# Electronic Supplementary Material (ESI) for RSC Advances.
# 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 
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data_SN2Mo6
_database_code_depnum_ccdc_archive 'CCDC 1414602'
_audit_update_record             
;
2015-07-22 deposited with the CCDC.
2015-09-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H44 Mo6 N6 O21'
_chemical_formula_weight         1568.49

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   14.3898(6)
_cell_length_b                   12.7305(5)
_cell_length_c                   14.4617(7)
_cell_angle_alpha                90
_cell_angle_beta                 111.279(2)
_cell_angle_gamma                90
_cell_volume                     2468.62(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.201
_cell_measurement_theta_max      30.034

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.110
_exptl_crystal_F_000             1540
_exptl_transmission_factor_min   0.6863
_exptl_transmission_factor_max   0.8467
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.566
_shelx_estimated_absorpt_T_min   0.651
_shelx_estimated_absorpt_T_max   0.745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS (Sheldrick, V2.10)'
_exptl_absorpt_special_details   'Blessing, Acta Cryst. (1995) A51, 33-38'
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            75596
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.201
_diffrn_reflns_theta_max         30.034
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7214
_reflns_number_gt                5961
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0288P)²+2.4689P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7214
_refine_ls_number_parameters     353
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0264
_refine_ls_wR_factor_ref         0.0665
_refine_ls_wR_factor_gt          0.0600
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_restrained_S_all      0.959
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.98977(2) 0.17836(2) 0.02792(2) 0.03573(6) Uani 1 1 d . . . . .
Mo2 Mo 0.97504(2) 0.03391(2) -0.16539(2) 0.03811(6) Uani 1 1 d . . . . .
Mo3 Mo 1.17010(2) 0.01630(2) 0.04028(2) 0.04013(6) Uani 1 1 d . . . . .
O1 O 1.0000 0.0000 0.0000 0.0303(4) Uani 1 2 d S . P . .
O2 O 0.97684(12) 0.17598(12) -0.10475(12) 0.0388(4) Uani 1 1 d . . . . .
O3 O 1.13154(12) 0.15450(12) 0.06668(12) 0.0393(4) Uani 1 1 d . . . . .
O4 O 0.84392(12) 0.02337(13) -0.16745(12) 0.0433(4) Uani 1 1 d . . . . .
O5 O 1.12052(13) 0.04671(13) -0.09543(13) 0.0423(4) Uani 1 1 d . . . . .
O6 O 0.98329(14) 0.30632(13) 0.05400(14) 0.0469(4) Uani 1 1 d . . . . .
O7 O 0.85423(12) 0.13133(13) -0.00865(13) 0.0420(4) Uani 1 1 d . . . . .
O8 O 0.99118(13) -0.11092(13) -0.15842(12) 0.0418(4) Uani 1 1 d . . . . .
O9 O 1.29476(13) 0.02558(16) 0.07576(17) 0.0596(5) Uani 1 1 d . . . . .
O10 O 0.96033(17) 0.06640(16) -0.28246(14) 0.0588(5) Uani 1 1 d . . . . .
O11 O 0.32212(15) 0.43257(15) -0.09304(15) 0.0535(5) Uani 1 1 d . . . . .
N1 N 0.32941(18) 0.24886(18) -0.06058(16) 0.0495(5) Uani 1 1 d . . . . .
N2 N 0.15587(17) 0.40332(18) -0.03473(18) 0.0502(5) Uani 1 1 d . . . . .
N3 N 0.26756(17) 0.70154(16) 0.18325(16) 0.0471(5) Uani 1 1 d . . . . .
C1 C 0.2522(2) 0.3054(2) -0.22865(19) 0.0475(6) Uani 1 1 d . . . . .
C2 C 0.33236(19) 0.2249(2) -0.2161(2) 0.0444(6) Uani 1 1 d . . . . .
C3 C 0.3620(2) 0.1782(2) -0.2870(2) 0.0550(7) Uani 1 1 d . . . . .
H3 H 0.3338 0.1984 -0.3532 0.066 Uiso 1 1 calc R U . . .
C4 C 0.4349(2) 0.1005(3) -0.2575(3) 0.0678(9) Uani 1 1 d . . . . .
H4 H 0.4549 0.0672 -0.3043 0.081 Uiso 1 1 calc R U . . .
C5 C 0.4772(2) 0.0729(3) -0.1593(3) 0.0706(10) Uani 1 1 d . . . . .
H5 H 0.5262 0.0213 -0.1406 0.085 Uiso 1 1 calc R U . . .
C6 C 0.4490(2) 0.1198(2) -0.0872(3) 0.0593(8) Uani 1 1 d . . . . .
