# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_raj01
_database_code_depnum_ccdc_archive 'CCDC 1515745'
_audit_update_record             
;
2016-11-08 deposited with the CCDC.
2017-05-22 downloaded from the CCDC.
;
_audit_creation_date             2016-07-15
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C40 H51 Li N2 O7 W'
_chemical_formula_sum            'C40 H51 Li N2 O7 W'
_chemical_formula_weight         862.61
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C132 H216 N48 O20 W4 Li1 '
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'
Li Li -0.0003 0.0001 '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 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   10.86235(11)
_cell_length_b                   18.91698(18)
_cell_length_c                   19.27237(18)
_cell_angle_alpha                90
_cell_angle_beta                 90.4081(9)
_cell_angle_gamma                90
_cell_volume                     3960.04(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    54851
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      31.9580
_cell_measurement_theta_min      2.1090
_exptl_absorpt_coefficient_mu    2.966
_exptl_absorpt_correction_T_max  0.736
_exptl_absorpt_correction_T_min  0.511
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1752.0
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 27 0.0561
0 -26 -7 0.0885
-1 -5 -27 0.0704
-14 -2 9 0.1292
0 7 -26 0.0575
0 26 -3 0.0664
15 1 -6 0.1078
0 -7 26 0.0838
14 -2 9 0.1438

_exptl_crystal_recrystallization_method 
"disordered from C37 to C40. Inside the disordred part ADP's were constrained to be same pairwise, equivalent bond length were restrained to be same"
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.126
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.8639 0.6356 27.1079 0.2378 0.1315 0.9624
0.0160 -25.7595 -7.0234 -0.8784 -0.4778 -0.0096
-0.8074 -5.0353 -26.6325 -0.3744 -0.2057 -0.9042
-13.9848 -2.0061 9.0032 -0.4369 0.8229 0.2767
-0.1982 6.5978 -26.3203 0.0214 -0.0431 -0.9988
-0.3434 26.4992 -2.9631 0.8219 0.4463 -0.3540
14.9851 1.0058 -6.0070 0.4569 -0.8781 -0.1563
-0.1263 -6.5990 26.3257 -0.0316 0.0617 0.9976
14.3731 -2.2391 8.9162 0.4381 -0.8039 0.4022

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            137501
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.080
_diffrn_reflns_theta_min         1.508
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -4.00  94.00   1.00    4.00    --   24.96  77.00 150.00   98
  2  ω      6.00  93.00   1.00    4.00    --   24.96  57.00 -90.00   87
  3  ω    -43.00  43.00   1.00    4.00    --   24.96 -57.00-150.00   86
  4  ω    -43.00  43.00   1.00    4.00    --   24.96 -57.00 120.00   86
  5  ω    -47.00  63.00   1.00    4.00    --   24.96 -19.00 -90.00  110
  6  ω     -4.00  94.00   1.00    4.00    --   24.96  77.00 -30.00   98
  7  ω      6.00  93.00   1.00    4.00    --   24.96  57.00  90.00   87
  8  ω    -44.00  54.00   1.00    4.00    --   24.96 -77.00  60.00   98
  9  ω    -20.00  65.00   1.00    4.00    --   24.96 -99.00-180.00   85
 10  ω     10.00  89.00   1.00    4.00    --   24.96-139.00  20.61   79
 11  ω    -97.00 -16.00   1.00    4.00    --  -23.50 153.00 -28.14   81
 12  ω    -94.00 -31.00   1.00    4.00    --  -23.50 -38.00  60.00   63
 13  ω     -4.00  94.00   1.00    4.00    --   24.96  77.00  30.00   98
 14  ω      7.00  85.00   1.00    4.00    --   24.96-133.00 -79.43   78
 15  ω     -4.00  94.00   1.00    4.00    --   24.96  77.00-150.00   98
 16  ω    -47.00  63.00   1.00    4.00    --   24.96 -19.00  90.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0311421000
_diffrn_orient_matrix_UB_12      0.0322041000
_diffrn_orient_matrix_UB_13      0.0070235000
_diffrn_orient_matrix_UB_21      -0.0572110000
_diffrn_orient_matrix_UB_22      0.0168023000
_diffrn_orient_matrix_UB_23      0.0062799000
_diffrn_orient_matrix_UB_31      0.0044576000
_diffrn_orient_matrix_UB_32      -0.0093246000
_diffrn_orient_matrix_UB_33      0.0355785000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10239
_reflns_number_total             11634
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_reflns_special_details          
;
 Atoms C38-C40 (part of thf) are disordered at 2 positions, ratio 83:17. 
 The ADP's of these atoms were constrained to be same pairwisely, 
 eqivalent bond lenght in this part were restrained to be same.

