# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_X8_16197
_database_code_depnum_ccdc_archive 'CCDC 1580349'
_audit_update_record             
;
2017-10-16 deposited with the CCDC.
2017-12-21 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            'C15 H12 N2'
_chemical_formula_weight         220.27

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'

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

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

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

_cell_length_a                   22.851(3)
_cell_length_b                   5.7145(6)
_cell_length_c                   16.970(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.174(3)
_cell_angle_gamma                90
_cell_volume                     2193.6(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4668
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      30.51

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_F_000             928
_exptl_transmission_factor_min   0.7006
_exptl_transmission_factor_max   0.7461
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.055
_exptl_absorpt_coefficient_mu    0.080
_shelx_estimated_absorpt_T_min   0.984
_shelx_estimated_absorpt_T_max   0.996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   
'I\mS micro-focus sealed tube, multilayer optics'
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            20936
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.801
_diffrn_reflns_theta_max         30.454
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3320
_reflns_number_gt                2700
_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       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_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          
; 
 Bruker X8 Kappa DUO four-circle diffractometer, Bruker APEX2 CCD. 
 The instrument was purchased with the help of funding from the 
 National Science Foundation (NSF) under Grant Number 
 CHE-0946721.  Please acknowledge this grant in all publications 
 of this structure. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0637P)²+1.9170P] 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         3320
_refine_ls_number_parameters     154
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0474
_refine_ls_wR_factor_ref         0.1298
_refine_ls_wR_factor_gt          0.1199
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.51761(6) 0.6387(2) 0.09477(8) 0.0221(3) Uani 1 1 d . . . . .
H1A H 0.5005 0.4895 0.1008 0.027 Uiso 1 1 calc R U . . .
H1B H 0.5077 0.7237 0.0466 0.027 Uiso 1 1 calc R U . . .
N1 N 0.55384(5) 0.72505(19) 0.15141(6) 0.0202(2) Uani 1 1 d . . . . .
N2 N 0.56716(4) 0.59558(18) 0.22091(6) 0.0162(2) Uani 1 1 d . . . . .
C2 C 0.62866(5) 0.6454(2) 0.26266(7) 0.0157(2) Uani 1 1 d . . . . .
H2 H 0.6385 0.8133 0.2747 0.019 Uiso 1 1 calc R U . . .
C3 C 0.62541(5) 0.4860(2) 0.33422(7) 0.0163(2) Uani 1 1 d . . . . .
C4 C 0.64548(5) 0.5054(2) 0.41481(7) 0.0180(2) Uani 1 1 d . . . . .
H4 H 0.6676 0.6379 0.4355 0.022 Uiso 1 1 calc R U . . .
C5 C 0.63223(5) 0.3243(2) 0.46514(7) 0.0204(3) Uani 1 1 d . . . . .
H5 H 0.6458 0.3339 0.5206 0.024 Uiso 1 1 calc R U . . .
C6 C 0.59963(5) 0.1309(2) 0.43500(7) 0.0198(2) Uani 1 1 d . . . . .
H6 H 0.5915 0.0096 0.4701 0.024 Uiso 1 1 calc R U . . .
C7 C 0.57852(5) 0.1121(2) 0.35328(7) 0.0175(2) Uani 1 1 d . . . . .
H7 H 0.5557 -0.0187 0.3326 0.021 Uiso 1 1 calc R U . . .
C8 C 0.59218(5) 0.2909(2) 0.30426(7) 0.0159(2) Uani 1 1 d . . . . .
C9 C 0.57579(5) 0.3325(2) 0.21552(7) 0.0157(2) Uani 1 1 d . . . . .
H9 H 0.5417 0.2405 0.1879 0.019 Uiso 1 1 calc R U . . .
C10 C 0.63345(5) 0.3230(2) 0.17892(7) 0.0148(2) Uani 1 1 d . . . . .
C11 C 0.65510(5) 0.1668(2) 0.12826(7) 0.0169(2) Uani 1 1 d . . . . .
H11 H 0.6337 0.0297 0.1106 0.020 Uiso 1 1 calc R U . . .
C12 C 0.70993(5) 0.2173(2) 0.10363(7) 0.0183(2) Uani 1 1 d . . . . .
H12 H 0.7256 0.1135 0.0682 0.022 Uiso 1 1 calc R U . . .
C13 C 0.74149(5) 0.4168(2) 0.13026(7) 0.0180(2) Uani 1 1 d . . . . .
H13 H 0.7780 0.4491 0.1118 0.022 Uiso 1 1 calc R U . . .
C14 C 0.72019(5) 0.5715(2) 0.18408(7) 0.0165(2) Uani 1 1 d . . . . .
H14 H 0.7421 0.7061 0.2034 0.020 Uiso 1 1 calc R U . . .
C15 C 0.66621(5) 0.5204(2) 0.20789(7) 0.0149(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.2753(17) . ?
C1 H1A 0.9500 . ?
C1 H1B 0.9500 . ?
N1 N2 1.3890(14) . ?
N2 C2 1.5082(15) . ?
N2 C9 1.5209(16) . ?
C2 C3 1.5282(16) . ?
C2 C15 1.5287(16) . ?
C2 H2 1.0000 . ?
C3 C4 1.3837(16) . ?
C3 C8 1.4029(16) . ?
C4 C5 1.4022(17) . ?
C4 H4 0.9500 . ?
C5 C6 1.3889(18) . ?
C5 H5 0.9500 . ?
C6 C7 1.4061(17) . ?
C6 H6 0.9500 . ?
C7 C8 1.3810(16) . ?
C7 H7 0.9500 . ?
C8 C9 1.5180(16) . ?
C9 C10 1.5355(15) . ?
C9 H9 1.0000 . ?
C10 C11 1.3788(16) . ?
C10 C15 1.4036(16) . ?
C11 C12 1.4059(16) . ?
C11 H11 0.9500 . ?
C12 C13 1.3895(17) . ?
C12 H12 0.9500 . ?
C13 C14 1.4070(16) . ?
C13 H13 0.9500 . ?
C14 C15 1.3827(15) . ?
C14 H14 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 H1A 120.0 . . ?
N1 C1 H1B 120.0 . . ?
H1A C1 H1B 120.0 . . ?
C1 N1 N2 118.32(11) . . ?
N1 N2 C2 112.06(9) . . ?
N1 N2 C9 119.35(10) . . ?
C2 N2 C9 95.43(8) . . ?
N2 C2 C3 96.53(8) . . ?
N2 C2 C15 101.09(9) . . ?
C3 C2 C15 107.44(9) . . ?
N2 C2 H2 116.4 . . ?
C3 C2 H2 116.4 . . ?
C15 C2 H2 116.4 . . ?
C4 C3 C8 120.54(11) . . ?
C4 C3 C2 133.70(11) . . ?
C8 C3 C2 105.69(10) . . ?
C3 C4 C5 118.22(11) . . ?
C3 C4 H4 120.9 . . ?
C5 C4 H4 120.9 . . ?
C6 C5 C4 120.92(11) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 C7 120.99(11) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C8 C7 C6 117.54(11) . . ?
C8 C7 H7 121.2 . . ?
C6 C7 H7 121.2 . . ?
C7 C8 C3 121.78(11) . . ?
C7 C8 C9 131.94(11) . . ?
C3 C8 C9 106.24(10) . . ?
C8 C9 N2 96.36(9) . . ?
C8 C9 C10 106.91(9) . . ?
N2 C9 C10 100.68(9) . . ?
C8 C9 H9 116.7 . . ?
N2 C9 H9 116.7 . . ?
C10 C9 H9 116.7 . . ?
C11 C10 C15 121.19(10) . . ?
C11 C10 C9 132.82(11) . . ?
C15 C10 C9 106.00(9) . . ?
C10 C11 C12 117.81(11) . . ?
C10 C11 H11 121.1 . . ?
C12 C11 H11 121.1 . . ?
C13 C12 C11 120.99(11) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C12 C13 C14 121.01(11) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C15 C14 C13 117.53(11) . . ?
C15 C14 H14 121.2 . . ?
C13 C14 H14 121.2 . . ?
C14 C15 C10 121.40(10) . . ?
C14 C15 C2 132.86(11) . . ?
C10 C15 C2 105.72(9) . . ?

_refine_diff_density_max         0.410
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.057

####################################################################### 
# 
# 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_X8_17012
_database_code_depnum_ccdc_archive 'CCDC 1580350'
_audit_update_record             
;
2017-10-16 deposited with the CCDC.
2017-12-21 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            'C27 H41 O2 W0.50'
_chemical_formula_weight         489.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'

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

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

_cell_length_a                   15.0937(12)
_cell_length_b                   17.6924(14)
_cell_length_c                   9.6626(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2580.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9834
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      28.90

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_F_000             1024
_exptl_transmission_factor_min   0.4565
_exptl_transmission_factor_max   0.5658
_exptl_crystal_size_max          0.312
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.069
_exptl_absorpt_coefficient_mu    2.279
_shelx_estimated_absorpt_T_min   0.537
_shelx_estimated_absorpt_T_max   0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   
'I\mS micro-focus sealed tube, multilayer optics'
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            114424
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.773
_diffrn_reflns_theta_max         33.191
_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             9878
_reflns_number_gt                8748
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.806
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    1.000