H6 H 0.4787 0.1012 -0.0207 0.071 Uiso 1 1 calc R U . . .
C7 C 0.37495(19) 0.1954(2) -0.1174(2) 0.0457(6) Uani 1 1 d . . . . .
C8 C 0.2678(2) 0.3326(2) -0.1174(2) 0.0455(6) Uani 1 1 d . . . . .
C9 C 0.1749(2) 0.3381(2) -0.0923(2) 0.0525(7) Uani 1 1 d . . . . .
H9 H 0.1260 0.2882 -0.1222 0.063 Uiso 1 1 calc R U . . .
C10 C 0.22702(19) 0.48291(19) 0.00461(19) 0.0420(5) Uani 1 1 d . . . . .
C11 C 0.3062(2) 0.49650(19) -0.02500(19) 0.0439(5) Uani 1 1 d . . . . .
C12 C 0.3740(2) 0.5795(2) 0.0130(2) 0.0526(7) Uani 1 1 d . . . . .
H12 H 0.4277 0.5874 -0.0077 0.063 Uiso 1 1 calc R U . . .
C13 C 0.3618(2) 0.6488(2) 0.0803(2) 0.0500(6) Uani 1 1 d . . . . .
H13 H 0.4059 0.7045 0.1039 0.060 Uiso 1 1 calc R U . . .
C14 C 0.28210(19) 0.63491(19) 0.11313(19) 0.0434(6) Uani 1 1 d . . . . .
C15 C 0.21398(18) 0.55176(18) 0.07675(17) 0.0387(5) Uani 1 1 d . . . . .
C16 C 0.13542(19) 0.5380(2) 0.11137(19) 0.0435(6) Uani 1 1 d . . . . .
H16 H 0.0898 0.4837 0.0868 0.052 Uiso 1 1 calc R U . . .
C17 C 0.1267(2) 0.6056(2) 0.1820(2) 0.0508(6) Uani 1 1 d . . . . .
H17 H 0.0760 0.5966 0.2068 0.061 Uiso 1 1 calc R U . . .
C18 C 0.1938(2) 0.6864(2) 0.2153(2) 0.0534(7) Uani 1 1 d . . . . .
H18 H 0.1869 0.7324 0.2624 0.064 Uiso 1 1 calc R U . . .
C19 C 0.3355(2) 0.7919(2) 0.2194(2) 0.0650(9) Uani 1 1 d . . . . .
H19A H 0.4023 0.7669 0.2525 0.098 Uiso 1 1 calc R U . . .
H19B H 0.3153 0.8322 0.2651 0.098 Uiso 1 1 calc R U . . .
H19C H 0.3329 0.8353 0.1643 0.098 Uiso 1 1 calc R U . . .
C20 C 0.3737(3) 0.2556(3) 0.0461(2) 0.0652(9) Uani 1 1 d . . . . .
H20A H 0.4286 0.3040 0.0644 0.098 Uiso 1 1 calc R U . . .
H20B H 0.3973 0.1876 0.0730 0.098 Uiso 1 1 calc R U . . .
H20C H 0.3248 0.2798 0.0720 0.098 Uiso 1 1 calc R U . . .
C21 C 0.2614(3) 0.4008(3) -0.2881(3) 0.0790(11) Uani 1 1 d . . . . .
H21A H 0.3270 0.4302 -0.2586 0.118 Uiso 1 1 calc R U . . .
H21B H 0.2127 0.4524 -0.2881 0.118 Uiso 1 1 calc R U . . .
H21C H 0.2502 0.3801 -0.3551 0.118 Uiso 1 1 calc R U . . .
C22 C 0.1501(2) 0.2520(4) -0.2800(2) 0.0803(12) Uani 1 1 d . . . . .
H22A H 0.1431 0.2320 -0.3462 0.120 Uiso 1 1 calc R U . . .
H22B H 0.0978 0.3002 -0.2826 0.120 Uiso 1 1 calc R U . . .
H22C H 0.1457 0.1907 -0.2432 0.120 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O6 1.6823(16) . ?
Mo1 O2 1.8595(17) . ?
Mo1 O7 1.9219(17) . ?
Mo1 O3 1.9334(16) . ?
Mo1 O8 1.9997(16) 3_755 ?
Mo1 O1 2.3202(2) . ?
Mo2 O10 1.6800(18) . ?
Mo2 O8 1.8565(17) . ?
Mo2 O4 1.8811(18) . ?
Mo2 O5 1.9736(17) . ?
Mo2 O2 2.0061(16) . ?
Mo2 O1 2.3265(2) . ?
Mo3 O9 1.6813(18) . ?
Mo3 O5 1.8693(18) . ?
Mo3 O3 1.9242(17) . ?
Mo3 O7 1.9360(17) 3_755 ?
Mo3 O4 1.9867(18) 3_755 ?
Mo3 O1 2.3106(2) . ?
O1 Mo3 2.3106(2) 3_755 ?
O1 Mo1 2.3202(2) 3_755 ?
O1 Mo2 2.3264(2) 3_755 ?
O4 Mo3 1.9868(18) 3_755 ?
O7 Mo3 1.9359(17) 3_755 ?
O8 Mo1 1.9997(16) 3_755 ?
O11 C11 1.359(3) . ?
O11 C8 1.468(3) . ?
N1 C7 1.400(4) . ?
N1 C8 1.438(3) . ?
N1 C20 1.443(3) . ?
N2 C9 1.274(3) . ?
N2 C10 1.406(3) . ?
N3 C18 1.318(4) . ?
N3 C14 1.395(3) . ?
N3 C19 1.477(4) . ?
C1 C2 1.504(4) . ?
C1 C21 1.522(4) . ?
C1 C22 1.543(4) . ?
C1 C8 1.579(4) . ?
C2 C3 1.380(4) . ?
C2 C7 1.385(4) . ?
C3 C4 1.392(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.372(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.384(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.383(4) . ?
C6 H6 0.9300 . ?
C8 C9 1.510(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.367(4) . ?
C10 C15 1.426(4) . ?
C11 C12 1.407(4) . ?
C12 C13 1.372(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.402(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.408(3) . ?
C15 C16 1.404(4) . ?
C16 C17 1.376(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.373(4) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?