 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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.262
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         11634
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0212
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0173P)²+3.0934P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0486
_refine_special_details          
"disorder of C37 to C40. Inside the disordred part ADP's were constrained to be same pairwise, equivalent bond length were restrained to be same."
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.54328(2) 0.56282(2) 0.80855(2) 0.01223(2) Uani 1 1 d . . . . .
O1 O 0.61380(14) 0.69770(7) 0.89602(7) 0.0219(3) Uani 1 1 d . . . . .
O2 O 0.43841(15) 0.67343(8) 0.69928(8) 0.0288(3) Uani 1 1 d . . . . .
O3 O 0.78925(16) 0.55200(10) 0.72038(10) 0.0387(4) Uani 1 1 d . . . . .
O4 O 0.66472(16) 0.48663(8) 0.93984(8) 0.0302(4) Uani 1 1 d . . . . .
O5 O 0.28150(15) 0.56144(10) 0.88085(9) 0.0369(4) Uani 1 1 d . . . . .
O6 O 0.49515(13) 0.18475(7) 0.61506(7) 0.0206(3) Uani 1 1 d . . . . .
O7 O 0.47281(14) 0.17035(7) 0.76759(7) 0.0232(3) Uani 1 1 d D . . . .
N1 N 0.49999(13) 0.39518(8) 0.75720(7) 0.0110(3) Uani 1 1 d . . . . .
N2 N 0.44151(14) 0.39814(8) 0.65208(7) 0.0121(3) Uani 1 1 d . . . . .
C1 C 0.47116(16) 0.35136(9) 0.70288(9) 0.0123(3) Uani 1 1 d . . . . .
C2 C 0.49160(16) 0.46853(9) 0.74276(9) 0.0128(3) Uani 1 1 d . . . . .
C3 C 0.45379(16) 0.46817(9) 0.67482(9) 0.0134(3) Uani 1 1 d . . . . .
H3 H 0.4383 0.5090 0.6474 0.016 Uiso 1 1 calc R U . . .
C4 C 0.53872(16) 0.36686(9) 0.82347(9) 0.0124(3) Uani 1 1 d . . . . .
C5 C 0.66311(17) 0.34951(10) 0.83354(9) 0.0153(3) Uani 1 1 d . . . . .
C6 C 0.69757(19) 0.32205(10) 0.89800(10) 0.0208(4) Uani 1 1 d . . . . .
H6 H 0.7807 0.3084 0.9058 0.025 Uiso 1 1 calc R U . . .
C7 C 0.6130(2) 0.31435(11) 0.95060(10) 0.0236(4) Uani 1 1 d . . . . .
H7 H 0.6387 0.2964 0.9944 0.028 Uiso 1 1 calc R U . . .
C8 C 0.4905(2) 0.33269(10) 0.93977(10) 0.0208(4) Uani 1 1 d . . . . .
H8 H 0.4333 0.3275 0.9765 0.025 Uiso 1 1 calc R U . . .
C9 C 0.45055(18) 0.35860(10) 0.87573(9) 0.0156(3) Uani 1 1 d . . . . .
C10 C 0.75806(17) 0.36011(11) 0.77694(10) 0.0191(4) Uani 1 1 d . . . . .
H10 H 0.7207 0.3913 0.7406 0.023 Uiso 1 1 calc R U . . .
C11 C 0.7909(2) 0.28976(14) 0.74273(14) 0.0356(6) Uani 1 1 d . . . . .
H11A H 0.8517 0.2979 0.7063 0.053 Uiso 1 1 calc R U . . .
H11B H 0.7166 0.2687 0.7223 0.053 Uiso 1 1 calc R U . . .
H11C H 0.8254 0.2576 0.7777 0.053 Uiso 1 1 calc R U . . .
C12 C 0.8750(2) 0.39644(14) 0.80433(12) 0.0304(5) Uani 1 1 d . . . . .
H12A H 0.8526 0.4402 0.8284 0.046 Uiso 1 1 calc R U . . .
H12B H 0.9292 0.4075 0.7654 0.046 Uiso 1 1 calc R U . . .
H12C H 0.9178 0.3648 0.8367 0.046 Uiso 1 1 calc R U . . .
C13 C 0.31538(18) 0.37419(10) 0.86230(10) 0.0181(4) Uani 1 1 d . . . . .
H13 H 0.3100 0.4120 0.8261 0.022 Uiso 1 1 calc R U . . .
C14 C 0.2479(2) 0.40025(13) 0.92660(11) 0.0293(5) Uani 1 1 d . . . . .
H14A H 0.1657 0.4171 0.9132 0.044 Uiso 1 1 calc R U . . .
H14B H 0.2944 0.4390 0.9480 0.044 Uiso 1 1 calc R U . . .
H14C H 0.2401 0.3614 0.9599 0.044 Uiso 1 1 calc R U . . .
C15 C 0.2502(2) 0.30800(12) 0.83376(12) 0.0274(5) Uani 1 1 d . . . . .
H15A H 0.2914 0.2923 0.7914 0.041 Uiso 1 1 calc R U . . .
H15B H 0.1641 0.3193 0.8232 0.041 Uiso 1 1 calc R U . . .
H15C H 0.2538 0.2702 0.8685 0.041 Uiso 1 1 calc R U . . .
C16 C 0.41089(17) 0.37940(9) 0.58162(9) 0.0121(3) Uani 1 1 d . . . . .
C17 C 0.50578(17) 0.37553(9) 0.53313(9) 0.0147(3) Uani 1 1 d . . . . .
C18 C 0.47396(19) 0.36005(10) 0.46454(9) 0.0178(4) Uani 1 1 d . . . . .
H18 H 0.5367 0.3571 0.4305 0.021 Uiso 1 1 calc R U . . .
C19 C 0.35264(19) 0.34896(10) 0.44521(10) 0.0194(4) Uani 1 1 d . . . . .
H19 H 0.3327 0.3384 0.3983 0.023 Uiso 1 1 calc R U . . .
C20 C 0.25987(18) 0.35316(10) 0.49421(10) 0.0181(4) Uani 1 1 d . . . . .
H20 H 0.1768 0.3454 0.4804 0.022 Uiso 1 1 calc R U . . .
C21 C 0.28691(17) 0.36861(9) 0.56358(9) 0.0145(3) Uani 1 1 d . . . . .
C22 C 0.64011(17) 0.38698(10) 0.55334(10) 0.0175(4) Uani 1 1 d . . . . .
H22 H 0.6442 0.3950 0.6046 0.021 Uiso 1 1 calc R U . . .
C23 C 0.6934(2) 0.45215(11) 0.51743(13) 0.0280(5) Uani 1 1 d . . . . .
H23A H 0.6927 0.4448 0.4671 0.042 Uiso 1 1 calc R U . . .
H23B H 0.7782 0.4597 0.5335 0.042 Uiso 1 1 calc R U . . .
H23C H 0.6434 0.4937 0.5287 0.042 Uiso 1 1 calc R U . . .
C24 C 0.7171(2) 0.32153(12) 0.53669(15) 0.0341(5) Uani 1 1 d . . . . .
H24A H 0.6820 0.2803 0.5601 0.051 Uiso 1 1 calc R U . . .
H24B H 0.8019 0.3288 0.5528 0.051 Uiso 1 1 calc R U . . .
H24C H 0.7166 0.3135 0.4864 0.051 Uiso 1 1 calc R U . . .
C25 C 0.18536(17) 0.37191(11) 0.61766(10) 0.0188(4) Uani 1 1 d . . . . .
H25 H 0.2166 0.4006 0.6576 0.023 Uiso 1 1 calc R U . . .
C26 C 0.0679(2) 0.40756(14) 0.59007(13) 0.0316(5) Uani 1 1 d . . . . .
H26A H 0.0890 0.4532 0.5692 0.047 Uiso 1 1 calc R U . . .
H26B H 0.0106 0.4151 0.6284 0.047 Uiso 1 1 calc R U . . .
H26C H 0.0292 0.3772 0.5550 0.047 Uiso 1 1 calc R U . . .
C27 C 0.1558(2) 0.29777(12) 0.64470(12) 0.0270(5) Uani 1 1 d . . . . .
H27A H 0.1240 0.2686 0.6065 0.041 Uiso 1 1 calc R U . . .
H27B H 0.0936 0.3011 0.6812 0.041 Uiso 1 1 calc R U . . .
H27C H 0.2308 0.2762 0.6637 0.041 Uiso 1 1 calc R U . . .
C28 C 0.58917(18) 0.64831(10) 0.86321(9) 0.0164(4) Uani 1 1 d . . . . .
C29 C 0.47491(18) 0.63079(10) 0.73683(10) 0.0181(4) Uani 1 1 d . . . . .
C30 C 0.70265(19) 0.55709(11) 0.75330(11) 0.0211(4) Uani 1 1 d . . . . .
C31 C 0.61908(19) 0.50885(10) 0.89078(10) 0.0189(4) Uani 1 1 d . . . . .
C32 C 0.37616(19) 0.56079(11) 0.85527(10) 0.0198(4) Uani 1 1 d . . . . .
C33 C 0.4104(2) 0.18233(11) 0.55696(11) 0.0247(4) Uani 1 1 d . . . . .
H33A H 0.4209 0.2245 0.5272 0.030 Uiso 1 1 calc R U . . .
H33B H 0.3244 0.1810 0.5735 0.030 Uiso 1 1 calc R U . . .
C34 C 0.44001(19) 0.11542(11) 0.51646(10) 0.0222(4) Uani 1 1 d . . . . .
H34A H 0.4869 0.1266 0.4740 0.027 Uiso 1 1 calc R U . . .
H34B H 0.3638 0.0900 0.5032 0.027 Uiso 1 1 calc R U . . .
C35 C 0.51770(19) 0.07159(10) 0.56703(11) 0.0217(4) Uani 1 1 d . . . . .
H35A H 0.4653 0.0419 0.5971 0.026 Uiso 1 1 calc R U . . .