_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       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_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          
; 
 Refined as a 2-component inversion twin. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0169P)²+0.8674P] 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_abs_structure_details 
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.240(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9878
_refine_ls_number_parameters     546
_refine_ls_number_restraints     1343
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0234
_refine_ls_wR_factor_ref         0.0511
_refine_ls_wR_factor_gt          0.0487
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.039
_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
W1 W 0.5056(2) 0.5028(3) 0.68313(2) 0.0214(3) Uani 0.4270(3) 1 d D U P A -2
C1 C 0.5102(9) 0.5036(15) 0.8758(4) 0.019(2) Uani 0.4270(3) 1 d D U P A -2
H1A H 0.5282 0.5470 0.9223 0.023 Uiso 0.4270(3) 1 calc R U P A -2
H1B H 0.4945 0.4606 0.9255 0.023 Uiso 0.4270(3) 1 calc R U P A -2
W2 W 0.5038(10) 0.5034(10) 0.58503(10) 0.0225(11) Uani 0.0730(3) 1 d D U P A -3
C2 C 0.509(2) 0.496(3) 0.3945(16) 0.019(2) Uani 0.0730(3) 1 d D U P A -3
H2A H 0.4592 0.5066 0.3414 0.023 Uiso 0.0730(3) 1 calc R U P A -3
H2B H 0.5615 0.4812 0.3517 0.023 Uiso 0.0730(3) 1 calc R U P A -3
O1 O 0.4489(13) 0.4106(6) 0.666(2) 0.028(2) Uani 0.5 1 d D U P A -1
C11 C 0.4063(13) 0.3396(11) 0.635(2) 0.029(2) Uani 0.5 1 d D U P A -1
C12 C 0.3371(8) 0.3192(6) 0.7242(13) 0.039(2) Uani 0.5 1 d D U P A -1
C13 C 0.2925(7) 0.2513(5) 0.6933(11) 0.049(2) Uani 0.5 1 d D U P A -1
H13 H 0.2461 0.2351 0.7492 0.059 Uiso 0.5 1 calc R U P A -1
C14 C 0.3175(8) 0.2092(5) 0.5809(11) 0.057(2) Uani 0.5 1 d D U P A -1
H14 H 0.2873 0.1646 0.5617 0.068 Uiso 0.5 1 calc R U P A -1
C15 C 0.3855(7) 0.2308(5) 0.4961(12) 0.050(2) Uani 0.5 1 d D U P A -1
H15 H 0.4002 0.2011 0.4201 0.060 Uiso 0.5 1 calc R U P A -1
C16 C 0.4327(7) 0.2962(6) 0.5220(11) 0.0331(19) Uani 0.5 1 d D U P A -1
C121 C 0.3115(7) 0.3647(6) 0.8487(12) 0.038(2) Uani 0.5 1 d D U P A -1
H121 H 0.3309 0.4165 0.8297 0.046 Uiso 0.5 1 calc R U P A -1
C122 C 0.3616(8) 0.3397(7) 0.9780(12) 0.045(3) Uani 0.5 1 d D U P A -1
H12A H 0.3434 0.3701 1.0553 0.068 Uiso 0.5 1 calc R U P A -1
H12B H 0.3487 0.2876 0.9968 0.068 Uiso 0.5 1 calc R U P A -1
H12C H 0.4241 0.3457 0.9633 0.068 Uiso 0.5 1 calc R U P A -1
C123 C 0.2122(6) 0.3695(7) 0.8786(15) 0.060(3) Uani 0.5 1 d D U P A -1
H12D H 0.2026 0.3997 0.9598 0.091 Uiso 0.5 1 calc R U P A -1
H12E H 0.1826 0.3922 0.8012 0.091 Uiso 0.5 1 calc R U P A -1
H12F H 0.1891 0.3196 0.8936 0.091 Uiso 0.5 1 calc R U P A -1
C161 C 0.5071(8) 0.3215(4) 0.4306(8) 0.0463(19) Uani 0.5 1 d D U P A -1
H161 H 0.5544 0.3415 0.4895 0.056 Uiso 0.5 1 calc R U P A -1
C162 C 0.4790(5) 0.3844(6) 0.3284(8) 0.072(2) Uani 0.5 1 d D U P A -1
H16A H 0.5288 0.3986 0.2724 0.108 Uiso 0.5 1 calc R U P A -1
H16B H 0.4322 0.3660 0.2701 0.108 Uiso 0.5 1 calc R U P A -1
H16C H 0.4585 0.4275 0.3794 0.108 Uiso 0.5 1 calc R U P A -1
C163 C 0.5475(8) 0.2607(7) 0.3349(15) 0.113(5) Uani 0.5 1 d D U P A -1
H16D H 0.5943 0.2826 0.2810 0.169 Uiso 0.5 1 calc R U P A -1
H16E H 0.5708 0.2201 0.3900 0.169 Uiso 0.5 1 calc R U P A -1
H16F H 0.5024 0.2414 0.2742 0.169 Uiso 0.5 1 calc R U P A -1
O2 O 0.3879(8) 0.5334(7) 0.613(2) 0.029(2) Uani 0.5 1 d D U P A -1
C21 C 0.3019(11) 0.5419(15) 0.637(2) 0.027(3) Uani 0.5 1 d D U P A -1
C22 C 0.2660(9) 0.5836(10) 0.7447(17) 0.035(2) Uani 0.5 1 d D U P A -1
C23 C 0.1738(8) 0.5842(8) 0.7630(14) 0.043(3) Uani 0.5 1 d D U P A -1
H23 H 0.1489 0.6117 0.8352 0.051 Uiso 0.5 1 calc R U P A -1
C24 C 0.1205(7) 0.5442(7) 0.6747(11) 0.045(2) Uani 0.5 1 d D U P A -1
H24 H 0.0595 0.5436 0.6881 0.054 Uiso 0.5 1 calc R U P A -1
C25 C 0.1572(7) 0.5051(9) 0.5664(10) 0.0406(19) Uani 0.5 1 d D U P A -1
H25 H 0.1200 0.4797 0.5055 0.049 Uiso 0.5 1 calc R U P A -1
C26 C 0.2477(7) 0.5022(11) 0.5449(12) 0.0310(18) Uani 0.5 1 d D U P A -1
C221 C 0.3238(11) 0.6302(7) 0.8362(17) 0.050(4) Uani 0.5 1 d D U P A -1
H221 H 0.3852 0.6175 0.8125 0.060 Uiso 0.5 1 calc R U P A -1
C222 C 0.3128(13) 0.6138(9) 0.9919(15) 0.090(5) Uani 0.5 1 d D U P A -1
H22A H 0.3520 0.6458 1.0438 0.135 Uiso 0.5 1 calc R U P A -1
H22B H 0.2527 0.6236 1.0189 0.135 Uiso 0.5 1 calc R U P A -1
H22C H 0.3269 0.5618 1.0099 0.135 Uiso 0.5 1 calc R U P A -1
C223 C 0.3126(17) 0.7144(8) 0.808(2) 0.146(9) Uani 0.5 1 d D U P A -1
H22D H 0.3506 0.7426 0.8687 0.220 Uiso 0.5 1 calc R U P A -1
H22E H 0.3280 0.7250 0.7137 0.220 Uiso 0.5 1 calc R U P A -1
H22F H 0.2521 0.7286 0.8243 0.220 Uiso 0.5 1 calc R U P A -1
C261 C 0.2897(7) 0.4631(6) 0.4238(10) 0.036(2) Uani 0.5 1 d D U P A -1
H261 H 0.3473 0.4438 0.4544 0.043 Uiso 0.5 1 calc R U P A -1
C262 C 0.3069(8) 0.5199(7) 0.3075(13) 0.053(3) Uani 0.5 1 d D U P A -1
H26A H 0.3338 0.4944 0.2305 0.079 Uiso 0.5 1 calc R U P A -1
H26B H 0.2519 0.5420 0.2787 0.079 Uiso 0.5 1 calc R U P A -1
H26C H 0.3459 0.5588 0.3402 0.079 Uiso 0.5 1 calc R U P A -1
C263 C 0.2365(8) 0.3962(6) 0.3706(13) 0.061(3) Uani 0.5 1 d D U P A -1
H26D H 0.2667 0.3738 0.2935 0.092 Uiso 0.5 1 calc R U P A -1
H26E H 0.2302 0.3595 0.4431 0.092 Uiso 0.5 1 calc R U P A -1
H26F H 0.1790 0.4131 0.3417 0.092 Uiso 0.5 1 calc R U P A -1
O3 O 0.5438(13) 0.6012(6) 0.669(2) 0.026(2) Uani 0.5 1 d D U P A -1
C31 C 0.6020(14) 0.6574(11) 0.655(2) 0.028(2) Uani 0.5 1 d D U P A -1
C32 C 0.6740(7) 0.6646(6) 0.7452(11) 0.0313(18) Uani 0.5 1 d D U P A -1
C33 C 0.7291(6) 0.7260(5) 0.7228(11) 0.0421(19) Uani 0.5 1 d D U P A -1
H33 H 0.7773 0.7332 0.7814 0.050 Uiso 0.5 1 calc R U P A -1
C34 C 0.7152(5) 0.7768(5) 0.6171(11) 0.0450(19) Uani 0.5 1 d D U P A -1
H34 H 0.7548 0.8165 0.6038 0.054 Uiso 0.5 1 calc R U P A -1
C35 C 0.6436(6) 0.7694(5) 0.5315(10) 0.0362(17) Uani 0.5 1 d D U P A -1
H35 H 0.6339 0.8046 0.4616 0.043 Uiso 0.5 1 calc R U P A -1
C36 C 0.5851(7) 0.7092(6) 0.5490(11) 0.0283(16) Uani 0.5 1 d D U P A -1
C321 C 0.6839(9) 0.6132(6) 0.8685(11) 0.049(3) Uani 0.5 1 d D U P A -1
H321 H 0.6596 0.5636 0.8442 0.059 Uiso 0.5 1 calc R U P A -1
C322 C 0.6293(12) 0.6454(10) 0.9910(16) 0.110(6) Uani 0.5 1 d D U P A -1
H32A H 0.6355 0.6128 1.0698 0.164 Uiso 0.5 1 calc R U P A -1
H32B H 0.6507 0.6950 1.0139 0.164 Uiso 0.5 1 calc R U P A -1
H32C H 0.5680 0.6484 0.9651 0.164 Uiso 0.5 1 calc R U P A -1
C323 C 0.7813(9) 0.6025(8) 0.9120(14) 0.080(4) Uani 0.5 1 d D U P A -1
H32D H 0.7842 0.5695 0.9907 0.121 Uiso 0.5 1 calc R U P A -1
H32E H 0.8140 0.5808 0.8367 0.121 Uiso 0.5 1 calc R U P A -1
H32F H 0.8065 0.6506 0.9358 0.121 Uiso 0.5 1 calc R U P A -1
C361 C 0.5024(8) 0.7043(4) 0.4619(9) 0.050(2) Uani 0.5 1 d D U P A -1
H361 H 0.4626 0.6667 0.5026 0.060 Uiso 0.5 1 calc R U P A -1
C362 C 0.5216(8) 0.6823(7) 0.3129(10) 0.093(4) Uani 0.5 1 d D U P A -1
H36A H 0.4670 0.6800 0.2620 0.140 Uiso 0.5 1 calc R U P A -1