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 Mo1 O2 104.73(8) . . ?
O6 Mo1 O7 103.30(8) . . ?
O2 Mo1 O7 89.97(7) . . ?
O6 Mo1 O3 103.04(8) . . ?
O2 Mo1 O3 89.80(7) . . ?
O7 Mo1 O3 152.81(7) . . ?
O6 Mo1 O8 101.76(8) . 3_755 ?
O2 Mo1 O8 153.50(7) . 3_755 ?
O7 Mo1 O8 84.48(7) . 3_755 ?
O3 Mo1 O8 83.69(7) . 3_755 ?
O6 Mo1 O1 177.19(6) . . ?
O2 Mo1 O1 78.08(5) . . ?
O7 Mo1 O1 76.67(5) . . ?
O3 Mo1 O1 76.69(5) . . ?
O8 Mo1 O1 75.43(5) 3_755 . ?
O10 Mo2 O8 105.47(9) . . ?
O10 Mo2 O4 104.05(9) . . ?
O8 Mo2 O4 92.00(8) . . ?
O10 Mo2 O5 102.63(9) . . ?
O8 Mo2 O5 88.04(7) . . ?
O4 Mo2 O5 152.29(7) . . ?
O10 Mo2 O2 101.27(8) . . ?
O8 Mo2 O2 152.90(7) . . ?
O4 Mo2 O2 85.70(7) . . ?
O5 Mo2 O2 81.86(7) . . ?
O10 Mo2 O1 176.17(7) . . ?
O8 Mo2 O1 77.90(5) . . ?
O4 Mo2 O1 77.45(5) . . ?
O5 Mo2 O1 75.47(5) . . ?
O2 Mo2 O1 75.24(5) . . ?
O9 Mo3 O5 105.33(10) . . ?
O9 Mo3 O3 103.17(9) . . ?
O5 Mo3 O3 89.50(7) . . ?
O9 Mo3 O7 102.81(9) . 3_755 ?
O5 Mo3 O7 89.18(7) . 3_755 ?
O3 Mo3 O7 153.38(7) . 3_755 ?
O9 Mo3 O4 101.00(9) . 3_755 ?
O5 Mo3 O4 153.66(7) . 3_755 ?
O3 Mo3 O4 85.14(7) . 3_755 ?
O7 Mo3 O4 84.35(7) 3_755 3_755 ?
O9 Mo3 O1 176.87(8) . . ?
O5 Mo3 O1 77.77(5) . . ?
O3 Mo3 O1 77.10(5) . . ?
O7 Mo3 O1 76.65(5) 3_755 . ?
O4 Mo3 O1 75.90(5) 3_755 . ?
Mo3 O1 Mo3 180.0 . 3_755 ?
Mo3 O1 Mo1 90.198(7) . 3_755 ?
Mo3 O1 Mo1 89.802(7) 3_755 3_755 ?
Mo3 O1 Mo1 89.802(7) . . ?
Mo3 O1 Mo1 90.198(7) 3_755 . ?
Mo1 O1 Mo1 180.0 3_755 . ?
Mo3 O1 Mo2 90.191(8) . 3_755 ?
Mo3 O1 Mo2 89.808(8) 3_755 3_755 ?
Mo1 O1 Mo2 90.080(7) 3_755 3_755 ?
Mo1 O1 Mo2 89.919(7) . 3_755 ?
Mo3 O1 Mo2 89.809(8) . . ?
Mo3 O1 Mo2 90.192(8) 3_755 . ?
Mo1 O1 Mo2 89.919(7) 3_755 . ?
Mo1 O1 Mo2 90.082(7) . . ?
Mo2 O1 Mo2 180.0 3_755 . ?
Mo1 O2 Mo2 116.50(8) . . ?
Mo3 O3 Mo1 115.85(8) . . ?
Mo2 O4 Mo3 116.21(8) . 3_755 ?
Mo3 O5 Mo2 116.79(9) . . ?
Mo1 O7 Mo3 116.48(8) . 3_755 ?
Mo2 O8 Mo1 116.69(8) . 3_755 ?
C11 O11 C8 118.6(2) . . ?
C7 N1 C8 110.3(2) . . ?
C7 N1 C20 122.5(3) . . ?
C8 N1 C20 120.6(2) . . ?
C9 N2 C10 115.9(2) . . ?
C18 N3 C14 121.3(2) . . ?
C18 N3 C19 120.2(3) . . ?
C14 N3 C19 118.5(3) . . ?
C2 C1 C21 113.1(2) . . ?
C2 C1 C22 108.2(3) . . ?
C21 C1 C22 110.0(3) . . ?
C2 C1 C8 101.9(2) . . ?
C21 C1 C8 113.0(3) . . ?
C22 C1 C8 110.2(2) . . ?
C3 C2 C7 120.6(3) . . ?
C3 C2 C1 129.3(3) . . ?
C7 C2 C1 110.1(2) . . ?
C2 C3 C4 118.6(3) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 H3 120.7 . . ?
C5 C4 C3 120.1(3) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 121.9(3) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C7 C6 C5 117.7(3) . . ?
C7 C6 H6 121.2 . . ?
C5 C6 H6 121.2 . . ?
C6 C7 C2 121.1(3) . . ?
C6 C7 N1 128.6(3) . . ?
C2 C7 N1 110.3(2) . . ?
N1 C8 O11 110.0(2) . . ?
N1 C8 C9 108.2(2) . . ?
O11 C8 C9 110.0(2) . . ?
N1 C8 C1 104.5(2) . . ?
O11 C8 C1 107.5(2) . . ?
C9 C8 C1 116.4(2) . . ?
N2 C9 C8 127.4(2) . . ?
N2 C9 H9 116.3 . . ?
C8 C9 H9 116.3 . . ?
C11 C10 N2 122.2(2) . . ?
C11 C10 C15 119.8(2) . . ?
N2 C10 C15 118.0(2) . . ?
O11 C11 C10 122.0(2) . . ?
O11 C11 C12 117.2(2) . . ?
C10 C11 C12 120.8(3) . . ?
C13 C12 C11 120.7(3) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C12 C13 C14 119.4(2) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
N3 C14 C13 121.7(2) . . ?
N3 C14 C15 117.4(2) . . ?
C13 C14 C15 120.8(2) . . ?
C16 C15 C14 120.1(2) . . ?
C16 C15 C10 121.4(2) . . ?
C14 C15 C10 118.5(2) . . ?
C17 C16 C15 119.3(3) . . ?
C17 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?
C18 C17 C16 119.2(3) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
N3 C18 C17 122.6(3) . . ?
N3 C18 H18 118.7 . . ?
C17 C18 H18 118.7 . . ?
N3 C19 H19A 109.5 . . ?
N3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N1 C20 H20A 109.5 . . ?
N1 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N1 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C1 C21 H21A 109.5 . . ?
C1 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C1 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C1 C22 H22A 109.5 . . ?
C1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C1 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