H35B H 0.5768 0.0411 0.5421 0.026 Uiso 1 1 calc R U . . .
C36 C 0.58362(18) 0.12830(11) 0.60866(11) 0.0202(4) Uani 1 1 d . . . . .
H36A H 0.6082 0.1102 0.6549 0.024 Uiso 1 1 calc R U . . .
H36B H 0.6581 0.1448 0.5841 0.024 Uiso 1 1 calc R U . . .
C37 C 0.5186(2) 0.17101(11) 0.83867(10) 0.0239(4) Uani 1 1 d D . . . .
H37A H 0.4922 0.2147 0.8625 0.029 Uiso 0.832(6) 1 calc R U P A 1
H37B H 0.6097 0.1692 0.8393 0.029 Uiso 0.832(6) 1 calc R U P A 1
H37C H 0.5131 0.2186 0.8598 0.029 Uiso 0.168(6) 1 calc R U P A 2
H37D H 0.6044 0.1536 0.8420 0.029 Uiso 0.168(6) 1 calc R U P A 2
C38A C 0.4662(3) 0.10686(17) 0.87474(15) 0.0264(7) Uani 0.832(6) 1 d D . P A 1
H38A H 0.4480 0.1169 0.9240 0.032 Uiso 0.832(6) 1 calc R U P A 1
H38B H 0.5229 0.0660 0.8720 0.032 Uiso 0.832(6) 1 calc R U P A 1
C38B C 0.4270(14) 0.1190(8) 0.8713(8) 0.0264(7) Uani 0.168(6) 1 d D . P A 2
H38C H 0.4659 0.0938 0.9108 0.032 Uiso 0.168(6) 1 calc R U P A 2
H38D H 0.3536 0.1444 0.8884 0.032 Uiso 0.168(6) 1 calc R U P A 2
C39A C 0.3477(3) 0.09373(18) 0.83265(15) 0.0297(7) Uani 0.832(6) 1 d D . P A 1
H39A H 0.3201 0.0440 0.8365 0.036 Uiso 0.832(6) 1 calc R U P A 1
H39B H 0.2805 0.1256 0.8474 0.036 Uiso 0.832(6) 1 calc R U P A 1
C39B C 0.3913(16) 0.0675(8) 0.8150(7) 0.0297(7) Uani 0.168(6) 1 d D . P A 2
H39C H 0.3142 0.0420 0.8257 0.036 Uiso 0.168(6) 1 calc R U P A 2
H39D H 0.4577 0.0332 0.8051 0.036 Uiso 0.168(6) 1 calc R U P A 2
C40A C 0.3904(6) 0.1108(3) 0.7597(4) 0.0356(13) Uani 0.832(6) 1 d D . P A 1
H40A H 0.4338 0.0699 0.7392 0.043 Uiso 0.832(6) 1 calc R U P A 1
H40B H 0.3195 0.1233 0.7296 0.043 Uiso 0.832(6) 1 calc R U P A 1
C40B C 0.374(4) 0.1203(19) 0.757(2) 0.0356(13) Uani 0.168(6) 1 d D . P A 2
H40C H 0.3810 0.0971 0.7110 0.043 Uiso 0.168(6) 1 calc R U P A 2
H40D H 0.2929 0.1438 0.7598 0.043 Uiso 0.168(6) 1 calc R U P A 2
Li1 Li 0.4846(4) 0.24045(19) 0.69692(18) 0.0232(7) 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
W1 C2 2.2570(18) . ?
W1 C28 1.9916(19) . ?
W1 C29 2.025(2) . ?
W1 C30 2.042(2) . ?
W1 C31 2.053(2) . ?
W1 C32 2.033(2) . ?
O1 C28 1.158(2) . ?
O2 C29 1.152(2) . ?
O3 C30 1.142(3) . ?
O4 C31 1.144(2) . ?
O5 C32 1.143(3) . ?
O6 C33 1.445(2) . ?
O6 C36 1.442(2) . ?
O6 Li1 1.901(4) . ?
O7 C37 1.454(2) . ?
O7 C40A 1.446(4) . ?
O7 C40B 1.444(16) . ?
O7 Li1 1.906(4) . ?
N1 C1 1.370(2) . ?
N1 C2 1.418(2) . ?
N1 C4 1.445(2) . ?
N2 C1 1.357(2) . ?
N2 C3 1.402(2) . ?
N2 C16 1.440(2) . ?
C1 Li1 2.106(4) . ?
C2 C3 1.369(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.403(3) . ?
C4 C9 1.403(2) . ?
C5 C6 1.395(3) . ?
C5 C10 1.520(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.381(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.389(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.394(3) . ?
C9 C13 1.518(3) . ?
C10 H10 1.0000 . ?
C10 C11 1.528(3) . ?
C10 C12 1.534(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13 1.0000 . ?
C13 C14 1.526(3) . ?
C13 C15 1.538(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.398(2) . ?
C16 C21 1.403(3) . ?
C17 C18 1.395(3) . ?
C17 C22 1.523(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.383(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.388(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.398(3) . ?
C21 C25 1.524(3) . ?
C22 H22 1.0000 . ?
C22 C23 1.530(3) . ?
C22 C24 1.529(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25 1.0000 . ?
C25 C26 1.535(3) . ?
C25 C27 1.531(3) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.522(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.529(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.516(3) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 H37C 0.9900 . ?
C37 H37D 0.9900 . ?
C37 C38A 1.512(4) . ?
C37 C38B 1.538(13) . ?
C38A H38A 0.9900 . ?
C38A H38B 0.9900 . ?
C38A C39A 1.536(4) . ?
C38B H38C 0.9900 . ?
C38B H38D 0.9900 . ?
C38B C39B 1.507(16) . ?
C39A H39A 0.9900 . ?
C39A H39B 0.9900 . ?
C39A C40A 1.517(7) . ?
C39B H39C 0.9900 . ?
C39B H39D 0.9900 . ?
C39B C40B 1.512(16) . ?
C40A H40A 0.9900 . ?
C40A H40B 0.9900 . ?
C40B H40C 0.9900 . ?
C40B H40D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C28 W1 C2 177.75(7) . . ?
C28 W1 C29 86.25(8) . . ?
C28 W1 C30 96.26(8) . . ?
C28 W1 C31 84.14(7) . . ?
C28 W1 C32 90.11(8) . . ?
C29 W1 C2 91.71(7) . . ?
C29 W1 C30 89.19(8) . . ?
C29 W1 C31 170.39(8) . . ?
C29 W1 C32 89.43(8) . . ?
C30 W1 C2 82.74(7) . . ?
C30 W1 C31 92.25(8) . . ?
C31 W1 C2 97.90(7) . . ?
C32 W1 C2 90.84(7) . . ?
C32 W1 C30 173.38(8) . . ?
C32 W1 C31 90.18(8) . . ?
C33 O6 Li1 128.22(17) . . ?
C36 O6 C33 109.34(14) . . ?
C36 O6 Li1 121.70(16) . . ?
C37 O7 Li1 130.02(16) . . ?
C40A O7 C37 108.2(3) . . ?
C40A O7 Li1 120.8(2) . . ?
C40B O7 C37 113.0(11) . . ?
C40B O7 Li1 114.0(8) . . ?
C1 N1 C2 115.35(14) . . ?
C1 N1 C4 120.98(15) . . ?
C2 N1 C4 123.65(14) . . ?
C1 N2 C3 111.66(14) . . ?
C1 N2 C16 124.89(15) . . ?
C3 N2 C16 123.26(14) . . ?
N1 C1 Li1 128.97(16) . . ?
N2 C1 N1 102.04(15) . . ?
N2 C1 Li1 128.78(16) . . ?
N1 C2 W1 130.37(12) . . ?
C3 C2 W1 127.79(13) . . ?
C3 C2 N1 101.60(15) . . ?
N2 C3 H3 125.3 . . ?
C2 C3 N2 109.33(15) . . ?
C2 C3 H3 125.3 . . ?
C5 C4 N1 118.89(15) . . ?
C5 C4 C9 122.43(16) . . ?
C9 C4 N1 118.67(16) . . ?
C4 C5 C10 121.86(16) . . ?
C6 C5 C4 117.54(17) . . ?
C6 C5 C10 120.60(17) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 C5 121.16(19) . . ?
C7 C6 H6 119.4 . . ?
C6 C7 H7 119.8 . . ?
C6 C7 C8 120.31(18) . . ?
C8 C7 H7 119.8 . . ?
C7 C8 H8 119.6 . . ?
C7 C8 C9 120.84(18) . . ?
C9 C8 H8 119.6 . . ?
C4 C9 C13 121.35(16) . . ?
C8 C9 C4 117.68(18) . . ?
C8 C9 C13 120.92(17) . . ?
C5 C10 H10 107.9 . . ?
C5 C10 C11 110.87(18) . . ?
C5 C10 C12 112.12(16) . . ?
C11 C10 H10 107.9 . . ?
C11 C10 C12 110.09(18) . . ?
C12 C10 H10 107.9 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13 108.0 . . ?
C9 C13 C14 113.21(17) . . ?
C9 C13 C15 110.17(16) . . ?
C14 C13 H13 108.0 . . ?
C14 C13 C15 109.33(17) . . ?
C15 C13 H13 108.0 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N2 118.47(16) . . ?
C17 C16 C21 122.52(16) . . ?
C21 C16 N2 118.96(15) . . ?
C16 C17 C22 122.09(16) . . ?
C18 C17 C16 117.74(17) . . ?
