# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_140930b
_database_code_depnum_ccdc_archive 'CCDC 1028584'
_audit_update_record             
;
2014-10-10 deposited with the CCDC.
2015-05-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H26 N4 O6 W'
_chemical_formula_weight         554.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 '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                   16.5081(7)
_cell_length_b                   23.4259(8)
_cell_length_c                   10.2617(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.433(3)
_cell_angle_gamma                90.00
_cell_volume                     3964.8(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5775
_cell_measurement_theta_min      5.3540
_cell_measurement_theta_max      71.3270

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2176
_exptl_absorpt_coefficient_mu    11.152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1079
_exptl_absorpt_correction_T_max  0.4690
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6937
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0850
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.68
_diffrn_reflns_theta_max         66.19
_reflns_number_total             6937
_reflns_number_gt                4900
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0001P)²+144.6593P] 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         6937
_refine_ls_number_parameters     489
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0840
_refine_ls_wR_factor_ref         0.2009
_refine_ls_wR_factor_gt          0.1897
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_restrained_S_all      1.178
_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
W1 W 0.35947(5) 0.39485(4) 0.18520(8) 0.0322(2) Uani 1 1 d . . .
W2 W 0.13290(5) 0.39128(3) 0.71485(8) 0.0318(2) Uani 1 1 d . . .
N1 N 0.1542(10) 0.3385(7) 0.0955(17) 0.049(4) Uani 1 1 d . . .
H1A H 0.1508 0.3404 0.0088 0.073 Uiso 1 1 d R . .
H1B H 0.2061 0.3372 0.1227 0.073 Uiso 1 1 d R . .
N2 N 0.0670(12) 0.3376(7) 0.3293(17) 0.057(5) Uani 1 1 d . . .
H2A H 0.1009 0.3669 0.3230 0.086 Uiso 1 1 calc R . .
H2B H 0.0540 0.3333 0.4121 0.086 Uiso 1 1 calc R . .
H2C H 0.0222 0.3442 0.2802 0.086 Uiso 1 1 calc R . .
N3 N 0.3489(10) 0.3434(7) 0.5491(16) 0.045(4) Uani 1 1 d . . .
H3A H 0.2969 0.3504 0.5621 0.067 Uiso 1 1 d R . .
H3B H 0.3570 0.3435 0.4639 0.067 Uiso 1 1 d R . .
N4 N 0.4045(16) 0.3352(9) 0.812(2) 0.087(8) Uani 1 1 d . . .
H4A H 0.4574 0.3373 0.7990 0.130 Uiso 1 1 calc R . .
H4B H 0.3966 0.3321 0.8968 0.130 Uiso 1 1 calc R . .
H4C H 0.3800 0.3665 0.7809 0.130 Uiso 1 1 calc R . .
N5 N 0.0592(12) 0.4403(8) 0.0966(16) 0.058(5) Uani 1 1 d . . .
H5A H 0.0888 0.4087 0.1057 0.087 Uiso 1 1 calc R . .
H5B H 0.0423 0.4442 0.0135 0.087 Uiso 1 1 calc R . .
H5C H 0.0165 0.4380 0.1464 0.087 Uiso 1 1 calc R . .
N6 N 0.1408(10) 0.4497(7) 0.3592(16) 0.042(4) Uani 1 1 d . . .
H6A H 0.1339 0.4551 0.4438 0.063 Uiso 1 1 d R . .
H6B H 0.1935 0.4474 0.3452 0.063 Uiso 1 1 d R . .
N7 N 0.4414(12) 0.4464(8) 0.5862(18) 0.063(5) Uani 1 1 d . . .
H7A H 0.4827 0.4448 0.6447 0.095 Uiso 1 1 calc R . .
H7B H 0.4603 0.4516 0.5071 0.095 Uiso 1 1 calc R . .
H7C H 0.4136 0.4139 0.5877 0.095 Uiso 1 1 calc R . .
N8 N 0.3632(10) 0.4553(7) 0.8412(16) 0.045(4) Uani 1 1 d . . .
H8A H 0.3113 0.4605 0.8580 0.067 Uiso 1 1 d R . .
H8B H 0.3925 0.4532 0.9160 0.067 Uiso 1 1 d R . .
O1 O 0.4574(7) 0.3945(6) 0.3247(13) 0.043(3) Uani 1 1 d . . .
O2 O 0.4415(8) 0.3452(5) 0.1045(13) 0.040(3) Uani 1 1 d . . .
O3 O 0.3149(8) 0.4596(5) 0.2887(13) 0.042(3) Uani 1 1 d . . .
O4 O 0.4157(7) 0.4684(5) 0.1079(12) 0.038(3) Uani 1 1 d . . .
O5 O 0.3026(8) 0.3482(5) 0.2809(12) 0.040(3) Uani 1 1 d . . .
O6 O 0.3008(8) 0.3915(6) 0.0410(13) 0.049(3) Uani 1 1 d . . .
O7 O 0.0297(8) 0.3992(5) 0.8255(13) 0.043(3) Uani 1 1 d . . .
O8 O 0.0494(8) 0.3454(5) 0.6164(13) 0.041(3) Uani 1 1 d . . .
O9 O 0.0872(7) 0.4665(5) 0.6191(12) 0.037(3) Uani 1 1 d . . .
O10 O 0.1810(7) 0.4554(5) 0.8211(13) 0.039(3) Uani 1 1 d . . .
O11 O 0.1965(8) 0.3837(6) 0.5804(14) 0.050(4) Uani 1 1 d . . .
O12 O 0.1754(8) 0.3415(5) 0.8253(13) 0.045(3) Uani 1 1 d . . .
C1 C 0.5171(12) 0.3575(8) 0.299(2) 0.041(5) Uani 1 1 d . . .