_refine_diff_density_max         0.696
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.075


####################################################################### 
# 
# 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_SN2W6
_database_code_depnum_ccdc_archive 'CCDC 1414603'
_audit_update_record             
;
2015-07-22 deposited with the CCDC.
2015-09-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H44 N6 O21 W6'
_chemical_formula_weight         2095.95

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'
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'
N N 0.0061 0.0033 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   14.410(3)
_cell_length_b                   12.743(3)
_cell_length_c                   14.549(3)
_cell_angle_alpha                90
_cell_angle_beta                 111.339(10)
_cell_angle_gamma                90
_cell_volume                     2488.5(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.703
_cell_measurement_theta_max      30.033

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.797
_exptl_crystal_F_000             1924
_exptl_transmission_factor_min   0.3256
_exptl_transmission_factor_max   0.5679
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    13.899
_shelx_estimated_absorpt_T_min   0.103
_shelx_estimated_absorpt_T_max   0.168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS (Sheldrick, V2.10)'
_exptl_absorpt_special_details   'Blessing, Acta Cryst. (1995) A51, 33-38'
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            124070
_diffrn_reflns_av_unetI/netI     0.0118
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.703
_diffrn_reflns_theta_max         30.033
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7253
_reflns_number_gt                6555
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0316P)²+6.9295P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7253
_refine_ls_number_parameters     353
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0208
_refine_ls_wR_factor_ref         0.0600
_refine_ls_wR_factor_gt          0.0563
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.98980(2) 0.17812(2) 0.03114(2) 0.02985(4) Uani 1 1 d . . . . .
W2 W 0.97669(2) 0.03788(2) -0.16368(2) 0.03245(4) Uani 1 1 d . . . . .
W3 W 1.17095(2) 0.01614(2) 0.04219(2) 0.03373(5) Uani 1 1 d . . . . .
O1 O 1.0000 0.0000 0.0000 0.0261(7) Uani 1 2 d S . P . .
O2 O 0.9739(2) 0.1746(2) -0.1050(2) 0.0343(6) Uani 1 1 d . . . . .
O3 O 1.1302(2) 0.1556(2) 0.0621(2) 0.0356(6) Uani 1 1 d . . . . .
O4 O 0.8441(2) 0.0204(2) -0.1659(2) 0.0382(6) Uani 1 1 d . . . . .
O5 O 1.1191(2) 0.0456(2) -0.0960(2) 0.0368(6) Uani 1 1 d . . . . .
O6 O 0.9824(3) 0.3079(2) 0.0551(2) 0.0432(7) Uani 1 1 d . . . . .
O7 O 0.8540(2) 0.1304(2) -0.0089(2) 0.0375(6) Uani 1 1 d . . . . .
O8 O 0.9902(2) -0.1112(2) -0.1569(2) 0.0363(6) Uani 1 1 d . . . . .
O9 O 1.2966(2) 0.0269(3) 0.0761(3) 0.0550(9) Uani 1 1 d . . . . .
O10 O 0.9597(3) 0.0687(3) -0.2825(2) 0.0568(9) Uani 1 1 d . . . . .
O11 O 0.3206(3) 0.4339(3) -0.0943(3) 0.0488(8) Uani 1 1 d . . . . .
N1 N 0.3278(3) 0.2504(3) -0.0617(3) 0.0442(8) Uani 1 1 d . . . . .
N2 N 0.1541(3) 0.4047(3) -0.0363(3) 0.0453(9) Uani 1 1 d . . . . .
N3 N 0.2673(3) 0.7005(3) 0.1830(3) 0.0436(9) Uani 1 1 d . . . . .
C1 C 0.2513(3) 0.3071(4) -0.2287(3) 0.0427(9) Uani 1 1 d . . . . .
C2 C 0.3319(3) 0.2262(4) -0.2157(3) 0.0396(9) Uani 1 1 d . . . . .
C3 C 0.3623(4) 0.1798(4) -0.2858(4) 0.0513(11) Uani 1 1 d . . . . .
H3 H 0.3349 0.2002 -0.3516 0.062 Uiso 1 1 calc R U . . .
C4 C 0.4346(4) 0.1018(5) -0.2560(5) 0.0612(15) Uani 1 1 d . . . . .
H4 H 0.4542 0.0680 -0.3026 0.073 Uiso 1 1 calc R U . . .
C5 C 0.4773(4) 0.0743(5) -0.1580(6) 0.0672(17) Uani 1 1 d . . . . .
H5 H 0.5266 0.0231 -0.1393 0.081 Uiso 1 1 calc R U . . .
C6 C 0.4484(4) 0.1215(4) -0.0858(4) 0.0545(12) Uani 1 1 d . . . . .
H6 H 0.4781 0.1033 -0.0195 0.065 Uiso 1 1 calc R U . . .
C7 C 0.3736(3) 0.1968(4) -0.1172(3) 0.0406(9) Uani 1 1 d . . . . .
C8 C 0.2667(4) 0.3339(4) -0.1181(3) 0.0413(9) Uani 1 1 d . . . . .
C9 C 0.1733(4) 0.3393(4) -0.0943(4) 0.0477(11) Uani 1 1 d . . . . .
H9 H 0.1242 0.2899 -0.1249 0.057 Uiso 1 1 calc R U . . .
C10 C 0.2253(3) 0.4836(3) 0.0034(3) 0.0381(9) Uani 1 1 d . . . . .
C11 C 0.3054(4) 0.4972(3) -0.0256(3) 0.0401(9) Uani 1 1 d . . . . .
C12 C 0.3730(4) 0.5805(4) 0.0118(4) 0.0481(11) Uani 1 1 d . . . . .
H12 H 0.4257 0.5896 -0.0099 0.058 Uiso 1 1 calc R U . . .
C13 C 0.3613(4) 0.6486(4) 0.0804(4) 0.0467(11) Uani 1 1 d . . . . .
H13 H 0.4059 0.7035 0.1052 0.056 Uiso 1 1 calc R U . . .
C14 C 0.2817(3) 0.6343(3) 0.1125(3) 0.0396(9) Uani 1 1 d . . . . .
C15 C 0.2133(3) 0.5513(3) 0.0757(3) 0.0363(8) Uani 1 1 d . . . . .
C16 C 0.1354(3) 0.5366(4) 0.1112(3) 0.0408(9) Uani 1 1 d . . . . .
H16 H 0.0898 0.4824 0.0872 0.049 Uiso 1 1 calc R U . . .
C17 C 0.1282(4) 0.6039(4) 0.1819(4) 0.0473(10) Uani 1 1 d . . . . .
H17 H 0.0781 0.5944 0.2072 0.057 Uiso 1 1 calc R U . . .
C18 C 0.1943(4) 0.6849(4) 0.2153(4) 0.0475(11) Uani 1 1 d . . . . .
H18 H 0.1873 0.7304 0.2624 0.057 Uiso 1 1 calc R U . . .
C19 C 0.3339(4) 0.7915(4) 0.2190(4) 0.0596(15) Uani 1 1 d . . . . .
H19A H 0.4013 0.7676 0.2499 0.089 Uiso 1 1 calc R U . . .
H19B H 0.3147 0.8298 0.2660 0.089 Uiso 1 1 calc R U . . .
H19C H 0.3291 0.8364 0.1644 0.089 Uiso 1 1 calc R U . . .
C20 C 0.3717(5) 0.2578(5) 0.0446(4) 0.0599(14) Uani 1 1 d . . . . .
H20A H 0.4243 0.3089 0.0627 0.090 Uiso 1 1 calc R U . . .
H20B H 0.3983 0.1908 0.0716 0.090 Uiso 1 1 calc R U . . .
H20C H 0.3217 0.2788 0.0701 0.090 Uiso 1 1 calc R U . . .
C21 C 0.2610(6) 0.4020(5) -0.2880(5) 0.0733(19) Uani 1 1 d . . . . .
H21A H 0.3272 0.4300 -0.2596 0.110 Uiso 1 1 calc R U . . .
H21B H 0.2137 0.4546 -0.2869 0.110 Uiso 1 1 calc R U . . .
H21C H 0.2482 0.3812 -0.3549 0.110 Uiso 1 1 calc R U . . .
C22 C 0.1498(4) 0.2531(7) -0.2810(4) 0.074(2) Uani 1 1 d . . . . .
H22A H 0.1432 0.2347 -0.3471 0.110 Uiso 1 1 calc R U . . .
H22B H 0.0971 0.3002 -0.2829 0.110 Uiso 1 1 calc R U . . .
H22C H 0.1460 0.1908 -0.2455 0.110 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O6 1.701(3) . ?
W1 O2 1.910(3) . ?
W1 O7 1.926(3) . ?
W1 O3 1.927(3) . ?
W1 O8 1.943(3) 3_755 ?
W1 O1 2.3296(5) . ?
W2 O10 1.701(3) . ?
W2 O8 1.909(3) . ?
W2 O4 1.912(3) . ?
W2 O5 1.928(3) . ?
W2 O2 1.947(3) . ?
W2 O1 2.3313(5) . ?
W3 O9 1.700(3) . ?
W3 O5 1.910(3) . ?
W3 O7 1.930(3) 3_755 ?
W3 O3 1.927(3) . ?
W3 O4 1.947(3) 3_755 ?
W3 O1 2.3211(6) . ?
O1 W3 2.3211(6) 3_755 ?
O1 W1 2.3296(5) 3_755 ?
O1 W2 2.3313(5) 3_755 ?
O4 W3 1.947(3) 3_755 ?
O7 W3 1.930(3) 3_755 ?
O8 W1 1.943(3) 3_755 ?
O11 C11 1.362(6) . ?
O11 C8 1.467(5) . ?
N1 C7 1.393(6) . ?
N1 C20 1.445(6) . ?
N1 C8 1.434(6) . ?
N2 C9 1.285(6) . ?
N2 C10 1.401(6) . ?
N3 C18 1.315(7) . ?
N3 C14 1.400(6) . ?
N3 C19 1.475(6) . ?
C1 C2 1.512(6) . ?
C1 C21 1.521(7) . ?
C1 C22 1.544(8) . ?
C1 C8 1.578(6) . ?
C2 C3 1.381(7) . ?
C2 C7 1.389(6) . ?
C3 C4 1.390(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.377(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.399(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.391(7) . ?
C6 H6 0.9300 . ?
C8 C9 1.509(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.377(6) . ?
C10 C15 1.419(6) . ?
C11 C12 1.410(6) . ?
C12 C13 1.379(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.399(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.411(6) . ?
C15 C16 1.409(6) . ?
C16 C17 1.372(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.369(7) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?