H36B H 0.5599 0.7193 0.2716 0.140 Uiso 0.5 1 calc R U P A -1
H36C H 0.5499 0.6337 0.3109 0.140 Uiso 0.5 1 calc R U P A -1
C363 C 0.4532(6) 0.7814(5) 0.4539(13) 0.079(3) Uani 0.5 1 d D U P A -1
H36D H 0.4011 0.7761 0.3978 0.118 Uiso 0.5 1 calc R U P A -1
H36E H 0.4366 0.7971 0.5454 0.118 Uiso 0.5 1 calc R U P A -1
H36F H 0.4917 0.8187 0.4136 0.118 Uiso 0.5 1 calc R U P A -1
O4 O 0.6105(7) 0.4516(6) 0.6130(17) 0.0204(14) Uani 0.5 1 d D U P A -1
C41 C 0.7012(11) 0.4518(16) 0.649(2) 0.029(3) Uani 0.5 1 d D U P A -1
C42 C 0.7242(8) 0.4048(9) 0.7599(16) 0.0287(19) Uani 0.5 1 d D U P A -1
C43 C 0.8137(7) 0.4009(8) 0.7928(13) 0.035(2) Uani 0.5 1 d D U P A -1
H43 H 0.8317 0.3704 0.8660 0.042 Uiso 0.5 1 calc R U P A -1
C44 C 0.8760(8) 0.4405(7) 0.7204(11) 0.040(2) Uani 0.5 1 d D U P A -1
H44 H 0.9351 0.4373 0.7467 0.047 Uiso 0.5 1 calc R U P A -1
C45 C 0.8531(7) 0.4853(8) 0.6087(10) 0.037(2) Uani 0.5 1 d D U P A -1
H45 H 0.8965 0.5112 0.5597 0.044 Uiso 0.5 1 calc R U P A -1
C46 C 0.7642(9) 0.4914(10) 0.5701(14) 0.033(2) Uani 0.5 1 d D U P A -1
C421 C 0.6578(9) 0.3543(7) 0.8308(14) 0.033(2) Uani 0.5 1 d D U P A -1
H421 H 0.5979 0.3693 0.8027 0.040 Uiso 0.5 1 calc R U P A -1
C422 C 0.6659(10) 0.3616(7) 0.9876(13) 0.048(3) Uani 0.5 1 d D U P A -1
H42A H 0.6233 0.3292 1.0314 0.072 Uiso 0.5 1 calc R U P A -1
H42B H 0.7245 0.3472 1.0158 0.072 Uiso 0.5 1 calc R U P A -1
H42C H 0.6550 0.4130 1.0143 0.072 Uiso 0.5 1 calc R U P A -1
C423 C 0.6745(9) 0.2719(6) 0.7846(13) 0.049(2) Uani 0.5 1 d D U P A -1
H42D H 0.6325 0.2391 0.8290 0.073 Uiso 0.5 1 calc R U P A -1
H42E H 0.6677 0.2682 0.6860 0.073 Uiso 0.5 1 calc R U P A -1
H42F H 0.7335 0.2572 0.8100 0.073 Uiso 0.5 1 calc R U P A -1
C461 C 0.7369(6) 0.5367(7) 0.4447(13) 0.037(2) Uani 0.5 1 d D U P A -1
H461 H 0.6782 0.5575 0.4652 0.045 Uiso 0.5 1 calc R U P A -1
C462 C 0.7258(8) 0.4855(7) 0.3180(15) 0.050(3) Uani 0.5 1 d D U P A -1
H46A H 0.7084 0.5155 0.2397 0.076 Uiso 0.5 1 calc R U P A -1
H46B H 0.7809 0.4607 0.2984 0.076 Uiso 0.5 1 calc R U P A -1
H46C H 0.6810 0.4483 0.3365 0.076 Uiso 0.5 1 calc R U P A -1
C463 C 0.7966(8) 0.6040(7) 0.4097(14) 0.055(3) Uani 0.5 1 d D U P A -1
H46D H 0.7742 0.6293 0.3290 0.083 Uiso 0.5 1 calc R U P A -1
H46E H 0.7975 0.6386 0.4862 0.083 Uiso 0.5 1 calc R U P A -1
H46F H 0.8557 0.5864 0.3919 0.083 Uiso 0.5 1 calc R U P A -1
C1S C 0.4849(8) 0.1285(9) 0.8893(19) 0.097(5) Uani 0.5 1 d D U P B -1
H1S1 H 0.4502 0.1655 0.8410 0.145 Uiso 0.5 1 calc R U P B -1
H1S2 H 0.4698 0.1293 0.9858 0.145 Uiso 0.5 1 calc R U P B -1
H1S3 H 0.5467 0.1401 0.8785 0.145 Uiso 0.5 1 calc R U P B -1
C2S C 0.4667(9) 0.0530(9) 0.8321(18) 0.108(5) Uani 0.5 1 d D U P B -1
H2S1 H 0.4037 0.0436 0.8408 0.130 Uiso 0.5 1 calc R U P B -1
H2S2 H 0.4802 0.0543 0.7340 0.130 Uiso 0.5 1 calc R U P B -1
C3S C 0.5135(6) -0.0115(7) 0.8922(9) 0.084(3) Uani 0.5 1 d D U P B -1
H3S1 H 0.4975 -0.0149 0.9892 0.101 Uiso 0.5 1 calc R U P B -1
H3S2 H 0.5766 -0.0012 0.8879 0.101 Uiso 0.5 1 calc R U P B -1
C4S C 0.4971(10) -0.0866(8) 0.8269(13) 0.090(3) Uani 0.5 1 d D U P B -1
H4S1 H 0.4340 -0.0969 0.8310 0.109 Uiso 0.5 1 calc R U P B -1
H4S2 H 0.5133 -0.0834 0.7299 0.109 Uiso 0.5 1 calc R U P B -1
C5S C 0.5445(9) -0.1509(9) 0.8887(19) 0.098(5) Uani 0.5 1 d D U P B -1
H5S1 H 0.5295 -0.1964 0.8397 0.148 Uiso 0.5 1 calc R U P B -1
H5S2 H 0.6072 -0.1424 0.8827 0.148 Uiso 0.5 1 calc R U P B -1
H5S3 H 0.5277 -0.1560 0.9841 0.148 Uiso 0.5 1 calc R U P B -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O3 1.840(10) . ?
W1 O1 1.849(11) . ?
W1 C1 1.863(4) . ?
W1 O4 1.944(10) . ?
W1 O2 1.977(12) . ?
C1 H1A 0.9300 . ?
C1 H1B 0.9300 . ?
W2 C2 1.848(16) . ?
W2 O2 1.849(14) . ?
W2 O4 1.872(14) . ?
W2 O1 2.000(13) . ?
W2 O3 2.003(13) . ?
C2 H2A 0.9300 . ?
C2 H2B 0.9300 . ?
O1 C11 1.442(19) . ?
C11 C16 1.393(12) . ?
C11 C12 1.402(12) . ?
C12 C13 1.409(10) . ?
C12 C121 1.498(12) . ?
C13 C14 1.369(12) . ?
C13 H13 0.9300 . ?
C14 C15 1.369(11) . ?
C14 H14 0.9300 . ?
C15 C16 1.382(10) . ?
C15 H15 0.9300 . ?
C16 C161 1.497(11) . ?
C121 C122 1.526(12) . ?
C121 C123 1.529(11) . ?
C121 H121 0.9800 . ?
C122 H12A 0.9600 . ?
C122 H12B 0.9600 . ?
C122 H12C 0.9600 . ?
C123 H12D 0.9600 . ?
C123 H12E 0.9600 . ?
C123 H12F 0.9600 . ?
C161 C163 1.544(10) . ?
C161 C162 1.546(11) . ?
C161 H161 0.9800 . ?
C162 H16A 0.9600 . ?
C162 H16B 0.9600 . ?
C162 H16C 0.9600 . ?
C163 H16D 0.9600 . ?
C163 H16E 0.9600 . ?
C163 H16F 0.9600 . ?
O2 C21 1.33(2) . ?
C21 C22 1.385(13) . ?
C21 C26 1.399(13) . ?
C22 C23 1.404(13) . ?
C22 C221 1.490(12) . ?
C23 C24 1.369(11) . ?
C23 H23 0.9300 . ?
C24 C25 1.372(12) . ?
C24 H24 0.9300 . ?
C25 C26 1.383(11) . ?
C25 H25 0.9300 . ?
C26 C261 1.499(11) . ?
C221 C223 1.524(14) . ?
C221 C222 1.541(14) . ?
C221 H221 0.9800 . ?
C222 H22A 0.9600 . ?
C222 H22B 0.9600 . ?
C222 H22C 0.9600 . ?
C223 H22D 0.9600 . ?
C223 H22E 0.9600 . ?
C223 H22F 0.9600 . ?
C261 C263 1.520(11) . ?
C261 C262 1.529(11) . ?
C261 H261 0.9800 . ?
C262 H26A 0.9600 . ?
C262 H26B 0.9600 . ?
C262 H26C 0.9600 . ?
C263 H26D 0.9600 . ?
C263 H26E 0.9600 . ?
C263 H26F 0.9600 . ?
O3 C31 1.33(2) . ?
C31 C32 1.397(12) . ?
C31 C36 1.399(12) . ?
C32 C33 1.385(11) . ?
C32 C321 1.506(11) . ?
C33 C34 1.377(11) . ?
C33 H33 0.9300 . ?
C34 C35 1.368(9) . ?
C34 H34 0.9300 . ?
C35 C36 1.393(10) . ?
C35 H35 0.9300 . ?
C36 C361 1.508(11) . ?
C321 C323 1.541(13) . ?
C321 C322 1.550(13) . ?
C321 H321 0.9800 . ?
C322 H32A 0.9600 . ?
C322 H32B 0.9600 . ?
C322 H32C 0.9600 . ?
C323 H32D 0.9600 . ?
C323 H32E 0.9600 . ?
C323 H32F 0.9600 . ?
C361 C362 1.519(11) . ?
C361 C363 1.555(10) . ?
C361 H361 0.9800 . ?
C362 H36A 0.9600 . ?
C362 H36B 0.9600 . ?
C362 H36C 0.9600 . ?
C363 H36D 0.9600 . ?
C363 H36E 0.9600 . ?
C363 H36F 0.9600 . ?
O4 C41 1.41(2) . ?
C41 C42 1.399(13) . ?
C41 C46 1.407(13) . ?
C42 C43 1.389(11) . ?
C42 C421 1.509(11) . ?
C43 C44 1.365(10) . ?
C43 H43 0.9300 . ?
C44 C45 1.382(10) . ?
C44 H44 0.9300 . ?
C45 C46 1.396(11) . ?
C45 H45 0.9300 . ?
C46 C461 1.510(11) . ?
C421 C422 1.525(12) . ?
C421 C423 1.545(12) . ?
C421 H421 0.9800 . ?
C422 H42A 0.9600 . ?
C422 H42B 0.9600 . ?
C422 H42C 0.9600 . ?
C423 H42D 0.9600 . ?
C423 H42E 0.9600 . ?
C423 H42F 0.9600 . ?
C461 C462 1.532(12) . ?
C461 C463 1.532(11) . ?
C461 H461 0.9800 . ?
C462 H46A 0.9600 . ?
C462 H46B 0.9600 . ?
C462 H46C 0.9600 . ?
C463 H46D 0.9600 . ?
C463 H46E 0.9600 . ?
C463 H46F 0.9600 . ?
C1S C2S 1.473(15) . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9600 . ?
C1S H1S3 0.9600 . ?
C2S C3S 1.461(16) . ?
C2S H2S1 0.9700 . ?
C2S H2S2 0.9700 . ?
C3S C4S 1.492(14) . ?
C3S H3S1 0.9700 . ?
C3S H3S2 0.9700 . ?
C4S C5S 1.472(15) . ?
C4S H4S1 0.9700 . ?
C4S H4S2 0.9700 . ?
C5S H5S1 0.9600 . ?
C5S H5S2 0.9600 . ?
C5S H5S3 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
O3 W1 O1 166.7(9) . . ?
O3 W1 O4 99.2(7) . . ?
O1 W1 O4 86.3(8) . . ?
O3 W1 O2 89.7(8) . . ?
O1 W1 O2 78.2(7) . . ?
O4 W1 O2 137.8(2) . . ?
W1 C1 H1A 120.0 . . ?