C2 C 0.5098(12) 0.3311(8) 0.176(2) 0.042(5) Uani 1 1 d . . .
C3 C 0.5671(13) 0.2930(9) 0.134(2) 0.052(6) Uani 1 1 d . . .
H3 H 0.5616 0.2757 0.0524 0.062 Uiso 1 1 calc R . .
C4 C 0.6326(13) 0.2817(9) 0.218(2) 0.054(6) Uani 1 1 d . . .
H4 H 0.6720 0.2562 0.1921 0.065 Uiso 1 1 calc R . .
C5 C 0.6412(13) 0.3064(9) 0.336(2) 0.052(6) Uani 1 1 d . . .
H5 H 0.6868 0.2978 0.3890 0.062 Uiso 1 1 calc R . .
C6 C 0.5831(12) 0.3453(9) 0.384(2) 0.049(5) Uani 1 1 d . . .
H6 H 0.5888 0.3615 0.4663 0.059 Uiso 1 1 calc R . .
C7 C 0.3370(12) 0.5137(8) 0.257(2) 0.043(5) Uani 1 1 d . . .
C8 C 0.3907(12) 0.5178(8) 0.156(2) 0.042(5) Uani 1 1 d . . .
C9 C 0.4139(13) 0.5720(9) 0.112(2) 0.050(5) Uani 1 1 d . . .
H9 H 0.4496 0.5757 0.0446 0.060 Uiso 1 1 calc R . .
C10 C 0.3822(13) 0.6200(9) 0.171(2) 0.052(6) Uani 1 1 d . . .
H10 H 0.3948 0.6559 0.1392 0.063 Uiso 1 1 calc R . .
C11 C 0.3334(13) 0.6158(9) 0.273(2) 0.055(6) Uani 1 1 d . . .
H11 H 0.3160 0.6490 0.3130 0.067 Uiso 1 1 calc R . .
C12 C 0.3082(12) 0.5618(9) 0.321(2) 0.048(5) Uani 1 1 d . . .
H12 H 0.2743 0.5587 0.3903 0.058 Uiso 1 1 calc R . .
C13 C -0.0280(12) 0.3604(8) 0.797(2) 0.042(5) Uani 1 1 d . . .
C14 C -0.0203(12) 0.3320(8) 0.676(2) 0.042(5) Uani 1 1 d . . .
C15 C -0.0754(12) 0.2933(9) 0.631(2) 0.049(5) Uani 1 1 d . . .
H15 H -0.0710 0.2751 0.5513 0.059 Uiso 1 1 calc R . .
C16 C -0.1420(13) 0.2819(9) 0.715(2) 0.054(6) Uani 1 1 d . . .
H16 H -0.1805 0.2551 0.6878 0.064 Uiso 1 1 calc R . .
C17 C -0.1517(13) 0.3082(9) 0.832(2) 0.055(6) Uani 1 1 d . . .
H17 H -0.1953 0.2996 0.8834 0.065 Uiso 1 1 calc R . .
C18 C -0.0929(13) 0.3488(9) 0.872(2) 0.050(5) Uani 1 1 d . . .
H18 H -0.0979 0.3679 0.9510 0.060 Uiso 1 1 calc R . .
C19 C 0.1153(12) 0.5149(8) 0.669(2) 0.040(5) Uani 1 1 d . . .
C20 C 0.1647(12) 0.5099(8) 0.783(2) 0.041(5) Uani 1 1 d . . .
C21 C 0.1980(12) 0.5560(8) 0.850(2) 0.046(5) Uani 1 1 d . . .
H21 H 0.2299 0.5517 0.9260 0.055 Uiso 1 1 calc R . .
C22 C 0.1804(13) 0.6110(9) 0.795(2) 0.054(6) Uani 1 1 d . . .
H22 H 0.1996 0.6434 0.8381 0.064 Uiso 1 1 calc R . .
C23 C 0.1353(13) 0.6173(9) 0.677(2) 0.052(5) Uani 1 1 d . . .
H23 H 0.1286 0.6532 0.6393 0.062 Uiso 1 1 calc R . .
C24 C 0.1010(13) 0.5701(8) 0.617(2) 0.047(5) Uani 1 1 d . . .
H24 H 0.0680 0.5744 0.5420 0.057 Uiso 1 1 calc R . .
C25 C 0.1129(14) 0.2863(9) 0.137(2) 0.049(5) Uani 1 1 d . . .
H25A H 0.1436 0.2531 0.1123 0.058 Uiso 1 1 calc R . .
H25B H 0.0595 0.2841 0.0946 0.058 Uiso 1 1 calc R . .
C26 C 0.1050(15) 0.2868(9) 0.2856(19) 0.051(6) Uani 1 1 d . . .
H26A H 0.0735 0.2539 0.3108 0.061 Uiso 1 1 calc R . .
H26B H 0.1585 0.2836 0.3278 0.061 Uiso 1 1 calc R . .
C27 C 0.3702(16) 0.2877(9) 0.604(2) 0.059(6) Uani 1 1 d . . .
H27A H 0.4227 0.2761 0.5737 0.071 Uiso 1 1 calc R . .
H27B H 0.3305 0.2597 0.5730 0.071 Uiso 1 1 calc R . .
C28 C 0.3731(19) 0.2890(10) 0.749(3) 0.074(8) Uani 1 1 d . . .
H28A H 0.3182 0.2840 0.7768 0.088 Uiso 1 1 calc R . .
H28B H 0.4039 0.2560 0.7795 0.088 Uiso 1 1 calc R . .
C29 C 0.1085(13) 0.4898(9) 0.1363(19) 0.047(5) Uani 1 1 d . . .
H29A H 0.0885 0.5235 0.0905 0.057 Uiso 1 1 calc R . .