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 O2 104.04(14) . . ?
O6 W1 O7 103.66(14) . . ?
O2 W1 O7 87.35(13) . . ?
O6 W1 O3 103.62(14) . . ?
O2 W1 O3 87.61(13) . . ?
O7 W1 O3 152.67(12) . . ?
O6 W1 O8 103.46(14) . 3_755 ?
O2 W1 O8 152.50(11) . 3_755 ?
O7 W1 O8 86.14(13) . 3_755 ?
O3 W1 O8 86.04(13) . 3_755 ?
O6 W1 O1 179.41(11) . . ?
O2 W1 O1 76.55(8) . . ?
O7 W1 O1 76.26(9) . . ?
O3 W1 O1 76.44(8) . . ?
O8 W1 O1 75.95(8) 3_755 . ?
O10 W2 O8 104.86(15) . . ?
O10 W2 O4 103.65(17) . . ?
O8 W2 O4 88.13(13) . . ?
O10 W2 O5 103.90(17) . . ?
O8 W2 O5 87.40(13) . . ?
O4 W2 O5 152.31(13) . . ?
O10 W2 O2 102.76(15) . . ?
O8 W2 O2 152.37(12) . . ?
O4 W2 O2 86.09(13) . . ?
O5 W2 O2 85.32(12) . . ?
O10 W2 O1 178.61(13) . . ?
O8 W2 O1 76.52(8) . . ?
O4 W2 O1 76.40(9) . . ?
O5 W2 O1 75.98(9) . . ?
O2 W2 O1 75.86(8) . . ?
O9 W3 O5 104.91(17) . . ?
O9 W3 O7 103.43(15) . 3_755 ?
O5 W3 O7 87.70(13) . 3_755 ?
O9 W3 O3 103.45(15) . . ?
O5 W3 O3 87.33(12) . . ?
O7 W3 O3 153.04(12) 3_755 . ?
O9 W3 O4 102.50(17) . 3_755 ?
O5 W3 O4 152.60(12) . 3_755 ?
O7 W3 O4 85.82(13) 3_755 3_755 ?
O3 W3 O4 86.51(13) . 3_755 ?
O9 W3 O1 178.52(14) . . ?
O5 W3 O1 76.57(9) . . ?
O7 W3 O1 76.41(8) 3_755 . ?
O3 W3 O1 76.66(8) . . ?
O4 W3 O1 76.03(8) 3_755 . ?
W3 O1 W3 180.0 3_755 . ?
W3 O1 W1 90.100(7) 3_755 . ?
W3 O1 W1 89.899(6) . . ?
W3 O1 W1 89.899(7) 3_755 3_755 ?
W3 O1 W1 90.102(7) . 3_755 ?
W1 O1 W1 180.0 . 3_755 ?
W3 O1 W2 89.792(12) 3_755 3_755 ?
W3 O1 W2 90.208(12) . 3_755 ?
W1 O1 W2 89.937(8) . 3_755 ?
W1 O1 W2 90.063(9) 3_755 3_755 ?
W3 O1 W2 90.209(12) 3_755 . ?
W3 O1 W2 89.791(12) . . ?
W1 O1 W2 90.063(9) . . ?
W1 O1 W2 89.937(9) 3_755 . ?
W2 O1 W2 180.0 3_755 . ?
W1 O2 W2 117.53(13) . . ?
W3 O3 W1 116.96(14) . . ?
W2 O4 W3 117.34(13) . 3_755 ?
W3 O5 W2 117.63(15) . . ?
W3 O7 W1 117.23(14) 3_755 . ?
W2 O8 W1 117.59(14) . 3_755 ?
C11 O11 C8 118.4(3) . . ?
C7 N1 C20 122.5(4) . . ?
C7 N1 C8 110.7(4) . . ?
C20 N1 C8 120.2(4) . . ?
C9 N2 C10 115.9(4) . . ?
C18 N3 C14 121.4(4) . . ?
C18 N3 C19 119.6(4) . . ?
C14 N3 C19 118.9(4) . . ?
C2 C1 C21 112.8(4) . . ?
C2 C1 C22 107.7(5) . . ?
C21 C1 C22 109.9(5) . . ?
C2 C1 C8 101.7(4) . . ?
C21 C1 C8 113.5(4) . . ?
C22 C1 C8 110.8(4) . . ?
C3 C2 C7 120.8(4) . . ?
C3 C2 C1 129.4(4) . . ?
C7 C2 C1 109.7(4) . . ?
C4 C3 C2 118.6(5) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C5 C4 C3 120.5(5) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 121.7(5) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C7 C6 C5 117.2(5) . . ?
C7 C6 H6 121.4 . . ?
C5 C6 H6 121.4 . . ?
N1 C7 C2 110.3(4) . . ?
N1 C7 C6 128.4(5) . . ?
C2 C7 C6 121.2(5) . . ?
N1 C8 O11 110.3(4) . . ?
N1 C8 C9 108.4(4) . . ?
O11 C8 C9 110.2(4) . . ?
N1 C8 C1 104.6(4) . . ?
O11 C8 C1 107.1(4) . . ?
C9 C8 C1 116.0(4) . . ?
N2 C9 C8 127.1(4) . . ?
N2 C9 H9 116.4 . . ?
C8 C9 H9 116.4 . . ?
C11 C10 C15 119.5(4) . . ?
C11 C10 N2 122.2(4) . . ?
C15 C10 N2 118.3(4) . . ?
O11 C11 C10 121.8(4) . . ?
O11 C11 C12 117.1(4) . . ?
C10 C11 C12 121.0(4) . . ?
C13 C12 C11 120.2(4) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C14 C13 C12 119.5(4) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 N3 121.6(4) . . ?
C13 C14 C15 121.0(4) . . ?
N3 C14 C15 117.4(4) . . ?
C10 C15 C16 121.2(4) . . ?
C10 C15 C14 118.8(4) . . ?
C16 C15 C14 120.0(4) . . ?
C17 C16 C15 118.7(4) . . ?
C17 C16 H16 120.7 . . ?
C15 C16 H16 120.7 . . ?
C18 C17 C16 120.3(5) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
N3 C18 C17 122.1(5) . . ?
N3 C18 H18 119.0 . . ?
C17 C18 H18 119.0 . . ?
N3 C19 H19A 109.5 . . ?
N3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N1 C20 H20A 109.5 . . ?
N1 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N1 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C1 C21 H21A 109.5 . . ?
C1 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C1 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C1 C22 H22A 109.5 . . ?
C1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C1 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