C18 C17 C22 120.17(17) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 C17 121.08(18) . . ?
C19 C18 H18 119.5 . . ?
C18 C19 H19 119.9 . . ?
C18 C19 C20 120.19(17) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 119.5 . . ?
C19 C20 C21 120.94(18) . . ?
C21 C20 H20 119.5 . . ?
C16 C21 C25 121.50(16) . . ?
C20 C21 C16 117.53(17) . . ?
C20 C21 C25 120.96(17) . . ?
C17 C22 H22 108.1 . . ?
C17 C22 C23 111.33(16) . . ?
C17 C22 C24 110.83(17) . . ?
C23 C22 H22 108.1 . . ?
C24 C22 H22 108.1 . . ?
C24 C22 C23 110.39(17) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 H25 107.8 . . ?
C21 C25 C26 112.64(17) . . ?
C21 C25 C27 110.48(16) . . ?
C26 C25 H25 107.8 . . ?
C27 C25 H25 107.8 . . ?
C27 C25 C26 110.15(18) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O1 C28 W1 178.49(17) . . ?
O2 C29 W1 174.97(17) . . ?
O3 C30 W1 177.02(19) . . ?
O4 C31 W1 171.71(16) . . ?
O5 C32 W1 178.15(19) . . ?
O6 C33 H33A 110.4 . . ?
O6 C33 H33B 110.4 . . ?
O6 C33 C34 106.75(16) . . ?
H33A C33 H33B 108.6 . . ?
C34 C33 H33A 110.4 . . ?
C34 C33 H33B 110.4 . . ?
C33 C34 H34A 111.0 . . ?
C33 C34 H34B 111.0 . . ?
C33 C34 C35 103.97(16) . . ?
H34A C34 H34B 109.0 . . ?
C35 C34 H34A 111.0 . . ?
C35 C34 H34B 111.0 . . ?
C34 C35 H35A 111.3 . . ?
C34 C35 H35B 111.3 . . ?
H35A C35 H35B 109.2 . . ?
C36 C35 C34 102.13(16) . . ?
C36 C35 H35A 111.3 . . ?
C36 C35 H35B 111.3 . . ?
O6 C36 C35 104.87(15) . . ?
O6 C36 H36A 110.8 . . ?
O6 C36 H36B 110.8 . . ?
C35 C36 H36A 110.8 . . ?
C35 C36 H36B 110.8 . . ?
H36A C36 H36B 108.8 . . ?
O7 C37 H37A 110.2 . . ?
O7 C37 H37B 110.2 . . ?
O7 C37 H37C 111.9 . . ?
O7 C37 H37D 111.9 . . ?
O7 C37 C38A 107.39(18) . . ?
O7 C37 C38B 99.3(6) . . ?
H37A C37 H37B 108.5 . . ?
H37C C37 H37D 109.6 . . ?
C38A C37 H37A 110.2 . . ?
C38A C37 H37B 110.2 . . ?
C38B C37 H37C 111.9 . . ?
C38B C37 H37D 111.9 . . ?
C37 C38A H38A 111.4 . . ?
C37 C38A H38B 111.4 . . ?
C37 C38A C39A 101.8(2) . . ?
H38A C38A H38B 109.3 . . ?
C39A C38A H38A 111.4 . . ?
C39A C38A H38B 111.4 . . ?
C37 C38B H38C 110.5 . . ?
C37 C38B H38D 110.5 . . ?
H38C C38B H38D 108.6 . . ?
C39B C38B C37 106.4(11) . . ?
C39B C38B H38C 110.5 . . ?
C39B C38B H38D 110.5 . . ?
C38A C39A H39A 111.5 . . ?
C38A C39A H39B 111.5 . . ?
H39A C39A H39B 109.3 . . ?
C40A C39A C38A 101.2(3) . . ?
C40A C39A H39A 111.5 . . ?
C40A C39A H39B 111.5 . . ?
C38B C39B H39C 112.2 . . ?
C38B C39B H39D 112.2 . . ?
C38B C39B C40B 97.9(19) . . ?
H39C C39B H39D 109.8 . . ?
C40B C39B H39C 112.2 . . ?
C40B C39B H39D 112.2 . . ?
O7 C40A C39A 105.2(5) . . ?
O7 C40A H40A 110.7 . . ?
O7 C40A H40B 110.7 . . ?
C39A C40A H40A 110.7 . . ?
C39A C40A H40B 110.7 . . ?
H40A C40A H40B 108.8 . . ?
O7 C40B C39B 103.8(14) . . ?
O7 C40B H40C 111.0 . . ?
O7 C40B H40D 111.0 . . ?
C39B C40B H40C 111.0 . . ?
C39B C40B H40D 111.0 . . ?
H40C C40B H40D 109.0 . . ?
O6 Li1 O7 102.25(18) . . ?
O6 Li1 C1 127.01(19) . . ?
O7 Li1 C1 130.47(19) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
W1 C2 C3 N2 174.79(12) . . . . ?
O6 C33 C34 C35 16.3(2) . . . . ?
O7 C37 C38A C39A -26.1(3) . . . . ?
O7 C37 C38B C39B 30.6(13) . . . . ?
N1 C2 C3 N2 -0.02(19) . . . . ?
N1 C4 C5 C6 -179.78(16) . . . . ?
N1 C4 C5 C10 0.4(3) . . . . ?
N1 C4 C9 C8 -178.58(16) . . . . ?
N1 C4 C9 C13 4.1(3) . . . . ?
N2 C16 C17 C18 -177.52(16) . . . . ?
N2 C16 C17 C22 3.0(3) . . . . ?
N2 C16 C21 C20 177.59(16) . . . . ?
N2 C16 C21 C25 -3.7(3) . . . . ?
C1 N1 C2 W1 -174.05(12) . . . . ?
C1 N1 C2 C3 0.6(2) . . . . ?
C1 N1 C4 C5 84.7(2) . . . . ?
C1 N1 C4 C9 -96.1(2) . . . . ?
C1 N2 C3 C2 -0.5(2) . . . . ?
C1 N2 C16 C17 -90.2(2) . . . . ?
C1 N2 C16 C21 92.3(2) . . . . ?
C2 N1 C1 N2 -0.86(19) . . . . ?
C2 N1 C1 Li1 174.28(18) . . . . ?
C2 N1 C4 C5 -93.9(2) . . . . ?
C2 N1 C4 C9 85.3(2) . . . . ?
C3 N2 C1 N1 0.81(18) . . . . ?
C3 N2 C1 Li1 -174.34(18) . . . . ?
C3 N2 C16 C17 84.4(2) . . . . ?
C3 N2 C16 C21 -93.0(2) . . . . ?
C4 N1 C1 N2 -179.50(15) . . . . ?
C4 N1 C1 Li1 -4.4(3) . . . . ?
C4 N1 C2 W1 4.5(2) . . . . ?
C4 N1 C2 C3 179.16(15) . . . . ?
C4 C5 C6 C7 -2.0(3) . . . . ?
C4 C5 C10 C11 -103.4(2) . . . . ?
C4 C5 C10 C12 133.2(2) . . . . ?
C4 C9 C13 C14 -149.45(18) . . . . ?
C4 C9 C13 C15 87.8(2) . . . . ?
C5 C4 C9 C8 0.6(3) . . . . ?
C5 C4 C9 C13 -176.78(17) . . . . ?
C5 C6 C7 C8 1.2(3) . . . . ?
C6 C5 C10 C11 76.8(2) . . . . ?
C6 C5 C10 C12 -46.7(3) . . . . ?
C6 C7 C8 C9 0.5(3) . . . . ?
C7 C8 C9 C4 -1.4(3) . . . . ?
C7 C8 C9 C13 176.00(18) . . . . ?
C8 C9 C13 C14 33.3(3) . . . . ?
C8 C9 C13 C15 -89.5(2) . . . . ?
C9 C4 C5 C6 1.1(3) . . . . ?
C9 C4 C5 C10 -178.75(17) . . . . ?
C10 C5 C6 C7 177.84(18) . . . . ?
C16 N2 C1 N1 175.99(15) . . . . ?
C16 N2 C1 Li1 0.8(3) . . . . ?
C16 N2 C3 C2 -175.80(16) . . . . ?
C16 C17 C18 C19 0.0(3) . . . . ?
C16 C17 C22 C23 -116.3(2) . . . . ?
C16 C17 C22 C24 120.4(2) . . . . ?
C16 C21 C25 C26 141.35(19) . . . . ?
C16 C21 C25 C27 -95.0(2) . . . . ?
C17 C16 C21 C20 0.3(3) . . . . ?
C17 C16 C21 C25 178.96(17) . . . . ?
C17 C18 C19 C20 0.1(3) . . . . ?
C18 C17 C22 C23 64.2(2) . . . . ?
C18 C17 C22 C24 -59.1(2) . . . . ?
C18 C19 C20 C21 0.0(3) . . . . ?
C19 C20 C21 C16 -0.2(3) . . . . ?
C19 C20 C21 C25 -178.87(18) . . . . ?
C20 C21 C25 C26 -40.0(3) . . . . ?
C20 C21 C25 C27 83.6(2) . . . . ?
C21 C16 C17 C18 -0.2(3) . . . . ?
C21 C16 C17 C22 -179.69(17) . . . . ?
C22 C17 C18 C19 179.52(18) . . . . ?
C33 O6 C36 C35 -26.9(2) . . . . ?
C33 C34 C35 C36 -31.4(2) . . . . ?
C34 C35 C36 O6 35.9(2) . . . . ?
C36 O6 C33 C34 6.4(2) . . . . ?
C37 O7 C40A C39A 22.4(6) . . . . ?
C37 O7 C40B C39B -23(4) . . . . ?
C37 C38A C39A C40A 38.2(4) . . . . ?
C37 C38B C39B C40B -44(2) . . . . ?
C38A C37 C38B C39B -87(2) . . . . ?
C38A C39A C40A O7 -37.8(6) . . . . ?
C38B C37 C38A C39A 40(2) . . . . ?
C38B C39B C40B O7 39(4) . . . . ?
C40A O7 C37 C38A 2.8(5) . . . . ?
C40A O7 C37 C38B -14.2(8) . . . . ?
C40A O7 C40B C39B 42(9) . . . . ?
C40B O7 C37 C38A 12(3) . . . . ?
C40B O7 C37 C38B -5(3) . . . . ?
C40B O7 C40A C39A -97(12) . . . . ?
Li1 O6 C33 C34 -163.70(19) . . . . ?
Li1 O6 C36 C35 143.99(19) . . . . ?
Li1 O7 C37 C38A 171.2(2) . . . . ?
Li1 O7 C37 C38B 154.3(7) . . . . ?
Li1 O7 C40A C39A -147.4(3) . . . . ?
Li1 O7 C40B C39B 175(2) . . . . ?