H29B H 0.1642 0.4836 0.1133 0.057 Uiso 1 1 calc R . .
C30 C 0.1052(12) 0.4992(8) 0.2837(19) 0.043(5) Uani 1 1 d . . .
H30A H 0.1348 0.5337 0.3076 0.052 Uiso 1 1 calc R . .
H30B H 0.0493 0.5045 0.3064 0.052 Uiso 1 1 calc R . .
C31 C 0.3890(14) 0.4932(10) 0.617(2) 0.056(6) Uani 1 1 d . . .
H31A H 0.3337 0.4840 0.5889 0.067 Uiso 1 1 calc R . .
H31B H 0.4053 0.5270 0.5702 0.067 Uiso 1 1 calc R . .
C32 C 0.3923(13) 0.5058(9) 0.763(2) 0.050(5) Uani 1 1 d . . .
H32A H 0.4476 0.5150 0.7912 0.060 Uiso 1 1 calc R . .
H32B H 0.3587 0.5387 0.7797 0.060 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
W1 O6 1.736(13) . ?
W1 O5 1.766(12) . ?
W1 O2 1.992(12) . ?
W1 O3 2.009(13) . ?
W1 O1 2.113(13) . ?
W1 O4 2.126(12) . ?
W2 O12 1.752(13) . ?
W2 O11 1.777(14) . ?
W2 O8 1.990(12) . ?
W2 O10 2.001(12) . ?
W2 O7 2.095(13) . ?
W2 O9 2.139(12) . ?
N1 C25 1.47(2) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N2 C26 1.43(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N3 C27 1.46(2) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N4 C28 1.35(3) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 H4C 0.8900 . ?
N5 C29 1.47(3) . ?
N5 H5A 0.8900 . ?
N5 H5B 0.8900 . ?
N5 H5C 0.8900 . ?
N6 C30 1.50(2) . ?
N6 H6A 0.8900 . ?
N6 H6B 0.8900 . ?
N7 C31 1.44(3) . ?
N7 H7A 0.8900 . ?
N7 H7B 0.8900 . ?
N7 H7C 0.8900 . ?
N8 C32 1.52(2) . ?
N8 H8A 0.8900 . ?
N8 H8B 0.8900 . ?
O1 C1 1.35(2) . ?
O2 C2 1.36(2) . ?
O3 C7 1.36(2) . ?
O4 C8 1.33(2) . ?
O7 C13 1.34(2) . ?
O8 C14 1.37(2) . ?
O9 C19 1.32(2) . ?
O10 C20 1.36(2) . ?
C1 C6 1.39(3) . ?
C1 C2 1.40(3) . ?
C2 C3 1.39(3) . ?
C3 C4 1.38(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.35(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.42(3) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.39(3) . ?
C7 C12 1.40(3) . ?
C8 C9 1.41(3) . ?
C9 C10 1.39(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.35(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.43(3) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C18 1.38(3) . ?
C13 C14 1.41(3) . ?
C14 C15 1.35(3) . ?
C15 C16 1.45(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.36(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.41(3) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C20 1.40(3) . ?
C19 C24 1.41(3) . ?
C20 C21 1.38(3) . ?
C21 C22 1.43(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.40(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.38(3) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C26 1.53(3) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.49(3) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.53(3) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C32 1.52(3) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 W1 O5 98.9(6) . . ?
O6 W1 O2 89.1(6) . . ?
O5 W1 O2 104.9(6) . . ?
O6 W1 O3 106.4(6) . . ?
O5 W1 O3 87.6(5) . . ?
O2 W1 O3 158.6(5) . . ?
O6 W1 O1 163.8(6) . . ?
O5 W1 O1 91.7(6) . . ?
O2 W1 O1 76.4(5) . . ?
O3 W1 O1 86.1(5) . . ?
O6 W1 O4 87.5(5) . . ?
O5 W1 O4 163.7(5) . . ?
O2 W1 O4 90.1(5) . . ?
O3 W1 O4 76.2(5) . . ?
O1 W1 O4 85.5(5) . . ?
O12 W2 O11 101.7(6) . . ?
O12 W2 O8 102.6(6) . . ?
O11 W2 O8 88.3(6) . . ?
O12 W2 O10 90.5(6) . . ?
O11 W2 O10 105.3(6) . . ?
O8 W2 O10 158.9(5) . . ?
O12 W2 O7 91.2(6) . . ?
O11 W2 O7 161.8(6) . . ?
O8 W2 O7 76.2(5) . . ?
O10 W2 O7 87.2(5) . . ?
O12 W2 O9 165.7(5) . . ?
O11 W2 O9 86.2(6) . . ?
O8 W2 O9 89.3(5) . . ?
O10 W2 O9 75.9(5) . . ?
O7 W2 O9 84.1(5) . . ?
C25 N1 H1A 108.9 . . ?
C25 N1 H1B 109.3 . . ?
H1A N1 H1B 109.5 . . ?
C26 N2 H2A 109.5 . . ?
C26 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C26 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C27 N3 H3A 108.9 . . ?
C27 N3 H3B 109.6 . . ?
H3A N3 H3B 109.5 . . ?
C28 N4 H4A 109.5 . . ?
C28 N4 H4B 109.5 . . ?
H4A N4 H4B 109.5 . . ?
C28 N4 H4C 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
C29 N5 H5A 109.5 . . ?
C29 N5 H5B 109.5 . . ?
H5A N5 H5B 109.5 . . ?
C29 N5 H5C 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
C30 N6 H6A 109.3 . . ?
C30 N6 H6B 109.1 . . ?
H6A N6 H6B 109.5 . . ?
C31 N7 H7A 109.5 . . ?
C31 N7 H7B 109.5 . . ?
H7A N7 H7B 109.5 . . ?