_refine_diff_density_max         1.383
_refine_diff_density_min         -1.466
_refine_diff_density_rms         0.205


####################################################################### 
# 
# 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_SP2W6
_database_code_depnum_ccdc_archive 'CCDC 1414604'
_audit_update_record             
;
2015-07-22 deposited with the CCDC.
2015-09-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C41 H47.50 N4.50 O21 W6'
_chemical_formula_weight         2042.43

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   10.4923(2)
_cell_length_b                   15.1018(3)
_cell_length_c                   16.1338(2)
_cell_angle_alpha                90
_cell_angle_beta                 104.6525(6)
_cell_angle_gamma                90
_cell_volume                     2473.30(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9884
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      29.96

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.743
_exptl_crystal_F_000             1874
_exptl_transmission_factor_min   0.3593
_exptl_transmission_factor_max   0.7460
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    13.979
_shelx_estimated_absorpt_T_min   0.102
_shelx_estimated_absorpt_T_max   0.605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS (Sheldrick, V2.10)'
_exptl_absorpt_special_details   'Blessing, Acta Cryst. (1995) A51, 33-38'
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37153
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.876
_diffrn_reflns_theta_max         30.037
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7227
_reflns_number_gt                6135
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0558P)²+3.2809P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7227
_refine_ls_number_parameters     340
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0320
_refine_ls_wR_factor_ref         0.1042
_refine_ls_wR_factor_gt          0.0908
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.70545(2) 0.56687(2) 1.02958(2) 0.03509(7) Uani 1 1 d . . . . .
W2 W 0.45944(2) 0.54649(2) 0.85809(2) 0.03835(8) Uani 1 1 d . . . . .
W3 W 0.59190(2) 0.36897(2) 0.96492(2) 0.03875(8) Uani 1 1 d . . . . .
O1 O 0.8547(4) 0.6179(3) 1.0506(3) 0.0493(11) Uani 1 1 d . . . . .
O2 O 0.6975(4) 0.5181(3) 1.1375(3) 0.0415(9) Uani 1 1 d . . . . .
O3 O 0.4086(4) 0.3417(3) 0.9479(3) 0.0416(9) Uani 1 1 d . . . . .
O4 O 0.6323(4) 0.5915(3) 0.9098(3) 0.0414(9) Uani 1 1 d . . . . .
O5 O 0.7401(4) 0.4488(3) 0.9961(3) 0.0418(9) Uani 1 1 d . . . . .
O6 O 0.5000 0.5000 1.0000 0.0326(11) Uani 1 2 d S . P . .
O7 O 0.4304(6) 0.5811(4) 0.7544(3) 0.0614(14) Uani 1 1 d . . . . .
O8 O 0.6067(4) 0.3580(3) 1.0857(3) 0.0435(10) Uani 1 1 d . . . . .
O9 O 0.5422(5) 0.4323(3) 0.8581(3) 0.0426(10) Uani 1 1 d . . . . .
O10 O 0.6602(6) 0.2734(4) 0.9395(4) 0.0648(14) Uani 1 1 d . . . . .
O11 O 0.0015(4) 0.4821(3) 0.2807(3) 0.0452(10) Uani 1 1 d . . . . .
C1 C 0.1064(7) 0.6247(4) 0.2834(4) 0.0457(14) Uani 1 1 d . . . . .
C2 C 0.1807(6) 0.6199(4) 0.3759(4) 0.0394(12) Uani 1 1 d . . . . .
C3 C 0.1850(7) 0.6787(4) 0.4423(4) 0.0484(15) Uani 1 1 d . . . . .
H3 H 0.1351 0.7303 0.4332 0.058 Uiso 1 1 calc R U . . .
C4 C 0.2661(8) 0.6590(6) 0.5240(5) 0.0574(18) Uani 1 1 d . . . . .
H4 H 0.2706 0.6980 0.5692 0.069 Uiso 1 1 calc R U . . .
C5 C 0.3378(8) 0.5830(6) 0.5368(5) 0.0600(19) Uani 1 1 d . . . . .
H5 H 0.3902 0.5704 0.5912 0.072 Uiso 1 1 calc R U . . .
C6 C 0.3348(7) 0.5233(5) 0.4698(5) 0.0530(16) Uani 1 1 d . . . . .
H6 H 0.3845 0.4716 0.4789 0.064 Uiso 1 1 calc R U . . .
C7 C 0.2560(6) 0.5436(4) 0.3905(4) 0.0376(12) Uani 1 1 d . . . . .
N8 N 0.2356(5) 0.4947(3) 0.3140(3) 0.0399(10) Uani 1 1 d . . . . .
C9 C 0.1142(6) 0.5252(4) 0.2572(4) 0.0374(11) Uani 1 1 d . . . . .