_olex2_date_sample_data_collection 2016-07-14
_olex2_exptl_crystal_mounting_method mounted
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.473
_oxdiff_exptl_absorpt_empirical_full_min 0.673
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2013-2
####################################################################### 
# 
# 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_Compound_8W
_database_code_depnum_ccdc_archive 'CCDC 1514800'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-05-22 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         'C32 H36 N2 O5 W'
_chemical_formula_sum            'C32 H36 N2 O5 W'
_chemical_formula_weight         712.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.4201 4.6430 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_H-M_alt        'C m c m'
_space_group_name_Hall           '-C 2c 2'

_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, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   11.250(2)
_cell_length_b                   13.869(2)
_cell_length_c                   19.759(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3082.9(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9980
_cell_measurement_theta_min      2.3175
_cell_measurement_theta_max      23.637

_exptl_crystal_description       lensoid
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_F_000             1424
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    2.047
_shelx_estimated_absorpt_T_min   0.650
_shelx_estimated_absorpt_T_max   0.685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3974
_exptl_absorpt_correction_T_max  0.4275
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.56086
_diffrn_radiation_type           AgK\a
_diffrn_source                   'INCOATEC Microsource'
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23603
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.627
_diffrn_reflns_theta_max         23.659
_diffrn_reflns_theta_full        19.665
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2539
_reflns_number_gt                2460
_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 v2012.2'
_computing_cell_refinement       'SAINT V8.35A'
_computing_data_reduction        'SAINT V8.35A'
_computing_structure_solution    
'SHELXT (G.M.Sheldrick,Acta Cryst.(2015)A71,3-8)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'
_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)+(0.0147P)²+1.7628P] 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         2539
_refine_ls_number_parameters     112
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0137
_refine_ls_R_factor_gt           0.0128
_refine_ls_wR_factor_ref         0.0308
_refine_ls_wR_factor_gt          0.0305
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_restrained_S_all      1.112
_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 0.5000 0.69661(2) 0.2500 0.01064(3) Uani 1 4 d S T P . .
N1 N 0.5000 0.92129(10) 0.30422(7) 0.0114(2) Uani 1 2 d S T P . .
C1 C 0.5000 0.85957(15) 0.2500 0.0095(4) Uani 1 4 d S T P . .
C2 C 0.5000 1.01731(12) 0.28412(8) 0.0174(3) Uani 1 2 d S T P . .
H2 H 0.5000 1.0722 0.3128 0.021 Uiso 1 2 calc R U P . .
C3 C 0.5000 0.89533(11) 0.37511(8) 0.0111(3) Uani 1 2 d S T P . .
C4 C 0.60964(11) 0.88614(8) 0.40828(6) 0.0130(2) Uani 1 1 d . . . . .
C5 C 0.72745(11) 0.89731(9) 0.37152(6) 0.0163(2) Uani 1 1 d . . . . .
H5 H 0.7120 0.8909 0.3219 0.020 Uiso 1 1 calc R U . . .
C6 C 0.77968(14) 0.99788(11) 0.38426(8) 0.0289(3) Uani 1 1 d . . . . .
H6A H 0.8544 1.0047 0.3592 0.043 Uiso 1 1 calc R U . . .
H6B H 0.7948 1.0062 0.4328 0.043 Uiso 1 1 calc R U . . .
H6C H 0.7232 1.0470 0.3689 0.043 Uiso 1 1 calc R U . . .
C7 C 0.81774(13) 0.81966(11) 0.39168(8) 0.0262(3) Uani 1 1 d . . . . .
H7A H 0.7806 0.7559 0.3882 0.039 Uiso 1 1 calc R U . . .
H7B H 0.8438 0.8307 0.4384 0.039 Uiso 1 1 calc R U . . .
H7C H 0.8865 0.8228 0.3613 0.039 Uiso 1 1 calc R U . . .
C8 C 0.60720(12) 0.86713(9) 0.47781(6) 0.0162(2) Uani 1 1 d . . . . .
H8 H 0.6798 0.8604 0.5019 0.019 Uiso 1 1 calc R U . . .
C9 C 0.5000 0.85801(13) 0.51198(8) 0.0178(3) Uani 1 2 d S T P . .
H9 H 0.5000 0.8454 0.5592 0.021 Uiso 1 2 calc R U P . .
O11 O 0.5000 0.46957(13) 0.2500 0.0221(4) Uani 1 4 d S T P . .
C11 C 0.5000 0.55264(18) 0.2500 0.0173(5) Uani 1 4 d S T P . .
O12 O 0.21631(13) 0.69059(10) 0.2500 0.0270(3) Uani 1 2 d S T P . .
C12 C 0.31788(18) 0.69513(12) 0.2500 0.0170(3) Uani 1 2 d S T P . .
O13 O 0.5000 0.66314(10) 0.09019(7) 0.0224(3) Uani 1 2 d S T P . .
C13 C 0.5000 0.68300(11) 0.14639(9) 0.0153(3) Uani 1 2 d S T 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 C11 1.997(2) . ?
W1 C12 2.049(2) 3_655 ?
W1 C12 2.049(2) . ?
W1 C13 2.0560(18) . ?
W1 C13 2.0560(18) 10_556 ?
W1 C1 2.260(2) . ?
N1 C1 1.3713(18) . ?
N1 C2 1.390(2) . ?
N1 C3 1.4462(19) . ?
C1 N1 1.3712(18) 10_556 ?
C2 C2 1.348(3) 10_556 ?
C2 H2 0.9500 . ?
C3 C4 1.4026(14) 12_655 ?
C3 C4 1.4027(14) . ?
C4 C8 1.3992(16) . ?
C4 C5 1.5193(17) . ?
C5 C7 1.5330(19) . ?
C5 C6 1.5343(19) . ?
C5 H5 1.0000 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.3878(15) . ?
C8 H8 0.9500 . ?
C9 C8 1.3878(15) 12_655 ?
C9 H9 0.9500 . ?
O11 C11 1.152(3) . ?
O12 C12 1.144(3) . ?
O13 C13 1.144(2) . ?