C31 N7 H7C 109.5 . . ?
H7A N7 H7C 109.5 . . ?
H7B N7 H7C 109.5 . . ?
C32 N8 H8A 108.9 . . ?
C32 N8 H8B 109.1 . . ?
H8A N8 H8B 109.5 . . ?
C1 O1 W1 114.6(12) . . ?
C2 O2 W1 118.5(12) . . ?
C7 O3 W1 117.9(12) . . ?
C8 O4 W1 114.8(12) . . ?
C13 O7 W2 114.1(12) . . ?
C14 O8 W2 118.3(12) . . ?
C19 O9 W2 114.7(11) . . ?
C20 O10 W2 118.7(12) . . ?
O1 C1 C6 124.7(19) . . ?
O1 C1 C2 115.0(17) . . ?
C6 C1 C2 120.2(19) . . ?
O2 C2 C3 123.1(19) . . ?
O2 C2 C1 114.7(17) . . ?
C3 C2 C1 122(2) . . ?
C4 C3 C2 117(2) . . ?
C4 C3 H3 121.5 . . ?
C2 C3 H3 121.5 . . ?
C5 C4 C3 122(2) . . ?
C5 C4 H4 119.0 . . ?
C3 C4 H4 119.0 . . ?
C4 C5 C6 122(2) . . ?
C4 C5 H5 118.8 . . ?
C6 C5 H5 118.8 . . ?
C1 C6 C5 116(2) . . ?
C1 C6 H6 122.0 . . ?
C5 C6 H6 122.0 . . ?
O3 C7 C8 115.3(18) . . ?
O3 C7 C12 122.5(19) . . ?
C8 C7 C12 122.1(19) . . ?
O4 C8 C7 115.6(17) . . ?
O4 C8 C9 124.9(19) . . ?
C7 C8 C9 119.4(19) . . ?
C10 C9 C8 118(2) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
C11 C10 C9 122(2) . . ?
C11 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
C10 C11 C12 121(2) . . ?
C10 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C7 C12 C11 116(2) . . ?
C7 C12 H12 121.8 . . ?
C11 C12 H12 121.8 . . ?
O7 C13 C18 125.0(19) . . ?
O7 C13 C14 115.0(17) . . ?
C18 C13 C14 119.9(19) . . ?
C15 C14 O8 124.6(19) . . ?
C15 C14 C13 122(2) . . ?
O8 C14 C13 113.2(17) . . ?
C14 C15 C16 116(2) . . ?
C14 C15 H15 122.1 . . ?
C16 C15 H15 122.1 . . ?
C17 C16 C15 124(2) . . ?
C17 C16 H16 117.9 . . ?
C15 C16 H16 117.9 . . ?
C16 C17 C18 117(2) . . ?
C16 C17 H17 121.4 . . ?
C18 C17 H17 121.4 . . ?
C13 C18 C17 121(2) . . ?
C13 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
O9 C19 C20 115.7(17) . . ?
O9 C19 C24 126.0(19) . . ?
C20 C19 C24 118.3(18) . . ?
O10 C20 C21 121.6(19) . . ?
O10 C20 C19 114.8(17) . . ?
C21 C20 C19 123.5(18) . . ?
C20 C21 C22 116(2) . . ?
C20 C21 H21 122.0 . . ?
C22 C21 H21 122.0 . . ?
C23 C22 C21 122(2) . . ?
C23 C22 H22 119.1 . . ?
C21 C22 H22 119.1 . . ?
C24 C23 C22 120(2) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C23 C24 C19 121(2) . . ?
C23 C24 H24 119.7 . . ?
C19 C24 H24 119.7 . . ?
N1 C25 C26 110.1(16) . . ?
N1 C25 H25A 109.6 . . ?
C26 C25 H25A 109.6 . . ?
N1 C25 H25B 109.6 . . ?
C26 C25 H25B 109.6 . . ?
H25A C25 H25B 108.2 . . ?
N2 C26 C25 112.0(18) . . ?
N2 C26 H26A 109.2 . . ?
C25 C26 H26A 109.2 . . ?
N2 C26 H26B 109.2 . . ?
C25 C26 H26B 109.2 . . ?
H26A C26 H26B 107.9 . . ?
N3 C27 C28 111.3(18) . . ?
N3 C27 H27A 109.4 . . ?
C28 C27 H27A 109.4 . . ?
N3 C27 H27B 109.4 . . ?
C28 C27 H27B 109.4 . . ?
H27A C27 H27B 108.0 . . ?
N4 C28 C27 119(2) . . ?
N4 C28 H28A 107.5 . . ?
C27 C28 H28A 107.5 . . ?
N4 C28 H28B 107.5 . . ?
C27 C28 H28B 107.5 . . ?
H28A C28 H28B 107.0 . . ?
N5 C29 C30 110.2(17) . . ?
N5 C29 H29A 109.6 . . ?
C30 C29 H29A 109.6 . . ?
N5 C29 H29B 109.6 . . ?
C30 C29 H29B 109.6 . . ?
H29A C29 H29B 108.1 . . ?
N6 C30 C29 111.7(16) . . ?
N6 C30 H30A 109.3 . . ?
C29 C30 H30A 109.3 . . ?
N6 C30 H30B 109.3 . . ?
C29 C30 H30B 109.3 . . ?
H30A C30 H30B 107.9 . . ?
N7 C31 C32 111.5(19) . . ?
N7 C31 H31A 109.3 . . ?
C32 C31 H31A 109.3 . . ?
N7 C31 H31B 109.3 . . ?
C32 C31 H31B 109.3 . . ?
H31A C31 H31B 108.0 . . ?
N8 C32 C31 111.7(17) . . ?
N8 C32 H32A 109.3 . . ?
C31 C32 H32A 109.3 . . ?