C10 C 0.1081(7) 0.5065(4) 0.1658(4) 0.0458(14) Uani 1 1 d . . . . .
H10 H 0.1483 0.5459 0.1361 0.055 Uiso 1 1 calc R U . . .
C11 C 0.0477(7) 0.4359(4) 0.1248(4) 0.0432(14) Uani 1 1 d . . . . .
H11 H 0.0465 0.4261 0.0677 0.052 Uiso 1 1 calc R U . . .
C12 C -0.0162(6) 0.3744(4) 0.1702(4) 0.0357(11) Uani 1 1 d . . . . .
C13 C -0.0383(6) 0.4011(4) 0.2480(4) 0.0381(12) Uani 1 1 d . . . . .
C14 C -0.1015(7) 0.3457(5) 0.2927(4) 0.0520(16) Uani 1 1 d . . . . .
H14 H -0.1181 0.3639 0.3441 0.062 Uiso 1 1 calc R U . . .
C15 C -0.1391(7) 0.2639(5) 0.2602(4) 0.0537(17) Uani 1 1 d . . . . .
H15 H -0.1836 0.2265 0.2891 0.064 Uiso 1 1 calc R U . . .
C16 C -0.1125(7) 0.2354(4) 0.1848(4) 0.0469(14) Uani 1 1 d . . . . .
N17 N -0.0539(5) 0.2914(3) 0.1405(3) 0.0415(11) Uani 1 1 d . . . . .
C18 C -0.0322(9) 0.6604(6) 0.2680(6) 0.079(3) Uani 1 1 d . . . . .
H18A H -0.0791 0.6276 0.3019 0.119 Uiso 1 1 calc R U . . .
H18B H -0.0766 0.6544 0.2085 0.119 Uiso 1 1 calc R U . . .
H18C H -0.0290 0.7217 0.2839 0.119 Uiso 1 1 calc R U . . .
C19 C 0.1894(13) 0.6819(5) 0.2370(6) 0.093(4) Uani 1 1 d . . . . .
H19A H 0.2087 0.7378 0.2658 0.140 Uiso 1 1 calc R U . . .
H19B H 0.1407 0.6916 0.1788 0.140 Uiso 1 1 calc R U . . .
H19C H 0.2702 0.6517 0.2377 0.140 Uiso 1 1 calc R U . . .
C20 C 0.2782(7) 0.4037(4) 0.3134(5) 0.0548(17) Uani 1 1 d . . . . .
H20A H 0.3691 0.3991 0.3442 0.082 Uiso 1 1 calc R U . . .
H20B H 0.2681 0.3846 0.2553 0.082 Uiso 1 1 calc R U . . .
H20C H 0.2256 0.3669 0.3402 0.082 Uiso 1 1 calc R U . . .
C21 C -0.1486(10) 0.1429(5) 0.1511(7) 0.077(3) Uani 1 1 d . . . . .
H21A H -0.2132 0.1461 0.0971 0.116 Uiso 1 1 calc R U . . .
H21B H -0.1842 0.1105 0.1913 0.116 Uiso 1 1 calc R U . . .
H21C H -0.0714 0.1132 0.1435 0.116 Uiso 1 1 calc R U . . .
C22 C -0.0242(8) 0.2619(5) 0.0600(5) 0.0575(18) Uani 1 1 d . . . . .
H22A H 0.0223 0.2066 0.0695 0.086 Uiso 1 1 calc R U . . .
H22B H 0.0293 0.3056 0.0416 0.086 Uiso 1 1 calc R U . . .
H22C H -0.1050 0.2544 0.0165 0.086 Uiso 1 1 calc R U . . .
C23 C 0.528(4) 0.023(2) 0.010(3) 0.068(9) Uiso 0.25 1 d . . P . .
H23A H 0.5290 0.0458 0.0653 0.103 Uiso 0.25 1 calc R U P . .
H23B H 0.4894 0.0663 -0.0331 0.103 Uiso 0.25 1 calc R U P . .
H23C H 0.6171 0.0116 0.0068 0.103 Uiso 0.25 1 calc R U P . .
C24 C 0.550(4) 0.060(2) 0.006(3) 0.079(11) Uiso 0.25 1 d D . P . .
N25 N 0.603(6) 0.126(3) 0.005(4) 0.16(2) Uiso 0.25 1 d D . P . .


_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 O1 1.701(4) . ?
W1 O2 1.911(4) . ?
W1 O3 1.921(4) 3_667 ?
W1 O5 1.924(4) . ?
W1 O4 1.926(4) . ?
W1 O6 2.3182(2) . ?
W2 O7 1.705(4) . ?
W2 O4 1.919(4) . ?
W2 O8 1.925(4) 3_667 ?
W2 O9 1.930(4) . ?
W2 O2 1.931(4) 3_667 ?
W2 O6 2.3287(2) . ?
W3 O10 1.706(5) . ?
W3 O3 1.917(4) . ?
W3 O8 1.923(4) . ?
W3 O9 1.925(4) . ?
W3 O5 1.931(4) . ?
W3 O6 2.3328(2) . ?
O2 W2 1.931(4) 3_667 ?
O3 W1 1.921(4) 3_667 ?
O6 W1 2.3182(2) 3_667 ?
O6 W2 2.3287(2) 3_667 ?
O6 W3 2.3328(2) 3_667 ?
O8 W2 1.925(4) 3_667 ?
O11 C13 1.354(7) . ?
O11 C9 1.481(7) . ?
C1 C2 1.501(9) . ?
C1 C18 1.512(10) . ?
C1 C19 1.546(11) . ?
C1 C9 1.568(8) . ?
C2 C3 1.383(8) . ?
C2 C7 1.384(8) . ?
C3 C4 1.407(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.359(11) . ?
C4 H4 0.9300 . ?
C5 C6 1.401(10) . ?
C5 H5 0.9300 . ?
C6 C7 1.372(9) . ?
C6 H6 0.9300 . ?
C7 N8 1.407(8) . ?
N8 C9 1.444(8) . ?
N8 C20 1.447(7) . ?
C9 C10 1.486(8) . ?
C10 C11 1.328(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.448(8) . ?
C11 H11 0.9300 . ?
C12 N17 1.365(7) . ?
C12 C13 1.393(8) . ?
C13 C14 1.379(8) . ?
C14 C15 1.362(10) . ?
C14 H14 0.9300 . ?
C15 C16 1.384(10) . ?
C15 H15 0.9300 . ?
C16 N17 1.351(8) . ?
C16 C21 1.513(10) . ?
N17 C22 1.479(8) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.493(19) 3_655 ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 N25 1.14(2) . ?
C24 C23 1.493(19) 3_655 ?