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
C11 W1 C12 89.42(5) . 3_655 ?
C11 W1 C12 89.42(5) . . ?
C12 W1 C12 178.85(9) 3_655 . ?
C11 W1 C13 84.73(4) . . ?
C12 W1 C13 89.947(4) 3_655 . ?
C12 W1 C13 89.947(4) . . ?
C11 W1 C13 84.73(4) . 10_556 ?
C12 W1 C13 89.947(5) 3_655 10_556 ?
C12 W1 C13 89.947(4) . 10_556 ?
C13 W1 C13 169.46(9) . 10_556 ?
C11 W1 C1 180.0 . . ?
C12 W1 C1 90.58(5) 3_655 . ?
C12 W1 C1 90.58(5) . . ?
C13 W1 C1 95.27(4) . . ?
C13 W1 C1 95.27(4) 10_556 . ?
C1 N1 C2 112.02(13) . . ?
C1 N1 C3 126.96(13) . . ?
C2 N1 C3 121.02(13) . . ?
N1 C1 N1 102.74(18) 10_556 . ?
N1 C1 W1 128.63(9) 10_556 . ?
N1 C1 W1 128.63(9) . . ?
C2 C2 N1 106.60(9) 10_556 . ?
C2 C2 H2 126.7 10_556 . ?
N1 C2 H2 126.7 . . ?
C4 C3 C4 123.14(14) 12_655 . ?
C4 C3 N1 118.37(7) 12_655 . ?
C4 C3 N1 118.38(7) . . ?
C8 C4 C3 117.30(12) . . ?
C8 C4 C5 120.39(11) . . ?
C3 C4 C5 122.31(10) . . ?
C4 C5 C7 112.46(10) . . ?
C4 C5 C6 110.39(10) . . ?
C7 C5 C6 110.01(12) . . ?
C4 C5 H5 107.9 . . ?
C7 C5 H5 107.9 . . ?
C6 C5 H5 107.9 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C4 120.79(12) . . ?
C9 C8 H8 119.6 . . ?
C4 C8 H8 119.6 . . ?
C8 C9 C8 120.67(15) 12_655 . ?
C8 C9 H9 119.7 12_655 . ?
C8 C9 H9 119.7 . . ?
O11 C11 W1 180.0 . . ?
O12 C12 W1 177.42(16) . . ?
O13 C13 W1 171.34(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N1 C1 N1 0.000(1) . . . 10_556 ?
C3 N1 C1 N1 180.000(0) . . . 10_556 ?
C2 N1 C1 W1 180.000(0) . . . . ?
C3 N1 C1 W1 0.000(1) . . . . ?
C1 N1 C2 C2 0.000(1) . . . 10_556 ?
C3 N1 C2 C2 180.000(1) . . . 10_556 ?
C1 N1 C3 C4 -91.84(12) . . . 12_655 ?
C2 N1 C3 C4 88.16(12) . . . 12_655 ?
C1 N1 C3 C4 91.84(12) . . . . ?
C2 N1 C3 C4 -88.16(12) . . . . ?
C4 C3 C4 C8 -0.2(2) 12_655 . . . ?
N1 C3 C4 C8 175.97(12) . . . . ?
C4 C3 C4 C5 -179.40(9) 12_655 . . . ?
N1 C3 C4 C5 -3.27(19) . . . . ?
C8 C4 C5 C7 44.58(15) . . . . ?
C3 C4 C5 C7 -136.20(13) . . . . ?
C8 C4 C5 C6 -78.70(14) . . . . ?
C3 C4 C5 C6 100.52(14) . . . . ?
C3 C4 C8 C9 -0.07(19) . . . . ?
C5 C4 C8 C9 179.18(13) . . . . ?
C4 C8 C9 C8 0.3(3) . . . 12_655 ?

_refine_diff_density_max         0.499
_refine_diff_density_min         -1.841
_refine_diff_density_rms         0.069

####################################################################### 
# 
# 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_Compound_7W
_database_code_depnum_ccdc_archive 'CCDC 1514801'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-05-22 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         'C27 H37 N2, C5 Cl O5 W, 2(C6 H6)'
_chemical_formula_sum            'C44 H49 Cl N2 O5 W'
_chemical_formula_weight         905.15

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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                   10.587(2)
_cell_length_b                   19.360(2)
_cell_length_c                   21.345(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.83(2)
_cell_angle_gamma                90
_cell_volume                     4265.7(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    98(2)
_cell_measurement_reflns_used    9887
_cell_measurement_theta_min      2.222
_cell_measurement_theta_max      22.563