N8 C32 H32B 109.3 . . ?
C31 C32 H32B 109.3 . . ?
H32A C32 H32B 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O6 W1 O1 C1 -34(3) . . . . ?
O5 W1 O1 C1 96.9(13) . . . . ?
O2 W1 O1 C1 -8.0(12) . . . . ?
O3 W1 O1 C1 -175.6(13) . . . . ?
O4 W1 O1 C1 -99.2(13) . . . . ?
O6 W1 O2 C2 179.6(13) . . . . ?
O5 W1 O2 C2 -81.4(13) . . . . ?
O3 W1 O2 C2 43(2) . . . . ?
O1 W1 O2 C2 6.8(12) . . . . ?
O4 W1 O2 C2 92.1(13) . . . . ?
O6 W1 O3 C7 -79.9(14) . . . . ?
O5 W1 O3 C7 -178.5(14) . . . . ?
O2 W1 O3 C7 55(2) . . . . ?
O1 W1 O3 C7 89.6(13) . . . . ?
O4 W1 O3 C7 3.3(12) . . . . ?
O6 W1 O4 C8 102.9(13) . . . . ?
O5 W1 O4 C8 -11(3) . . . . ?
O2 W1 O4 C8 -168.0(13) . . . . ?
O3 W1 O4 C8 -4.6(12) . . . . ?
O1 W1 O4 C8 -91.7(13) . . . . ?
O12 W2 O7 C13 -86.5(13) . . . . ?
O11 W2 O7 C13 49(2) . . . . ?
O8 W2 O7 C13 16.2(13) . . . . ?
O10 W2 O7 C13 -176.9(13) . . . . ?
O9 W2 O7 C13 107.0(13) . . . . ?
O12 W2 O8 C14 74.7(13) . . . . ?
O11 W2 O8 C14 176.3(13) . . . . ?
O10 W2 O8 C14 -52(2) . . . . ?
O7 W2 O8 C14 -13.4(12) . . . . ?
O9 W2 O8 C14 -97.4(13) . . . . ?
O12 W2 O9 C19 21(3) . . . . ?
O11 W2 O9 C19 -103.0(13) . . . . ?
O8 W2 O9 C19 168.6(13) . . . . ?
O10 W2 O9 C19 3.8(12) . . . . ?
O7 W2 O9 C19 92.4(13) . . . . ?
O12 W2 O10 C20 -177.2(14) . . . . ?
O11 W2 O10 C20 80.6(14) . . . . ?
O8 W2 O10 C20 -48(2) . . . . ?
O7 W2 O10 C20 -86.0(13) . . . . ?
O9 W2 O10 C20 -1.4(13) . . . . ?
W1 O1 C1 C6 -172.6(16) . . . . ?
W1 O1 C1 C2 8(2) . . . . ?
W1 O2 C2 C3 174.2(15) . . . . ?
W1 O2 C2 C1 -5(2) . . . . ?
O1 C1 C2 O2 -3(2) . . . . ?
C6 C1 C2 O2 178.0(17) . . . . ?
O1 C1 C2 C3 178.6(18) . . . . ?
C6 C1 C2 C3 -1(3) . . . . ?
O2 C2 C3 C4 -178.7(18) . . . . ?
C1 C2 C3 C4 0(3) . . . . ?
C2 C3 C4 C5 0(3) . . . . ?
C3 C4 C5 C6 1(4) . . . . ?
O1 C1 C6 C5 -177.9(18) . . . . ?
C2 C1 C6 C5 1(3) . . . . ?
C4 C5 C6 C1 -2(3) . . . . ?
W1 O3 C7 C8 -2(2) . . . . ?
W1 O3 C7 C12 178.6(15) . . . . ?
W1 O4 C8 C7 5(2) . . . . ?
W1 O4 C8 C9 -174.2(16) . . . . ?
O3 C7 C8 O4 -3(3) . . . . ?
C12 C7 C8 O4 177.2(18) . . . . ?
O3 C7 C8 C9 176.9(17) . . . . ?
C12 C7 C8 C9 -3(3) . . . . ?
O4 C8 C9 C10 179.5(19) . . . . ?
C7 C8 C9 C10 0(3) . . . . ?
C8 C9 C10 C11 3(3) . . . . ?
C9 C10 C11 C12 -4(3) . . . . ?
O3 C7 C12 C11 -177.2(18) . . . . ?
C8 C7 C12 C11 3(3) . . . . ?
C10 C11 C12 C7 1(3) . . . . ?
W2 O7 C13 C18 165.5(17) . . . . ?
W2 O7 C13 C14 -17(2) . . . . ?
W2 O8 C14 C15 -167.9(16) . . . . ?
W2 O8 C14 C13 9(2) . . . . ?
O7 C13 C14 C15 -177.4(18) . . . . ?
C18 C13 C14 C15 0(3) . . . . ?
O7 C13 C14 O8 6(3) . . . . ?
C18 C13 C14 O8 -176.2(18) . . . . ?
O8 C14 C15 C16 175.0(18) . . . . ?
C13 C14 C15 C16 -1(3) . . . . ?
C14 C15 C16 C17 1(3) . . . . ?
C15 C16 C17 C18 0(3) . . . . ?
O7 C13 C18 C17 178.4(19) . . . . ?
C14 C13 C18 C17 1(3) . . . . ?
C16 C17 C18 C13 -1(3) . . . . ?
W2 O9 C19 C20 -5(2) . . . . ?
W2 O9 C19 C24 173.7(16) . . . . ?
W2 O10 C20 C21 -178.0(15) . . . . ?
W2 O10 C20 C19 -1(2) . . . . ?
O9 C19 C20 O10 4(3) . . . . ?
C24 C19 C20 O10 -174.9(17) . . . . ?