W1 C1 H1B 120.0 . . ?
H1A C1 H1B 120.0 . . ?
O2 W2 O4 158.9(8) . . ?
O2 W2 O1 77.6(9) . . ?
O4 W2 O1 84.1(10) . . ?
O2 W2 O3 88.7(10) . . ?
O4 W2 O3 96.0(9) . . ?
O1 W2 O3 132.5(3) . . ?
W2 C2 H2A 120.0 . . ?
W2 C2 H2B 120.0 . . ?
H2A C2 H2B 120.0 . . ?
C16 C11 C12 123.6(11) . . ?
C16 C11 O1 121.2(13) . . ?
C12 C11 O1 115.3(13) . . ?
C11 C12 C13 116.5(9) . . ?
C11 C12 C121 123.2(9) . . ?
C13 C12 C121 120.3(9) . . ?
C14 C13 C12 120.0(8) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C15 C14 C13 122.0(8) . . ?
C15 C14 H14 119.0 . . ?
C13 C14 H14 119.0 . . ?
C14 C15 C16 120.8(8) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 H15 119.6 . . ?
C15 C16 C11 117.2(9) . . ?
C15 C16 C161 122.0(8) . . ?
C11 C16 C161 120.8(8) . . ?
C12 C121 C122 112.0(10) . . ?
C12 C121 C123 115.8(9) . . ?
C122 C121 C123 110.3(9) . . ?
C12 C121 H121 106.0 . . ?
C122 C121 H121 106.0 . . ?
C123 C121 H121 106.0 . . ?
C121 C122 H12A 109.5 . . ?
C121 C122 H12B 109.5 . . ?
H12A C122 H12B 109.5 . . ?
C121 C122 H12C 109.5 . . ?
H12A C122 H12C 109.5 . . ?
H12B C122 H12C 109.5 . . ?
C121 C123 H12D 109.5 . . ?
C121 C123 H12E 109.5 . . ?
H12D C123 H12E 109.5 . . ?
C121 C123 H12F 109.5 . . ?
H12D C123 H12F 109.5 . . ?
H12E C123 H12F 109.5 . . ?
C16 C161 C163 116.2(8) . . ?
C16 C161 C162 112.7(9) . . ?
C163 C161 C162 103.2(8) . . ?
C16 C161 H161 108.2 . . ?
C163 C161 H161 108.2 . . ?
C162 C161 H161 108.2 . . ?
C161 C162 H16A 109.5 . . ?
C161 C162 H16B 109.5 . . ?
H16A C162 H16B 109.5 . . ?
C161 C162 H16C 109.5 . . ?
H16A C162 H16C 109.5 . . ?
H16B C162 H16C 109.5 . . ?
C161 C163 H16D 109.5 . . ?
C161 C163 H16E 109.5 . . ?
H16D C163 H16E 109.5 . . ?
C161 C163 H16F 109.5 . . ?
H16D C163 H16F 109.5 . . ?
H16E C163 H16F 109.5 . . ?
O2 C21 C22 124.9(15) . . ?
O2 C21 C26 113.9(14) . . ?
C22 C21 C26 121.2(12) . . ?
C21 C22 C23 119.1(11) . . ?
C21 C22 C221 120.8(13) . . ?
C23 C22 C221 120.1(11) . . ?
C24 C23 C22 120.0(10) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C25 119.9(9) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C24 C25 C26 122.2(10) . . ?
C24 C25 H25 118.9 . . ?
C26 C25 H25 118.9 . . ?
C25 C26 C21 117.5(11) . . ?
C25 C26 C261 123.6(9) . . ?
C21 C26 C261 118.8(10) . . ?
C22 C221 C223 111.7(13) . . ?
C22 C221 C222 114.4(12) . . ?
C223 C221 C222 110.2(13) . . ?
C22 C221 H221 106.7 . . ?
C223 C221 H221 106.7 . . ?
C222 C221 H221 106.7 . . ?
C221 C222 H22A 109.5 . . ?
C221 C222 H22B 109.5 . . ?
H22A C222 H22B 109.5 . . ?
C221 C222 H22C 109.5 . . ?
H22A C222 H22C 109.5 . . ?
H22B C222 H22C 109.5 . . ?
C221 C223 H22D 109.5 . . ?
C221 C223 H22E 109.5 . . ?
H22D C223 H22E 109.5 . . ?
C221 C223 H22F 109.5 . . ?
H22D C223 H22F 109.5 . . ?
H22E C223 H22F 109.5 . . ?
C26 C261 C263 113.5(9) . . ?
C26 C261 C262 110.1(10) . . ?
C263 C261 C262 110.6(9) . . ?
C26 C261 H261 107.5 . . ?
C263 C261 H261 107.5 . . ?
C262 C261 H261 107.5 . . ?
C261 C262 H26A 109.5 . . ?
C261 C262 H26B 109.5 . . ?
H26A C262 H26B 109.5 . . ?
C261 C262 H26C 109.5 . . ?
H26A C262 H26C 109.5 . . ?
H26B C262 H26C 109.5 . . ?
C261 C263 H26D 109.5 . . ?
C261 C263 H26E 109.5 . . ?
H26D C263 H26E 109.5 . . ?
C261 C263 H26F 109.5 . . ?
H26D C263 H26F 109.5 . . ?
H26E C263 H26F 109.5 . . ?
O3 C31 C32 121.4(14) . . ?
O3 C31 C36 116.0(14) . . ?
C32 C31 C36 122.6(11) . . ?
C33 C32 C31 116.1(9) . . ?
C33 C32 C321 122.5(9) . . ?
C31 C32 C321 121.0(10) . . ?
C34 C33 C32 122.5(7) . . ?
C34 C33 H33 118.8 . . ?
C32 C33 H33 118.8 . . ?
C35 C34 C33 120.4(7) . . ?
C35 C34 H34 119.8 . . ?
C33 C34 H34 119.8 . . ?
C34 C35 C36 120.1(7) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C35 C36 C31 118.3(8) . . ?
C35 C36 C361 120.0(9) . . ?
C31 C36 C361 121.5(10) . . ?
C32 C321 C323 112.6(9) . . ?
C32 C321 C322 109.2(10) . . ?
C323 C321 C322 110.1(11) . . ?
C32 C321 H321 108.2 . . ?
C323 C321 H321 108.2 . . ?
C322 C321 H321 108.2 . . ?
C321 C322 H32A 109.5 . . ?
C321 C322 H32B 109.5 . . ?
H32A C322 H32B 109.5 . . ?
C321 C322 H32C 109.5 . . ?
H32A C322 H32C 109.5 . . ?
H32B C322 H32C 109.5 . . ?
C321 C323 H32D 109.5 . . ?
C321 C323 H32E 109.5 . . ?
H32D C323 H32E 109.5 . . ?
C321 C323 H32F 109.5 . . ?
H32D C323 H32F 109.5 . . ?
H32E C323 H32F 109.5 . . ?
C36 C361 C362 112.7(10) . . ?
C36 C361 C363 111.9(7) . . ?
C362 C361 C363 105.6(8) . . ?
C36 C361 H361 108.9 . . ?
C362 C361 H361 108.9 . . ?
C363 C361 H361 108.9 . . ?
C361 C362 H36A 109.5 . . ?
C361 C362 H36B 109.5 . . ?
H36A C362 H36B 109.5 . . ?
C361 C362 H36C 109.5 . . ?
H36A C362 H36C 109.5 . . ?
H36B C362 H36C 109.5 . . ?
C361 C363 H36D 109.5 . . ?
C361 C363 H36E 109.5 . . ?
H36D C363 H36E 109.5 . . ?
C361 C363 H36F 109.5 . . ?
H36D C363 H36F 109.5 . . ?
H36E C363 H36F 109.5 . . ?
C42 C41 C46 122.9(12) . . ?
C42 C41 O4 115.3(13) . . ?
C46 C41 O4 121.5(13) . . ?
C43 C42 C41 116.5(10) . . ?
C43 C42 C421 120.9(9) . . ?
C41 C42 C421 122.3(11) . . ?
C44 C43 C42 121.7(9) . . ?
C44 C43 H43 119.1 . . ?
C42 C43 H43 119.1 . . ?
C43 C44 C45 121.5(9) . . ?
C43 C44 H44 119.3 . . ?
C45 C44 H44 119.3 . . ?
C44 C45 C46 119.5(9) . . ?
C44 C45 H45 120.2 . . ?
C46 C45 H45 120.2 . . ?
C45 C46 C41 117.8(10) . . ?
C45 C46 C461 121.2(10) . . ?
C41 C46 C461 121.0(11) . . ?
C42 C421 C422 110.3(10) . . ?
C42 C421 C423 108.6(11) . . ?
C422 C421 C423 110.7(9) . . ?
C42 C421 H421 109.0 . . ?
C422 C421 H421 109.0 . . ?
C423 C421 H421 109.0 . . ?
C421 C422 H42A 109.5 . . ?
C421 C422 H42B 109.5 . . ?
H42A C422 H42B 109.5 . . ?
C421 C422 H42C 109.5 . . ?
H42A C422 H42C 109.5 . . ?
H42B C422 H42C 109.5 . . ?
C421 C423 H42D 109.5 . . ?
C421 C423 H42E 109.5 . . ?
H42D C423 H42E 109.5 . . ?
C421 C423 H42F 109.5 . . ?
H42D C423 H42F 109.5 . . ?
H42E C423 H42F 109.5 . . ?
C46 C461 C462 110.9(10) . . ?
C46 C461 C463 115.4(8) . . ?
C462 C461 C463 110.3(10) . . ?
C46 C461 H461 106.5 . . ?
C462 C461 H461 106.5 . . ?
C463 C461 H461 106.5 . . ?
C461 C462 H46A 109.5 . . ?
C461 C462 H46B 109.5 . . ?
H46A C462 H46B 109.5 . . ?
C461 C462 H46C 109.5 . . ?
H46A C462 H46C 109.5 . . ?
H46B C462 H46C 109.5 . . ?
C461 C463 H46D 109.5 . . ?
C461 C463 H46E 109.5 . . ?
H46D C463 H46E 109.5 . . ?
C461 C463 H46F 109.5 . . ?
H46D C463 H46F 109.5 . . ?
H46E C463 H46F 109.5 . . ?
C2S C1S H1S1 109.5 . . ?
C2S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
C2S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
C3S C2S C1S 118.0(12) . . ?
C3S C2S H2S1 107.8 . . ?
C1S C2S H2S1 107.8 . . ?
C3S C2S H2S2 107.8 . . ?
C1S C2S H2S2 107.8 . . ?
H2S1 C2S H2S2 107.2 . . ?
C2S C3S C4S 116.5(10) . . ?
C2S C3S H3S1 108.2 . . ?
C4S C3S H3S1 108.2 . . ?
C2S C3S H3S2 108.2 . . ?
C4S C3S H3S2 108.2 . . ?
H3S1 C3S H3S2 107.3 . . ?
C5S C4S C3S 115.9(11) . . ?
C5S C4S H4S1 108.3 . . ?
C3S C4S H4S1 108.3 . . ?
C5S C4S H4S2 108.3 . . ?
C3S C4S H4S2 108.3 . . ?
H4S1 C4S H4S2 107.4 . . ?
C4S C5S H5S1 109.5 . . ?
C4S C5S H5S2 109.5 . . ?
H5S1 C5S H5S2 109.5 . . ?
C4S C5S H5S3 109.5 . . ?
H5S1 C5S H5S3 109.5 . . ?
H5S2 C5S H5S3 109.5 . . ?