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 W1 O2 104.1(2) . . ?
O1 W1 O3 102.9(2) . 3_667 ?
O2 W1 O3 86.10(19) . 3_667 ?
O1 W1 O5 104.2(2) . . ?
O2 W1 O5 87.3(2) . . ?
O3 W1 O5 152.87(18) 3_667 . ?
O1 W1 O4 103.0(2) . . ?
O2 W1 O4 152.87(18) . . ?
O3 W1 O4 86.65(19) 3_667 . ?
O5 W1 O4 87.3(2) . . ?
O1 W1 O6 178.86(18) . . ?
O2 W1 O6 76.55(12) . . ?
O3 W1 O6 76.15(13) 3_667 . ?
O5 W1 O6 76.72(13) . . ?
O4 W1 O6 76.33(12) . . ?
O7 W2 O4 103.5(2) . . ?
O7 W2 O8 103.7(2) . 3_667 ?
O4 W2 O8 86.77(19) . 3_667 ?
O7 W2 O9 104.0(2) . . ?
O4 W2 O9 86.6(2) . . ?
O8 W2 O9 152.32(17) 3_667 . ?
O7 W2 O2 104.4(2) . 3_667 ?
O4 W2 O2 152.12(17) . 3_667 ?
O8 W2 O2 87.06(19) 3_667 3_667 ?
O9 W2 O2 86.37(19) . 3_667 ?
O7 W2 O6 179.6(2) . . ?
O4 W2 O6 76.21(12) . . ?
O8 W2 O6 76.17(12) 3_667 . ?
O9 W2 O6 76.16(12) . . ?
O2 W2 O6 75.92(12) 3_667 . ?
O10 W3 O3 104.6(2) . . ?
O10 W3 O8 103.8(2) . . ?
O3 W3 O8 86.99(19) . . ?
O10 W3 O9 103.9(2) . . ?
O3 W3 O9 86.80(19) . . ?
O8 W3 O9 152.25(18) . . ?
O10 W3 O5 103.4(2) . . ?
O3 W3 O5 152.08(17) . . ?
O8 W3 O5 86.34(19) . . ?
O9 W3 O5 86.6(2) . . ?
O10 W3 O6 179.6(2) . . ?
O3 W3 O6 75.85(12) . . ?
O8 W3 O6 76.10(13) . . ?
O9 W3 O6 76.15(12) . . ?
O5 W3 O6 76.23(12) . . ?
W1 O2 W2 117.5(2) . 3_667 ?
W3 O3 W1 118.0(2) . 3_667 ?
W2 O4 W1 117.4(2) . . ?
W1 O5 W3 117.1(2) . . ?
W1 O6 W1 180.0 . 3_667 ?
W1 O6 W2 89.988(8) . 3_667 ?
W1 O6 W2 90.013(8) 3_667 3_667 ?
W1 O6 W2 90.012(8) . . ?
W1 O6 W2 89.987(8) 3_667 . ?
W2 O6 W2 180.0 3_667 . ?
W1 O6 W3 90.027(8) . 3_667 ?
W1 O6 W3 89.971(9) 3_667 3_667 ?
W2 O6 W3 90.062(9) 3_667 3_667 ?
W2 O6 W3 89.938(9) . 3_667 ?
W1 O6 W3 89.974(8) . . ?
W1 O6 W3 90.027(8) 3_667 . ?
W2 O6 W3 89.937(9) 3_667 . ?
W2 O6 W3 90.063(9) . . ?
W3 O6 W3 180.0 3_667 . ?
W3 O8 W2 117.8(2) . 3_667 ?
W3 O9 W2 117.6(2) . . ?
C13 O11 C9 119.0(4) . . ?
C2 C1 C18 114.6(6) . . ?
C2 C1 C19 107.1(6) . . ?
C18 C1 C19 111.0(7) . . ?
C2 C1 C9 100.0(5) . . ?
C18 C1 C9 114.2(6) . . ?
C19 C1 C9 109.3(6) . . ?
C3 C2 C7 119.9(6) . . ?
C3 C2 C1 130.3(6) . . ?
C7 C2 C1 109.8(5) . . ?
C2 C3 C4 118.9(6) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C5 C4 C3 120.1(7) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 121.5(7) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C7 C6 C5 117.8(7) . . ?
C7 C6 H6 121.1 . . ?
C5 C6 H6 121.1 . . ?
C6 C7 C2 121.9(6) . . ?
C6 C7 N8 128.6(6) . . ?
C2 C7 N8 109.5(5) . . ?
C7 N8 C9 107.7(4) . . ?
C7 N8 C20 121.7(5) . . ?
C9 N8 C20 121.5(5) . . ?
N8 C9 O11 109.3(5) . . ?
N8 C9 C10 112.3(5) . . ?
O11 C9 C10 109.5(5) . . ?
N8 C9 C1 103.4(5) . . ?
O11 C9 C1 104.7(5) . . ?
C10 C9 C1 117.2(5) . . ?
C11 C10 C9 122.8(6) . . ?
C11 C10 H10 118.6 . . ?
C9 C10 H10 118.6 . . ?
C10 C11 C12 119.1(6) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 H11 120.5 . . ?
N17 C12 C13 118.9(5) . . ?
N17 C12 C11 122.8(5) . . ?
C13 C12 C11 118.3(5) . . ?
O11 C13 C14 119.1(5) . . ?
O11 C13 C12 120.4(5) . . ?
C14 C13 C12 120.5(6) . . ?
C15 C14 C13 118.7(6) . . ?
C15 C14 H14 120.7 . . ?
C13 C14 H14 120.7 . . ?
C14 C15 C16 121.2(6) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 H15 119.4 . . ?
N17 C16 C15 119.4(6) . . ?
N17 C16 C21 119.6(7) . . ?
C15 C16 C21 121.0(7) . . ?
C16 N17 C12 121.3(5) . . ?
C16 N17 C22 120.1(6) . . ?
C12 N17 C22 118.6(5) . . ?
C1 C18 H18A 109.5 . . ?
C1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C1 C19 H19A 109.5 . . ?
C1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N8 C20 H20A 109.5 . . ?
N8 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N8 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N17 C22 H22A 109.5 . . ?
N17 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N17 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 H23A 109.5 3_655 . ?
C24 C23 H23B 109.5 3_655 . ?
H23A C23 H23B 109.5 . . ?
C24 C23 H23C 109.5 3_655 . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N25 C24 C23 170(6) . 3_655 ?

_refine_diff_density_max         1.375
_refine_diff_density_min         -2.491
_refine_diff_density_rms         0.575




#===END 