O9 C19 C20 C21 -178.7(18) . . . . ?
C24 C19 C20 C21 2(3) . . . . ?
O10 C20 C21 C22 175.8(18) . . . . ?
C19 C20 C21 C22 -1(3) . . . . ?
C20 C21 C22 C23 -3(3) . . . . ?
C21 C22 C23 C24 5(3) . . . . ?
C22 C23 C24 C19 -4(3) . . . . ?
O9 C19 C24 C23 -179(2) . . . . ?
C20 C19 C24 C23 1(3) . . . . ?
N1 C25 C26 N2 54(3) . . . . ?
N3 C27 C28 N4 -39(4) . . . . ?
N5 C29 C30 N6 63(2) . . . . ?
N7 C31 C32 N8 -62(2) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        66.19
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         2.909
_refine_diff_density_min         -1.749
_refine_diff_density_rms         0.212
####################################################################### 
# 
# 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_140929e
_database_code_depnum_ccdc_archive 'CCDC 1028585'
_audit_update_record             
;
2014-10-10 deposited with the CCDC.
2015-05-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H30 N5 O6 W'
_chemical_formula_weight         584.31

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'
W W -0.8490 6.8722 '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                   7.1077(6)
_cell_length_b                   30.734(3)
_cell_length_c                   9.8061(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.769(2)
_cell_angle_gamma                90.00
_cell_volume                     2089.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2606
_cell_measurement_theta_min      3.2410
_cell_measurement_theta_max      24.5720

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.35
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1156
_exptl_absorpt_coefficient_mu    5.573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1882
_exptl_absorpt_correction_T_max  0.2458
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12915
_diffrn_reflns_av_R_equivalents  0.0944
_diffrn_reflns_av_sigmaI/netI    0.0962
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         25.02
_reflns_number_total             3694
_reflns_number_gt                2844
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0352P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3694
_refine_ls_number_parameters     264
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0577
_refine_ls_wR_factor_ref         0.1171
_refine_ls_wR_factor_gt          0.1067
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_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
W1 W 0.79414(7) 0.647609(12) 0.43553(4) 0.02753(16) Uani 1 1 d . . .
N1 N 0.3265(13) 0.5880(3) 0.6024(7) 0.033(2) Uani 1 1 d . . .
H1A H 0.2423 0.6059 0.5498 0.049 Uiso 1 1 d R . .
H1B H 0.4460 0.5966 0.6020 0.049 Uiso 1 1 d R . .
N2 N 0.2856(14) 0.6344(3) 0.9529(8) 0.042(2) Uani 1 1 d . . .
H2A H 0.1634 0.6300 0.9577 0.062 Uiso 1 1 calc R . .
H2B H 0.3248 0.6602 0.9899 0.062 Uiso 1 1 calc R . .
H2C H 0.3592 0.6135 1.0002 0.062 Uiso 1 1 calc R . .
N3 N 0.3550(14) 0.7049(3) 0.1491(8) 0.039(2) Uani 1 1 d . . .
H3A H 0.3784 0.7292 0.1064 0.059 Uiso 1 1 d R . .
H3B H 0.4579 0.6980 0.2153 0.059 Uiso 1 1 d R . .
N4 N 0.3501(15) 0.7248(3) 0.4657(8) 0.051(3) Uani 1 1 d . . .
H4A H 0.2939 0.7012 0.4910 0.077 Uiso 1 1 d R . .
H4B H 0.4650 0.7177 0.4503 0.077 Uiso 1 1 d R . .
N5 N 0.2551(13) 0.5041(3) 0.4826(8) 0.039(2) Uani 1 1 d . . .
H5A H 0.2877 0.5236 0.5508 0.059 Uiso 1 1 calc R . .
H5B H 0.3042 0.5120 0.4103 0.059 Uiso 1 1 calc R . .
H5C H 0.3014 0.4781 0.5134 0.059 Uiso 1 1 calc R . .
O1 O 0.7553(10) 0.6869(2) 0.5857(6) 0.0312(17) Uani 1 1 d . . .
O2 O 0.7846(11) 0.6054(2) 0.6065(6) 0.0381(19) Uani 1 1 d . . .
O3 O 0.4942(10) 0.6326(2) 0.3894(7) 0.0312(17) Uani 1 1 d . . .
O4 O 0.7739(11) 0.5945(2) 0.3185(7) 0.0363(19) Uani 1 1 d . . .
O5 O 1.0444(11) 0.6437(2) 0.4682(7) 0.042(2) Uani 1 1 d . . .
O6 O 0.7437(12) 0.6896(2) 0.3143(7) 0.041(2) Uani 1 1 d . . .
C1 C 0.7650(16) 0.6710(3) 0.7171(10) 0.033(3) Uani 1 1 d . . .
C2 C 0.7851(15) 0.6249(4) 0.7256(9) 0.031(3) Uani 1 1 d . . .
C3 C 0.7994(17) 0.6058(4) 0.8542(11) 0.048(3) Uani 1 1 d . . .
H3 H 0.8148 0.5758 0.8642 0.058 Uiso 1 1 calc R . .
C4 C 0.7906(17) 0.6319(6) 0.9706(11) 0.065(5) Uani 1 1 d . . .
H4 H 0.7991 0.6189 1.0574 0.078 Uiso 1 1 calc R . .
C5 C 0.770(2) 0.6766(5) 0.9582(12) 0.060(4) Uani 1 1 d . . .
H5 H 0.7606 0.6932 1.0358 0.072 Uiso 1 1 calc R . .
C6 C 0.7620(15) 0.6967(4) 0.8303(11) 0.045(3) Uani 1 1 d . . .
H6 H 0.7551 0.7269 0.8219 0.054 Uiso 1 1 calc R . .