_refine_diff_density_max         0.686
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.058


# start Validation Reply Form 
_vrf_PLAT308_X8_17012            
; 
PROBLEM: Single Bonded Metal Atom in Structure  (Unusual)         W1 Check 
RESPONSE: These atoms are actually connected to the oxygen atoms of each 
of the four aryloxide ligands. They were solved in part -1, and seem to 
present connectivity issues for CheckCIF. In the .RES file, appropriate 
"BIND" commands have been used to connect each tungsten to the oxygen atoms. 
;
_vrf_PLAT220_X8_17012            
; 
PROBLEM: Non-Solvent Resd 1   C   Ueq(max)/Ueq(min) Range        8.2 Ratio 
RESPONSE: The data are not of high quality, and the size of the thermal 
ellipsoids do vary. They are particularly large for the isopropyl groups 
and the pentane of crystallization, which may suffer from some thermal 
motion. Further disorder to try to decrease the ellipsoid sizes has not 
modeled due to the relatively poor data quality. 
;
# end Validation Reply Form 
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_X8_16249
_database_code_depnum_ccdc_archive 'CCDC 1580351'
_audit_update_record             
;
2017-10-16 deposited with the CCDC.
2017-12-21 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            'C68 H87 O4 P W'
_chemical_formula_weight         1183.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   13.4644(6)
_cell_length_b                   13.7709(6)
_cell_length_c                   18.7517(8)
_cell_angle_alpha                106.468(2)
_cell_angle_beta                 110.976(2)
_cell_angle_gamma                96.554(2)
_cell_volume                     3021.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9450
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      33.34