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_F_000             1832
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.815
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6958
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS-2008/2
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      98(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'INCOATEC Microsource'
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            98396
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_av_R_equivalents  0.0892
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.437
_diffrn_reflns_theta_max         28.346
_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             10642
_reflns_number_gt                8191
_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 v2012.2'
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_reduction        'SAINT V7.68A'
_computing_structure_solution    
'SHELXT (G.M.Sheldrick,Acta Cryst.(2015)A71,3-8)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'
_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)+(0.0228P)²+1.2899P] 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         10642
_refine_ls_number_parameters     486
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0370
_refine_ls_wR_factor_ref         0.0690
_refine_ls_wR_factor_gt          0.0645
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.004
_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 0.97388(2) 0.75906(2) 0.83216(2) 0.02306(5) Uani 1 1 d . . . . .
Cl1 Cl 0.85268(8) 0.78928(5) 0.91971(4) 0.0306(2) Uani 1 1 d . . . . .
O1 O 0.9682(3) 0.91097(13) 0.77550(13) 0.0465(7) Uani 1 1 d . . . . .
O2 O 0.7079(3) 0.75281(13) 0.72894(13) 0.0455(7) Uani 1 1 d . . . . .
O3 O 1.1201(3) 0.71509(15) 0.72690(13) 0.0448(7) Uani 1 1 d . . . . .
O4 O 0.9777(3) 0.59788(14) 0.86101(14) 0.0540(8) Uani 1 1 d . . . . .
O5 O 1.2401(3) 0.78470(16) 0.93314(13) 0.0462(7) Uani 1 1 d . . . . .
N1 N 0.3793(2) 0.77553(12) 0.61541(12) 0.0187(6) Uani 1 1 d . . . . .
N2 N 0.4245(3) 0.66630(13) 0.62173(12) 0.0197(6) Uani 1 1 d . . . . .
C1 C 0.3957(3) 0.71944(15) 0.58124(15) 0.0202(7) Uani 1 1 d . . . . .
H1 H 0.3882 0.7178 0.5361 0.024 Uiso 1 1 calc R U . . .
C2 C 0.3977(3) 0.75714(16) 0.67909(14) 0.0217(7) Uani 1 1 d . . . . .
H2 H 0.3916 0.7868 0.7138 0.026 Uiso 1 1 calc R U . . .
C3 C 0.4257(3) 0.68940(16) 0.68305(15) 0.0232(7) Uani 1 1 d . . . . .
H3 H 0.4433 0.6623 0.7211 0.028 Uiso 1 1 calc R U . . .
C4 C 0.3407(3) 0.84366(15) 0.58905(15) 0.0208(7) Uani 1 1 d . . . . .
C5 C 0.4372(3) 0.88844(16) 0.57823(15) 0.0222(7) Uani 1 1 d . . . . .
C6 C 0.3965(4) 0.95367(17) 0.55501(17) 0.0316(9) Uani 1 1 d . . . . .
H6 H 0.4586 0.9861 0.5471 0.038 Uiso 1 1 calc R U . . .
C7 C 0.2666(4) 0.97234(19) 0.5431(2) 0.0414(10) Uani 1 1 d . . . . .
H7 H 0.2411 1.0173 0.5275 0.050 Uiso 1 1 calc R U . . .
C8 C 0.1743(4) 0.92603(19) 0.55385(19) 0.0373(10) Uani 1 1 d . . . . .
H8 H 0.0857 0.9394 0.5450 0.045 Uiso 1 1 calc R U . . .
C9 C 0.2094(3) 0.86010(18) 0.57739(16) 0.0270(8) Uani 1 1 d . . . . .
C10 C 0.5783(3) 0.86781(17) 0.59050(16) 0.0254(7) Uani 1 1 d . . . . .
H10 H 0.5925 0.8294 0.6226 0.030 Uiso 1 1 calc R U . . .
C11 C 0.6715(3) 0.92653(19) 0.61763(18) 0.0352(9) Uani 1 1 d . . . . .
H11A H 0.6698 0.9616 0.5843 0.053 Uiso 1 1 calc R U . . .
H11B H 0.7596 0.9081 0.6314 0.053 Uiso 1 1 calc R U . . .
H11C H 0.6449 0.9474 0.6545 0.053 Uiso 1 1 calc R U . . .
C12 C 0.6107(3) 0.84074(18) 0.52867(17) 0.0329(9) Uani 1 1 d . . . . .
H12A H 0.5500 0.8038 0.5108 0.049 Uiso 1 1 calc R U . . .
H12B H 0.6993 0.8226 0.5381 0.049 Uiso 1 1 calc R U . . .
H12C H 0.6034 0.8785 0.4974 0.049 Uiso 1 1 calc R U . . .
C13 C 0.0069(4) 0.8417(2) 0.6195(2) 0.0445(11) Uani 1 1 d . . . . .
H13A H 0.0504 0.8654 0.6590 0.067 Uiso 1 1 calc R U . . .
H13B H -0.0504 0.8058 0.6299 0.067 Uiso 1 1 calc R U . . .
H13C H -0.0442 0.8751 0.5898 0.067 Uiso 1 1 calc R U . . .
C14 C 0.1076(3) 0.80878(18) 0.58820(17) 0.0286(8) Uani 1 1 d . . . . .
H14 H 0.1529 0.7721 0.6179 0.034 Uiso 1 1 calc R U . . .
C15 C 0.0433(4) 0.7739(2) 0.5250(2) 0.0499(11) Uani 1 1 d . . . . .
H15A H -0.0014 0.8088 0.4948 0.075 Uiso 1 1 calc R U . . .
H15B H -0.0193 0.7396 0.5329 0.075 Uiso 1 1 calc R U . . .
H15C H 0.1096 0.7511 0.5067 0.075 Uiso 1 1 calc R U . . .
C16 C 0.4420(4) 0.59502(16) 0.60385(15) 0.0253(8) Uani 1 1 d . . . . .
C17 C 0.3300(4) 0.55572(17) 0.58208(16) 0.0284(8) Uani 1 1 d . . . . .
C18 C 0.3495(4) 0.48697(18) 0.56661(17) 0.0367(9) Uani 1 1 d . . . . .
H18 H 0.2767 0.4579 0.5520 0.044 Uiso 1 1 calc R U . . .
C19 C 0.4726(4) 0.46051(18) 0.57219(17) 0.0385(10) Uani 1 1 d . . . . .
H19 H 0.4836 0.4137 0.5611 0.046 Uiso 1 1 calc R U . . .
C20 C 0.5795(4) 0.50169(18) 0.59379(17) 0.0347(9) Uani 1 1 d . . . . .
H20 H 0.6635 0.4826 0.5975 0.042 Uiso 1 1 calc R U . . .
C21 C 0.5678(4) 0.57038(17) 0.61034(16) 0.0290(8) Uani 1 1 d . . . . .
C22 C 0.1202(4) 0.5485(2) 0.6183(2) 0.0518(12) Uani 1 1 d . . . . .
H22A H 0.1133 0.4991 0.6078 0.078 Uiso 1 1 calc R U . . .
H22B H 0.0333 0.5685 0.6121 0.078 Uiso 1 1 calc R U . . .
H22C H 0.1661 0.5545 0.6632 0.078 Uiso 1 1 calc R U . . .
C23 C 0.1945(4) 0.58471(19) 0.57462(17) 0.0335(9) Uani 1 1 d . . . . .
H23 H 0.2030 0.6344 0.5876 0.040 Uiso 1 1 calc R U . . .
C24 C 0.1210(4) 0.5817(2) 0.50418(19) 0.0468(11) Uani 1 1 d . . . . .
H24A H 0.1692 0.6074 0.4776 0.070 Uiso 1 1 calc R U . . .
H24B H 0.0349 0.6023 0.5000 0.070 Uiso 1 1 calc R U . . .
H24C H 0.1118 0.5335 0.4900 0.070 Uiso 1 1 calc R U . . .
C25 C 0.7916(4) 0.5821(2) 0.6832(2) 0.0518(12) Uani 1 1 d . . . . .
H25A H 0.7566 0.5682 0.7200 0.078 Uiso 1 1 calc R U . . .
H25B H 0.8627 0.6150 0.6973 0.078 Uiso 1 1 calc R U . . .
H25C H 0.8242 0.5413 0.6646 0.078 Uiso 1 1 calc R U . . .
C26 C 0.6856(4) 0.61602(19) 0.63292(18) 0.0350(9) Uani 1 1 d . . . . .
H26 H 0.6559 0.6576 0.6535 0.042 Uiso 1 1 calc R U . . .
C27 C 0.7378(4) 0.6415(3) 0.5766(2) 0.0626(14) Uani 1 1 d . . . . .
H27A H 0.8107 0.6728 0.5921 0.094 Uiso 1 1 calc R U . . .
H27B H 0.6693 0.6661 0.5464 0.094 Uiso 1 1 calc R U . . .
H27C H 0.7671 0.6020 0.5548 0.094 Uiso 1 1 calc R U . . .
C28 C 0.9717(4) 0.85801(19) 0.79968(17) 0.0315(8) Uani 1 1 d . . . . .
C29 C 0.8019(4) 0.75198(17) 0.76756(17) 0.0305(8) Uani 1 1 d . . . . .
C30 C 1.0661(4) 0.73251(19) 0.76618(18) 0.0335(8) Uani 1 1 d . . . . .
C31 C 0.9740(4) 0.6567(2) 0.85355(18) 0.0356(9) Uani 1 1 d . . . . .
C32 C 1.1432(4) 0.77512(19) 0.89783(17) 0.0316(8) Uani 1 1 d . . . . .
C33 C 0.3241(5) 0.8809(3) 0.7970(3) 0.0592(14) Uani 1 1 d . . . . .
H33 H 0.2406 0.8695 0.8034 0.071 Uiso 1 1 calc R U . . .
C34 C 0.3368(5) 0.9243(2) 0.7482(2) 0.0601(15) Uani 1 1 d . . . . .
H34 H 0.2619 0.9432 0.7206 0.072 Uiso 1 1 calc R U . . .
C35 C 0.4561(5) 0.9404(2) 0.7390(2) 0.0532(13) Uani 1 1 d . . . . .
H35 H 0.4652 0.9710 0.7056 0.064 Uiso 1 1 calc R U . . .
C36 C 0.5623(4) 0.9122(2) 0.7781(2) 0.0497(12) Uani 1 1 d . . . . .
H36 H 0.6459 0.9228 0.7713 0.060 Uiso 1 1 calc R U . . .
C37 C 0.5509(4) 0.8694(2) 0.8265(2) 0.0479(11) Uani 1 1 d . . . . .
H37 H 0.6261 0.8500 0.8535 0.058 Uiso 1 1 calc R U . . .
C38 C 0.4328(5) 0.8540(2) 0.8366(2) 0.0535(13) Uani 1 1 d . . . . .
H38 H 0.4250 0.8246 0.8711 0.064 Uiso 1 1 calc R U . . .
C39 C -0.0401(6) 0.1671(3) 0.6391(2) 0.0628(15) Uani 1 1 d . . . . .
H39 H -0.0744 0.2093 0.6198 0.075 Uiso 1 1 calc R U . . .
C40 C -0.1202(5) 0.1180(3) 0.6538(3) 0.0705(16) Uani 1 1 d . . . . .
H40 H -0.2112 0.1253 0.6426 0.085 Uiso 1 1 calc R U . . .
C41 C -0.0737(5) 0.0592(3) 0.6839(3) 0.0792(18) Uani 1 1 d . . . . .
H41 H -0.1313 0.0264 0.6953 0.095 Uiso 1 1 calc R U . . .
C42 C 0.0558(5) 0.0468(2) 0.6978(3) 0.0707(16) Uani 1 1 d . . . . .
H42 H 0.0888 0.0058 0.7199 0.085 Uiso 1 1 calc R U . . .
C43 C 0.1391(4) 0.0936(2) 0.6801(2) 0.0540(12) Uani 1 1 d . . . . .
H43 H 0.2289 0.0834 0.6869 0.065 Uiso 1 1 calc R U . . .
C44 C 0.0923(5) 0.1551(3) 0.6525(2) 0.0605(14) Uani 1 1 d . . . . .
H44 H 0.1497 0.1890 0.6427 0.073 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 C30 1.952(4) . ?
W1 C29 2.030(4) . ?
W1 C31 2.034(4) . ?
W1 C28 2.036(4) . ?
W1 C32 2.039(4) . ?
W1 Cl1 2.5585(9) . ?
O1 C28 1.145(4) . ?
O2 C29 1.143(4) . ?
O3 C30 1.165(4) . ?
O4 C31 1.149(4) . ?
O5 C32 1.145(4) . ?
N1 C1 1.341(4) . ?
N1 C2 1.377(4) . ?
N1 C4 1.457(4) . ?
N2 C1 1.335(4) . ?
N2 C3 1.380(4) . ?
N2 C16 1.455(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.343(4) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 C9 1.394(4) . ?
C4 C5 1.398(4) . ?
C5 C6 1.389(4) . ?
C5 C10 1.513(4) . ?
C6 C7 1.390(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.383(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.392(5) . ?
C8 H8 0.9500 . ?
C9 C14 1.520(5) . ?
C10 C12 1.528(4) . ?
C10 C11 1.532(4) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.518(5) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.527(5) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C21 1.393(5) . ?
C16 C17 1.399(5) . ?
C17 C18 1.398(5) . ?
C17 C23 1.515(5) . ?
C18 C19 1.380(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.378(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.389(5) . ?
C20 H20 0.9500 . ?
C21 C26 1.517(5) . ?
C22 C23 1.518(5) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.533(5) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.519(5) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.513(6) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C33 C34 1.369(7) . ?
C33 C38 1.370(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.356(7) . ?
C34 H34 0.9500 . ?
C35 C36 1.356(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.351(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.348(6) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C40 1.355(7) . ?
C39 C44 1.386(7) . ?
C39 H39 0.9500 . ?
C40 C41 1.346(7) . ?
C40 H40 0.9500 . ?
C41 C42 1.357(7) . ?
C41 H41 0.9500 . ?
C42 C43 1.375(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.370(6) . ?
C43 H43 0.9500 . ?
C44 H44 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
C30 W1 C29 90.50(15) . . ?
C30 W1 C31 85.97(15) . . ?
C29 W1 C31 92.44(14) . . ?
C30 W1 C28 88.39(15) . . ?
C29 W1 C28 83.77(14) . . ?
C31 W1 C28 173.17(14) . . ?
C30 W1 C32 91.84(15) . . ?
C29 W1 C32 174.99(14) . . ?
C31 W1 C32 92.15(15) . . ?
C28 W1 C32 91.87(14) . . ?
C30 W1 Cl1 177.94(11) . . ?
C29 W1 Cl1 89.55(10) . . ?
C31 W1 Cl1 91.97(11) . . ?
C28 W1 Cl1 93.67(11) . . ?
C32 W1 Cl1 88.27(10) . . ?
C1 N1 C2 108.7(3) . . ?
C1 N1 C4 125.6(3) . . ?
C2 N1 C4 125.6(3) . . ?
C1 N2 C3 108.5(3) . . ?
C1 N2 C16 125.8(3) . . ?
C3 N2 C16 125.5(3) . . ?
N2 C1 N1 108.1(3) . . ?
N2 C1 H1 126.0 . . ?
N1 C1 H1 126.0 . . ?
C3 C2 N1 107.2(3) . . ?
C3 C2 H2 126.4 . . ?
N1 C2 H2 126.4 . . ?
C2 C3 N2 107.5(3) . . ?
C2 C3 H3 126.2 . . ?
N2 C3 H3 126.2 . . ?
C9 C4 C5 124.4(3) . . ?
C9 C4 N1 117.3(3) . . ?
C5 C4 N1 118.2(3) . . ?
C6 C5 C4 116.3(3) . . ?
C6 C5 C10 121.2(3) . . ?
C4 C5 C10 122.5(3) . . ?
C5 C6 C7 121.1(3) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C8 C7 C6 120.6(3) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C7 C8 C9 120.8(3) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
C8 C9 C4 116.7(3) . . ?
C8 C9 C14 120.9(3) . . ?
C4 C9 C14 122.4(3) . . ?
C5 C10 C12 110.1(3) . . ?
C5 C10 C11 113.5(3) . . ?
C12 C10 C11 109.4(3) . . ?
C5 C10 H10 107.9 . . ?
C12 C10 H10 107.9 . . ?
C11 C10 H10 107.9 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C13 C14 C9 112.5(3) . . ?
C13 C14 C15 110.8(3) . . ?
C9 C14 C15 110.2(3) . . ?
C13 C14 H14 107.7 . . ?
C9 C14 H14 107.7 . . ?
C15 C14 H14 107.7 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C16 C17 124.6(3) . . ?
C21 C16 N2 118.3(3) . . ?
C17 C16 N2 117.1(3) . . ?
C18 C17 C16 115.9(3) . . ?
C18 C17 C23 121.0(3) . . ?
C16 C17 C23 123.1(3) . . ?
C19 C18 C17 121.3(4) . . ?
C19 C18 H18 119.3 . . ?
C17 C18 H18 119.3 . . ?
C20 C19 C18 120.3(3) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C19 C20 C21 121.7(4) . . ?
C19 C20 H20 119.1 . . ?
C21 C20 H20 119.1 . . ?
C20 C21 C16 116.1(3) . . ?
C20 C21 C26 121.7(3) . . ?
C16 C21 C26 122.2(3) . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C23 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C17 C23 C22 111.8(3) . . ?
C17 C23 C24 110.6(3) . . ?
C22 C23 C24 111.4(3) . . ?
C17 C23 H23 107.6 . . ?
C22 C23 H23 107.6 . . ?
C24 C23 H23 107.6 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 H25A 109.5 . . ?
C26 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C26 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C21 110.9(3) . . ?
C27 C26 C25 111.0(3) . . ?
C21 C26 C25 113.5(3) . . ?
C27 C26 H26 107.0 . . ?
C21 C26 H26 107.0 . . ?
C25 C26 H26 107.0 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O1 C28 W1 173.3(3) . . ?
O2 C29 W1 174.4(3) . . ?
O3 C30 W1 178.4(3) . . ?
O4 C31 W1 174.3(3) . . ?
O5 C32 W1 177.8(3) . . ?
C34 C33 C38 119.4(4) . . ?
C34 C33 H33 120.3 . . ?
C38 C33 H33 120.3 . . ?
C35 C34 C33 120.2(4) . . ?
C35 C34 H34 119.9 . . ?
C33 C34 H34 119.9 . . ?
C34 C35 C36 119.4(4) . . ?
C34 C35 H35 120.3 . . ?
C36 C35 H35 120.3 . . ?
C37 C36 C35 120.9(4) . . ?
C37 C36 H36 119.5 . . ?
C35 C36 H36 119.5 . . ?
C38 C37 C36 120.0(4) . . ?
C38 C37 H37 120.0 . . ?
C36 C37 H37 120.0 . . ?
C37 C38 C33 120.0(4) . . ?
C37 C38 H38 120.0 . . ?
C33 C38 H38 120.0 . . ?
C40 C39 C44 119.4(5) . . ?
C40 C39 H39 120.3 . . ?
C44 C39 H39 120.3 . . ?
C41 C40 C39 121.4(5) . . ?
C41 C40 H40 119.3 . . ?
C39 C40 H40 119.3 . . ?
C40 C41 C42 119.9(5) . . ?
C40 C41 H41 120.0 . . ?
C42 C41 H41 120.0 . . ?
C41 C42 C43 120.1(5) . . ?
C41 C42 H42 120.0 . . ?
C43 C42 H42 120.0 . . ?
C44 C43 C42 119.8(4) . . ?
C44 C43 H43 120.1 . . ?
C42 C43 H43 120.1 . . ?
C43 C44 C39 119.1(4) . . ?
C43 C44 H44 120.4 . . ?
C39 C44 H44 120.4 . . ?