C7 C 0.4460(16) 0.5993(3) 0.3045(9) 0.028(2) Uani 1 1 d . . .
C8 C 0.5983(18) 0.5771(3) 0.2656(9) 0.031(3) Uani 1 1 d . . .
C9 C 0.5643(19) 0.5410(3) 0.1807(10) 0.041(3) Uani 1 1 d . . .
H9 H 0.6666 0.5260 0.1580 0.050 Uiso 1 1 calc R . .
C10 C 0.379(2) 0.5276(4) 0.1300(10) 0.045(3) Uani 1 1 d . . .
H10 H 0.3554 0.5041 0.0686 0.054 Uiso 1 1 calc R . .
C11 C 0.227(2) 0.5477(4) 0.1675(10) 0.046(3) Uani 1 1 d . . .
H11 H 0.1028 0.5371 0.1350 0.055 Uiso 1 1 calc R . .
C12 C 0.2568(18) 0.5840(3) 0.2540(10) 0.037(3) Uani 1 1 d . . .
H12 H 0.1530 0.5980 0.2782 0.044 Uiso 1 1 calc R . .
C13 C 0.2985(16) 0.5892(3) 0.7496(9) 0.031(3) Uani 1 1 d . . .
H13A H 0.1762 0.5756 0.7519 0.037 Uiso 1 1 calc R . .
H13B H 0.3996 0.5722 0.8086 0.037 Uiso 1 1 calc R . .
C14 C 0.3008(16) 0.6334(3) 0.8083(9) 0.030(2) Uani 1 1 d . . .
H14A H 0.4197 0.6477 0.8006 0.036 Uiso 1 1 calc R . .
H14B H 0.1945 0.6499 0.7528 0.036 Uiso 1 1 calc R . .
C15 C 0.1907(18) 0.7119(4) 0.2137(10) 0.047(3) Uani 1 1 d . . .
H15A H 0.1493 0.6840 0.2428 0.056 Uiso 1 1 calc R . .
H15B H 0.0849 0.7238 0.1438 0.056 Uiso 1 1 calc R . .
C16 C 0.2310(18) 0.7421(3) 0.3387(10) 0.044(3) Uani 1 1 d . . .
H16A H 0.2926 0.7681 0.3133 0.053 Uiso 1 1 calc R . .
H16B H 0.1085 0.7509 0.3582 0.053 Uiso 1 1 calc R . .
C17 C 0.0491(16) 0.5018(4) 0.4395(10) 0.036(3) Uani 1 1 d . . .
H17A H 0.0143 0.4768 0.3787 0.044 Uiso 1 1 calc R . .
H17B H 0.0024 0.5277 0.3859 0.044 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
W1 O6 1.738(6) . ?
W1 O5 1.741(8) . ?
W1 O1 1.971(6) . ?
W1 O4 1.983(7) . ?
W1 O3 2.130(7) . ?
W1 O2 2.133(6) . ?
N1 C13 1.500(11) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N2 C14 1.447(11) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N3 C15 1.462(14) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N4 C16 1.444(12) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N5 C17 1.433(13) . ?
N5 H5A 0.8900 . ?
N5 H5B 0.8900 . ?
N5 H5C 0.8900 . ?
O1 C1 1.366(11) . ?
O2 C2 1.312(11) . ?
O3 C7 1.317(11) . ?
O4 C8 1.351(13) . ?
C1 C6 1.368(14) . ?
C1 C2 1.422(15) . ?
C2 C3 1.375(13) . ?
C3 C4 1.408(17) . ?
C3 H3 0.9300 . ?
C4 C5 1.38(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.389(16) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.401(15) . ?
C7 C12 1.407(15) . ?
C8 C9 1.376(13) . ?
C9 C10 1.367(16) . ?
C9 H9 0.9300 . ?
C10 C11 1.362(17) . ?
C10 H10 0.9300 . ?
C11 C12 1.388(14) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.473(12) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.514(13) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C17 1.508(19) 3_566 ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 W1 O5 103.1(4) . . ?
O6 W1 O1 90.8(3) . . ?
O5 W1 O1 102.2(3) . . ?
O6 W1 O4 103.8(3) . . ?
O5 W1 O4 89.4(3) . . ?
O1 W1 O4 158.9(3) . . ?
O6 W1 O3 88.3(3) . . ?
O5 W1 O3 163.4(3) . . ?
O1 W1 O3 89.6(3) . . ?
O4 W1 O3 76.0(3) . . ?
O6 W1 O2 162.2(3) . . ?
O5 W1 O2 91.2(3) . . ?
O1 W1 O2 75.6(3) . . ?
O4 W1 O2 86.7(3) . . ?
O3 W1 O2 80.3(3) . . ?
C13 N1 H1A 109.1 . . ?
C13 N1 H1B 109.0 . . ?
H1A N1 H1B 109.5 . . ?
C14 N2 H2A 109.5 . . ?
C14 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C14 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C15 N3 H3A 109.2 . . ?
C15 N3 H3B 109.0 . . ?
H3A N3 H3B 109.5 . . ?
C16 N4 H4A 109.1 . . ?
C16 N4 H4B 109.2 . . ?
H4A N4 H4B 109.5 . . ?
C17 N5 H5A 109.5 . . ?
C17 N5 H5B 109.5 . . ?
H5A N5 H5B 109.5 . . ?
C17 N5 H5C 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
C1 O1 W1 119.9(6) . . ?
C2 O2 W1 115.2(6) . . ?
C7 O3 W1 114.2(6) . . ?
C8 O4 W1 119.4(7) . . ?
O1 C1 C6 123.4(10) . . ?
O1 C1 C2 113.3(8) . . ?
C6 C1 C2 123.3(10) . . ?
O2 C2 C3 127.2(11) . . ?