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_F_000             1232
_exptl_transmission_factor_min   0.4774
_exptl_transmission_factor_max   0.5681
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.079
_exptl_absorpt_coefficient_mu    1.984
_shelx_estimated_absorpt_T_min   0.672
_shelx_estimated_absorpt_T_max   0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   
'I\mS micro-focus sealed tube, multilayer optics'
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            344550
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.241
_diffrn_reflns_theta_max         37.166
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             30460
_reflns_number_gt                26858
_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       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_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          
; 
 Bruker X8 Kappa DUO four-circle diffractometer, Bruker APEX2 CCD. 
 The instrument was purchased with the help of funding from the 
 National Science Foundation (NSF) under Grant Number 
 CHE-0946721.  Please acknowledge this grant in all publications 
 of this structure. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0309P)²+1.2009P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         30460
_refine_ls_number_parameters     709
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0257
_refine_ls_wR_factor_ref         0.0616
_refine_ls_wR_factor_gt          0.0588
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.006
_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 0.48083(2) 0.53184(2) 0.75365(2) 0.01247(1) Uani 1 1 d . . . . .
C1 C 0.45565(11) 0.48369(10) 0.65033(8) 0.0173(2) Uani 1 1 d D . . . .
H1 H 0.4449(16) 0.4588(15) 0.5969(9) 0.021(5) Uiso 1 1 d D . . . .
O1 O 0.37968(7) 0.62564(7) 0.75868(6) 0.01543(15) Uani 1 1 d . . . . .
C11 C 0.27118(10) 0.61188(9) 0.71506(7) 0.01459(19) Uani 1 1 d . . . . .
C12 C 0.23144(11) 0.61917(10) 0.63615(8) 0.0170(2) Uani 1 1 d . . . . .
C13 C 0.11872(11) 0.60089(11) 0.59301(8) 0.0205(2) Uani 1 1 d . . . . .
H13 H 0.0913 0.6032 0.5394 0.025 Uiso 1 1 calc R U . . .
C14 C 0.04510(11) 0.57937(12) 0.62606(9) 0.0223(2) Uani 1 1 d . . . . .
H14 H -0.0316 0.5653 0.5950 0.027 Uiso 1 1 calc R U . . .
C15 C 0.08521(11) 0.57873(11) 0.70513(9) 0.0206(2) Uani 1 1 d . . . . .
H15 H 0.0353 0.5669 0.7287 0.025 Uiso 1 1 calc R U . . .
C16 C 0.19753(10) 0.59509(10) 0.75082(8) 0.0161(2) Uani 1 1 d . . . . .
C17 C 0.23842(11) 0.59811(11) 0.83805(8) 0.0189(2) Uani 1 1 d . . . . .
H17 H 0.3202 0.6117 0.8608 0.023 Uiso 1 1 calc R U . . .
C171 C 0.20734(14) 0.68700(13) 0.89016(9) 0.0262(3) Uani 1 1 d . . . . .
H17A H 0.1274 0.6751 0.8688 0.039 Uiso 1 1 calc R U . . .
H17B H 0.2387 0.7536 0.8883 0.039 Uiso 1 1 calc R U . . .
H17C H 0.2361 0.6890 0.9467 0.039 Uiso 1 1 calc R U . . .
C172 C 0.19366(13) 0.49452(13) 0.84307(10) 0.0258(3) Uani 1 1 d . . . . .
H17D H 0.1137 0.4813 0.8234 0.039 Uiso 1 1 calc R U . . .
H17E H 0.2254 0.4976 0.8998 0.039 Uiso 1 1 calc R U . . .
H17F H 0.2130 0.4381 0.8092 0.039 Uiso 1 1 calc R U . . .
C18 C 0.30961(12) 0.65380(12) 0.60192(9) 0.0214(2) Uani 1 1 d . . . . .
H18 H 0.3803 0.6359 0.6286 0.026 Uiso 1 1 calc R U . . .
C181 C 0.26910(17) 0.59997(19) 0.51019(11) 0.0425(5) Uani 1 1 d . . . . .
H18A H 0.2506 0.5242 0.4966 0.064 Uiso 1 1 calc R U . . .
H18B H 0.3267 0.6191 0.4928 0.064 Uiso 1 1 calc R U . . .
H18C H 0.2039 0.6220 0.4821 0.064 Uiso 1 1 calc R U . . .
C182 C 0.33275(17) 0.77228(15) 0.62423(14) 0.0382(4) Uani 1 1 d . . . . .
H18D H 0.2640 0.7924 0.6013 0.057 Uiso 1 1 calc R U . . .
H18E H 0.3834 0.7944 0.6020 0.057 Uiso 1 1 calc R U . . .
H18F H 0.3657 0.8059 0.6837 0.057 Uiso 1 1 calc R U . . .
O2 O 0.37907(8) 0.43408(7) 0.76936(6) 0.01726(16) Uani 1 1 d . . . . .
C21 C 0.33970(10) 0.33051(10) 0.74684(8) 0.0164(2) Uani 1 1 d . . . . .
C22 C 0.26098(11) 0.27107(10) 0.66726(8) 0.0173(2) Uani 1 1 d . . . . .
C23 C 0.22500(12) 0.16378(11) 0.64797(9) 0.0225(2) Uani 1 1 d . . . . .
H23 H 0.1730 0.1227 0.5944 0.027 Uiso 1 1 calc R U . . .
C24 C 0.26330(13) 0.11558(12) 0.70497(10) 0.0258(3) Uani 1 1 d . . . . .
H24 H 0.2395 0.0423 0.6902 0.031 Uiso 1 1 calc R U . . .
C25 C 0.33686(13) 0.17624(13) 0.78380(11) 0.0269(3) Uani 1 1 d . . . . .
H25 H 0.3616 0.1438 0.8233 0.032 Uiso 1 1 calc R U . . .
C26 C 0.37541(12) 0.28368(12) 0.80655(9) 0.0235(3) Uani 1 1 d . . . . .
C27 C 0.45251(14) 0.35022(15) 0.89445(10) 0.0345(4) Uani 1 1 d . . . . .
H27 H 0.4657 0.4244 0.8971 0.041 Uiso 1 1 calc R U . . .
C271 C 0.40018(18) 0.34429(18) 0.95383(12) 0.0430(5) Uani 1 1 d . . . . .
H27A H 0.3879 0.2729 0.9541 0.065 Uiso 1 1 calc R U . . .
H27B H 0.3300 0.3640 0.9366 0.065 Uiso 1 1 calc R U . . .
H27C H 0.4492 0.3922 1.0088 0.065 Uiso 1 1 calc R U . . .
C272 C 0.56186(18) 0.3242(3) 0.92080(15) 0.0591(7) Uani 1 1 d . . . . .
H27D H 0.5522 0.2516 0.9187 0.089 Uiso 1 1 calc R U . . .
H27E H 0.6088 0.3706 0.9767 0.089 Uiso 1 1 calc R U . . .
H27F H 0.5963 0.3332 0.8843 0.089 Uiso 1 1 calc R U . . .
C28 C 0.21426(11) 0.32168(11) 0.60444(8) 0.0195(2) Uani 1 1 d . . . . .
H28 H 0.2535 0.3971 0.6291 0.023 Uiso 1 1 calc R U . . .
C281 C 0.23299(14) 0.27393(14) 0.52758(9) 0.0300(3) Uani 1 1 d . . . . .
H28A H 0.3119 0.2845 0.5417 0.045 Uiso 1 1 calc R U . . .
H28B H 0.2008 0.3076 0.4882 0.045 Uiso 1 1 calc R U . . .
H28C H 0.1984 0.1990 0.5036 0.045 Uiso 1 1 calc R U . . .
C282 C 0.09212(13) 0.31549(14) 0.58224(10) 0.0275(3) Uani 1 1 d . . . . .
H28D H 0.0507 0.2426 0.5531 0.041 Uiso 1 1 calc R U . . .
H28E H 0.0669 0.3566 0.5473 0.041 Uiso 1 1 calc R U . . .
H28F H 0.0805 0.3433 0.6321 0.041 Uiso 1 1 calc R U . . .
O3 O 0.59757(8) 0.46547(8) 0.80244(6) 0.01825(17) Uani 1 1 d . . . . .
C31 C 0.68271(10) 0.44485(10) 0.78314(8) 0.0173(2) Uani 1 1 d . . . . .
C32 C 0.66713(11) 0.35779(11) 0.71510(9) 0.0195(2) Uani 1 1 d . . . . .
C33 C 0.75673(12) 0.34305(12) 0.69587(10) 0.0245(3) Uani 1 1 d . . . . .
H33 H 0.7471 0.2858 0.6495 0.029 Uiso 1 1 calc R U . . .
C34 C 0.85958(12) 0.41055(13) 0.74330(11) 0.0270(3) Uani 1 1 d . . . . .
H34 H 0.9191 0.4007 0.7284 0.032 Uiso 1 1 calc R U . . .
C35 C 0.87503(12) 0.49224(13) 0.81245(10) 0.0259(3) Uani 1 1 d . . . . .
H35 H 0.9462 0.5365 0.8458 0.031 Uiso 1 1 calc R U . . .
C36 C 0.78820(11) 0.51089(12) 0.83408(9) 0.0214(2) Uani 1 1 d . . . . .
C37 C 0.80738(12) 0.59659(13) 0.91285(10) 0.0263(3) Uani 1 1 d D U . . .
H37 H 0.7339 0.6013 0.9130 0.032 Uiso 1 1 calc R U . A 1
C371 C 0.8709(3) 0.5655(2) 0.98649(14) 0.0373(7) Uani 0.820(8) 1 d D U P B 1
H37A H 0.9438 0.5609 0.9885 0.056 Uiso 0.820(8) 1 calc R U P B 1
H37B H 0.8308 0.4977 0.9807 0.056 Uiso 0.820(8) 1 calc R U P B 1
H37C H 0.8782 0.6183 1.0369 0.056 Uiso 0.820(8) 1 calc R U P B 1
C372 C 0.8653(2) 0.70401(17) 0.92336(15) 0.0318(5) Uani 0.820(8) 1 d D U P B 1
H37D H 0.9377 0.7021 0.9231 0.048 Uiso 0.820(8) 1 calc R U P B 1
H37E H 0.8737 0.7542 0.9753 0.048 Uiso 0.820(8) 1 calc R U P B 1
H37F H 0.8218 0.7252 0.8785 0.048 Uiso 0.820(8) 1 calc R U P B 1
C373 C 0.8093(12) 0.5464(10) 0.9710(7) 0.039(3) Uani 0.180(8) 1 d D U P B 2
H37G H 0.8672 0.5082 0.9780 0.058 Uiso 0.180(8) 1 calc R U P B 2
H37H H 0.7383 0.4977 0.9512 0.058 Uiso 0.180(8) 1 calc R U P B 2
H37I H 0.8237 0.5993 1.0235 0.058 Uiso 0.180(8) 1 calc R U P B 2
C374 C 0.9124(10) 0.6794(11) 0.9358(7) 0.042(4) Uani 0.180(8) 1 d D . P B 2
H37J H 0.9136 0.7452 0.9743 0.064 Uiso 0.180(8) 1 calc R U P B 2
H37K H 0.9130 0.6904 0.8865 0.064 Uiso 0.180(8) 1 calc R U P B 2
H37L H 0.9772 0.6549 0.9612 0.064 Uiso 0.180(8) 1 calc R U P B 2
C38 C 0.55754(12) 0.27919(11) 0.66583(10) 0.0237(3) Uani 1 1 d . . . . .
H38 H 0.5001 0.3143 0.6754 0.028 Uiso 1 1 calc R U . . .
C381 C 0.52817(14) 0.24167(14) 0.57442(11) 0.0332(4) Uani 1 1 d . . . . .
H38A H 0.5334 0.3020 0.5570 0.050 Uiso 1 1 calc R U . . .
H38B H 0.4532 0.1980 0.5450 0.050 Uiso 1 1 calc R U . . .
H38C H 0.5791 0.2009 0.5626 0.050 Uiso 1 1 calc R U . . .
C382 C 0.55597(15) 0.18676(14) 0.69582(13) 0.0350(4) Uani 1 1 d . . . . .
H38D H 0.6126 0.1515 0.6881 0.052 Uiso 1 1 calc R U . . .
H38E H 0.4839 0.1376 0.6647 0.052 Uiso 1 1 calc R U . . .
H38F H 0.5704 0.2120 0.7538 0.052 Uiso 1 1 calc R U . . .
