc PR . .
H43C H 0.9685 0.3020 0.0994 0.416 Uiso 0.50 1 calc PR . .
C44 C 1.0091(17) 0.4540(19) 0.217(2) 0.39(3) Uani 0.50 1 d PDU . .
H44A H 1.0235 0.4590 0.2667 0.590 Uiso 0.50 1 calc PR . .
H44B H 0.9773 0.4885 0.1913 0.590 Uiso 0.50 1 calc PR . .
H44C H 1.0328 0.4802 0.2065 0.590 Uiso 0.50 1 calc PR . .
C45 C 1.0454(8) 0.302(2) 0.2175(18) 0.34(2) Uani 0.50 1 d PDU . .
H45A H 1.0637 0.2904 0.2674 0.514 Uiso 0.50 1 calc PR . .
H45B H 1.0665 0.3394 0.2075 0.514 Uiso 0.50 1 calc PR . .
H45C H 1.0370 0.2431 0.1926 0.514 Uiso 0.50 1 calc PR . .
N41 N 0.9995(6) 0.3525(16) 0.1955(11) 0.215(9) Uani 0.50 1 d PDU . .
O41 O 0.8943(3) 0.4283(4) 0.1205(3) 0.0586(17) Uani 0.50 1 d PDU . .
H41 H 0.8892 0.3936 0.0880 0.088 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
O1 Si2 1.620(3) . ?
O1 Si1 1.626(3) . ?
O2 Si2 1.616(3) . ?
O2 Si3 1.626(2) . ?
O3 Si3 1.621(2) . ?
O3 Si4 1.624(2) . ?
O4 Si4 1.612(2) . ?
O4 Si1 1.628(2) . ?
O5 Si1 1.581(2) . ?
O6 Si2 1.607(2) . ?
O7 Si3 1.580(2) . ?
O8 Si4 1.585(2) . ?
O9 Si1 1.623(2) . ?
O9 Si3 1.627(2) 7_665 ?
O10 Si2 1.616(2) . ?
O10 Si4 1.624(2) 7_665 ?
Si3 O9 1.627(2) 7_665 ?
Si4 O10 1.624(2) 7_665 ?
C11 O11 1.397(7) . ?
C11 C12 1.425(8) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N11 1.459(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N11 1.410(7) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 N11 1.502(7) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 N11 1.491(9) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
O11 H11 0.8400 . ?
C21 O21 1.446(8) . ?
C21 C22 1.505(9) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 N21 1.481(7) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 N21 1.405(8) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 N21 1.502(8) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 N21 1.502(9) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
O21 H21 0.8400 . ?
C31 O31 1.450(16) . ?
C31 C32 1.486(13) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 N31 1.467(9) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 N31 1.424(7) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 N31 1.523(10) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 N31 1.487(11) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
O31 H31 0.8400 . ?
C41 O41 1.377(11) . ?
C41 C42 1.477(13) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 N41 1.461(14) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 N41 1.456(15) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 N41 1.519(16) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 N41 1.442(15) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
O41 H41 0.8400 . ?
 
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
Si2 O1 Si1 148.19(16) . . ?
Si2 O2 Si3 148.97(17) . . ?
Si3 O3 Si4 149.77(16) . . ?
Si4 O4 Si1 150.70(17) . . ?
Si1 O9 Si3 148.50(16) . 7_665 ?
Si2 O10 Si4 146.72(15) . 7_665 ?
O5 Si1 O9 110.96(13) . . ?
O5 Si1 O1 110.83(13) . . ?
O9 Si1 O1 108.00(13) . . ?
O5 Si1 O4 110.89(13) . . ?
O9 Si1 O4 108.33(12) . . ?
O1 Si1 O4 107.70(13) . . ?
O6 Si2 O10 108.91(12) . . ?
O6 Si2 O2 109.72(14) . . ?
O10 Si2 O2 109.14(13) . . ?
O6 Si2 O1 109.82(13) . . ?
O10 Si2 O1 109.20(14) . . ?
O2 Si2 O1 110.03(13) . . ?
O7 Si3 O3 110.71(13) . . ?
O7 Si3 O2 111.14(13) . . ?
O3 Si3 O2 107.89(13) . . ?
O7 Si3 O9 111.29(13) . 7_665 ?
O3 Si3 O9 107.80(13) . 7_665 ?
O2 Si3 O9 107.86(13) . 7_665 ?
O8 Si4 O4 110.96(13) . . ?
O8 Si4 O10 110.11(12) . 7_665 ?
O4 Si4 O10 108.17(13) . 7_665 ?
O8 Si4 O3 110.54(13) . . ?