O2 C2 C1 115.1(8) . . ?
C3 C2 C1 117.7(10) . . ?
C2 C3 C4 119.5(12) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 121.2(11) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C4 C5 C6 120.3(11) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C1 C6 C5 118.0(12) . . ?
C1 C6 H6 121.0 . . ?
C5 C6 H6 121.0 . . ?
O3 C7 C8 116.2(10) . . ?
O3 C7 C12 125.2(10) . . ?
C8 C7 C12 118.6(10) . . ?
O4 C8 C9 125.1(11) . . ?
O4 C8 C7 114.0(9) . . ?
C9 C8 C7 120.9(11) . . ?
C10 C9 C8 119.4(11) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C11 C10 C9 121.4(11) . . ?
C11 C10 H10 119.3 . . ?
C9 C10 H10 119.3 . . ?
C10 C11 C12 120.5(12) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C11 C12 C7 119.2(11) . . ?
C11 C12 H12 120.4 . . ?
C7 C12 H12 120.4 . . ?
C14 C13 N1 114.0(8) . . ?
C14 C13 H13A 108.8 . . ?
N1 C13 H13A 108.8 . . ?
C14 C13 H13B 108.8 . . ?
N1 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
N2 C14 C13 113.9(8) . . ?
N2 C14 H14A 108.8 . . ?
C13 C14 H14A 108.8 . . ?
N2 C14 H14B 108.8 . . ?
C13 C14 H14B 108.8 . . ?
H14A C14 H14B 107.7 . . ?
N3 C15 C16 114.6(10) . . ?
N3 C15 H15A 108.6 . . ?
C16 C15 H15A 108.6 . . ?
N3 C15 H15B 108.6 . . ?
C16 C15 H15B 108.6 . . ?
H15A C15 H15B 107.6 . . ?
N4 C16 C15 116.2(9) . . ?
N4 C16 H16A 108.2 . . ?
C15 C16 H16A 108.2 . . ?
N4 C16 H16B 108.2 . . ?
C15 C16 H16B 108.2 . . ?
H16A C16 H16B 107.4 . . ?
N5 C17 C17 113.1(10) . 3_566 ?
N5 C17 H17A 109.0 . . ?
C17 C17 H17A 109.0 3_566 . ?
N5 C17 H17B 109.0 . . ?
C17 C17 H17B 109.0 3_566 . ?
H17A C17 H17B 107.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O6 W1 O1 C1 176.0(8) . . . . ?
O5 W1 O1 C1 -80.4(7) . . . . ?
O4 W1 O1 C1 41.6(12) . . . . ?
O3 W1 O1 C1 87.8(7) . . . . ?
O2 W1 O1 C1 7.7(7) . . . . ?
O6 W1 O2 C2 -49.9(14) . . . . ?
O5 W1 O2 C2 93.7(7) . . . . ?
O1 W1 O2 C2 -8.6(7) . . . . ?
O4 W1 O2 C2 -177.0(7) . . . . ?
O3 W1 O2 C2 -100.7(7) . . . . ?
O6 W1 O3 C7 101.0(6) . . . . ?
O5 W1 O3 C7 -32.7(13) . . . . ?
O1 W1 O3 C7 -168.2(6) . . . . ?
O4 W1 O3 C7 -3.7(6) . . . . ?
O2 W1 O3 C7 -92.8(6) . . . . ?
O6 W1 O4 C8 -81.9(7) . . . . ?
O5 W1 O4 C8 174.8(6) . . . . ?
O1 W1 O4 C8 50.7(11) . . . . ?
O3 W1 O4 C8 2.8(6) . . . . ?
O2 W1 O4 C8 83.6(7) . . . . ?
W1 O1 C1 C6 172.2(8) . . . . ?
W1 O1 C1 C2 -5.8(12) . . . . ?
W1 O2 C2 C3 -172.9(9) . . . . ?
W1 O2 C2 C1 8.3(11) . . . . ?
O1 C1 C2 O2 -2.1(13) . . . . ?
C6 C1 C2 O2 179.9(10) . . . . ?
O1 C1 C2 C3 178.9(9) . . . . ?
C6 C1 C2 C3 0.9(16) . . . . ?
O2 C2 C3 C4 -177.8(11) . . . . ?
C1 C2 C3 C4 1.0(16) . . . . ?
C2 C3 C4 C5 -0.6(18) . . . . ?
C3 C4 C5 C6 -2(2) . . . . ?
O1 C1 C6 C5 179.0(11) . . . . ?
C2 C1 C6 C5 -3.2(17) . . . . ?
C4 C5 C6 C1 3.6(18) . . . . ?
W1 O3 C7 C8 4.2(10) . . . . ?
W1 O3 C7 C12 -177.4(7) . . . . ?
W1 O4 C8 C9 178.5(7) . . . . ?
W1 O4 C8 C7 -1.5(10) . . . . ?
O3 C7 C8 O4 -2.0(12) . . . . ?
C12 C7 C8 O4 179.5(8) . . . . ?
O3 C7 C8 C9 178.0(8) . . . . ?
C12 C7 C8 C9 -0.5(14) . . . . ?
O4 C8 C9 C10 -177.8(9) . . . . ?
C7 C8 C9 C10 2.2(15) . . . . ?
C8 C9 C10 C11 -3.5(16) . . . . ?
C9 C10 C11 C12 2.9(17) . . . . ?
C10 C11 C12 C7 -1.1(15) . . . . ?
O3 C7 C12 C11 -178.5(9) . . . . ?
C8 C7 C12 C11 -0.1(14) . . . . ?
N1 C13 C14 N2 -176.4(9) . . . . ?
N3 C15 C16 N4 -73.1(13) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.960
_refine_diff_density_min         -2.949
_refine_diff_density_rms         0.193