O4 O 0.59597(7) 0.66199(7) 0.80195(5) 0.01510(15) Uani 1 1 d . . . . .
C41 C 0.60523(10) 0.74959(10) 0.78281(8) 0.0164(2) Uani 1 1 d . . . . .
C42 C 0.64253(11) 0.75411(11) 0.72224(8) 0.0198(2) Uani 1 1 d . . . . .
C43 C 0.64652(14) 0.84552(13) 0.70353(10) 0.0284(3) Uani 1 1 d . . . . .
H43 H 0.6696 0.8493 0.6619 0.034 Uiso 1 1 calc R U . . .
C44 C 0.61751(16) 0.93075(13) 0.74438(12) 0.0329(3) Uani 1 1 d . . . . .
H44 H 0.6191 0.9915 0.7299 0.039 Uiso 1 1 calc R U . . .
C45 C 0.58615(14) 0.92664(12) 0.80655(11) 0.0280(3) Uani 1 1 d . . . . .
H45 H 0.5682 0.9858 0.8354 0.034 Uiso 1 1 calc R U . . .
C46 C 0.58043(11) 0.83752(10) 0.82741(9) 0.0199(2) Uani 1 1 d . . . . .
C47 C 0.55234(12) 0.83583(11) 0.89850(9) 0.0217(2) Uani 1 1 d . . . . .
H47 H 0.5377 0.7618 0.8959 0.026 Uiso 1 1 calc R U . . .
C471 C 0.65083(14) 0.89866(15) 0.97875(10) 0.0329(3) Uani 1 1 d . . . . .
H47A H 0.7145 0.8697 0.9804 0.049 Uiso 1 1 calc R U . . .
H47B H 0.6336 0.8950 1.0246 0.049 Uiso 1 1 calc R U . . .
H47C H 0.6675 0.9716 0.9826 0.049 Uiso 1 1 calc R U . . .
C472 C 0.45076(14) 0.87557(15) 0.89620(11) 0.0338(4) Uani 1 1 d . . . . .
H47D H 0.4641 0.9491 0.9010 0.051 Uiso 1 1 calc R U . . .
H47E H 0.4342 0.8688 0.9416 0.051 Uiso 1 1 calc R U . . .
H47F H 0.3886 0.8345 0.8445 0.051 Uiso 1 1 calc R U . . .
C48 C 0.67788(12) 0.66336(12) 0.67815(9) 0.0227(2) Uani 1 1 d . . . . .
H48 H 0.6658 0.6049 0.6981 0.027 Uiso 1 1 calc R U . . .
C481 C 0.60859(14) 0.62488(15) 0.58615(10) 0.0305(3) Uani 1 1 d . . . . .
H48A H 0.5308 0.6064 0.5754 0.046 Uiso 1 1 calc R U . . .
H48B H 0.6292 0.5634 0.5592 0.046 Uiso 1 1 calc R U . . .
H48C H 0.6214 0.6802 0.5649 0.046 Uiso 1 1 calc R U . . .
C482 C 0.79981(14) 0.69302(16) 0.69615(11) 0.0337(4) Uani 1 1 d . . . . .
H48D H 0.8134 0.7502 0.6769 0.051 Uiso 1 1 calc R U . . .
H48E H 0.8206 0.6325 0.6681 0.051 Uiso 1 1 calc R U . . .
H48F H 0.8434 0.7153 0.7550 0.051 Uiso 1 1 calc R U . . .
P1 P -0.02409(3) 0.11485(3) 0.75606(2) 0.01729(6) Uani 1 1 d . . . . .
C5 C 0.07559(12) 0.23416(11) 0.79015(10) 0.0247(3) Uani 1 1 d . . . . .
H5A H 0.0399 0.2924 0.7939 0.037 Uiso 1 1 calc R U . . .
H5B H 0.1093 0.2309 0.7513 0.037 Uiso 1 1 calc R U . . .
H5C H 0.1322 0.2446 0.8439 0.037 Uiso 1 1 calc R U . . .
C61 C -0.12674(11) 0.09444(10) 0.65747(8) 0.0194(2) Uani 1 1 d . . . . .
C62 C -0.09620(14) 0.11993(16) 0.60029(11) 0.0325(3) Uani 1 1 d . . . . .
H62 H -0.0222 0.1528 0.6150 0.039 Uiso 1 1 calc R U . . .
C63 C -0.17412(16) 0.09717(18) 0.52174(12) 0.0400(4) Uani 1 1 d . . . . .
H63 H -0.1535 0.1150 0.4827 0.048 Uiso 1 1 calc R U . . .
C64 C -0.28137(15) 0.04879(14) 0.50016(10) 0.0326(3) Uani 1 1 d . . . . .
H64 H -0.3345 0.0335 0.4464 0.039 Uiso 1 1 calc R U . . .
C65 C -0.31181(13) 0.02250(12) 0.55653(10) 0.0278(3) Uani 1 1 d . . . . .
H65 H -0.3857 -0.0112 0.5412 0.033 Uiso 1 1 calc R U . . .
C66 C -0.23457(12) 0.04514(11) 0.63584(9) 0.0225(2) Uani 1 1 d . . . . .
H66 H -0.2555 0.0271 0.6746 0.027 Uiso 1 1 calc R U . . .
C71 C -0.08475(12) 0.12062(11) 0.82733(8) 0.0210(2) Uani 1 1 d . . . . .
C72 C -0.12966(14) 0.20543(13) 0.84930(10) 0.0273(3) Uani 1 1 d . . . . .
H72 H -0.1285 0.2584 0.8262 0.033 Uiso 1 1 calc R U . . .
C73 C -0.17575(15) 0.21097(15) 0.90524(11) 0.0338(4) Uani 1 1 d . . . . .
H73 H -0.2065 0.2680 0.9205 0.041 Uiso 1 1 calc R U . . .
C74 C -0.17715(16) 0.13390(15) 0.93898(11) 0.0357(4) Uani 1 1 d . . . . .
H74 H -0.2081 0.1388 0.9778 0.043 Uiso 1 1 calc R U . . .
C75 C -0.13398(17) 0.04983(15) 0.91678(12) 0.0359(4) Uani 1 1 d . . . . .
H75 H -0.1358 -0.0030 0.9400 0.043 Uiso 1 1 calc R U . . .
C76 C -0.08785(14) 0.04227(13) 0.86055(11) 0.0289(3) Uani 1 1 d . . . . .
H76 H -0.0587 -0.0158 0.8448 0.035 Uiso 1 1 calc R U . . .
C81 C 0.04163(11) 0.00903(10) 0.74825(8) 0.0184(2) Uani 1 1 d . . . . .
C82 C 0.13335(12) 0.01299(12) 0.81529(9) 0.0238(3) Uani 1 1 d . . . . .
H82 H 0.1600 0.0709 0.8648 0.029 Uiso 1 1 calc R U . . .
C83 C 0.18528(13) -0.06822(12) 0.80916(10) 0.0268(3) Uani 1 1 d . . . . .
H83 H 0.2474 -0.0663 0.8548 0.032 Uiso 1 1 calc R U . . .
C84 C 0.14705(13) -0.15219(12) 0.73680(10) 0.0275(3) Uani 1 1 d . . . . .
H84 H 0.1833 -0.2075 0.7330 0.033 Uiso 1 1 calc R U . . .
C85 C 0.05624(14) -0.15592(12) 0.66994(10) 0.0290(3) Uani 1 1 d . . . . .
H85 H 0.0307 -0.2135 0.6203 0.035 Uiso 1 1 calc R U . . .
C86 C 0.00265(12) -0.07554(11) 0.67545(9) 0.0242(3) Uani 1 1 d . . . . .
H86 H -0.0601 -0.0782 0.6299 0.029 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 C1 1.7487(13) . ?
W1 O2 1.9670(9) . ?
W1 O4 1.9688(9) . ?
W1 O3 1.9787(9) . ?
W1 O1 1.9892(9) . ?
C1 H1 0.913(14) . ?
O1 C11 1.3538(15) . ?
C11 C16 1.4135(18) . ?
C11 C12 1.4197(18) . ?
C12 C13 1.3927(18) . ?
C12 C18 1.513(2) . ?
C13 C14 1.390(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.387(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.3990(18) . ?
C15 H15 0.9500 . ?
C16 C17 1.5140(18) . ?
C17 C172 1.525(2) . ?
C17 C171 1.536(2) . ?
C17 H17 1.0000 . ?
C171 H17A 0.9800 . ?
C171 H17B 0.9800 . ?
C171 H17C 0.9800 . ?
C172 H17D 0.9800 . ?
C172 H17E 0.9800 . ?
C172 H17F 0.9800 . ?
C18 C181 1.523(2) . ?
C18 C182 1.529(2) . ?
C18 H18 1.0000 . ?
C181 H18A 0.9800 . ?
C181 H18B 0.9800 . ?
C181 H18C 0.9800 . ?
C182 H18D 0.9800 . ?
C182 H18E 0.9800 . ?
C182 H18F 0.9800 . ?
O2 C21 1.3488(16) . ?
C21 C26 1.4125(19) . ?
C21 C22 1.4133(18) . ?
C22 C23 1.3987(19) . ?
C22 C28 1.5179(19) . ?
C23 C24 1.391(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.388(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.396(2) . ?
C25 H25 0.9500 . ?
C26 C27 1.528(2) . ?
C27 C272 1.497(3) . ?
C27 C271 1.531(3) . ?
C27 H27 1.0000 . ?
C271 H27A 0.9800 . ?
C271 H27B 0.9800 . ?
C271 H27C 0.9800 . ?
C272 H27D 0.9800 . ?
C272 H27E 0.9800 . ?
C272 H27F 0.9800 . ?
C28 C281 1.528(2) . ?
C28 C282 1.531(2) . ?
C28 H28 1.0000 . ?
C281 H28A 0.9800 . ?
C281 H28B 0.9800 . ?
C281 H28C 0.9800 . ?
C282 H28D 0.9800 . ?
C282 H28E 0.9800 . ?
C282 H28F 0.9800 . ?
O3 C31 1.3561(16) . ?
C31 C32 1.412(2) . ?
C31 C36 1.4135(19) . ?
C32 C33 1.397(2) . ?
C32 C38 1.515(2) . ?
C33 C34 1.389(2) . ?
C33 H33 0.9500 . ?
C34 C35 1.384(2) . ?
C34 H34 0.9500 . ?
C35 C36 1.395(2) . ?
C35 H35 0.9500 . ?
C36 C37 1.520(2) . ?
C37 C373 1.442(9) . ?
C37 C372 1.515(3) . ?
C37 C371 1.547(3) . ?
C37 C374 1.550(9) . ?
C37 H37 1.0000 . ?
C371 H37A 0.9800 . ?
C371 H37B 0.9800 . ?
C371 H37C 0.9800 . ?
C372 H37D 0.9800 . ?
C372 H37E 0.9800 . ?
C372 H37F 0.9800 . ?
C373 H37G 0.9800 . ?
C373 H37H 0.9800 . ?
C373 H37I 0.9800 . ?
C374 H37J 0.9800 . ?
C374 H37K 0.9800 . ?
C374 H37L 0.9800 . ?
C38 C381 1.526(2) . ?
C38 C382 1.531(2) . ?
C38 H38 1.0000 . ?
C381 H38A 0.9800 . ?
C381 H38B 0.9800 . ?
C381 H38C 0.9800 . ?
C382 H38D 0.9800 . ?
C382 H38E 0.9800 . ?
C382 H38F 0.9800 . ?
O4 C41 1.3575(16) . ?
C41 C42 1.4098(19) . ?
C41 C46 1.4125(19) . ?
C42 C43 1.400(2) . ?
C42 C48 1.518(2) . ?
C43 C44 1.388(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.387(2) . ?
C44 H44 0.9500 . ?
C45 C46 1.392(2) . ?
C45 H45 0.9500 . ?
C46 C47 1.516(2) . ?
C47 C472 1.521(2) . ?
C47 C471 1.531(2) . ?
C47 H47 1.0000 . ?
C471 H47A 0.9800 . ?
C471 H47B 0.9800 . ?
C471 H47C 0.9800 . ?
C472 H47D 0.9800 . ?
C472 H47E 0.9800 . ?
C472 H47F 0.9800 . ?
C48 C481 1.531(2) . ?
C48 C482 1.532(2) . ?
C48 H48 1.0000 . ?
C481 H48A 0.9800 . ?
C481 H48B 0.9800 . ?
C481 H48C 0.9800 . ?
C482 H48D 0.9800 . ?
C482 H48E 0.9800 . ?
C482 H48F 0.9800 . ?
P1 C81 1.7871(14) . ?
P1 C61 1.7874(14) . ?
P1 C71 1.7876(15) . ?
P1 C5 1.7878(15) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C61 C66 1.389(2) . ?
C61 C62 1.392(2) . ?
C62 C63 1.388(2) . ?
C62 H62 0.9500 . ?
C63 C64 1.379(3) . ?
C63 H63 0.9500 . ?
C64 C65 1.382(3) . ?
C64 H64 0.9500 . ?
C65 C66 1.395(2) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C71 C76 1.394(2) . ?
C71 C72 1.402(2) . ?
C72 C73 1.387(2) . ?
C72 H72 0.9500 . ?
C73 C74 1.383(3) . ?
C73 H73 0.9500 . ?
C74 C75 1.380(3) . ?
C74 H74 0.9500 . ?
C75 C76 1.389(2) . ?
C75 H75 0.9500 . ?
C76 H76 0.9500 . ?
C81 C86 1.3934(19) . ?
C81 C82 1.3937(19) . ?
C82 C83 1.384(2) . ?
C82 H82 0.9500 . ?
C83 C84 1.385(2) . ?
C83 H83 0.9500 . ?
C84 C85 1.386(2) . ?
C84 H84 0.9500 . ?
C85 C86 1.388(2) . ?
C85 H85 0.9500 . ?
C86 H86 0.9500 . ?