O4 Si4 O3 108.41(13) . . ?
O10 Si4 O3 108.57(14) 7_665 . ?
O11 C11 C12 122.1(6) . . ?
O11 C11 H11A 106.8 . . ?
C12 C11 H11A 106.8 . . ?
O11 C11 H11B 106.8 . . ?
C12 C11 H11B 106.8 . . ?
H11A C11 H11B 106.6 . . ?
C11 C12 N11 122.3(6) . . ?
C11 C12 H12A 106.8 . . ?
N11 C12 H12A 106.8 . . ?
C11 C12 H12B 106.8 . . ?
N11 C12 H12B 106.8 . . ?
H12A C12 H12B 106.6 . . ?
N11 C13 H13A 109.5 . . ?
N11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N11 C14 H14A 109.5 . . ?
N11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N11 C15 H15A 109.5 . . ?
N11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 N11 C12 115.4(6) . . ?
C13 N11 C15 99.9(9) . . ?
C12 N11 C15 113.1(7) . . ?
C13 N11 C14 109.2(6) . . ?
C12 N11 C14 113.5(5) . . ?
C15 N11 C14 104.5(7) . . ?
C11 O11 H11 109.5 . . ?
O21 C21 C22 114.3(7) . . ?
O21 C21 H21A 108.7 . . ?
C22 C21 H21A 108.7 . . ?
O21 C21 H21B 108.7 . . ?
C22 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
N21 C22 C21 115.2(6) . . ?
N21 C22 H22A 108.5 . . ?
C21 C22 H22A 108.5 . . ?
N21 C22 H22B 108.5 . . ?
C21 C22 H22B 108.5 . . ?
H22A C22 H22B 107.5 . . ?
N21 C23 H23A 109.5 . . ?
N21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N21 C24 H24A 109.5 . . ?
N21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N21 C25 H25A 109.5 . . ?
N21 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N21 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 N21 C22 119.8(6) . . ?
C23 N21 C24 108.0(6) . . ?
C22 N21 C24 111.9(5) . . ?
C23 N21 C25 100.8(7) . . ?
C22 N21 C25 108.7(5) . . ?
C24 N21 C25 106.4(7) . . ?
C21 O21 H21 109.5 . . ?
O31 C31 C32 127.4(12) . . ?
O31 C31 H31A 105.5 . . ?
C32 C31 H31A 105.5 . . ?
O31 C31 H31B 105.5 . . ?
C32 C31 H31B 105.5 . . ?
H31A C31 H31B 106.0 . . ?
N31 C32 C31 127.4(11) . . ?
N31 C32 H32A 105.4 . . ?
C31 C32 H32A 105.4 . . ?
N31 C32 H32B 105.4 . . ?
C31 C32 H32B 105.4 . . ?
H32A C32 H32B 106.0 . . ?
N31 C33 H33A 109.5 . . ?
N31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N31 C34 H34A 109.5 . . ?
N31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N31 C35 H35A 109.5 . . ?
N31 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
N31 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 N31 C32 107.5(7) . . ?
C33 N31 C35 98.7(7) . . ?
C32 N31 C35 114.2(11) . . ?
C33 N31 C34 105.8(7) . . ?
C32 N31 C34 121.5(9) . . ?
C35 N31 C34 106.5(10) . . ?
C31 O31 H31 109.5 . . ?
O41 C41 C42 119.3(11) . . ?
O41 C41 H41A 107.5 . . ?
C42 C41 H41A 107.5 . . ?
O41 C41 H41B 107.5 . . ?
C42 C41 H41B 107.5 . . ?
H41A C41 H41B 107.0 . . ?
N41 C42 C41 118.1(13) . . ?
N41 C42 H42A 107.8 . . ?
C41 C42 H42A 107.8 . . ?
N41 C42 H42B 107.8 . . ?
C41 C42 H42B 107.8 . . ?
H42A C42 H42B 107.1 . . ?
N41 C43 H43A 109.5 . . ?
N41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
N41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N41 C44 H44A 109.5 . . ?
N41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
N41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N41 C45 H45A 109.5 . . ?
N41 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
N41 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C45 N41 C43 98.6(16) . . ?
C45 N41 C42 123.8(17) . . ?
C43 N41 C42 108.2(15) . . ?
C45 N41 C44 112.5(19) . . ?
C43 N41 C44 99.5(18) . . ?
C42 N41 C44 110.5(18) . . ?
C41 O41 H41 109.5 . . ?
 
_diffrn_measured_fraction_theta_max    0.998
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.998
_refine_diff_density_max    1.167
_refine_diff_density_min   -0.864
_refine_diff_density_rms    0.129