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
C1 W1 O2 106.34(5) . . ?
C1 W1 O4 105.89(5) . . ?
O2 W1 O4 147.74(4) . . ?
C1 W1 O3 102.43(5) . . ?
O2 W1 O3 87.74(4) . . ?
O4 W1 O3 86.76(4) . . ?
C1 W1 O1 103.92(5) . . ?
O2 W1 O1 86.11(4) . . ?
O4 W1 O1 84.89(4) . . ?
O3 W1 O1 153.63(4) . . ?
W1 C1 H1 178.1(12) . . ?
C11 O1 W1 132.20(8) . . ?
O1 C11 C16 118.96(11) . . ?
O1 C11 C12 121.05(11) . . ?
C16 C11 C12 119.91(11) . . ?
C13 C12 C11 118.53(12) . . ?
C13 C12 C18 120.38(12) . . ?
C11 C12 C18 120.94(11) . . ?
C14 C13 C12 121.94(13) . . ?
C14 C13 H13 119.0 . . ?
C12 C13 H13 119.0 . . ?
C15 C14 C13 119.03(12) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
C14 C15 C16 121.42(13) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 H15 119.3 . . ?
C15 C16 C11 118.96(12) . . ?
C15 C16 C17 119.82(12) . . ?
C11 C16 C17 121.20(11) . . ?
C16 C17 C172 111.59(12) . . ?
C16 C17 C171 110.57(11) . . ?
C172 C17 C171 109.92(12) . . ?
C16 C17 H17 108.2 . . ?
C172 C17 H17 108.2 . . ?
C171 C17 H17 108.2 . . ?
C17 C171 H17A 109.5 . . ?
C17 C171 H17B 109.5 . . ?
H17A C171 H17B 109.5 . . ?
C17 C171 H17C 109.5 . . ?
H17A C171 H17C 109.5 . . ?
H17B C171 H17C 109.5 . . ?
C17 C172 H17D 109.5 . . ?
C17 C172 H17E 109.5 . . ?
H17D C172 H17E 109.5 . . ?
C17 C172 H17F 109.5 . . ?
H17D C172 H17F 109.5 . . ?
H17E C172 H17F 109.5 . . ?
C12 C18 C181 113.41(13) . . ?
C12 C18 C182 109.67(13) . . ?
C181 C18 C182 110.47(15) . . ?
C12 C18 H18 107.7 . . ?
C181 C18 H18 107.7 . . ?
C182 C18 H18 107.7 . . ?
C18 C181 H18A 109.5 . . ?
C18 C181 H18B 109.5 . . ?
H18A C181 H18B 109.5 . . ?
C18 C181 H18C 109.5 . . ?
H18A C181 H18C 109.5 . . ?
H18B C181 H18C 109.5 . . ?
C18 C182 H18D 109.5 . . ?
C18 C182 H18E 109.5 . . ?
H18D C182 H18E 109.5 . . ?
C18 C182 H18F 109.5 . . ?
H18D C182 H18F 109.5 . . ?
H18E C182 H18F 109.5 . . ?
C21 O2 W1 139.72(9) . . ?
O2 C21 C26 117.91(12) . . ?
O2 C21 C22 121.38(11) . . ?
C26 C21 C22 120.63(12) . . ?
C23 C22 C21 118.19(12) . . ?
C23 C22 C28 120.39(12) . . ?
C21 C22 C28 121.41(12) . . ?
C24 C23 C22 121.83(14) . . ?
C24 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
C25 C24 C23 118.98(14) . . ?
C25 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?
C24 C25 C26 121.65(14) . . ?
C24 C25 H25 119.2 . . ?
C26 C25 H25 119.2 . . ?
C25 C26 C21 118.57(14) . . ?
C25 C26 C27 121.07(13) . . ?
C21 C26 C27 120.34(13) . . ?
C272 C27 C26 112.88(19) . . ?
C272 C27 C271 110.72(16) . . ?
C26 C27 C271 111.66(14) . . ?
C272 C27 H27 107.1 . . ?
C26 C27 H27 107.1 . . ?
C271 C27 H27 107.1 . . ?
C27 C271 H27A 109.5 . . ?
C27 C271 H27B 109.5 . . ?
H27A C271 H27B 109.5 . . ?
C27 C271 H27C 109.5 . . ?
H27A C271 H27C 109.5 . . ?
H27B C271 H27C 109.5 . . ?
C27 C272 H27D 109.5 . . ?
C27 C272 H27E 109.5 . . ?
H27D C272 H27E 109.5 . . ?
C27 C272 H27F 109.5 . . ?
H27D C272 H27F 109.5 . . ?
H27E C272 H27F 109.5 . . ?
C22 C28 C281 111.78(12) . . ?
C22 C28 C282 111.64(12) . . ?
C281 C28 C282 110.08(12) . . ?
C22 C28 H28 107.7 . . ?
C281 C28 H28 107.7 . . ?
C282 C28 H28 107.7 . . ?
C28 C281 H28A 109.5 . . ?
C28 C281 H28B 109.5 . . ?
H28A C281 H28B 109.5 . . ?
C28 C281 H28C 109.5 . . ?
H28A C281 H28C 109.5 . . ?
H28B C281 H28C 109.5 . . ?
C28 C282 H28D 109.5 . . ?
C28 C282 H28E 109.5 . . ?
H28D C282 H28E 109.5 . . ?
C28 C282 H28F 109.5 . . ?
H28D C282 H28F 109.5 . . ?
H28E C282 H28F 109.5 . . ?
C31 O3 W1 129.56(8) . . ?
O3 C31 C32 120.88(12) . . ?
O3 C31 C36 118.46(12) . . ?
C32 C31 C36 120.64(12) . . ?
C33 C32 C31 118.41(13) . . ?
C33 C32 C38 120.29(13) . . ?
C31 C32 C38 121.25(12) . . ?
C34 C33 C32 121.24(14) . . ?
C34 C33 H33 119.4 . . ?
C32 C33 H33 119.4 . . ?
C35 C34 C33 119.71(14) . . ?
C35 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C34 C35 C36 121.33(14) . . ?
C34 C35 H35 119.3 . . ?
C36 C35 H35 119.3 . . ?
C35 C36 C31 118.48(14) . . ?
C35 C36 C37 120.86(13) . . ?
C31 C36 C37 120.59(13) . . ?
C373 C37 C36 106.7(5) . . ?
C372 C37 C36 115.02(15) . . ?
C372 C37 C371 109.99(17) . . ?
C36 C37 C371 109.64(15) . . ?
C373 C37 C374 116.5(7) . . ?
C36 C37 C374 107.6(5) . . ?
C372 C37 H37 107.3 . . ?
C36 C37 H37 107.3 . . ?
C371 C37 H37 107.3 . . ?
C37 C371 H37A 109.5 . . ?
C37 C371 H37B 109.5 . . ?
H37A C371 H37B 109.5 . . ?
C37 C371 H37C 109.5 . . ?
H37A C371 H37C 109.5 . . ?
H37B C371 H37C 109.5 . . ?
C37 C372 H37D 109.5 . . ?
C37 C372 H37E 109.5 . . ?
H37D C372 H37E 109.5 . . ?
C37 C372 H37F 109.5 . . ?
H37D C372 H37F 109.5 . . ?
H37E C372 H37F 109.5 . . ?
C37 C373 H37G 109.5 . . ?
C37 C373 H37H 109.5 . . ?
H37G C373 H37H 109.5 . . ?
C37 C373 H37I 109.5 . . ?
H37G C373 H37I 109.5 . . ?
H37H C373 H37I 109.5 . . ?
C37 C374 H37J 109.5 . . ?
C37 C374 H37K 109.5 . . ?
H37J C374 H37K 109.5 . . ?
C37 C374 H37L 109.5 . . ?
H37J C374 H37L 109.5 . . ?
H37K C374 H37L 109.5 . . ?
C32 C38 C381 112.73(13) . . ?
C32 C38 C382 110.22(13) . . ?
C381 C38 C382 110.71(14) . . ?
C32 C38 H38 107.7 . . ?
C381 C38 H38 107.7 . . ?
C382 C38 H38 107.7 . . ?
C38 C381 H38A 109.5 . . ?
C38 C381 H38B 109.5 . . ?
H38A C381 H38B 109.5 . . ?
C38 C381 H38C 109.5 . . ?
H38A C381 H38C 109.5 . . ?
H38B C381 H38C 109.5 . . ?
C38 C382 H38D 109.5 . . ?
C38 C382 H38E 109.5 . . ?
H38D C382 H38E 109.5 . . ?
C38 C382 H38F 109.5 . . ?
H38D C382 H38F 109.5 . . ?
H38E C382 H38F 109.5 . . ?
C41 O4 W1 133.00(8) . . ?
O4 C41 C42 120.99(12) . . ?
O4 C41 C46 118.15(12) . . ?
C42 C41 C46 120.82(12) . . ?
C43 C42 C41 118.04(13) . . ?
C43 C42 C48 120.31(13) . . ?
C41 C42 C48 121.65(12) . . ?
C44 C43 C42 121.55(15) . . ?
C44 C43 H43 119.2 . . ?
C42 C43 H43 119.2 . . ?
C45 C44 C43 119.52(15) . . ?
C45 C44 H44 120.2 . . ?
C43 C44 H44 120.2 . . ?
C44 C45 C46 121.23(15) . . ?
C44 C45 H45 119.4 . . ?
C46 C45 H45 119.4 . . ?
C45 C46 C41 118.66(13) . . ?
C45 C46 C47 120.85(13) . . ?
C41 C46 C47 120.44(12) . . ?
C46 C47 C472 113.16(13) . . ?
C46 C47 C471 109.62(13) . . ?
C472 C47 C471 110.58(13) . . ?
C46 C47 H47 107.8 . . ?
C472 C47 H47 107.8 . . ?
C471 C47 H47 107.8 . . ?
C47 C471 H47A 109.5 . . ?
C47 C471 H47B 109.5 . . ?
H47A C471 H47B 109.5 . . ?
C47 C471 H47C 109.5 . . ?
H47A C471 H47C 109.5 . . ?
H47B C471 H47C 109.5 . . ?
C47 C472 H47D 109.5 . . ?
C47 C472 H47E 109.5 . . ?
H47D C472 H47E 109.5 . . ?
C47 C472 H47F 109.5 . . ?
H47D C472 H47F 109.5 . . ?
H47E C472 H47F 109.5 . . ?
C42 C48 C481 110.73(13) . . ?
C42 C48 C482 111.37(13) . . ?
C481 C48 C482 110.21(13) . . ?
C42 C48 H48 108.1 . . ?
C481 C48 H48 108.1 . . ?
C482 C48 H48 108.1 . . ?
C48 C481 H48A 109.5 . . ?
C48 C481 H48B 109.5 . . ?
H48A C481 H48B 109.5 . . ?
C48 C481 H48C 109.5 . . ?
H48A C481 H48C 109.5 . . ?
H48B C481 H48C 109.5 . . ?
C48 C482 H48D 109.5 . . ?
C48 C482 H48E 109.5 . . ?
H48D C482 H48E 109.5 . . ?
C48 C482 H48F 109.5 . . ?
H48D C482 H48F 109.5 . . ?
H48E C482 H48F 109.5 . . ?
C81 P1 C61 108.37(6) . . ?
C81 P1 C71 109.92(7) . . ?
C61 P1 C71 110.31(7) . . ?
C81 P1 C5 109.05(7) . . ?
C61 P1 C5 109.75(7) . . ?
C71 P1 C5 109.41(7) . . ?
P1 C5 H5A 109.5 . . ?
P1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
P1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C66 C61 C62 120.24(14) . . ?
C66 C61 P1 120.06(11) . . ?
C62 C61 P1 119.46(11) . . ?
C63 C62 C61 119.80(16) . . ?
C63 C62 H62 120.1 . . ?
C61 C62 H62 120.1 . . ?
C64 C63 C62 120.14(17) . . ?
C64 C63 H63 119.9 . . ?
C62 C63 H63 119.9 . . ?
C63 C64 C65 120.24(16) . . ?
C63 C64 H64 119.9 . . ?
C65 C64 H64 119.9 . . ?
C64 C65 C66 120.36(15) . . ?
C64 C65 H65 119.8 . . ?
C66 C65 H65 119.8 . . ?
C61 C66 C65 119.22(15) . . ?
C61 C66 H66 120.4 . . ?
C65 C66 H66 120.4 . . ?
C76 C71 C72 120.31(14) . . ?
C76 C71 P1 120.84(11) . . ?
C72 C71 P1 118.86(12) . . ?
C73 C72 C71 119.14(16) . . ?
C73 C72 H72 120.4 . . ?
C71 C72 H72 120.4 . . ?
C74 C73 C72 120.36(16) . . ?
C74 C73 H73 119.8 . . ?
C72 C73 H73 119.8 . . ?
C75 C74 C73 120.56(16) . . ?
C75 C74 H74 119.7 . . ?
C73 C74 H74 119.7 . . ?
C74 C75 C76 120.15(17) . . ?
C74 C75 H75 119.9 . . ?
C76 C75 H75 119.9 . . ?
C75 C76 C71 119.48(16) . . ?
C75 C76 H76 120.3 . . ?
C71 C76 H76 120.3 . . ?
C86 C81 C82 120.46(13) . . ?
C86 C81 P1 120.28(10) . . ?
C82 C81 P1 119.26(10) . . ?
C83 C82 C81 119.43(13) . . ?
C83 C82 H82 120.3 . . ?
C81 C82 H82 120.3 . . ?
C82 C83 C84 120.27(14) . . ?
C82 C83 H83 119.9 . . ?
C84 C83 H83 119.9 . . ?
C83 C84 C85 120.36(14) . . ?
C83 C84 H84 119.8 . . ?
C85 C84 H84 119.8 . . ?
C84 C85 C86 120.01(14) . . ?
C84 C85 H85 120.0 . . ?
C86 C85 H85 120.0 . . ?
C85 C86 C81 119.47(13) . . ?
C85 C86 H86 120.3 . . ?
C81 C86 H86 120.3 . . ?

_refine_diff_density_max         1.784
_refine_diff_density_min         -1.812
_refine_diff_density_rms         0.096


# start Validation Reply Form
_vrf_PLAT412_X8_16249            
;
PROBLEM: Short Intra XH3 .. XHn     H37    ..  H37H    ..       1.77 Ang.  
RESPONSE: H37 is positioned according to the major part of this 
disordered isopropyl group.
;
# end Validation Reply Form
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