_refine_diff_density_max         0.554
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.106

####################################################################### 
# 
# 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_Compound_4W
_database_code_depnum_ccdc_archive 'CCDC 1514798'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-05-22 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         'C58 H72 Cl4 N4 O4 Si2 W, C5 H5 N, C H2 Cl2'
_chemical_formula_sum            'C64 H79 Cl6 N5 O4 Si2 W'
_chemical_formula_weight         1435.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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           7
_space_group_name_H-M_alt        'P n'
_space_group_name_Hall           'P -2yac'

_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, z+1/2'

_cell_length_a                   12.696(2)
_cell_length_b                   16.539(3)
_cell_length_c                   16.499(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.35(2)
_cell_angle_gamma                90
_cell_volume                     3370.8(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9867
_cell_measurement_theta_min      2.301
_cell_measurement_theta_max      27.471

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_F_000             1468
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.371
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.074
_exptl_absorpt_coefficient_mu    2.035
_shelx_estimated_absorpt_T_min   0.519
_shelx_estimated_absorpt_T_max   0.864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2002
_exptl_absorpt_correction_T_max  0.2616
_exptl_absorpt_process_details   SADABS-2016/1
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'INCOATEC Microsource'
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            57844
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.231
_diffrn_reflns_theta_max         27.487
_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             15424
_reflns_number_gt                14942
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.997
_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 v2012.2'
_computing_cell_refinement       'SAINT V8.30C'
_computing_data_reduction        'SAINT V8.30C'
_computing_structure_solution    
'SHELXT (G.M.Sheldrick,Acta Cryst.(2015)A71,3-8)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'
_refine_special_details          
;
 Refined as a 2-component perfect 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)+(0.0222P)²+1.0206P] 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_abs_structure_details 
;
 Flack x determined using 7215 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0060(14)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         15424
_refine_ls_number_parameters     829
_refine_ls_number_restraints     377
_refine_ls_R_factor_all          0.0196
_refine_ls_R_factor_gt           0.0185
_refine_ls_wR_factor_ref         0.0447
_refine_ls_wR_factor_gt          0.0442
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.063
_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 0.48723(2) 0.25538(2) 0.39210(3) 0.01785(3) Uani 1 1 d . . . . .
Cl1 Cl 0.78201(7) 0.32359(5) 0.49810(6) 0.02304(16) Uani 1 1 d . . . . .
Cl2 Cl 0.62078(8) 0.31509(5) 0.61993(6) 0.02447(17) Uani 1 1 d . . . . .
Cl3 Cl 0.18908(7) 0.20904(5) 0.28189(6) 0.03030(19) Uani 1 1 d . . . . .
Cl4 Cl 0.35588(8) 0.18921(5) 0.16509(6) 0.02934(19) Uani 1 1 d . . . . .
Si1 Si 0.64520(15) 0.25486(6) 0.51138(11) 0.0174(3) Uani 1 1 d . . . . .
Si2 Si 0.33585(14) 0.26048(7) 0.26746(11) 0.0172(3) Uani 1 1 d . . . . .
O55 O 0.6455(5) 0.24301(17) 0.2677(3) 0.0314(10) Uani 1 1 d . . . . .
O56 O 0.4260(2) 0.06933(16) 0.3884(2) 0.0438(7) Uani 1 1 d . . . . .
O57 O 0.3167(5) 0.2575(2) 0.5043(4) 0.0427(13) Uani 1 1 d . . . . .
O58 O 0.5061(2) 0.44534(15) 0.42272(17) 0.0351(6) Uani 1 1 d . . . . .
N1 N 0.7896(2) 0.10881(16) 0.53036(17) 0.0209(6) Uani 1 1 d . . . . .
N2 N 0.7171(2) 0.11879(16) 0.63580(17) 0.0222(6) Uani 1 1 d . . . . .
N3 N 0.1952(2) 0.40882(15) 0.21762(17) 0.0184(5) Uani 1 1 d . . . . .
N4 N 0.3302(2) 0.40671(15) 0.15859(16) 0.0179(5) Uani 1 1 d . . . . .
C1 C 0.7249(3) 0.15732(18) 0.5645(2) 0.0180(6) Uani 1 1 d . . . . .
C2 C 0.8360(3) 0.12419(18) 0.4578(2) 0.0200(6) Uani 1 1 d . . . . .
C3 C 0.7852(3) 0.09130(19) 0.3805(2) 0.0226(6) Uani 1 1 d . . . . .
C4 C 0.6854(3) 0.0381(2) 0.3691(2) 0.0297(8) Uani 1 1 d . . . . .
H4 H 0.6419 0.0565 0.4090 0.036 Uiso 1 1 calc R U . . .
C5 C 0.7200(4) -0.0504(3) 0.3896(4) 0.0679(18) Uani 1 1 d . . . . .
H5A H 0.6558 -0.0833 0.3895 0.102 Uiso 1 1 calc R U . . .
H5B H 0.7695 -0.0529 0.4448 0.102 Uiso 1 1 calc R U . . .
H5C H 0.7565 -0.0711 0.3477 0.102 Uiso 1 1 calc R U . . .
C6 C 0.6123(3) 0.0395(2) 0.2809(2) 0.0337(8) Uani 1 1 d . . . . .
H6A H 0.5923 0.0954 0.2648 0.051 Uiso 1 1 calc R U . . .
H6B H 0.5467 0.0079 0.2800 0.051 Uiso 1 1 calc R U . . .
H6C H 0.6512 0.0160 0.2417 0.051 Uiso 1 1 calc R U . . .
C7 C 0.8355(3) 0.1040(2) 0.3148(2) 0.0255(7) Uani 1 1 d . . . . .
H7 H 0.8026 0.0842 0.2609 0.031 Uiso 1 1 calc R U . . .
C8 C 0.9333(3) 0.1452(2) 0.3275(2) 0.0278(7) Uani 1 1 d . . . . .
H8 H 0.9662 0.1536 0.2819 0.033 Uiso 1 1 calc R U . . .
C9 C 0.9833(3) 0.17403(19) 0.4054(2) 0.0252(7) Uani 1 1 d . . . . .
H9 H 1.0508 0.2012 0.4129 0.030 Uiso 1 1 calc R U . . .
C10 C 0.9364(3) 0.16398(18) 0.4733(2) 0.0208(6) Uani 1 1 d . . . . .
C11 C 0.9961(3) 0.1918(2) 0.5598(2) 0.0238(7) Uani 1 1 d . . . . .
H11 H 0.9414 0.1996 0.5940 0.029 Uiso 1 1 calc R U . . .
C12 C 1.0565(3) 0.2715(2) 0.5593(2) 0.0287(7) Uani 1 1 d . . . . .
H12A H 1.1167 0.2636 0.5322 0.043 Uiso 1 1 calc R U . . .
H12B H 1.0848 0.2897 0.6168 0.043 Uiso 1 1 calc R U . . .
H12C H 1.0069 0.3123 0.5288 0.043 Uiso 1 1 calc R U . . .
C13 C 1.0766(4) 0.1264(2) 0.6022(3) 0.0386(9) Uani 1 1 d . . . . .
H13A H 1.0378 0.0755 0.6045 0.058 Uiso 1 1 calc R U . . .
H13B H 1.1114 0.1437 0.6589 0.058 Uiso 1 1 calc R U . . .
H13C H 1.1319 0.1183 0.5702 0.058 Uiso 1 1 calc R U . . .
C14 C 0.8225(3) 0.0426(2) 0.5803(2) 0.0296(8) Uani 1 1 d . . . . .
H14 H 0.8687 0.0005 0.5701 0.035 Uiso 1 1 calc R U . . .
C15 C 0.7778(3) 0.0480(2) 0.6459(2) 0.0294(8) Uani 1 1 d . . . . .
H15 H 0.7859 0.0108 0.6908 0.035 Uiso 1 1 calc R U . . .
C16 C 0.6710(3) 0.1482(2) 0.7041(2) 0.0250(7) Uani 1 1 d . . . . .
C17 C 0.7404(3) 0.1895(2) 0.7685(2) 0.0298(8) Uani 1 1 d . . . . .
C18 C 0.8590(3) 0.2049(3) 0.7705(3) 0.0415(10) Uani 1 1 d . . . . .
H18 H 0.8732 0.1869 0.7161 0.050 Uiso 1 1 calc R U . . .
C19 C 0.8887(4) 0.2950(3) 0.7824(4) 0.0708(17) Uani 1 1 d . . . . .
H19A H 0.9622 0.3034 0.7746 0.106 Uiso 1 1 calc R U . . .
H19B H 0.8856 0.3117 0.8388 0.106 Uiso 1 1 calc R U . . .
H19C H 0.8375 0.3272 0.7415 0.106 Uiso 1 1 calc R U . . .
C20 C 0.9307(4) 0.1557(3) 0.8398(3) 0.0587(13) Uani 1 1 d . . . . .
H20A H 0.9070 0.0991 0.8354 0.088 Uiso 1 1 calc R U . . .
H20B H 0.9253 0.1774 0.8940 0.088 Uiso 1 1 calc R U . . .
H20C H 1.0060 0.1588 0.8348 0.088 Uiso 1 1 calc R U . . .
C21 C 0.6965(4) 0.2170(3) 0.8337(3) 0.0388(10) Uani 1 1 d . . . . .
H21 H 0.7407 0.2465 0.8782 0.047 Uiso 1 1 calc R U . . .
C22 C 0.5911(4) 0.2020(3) 0.8340(3) 0.0427(10) Uani 1 1 d . . . . .
H22 H 0.5626 0.2218 0.8786 0.051 Uiso 1 1 calc R U . . .
C23 C 0.5252(4) 0.1588(2) 0.7711(3) 0.0387(10) Uani 1 1 d . . . . .
H23 H 0.4527 0.1477 0.7739 0.046 Uiso 1 1 calc R U . . .
C24 C 0.5634(3) 0.1305(2) 0.7022(2) 0.0283(8) Uani 1 1 d . . . . .
C25 C 0.4934(3) 0.0828(2) 0.6327(3) 0.0337(9) Uani 1 1 d . . . . .
H25 H 0.5119 0.0999 0.5796 0.040 Uiso 1 1 calc R U . . .
C26 C 0.5146(4) -0.0087(3) 0.6428(4) 0.0559(13) Uani 1 1 d . . . . .
H26A H 0.4675 -0.0375 0.5964 0.084 Uiso 1 1 calc R U . . .
H26B H 0.4994 -0.0270 0.6954 0.084 Uiso 1 1 calc R U . . .
H26C H 0.5905 -0.0199 0.6430 0.084 Uiso 1 1 calc R U . . .
C27 C 0.3716(3) 0.0985(3) 0.6238(3) 0.0464(11) Uani 1 1 d . . . . .
H27A H 0.3585 0.1568 0.6244 0.070 Uiso 1 1 calc R U . . .
H27B H 0.3481 0.0730 0.6703 0.070 Uiso 1 1 calc R U . . .
H27C H 0.3308 0.0755 0.5711 0.070 Uiso 1 1 calc R U . . .
C28 C 0.2805(2) 0.36160(18) 0.20815(19) 0.0170(6) Uani 1 1 d . . . . .
C29 C 0.1063(3) 0.39005(19) 0.2569(2) 0.0199(6) Uani 1 1 d . . . . .
C30 C 0.1124(3) 0.41892(19) 0.3376(2) 0.0240(7) Uani 1 1 d . . . . .
C31 C 0.2104(3) 0.4638(2) 0.3868(2) 0.0311(8) Uani 1 1 d . . . . .
H31 H 0.2753 0.4457 0.3669 0.037 Uiso 1 1 calc R U . . .
C32 C 0.1961(4) 0.5561(3) 0.3713(3) 0.0495(12) Uani 1 1 d . . . . .
H32A H 0.1848 0.5671 0.3116 0.074 Uiso 1 1 calc R U . . .
H32B H 0.2612 0.5844 0.4015 0.074 Uiso 1 1 calc R U . . .
H32C H 0.1333 0.5750 0.3911 0.074 Uiso 1 1 calc R U . . .
C33 C 0.2321(4) 0.4483(2) 0.4808(2) 0.0404(9) Uani 1 1 d . . . . .
H33A H 0.1757 0.4745 0.5033 0.061 Uiso 1 1 calc R U . . .
H33B H 0.3029 0.4705 0.5081 0.061 Uiso 1 1 calc R U . . .
H33C H 0.2314 0.3899 0.4911 0.061 Uiso 1 1 calc R U . . .
C34 C 0.0217(3) 0.4062(2) 0.3701(2) 0.0318(8) Uani 1 1 d . . . . .
H34 H 0.0222 0.4247 0.4248 0.038 Uiso 1 1 calc R U . . .
C35 C -0.0687(3) 0.3675(2) 0.3246(3) 0.0365(9) Uani 1 1 d . . . . .
H35 H -0.1292 0.3591 0.3484 0.044 Uiso 1 1 calc R U . . .
C36 C -0.0725(3) 0.3407(2) 0.2449(3) 0.0344(9) Uani 1 1 d . . . . .
H36 H -0.1357 0.3143 0.2144 0.041 Uiso 1 1 calc R U . . .
C37 C 0.0150(3) 0.3519(2) 0.2084(2) 0.0257(7) Uani 1 1 d . . . . .
C38 C 0.0100(3) 0.3252(2) 0.1193(2) 0.0321(8) Uani 1 1 d . . . . .
H38 H 0.0858 0.3217 0.1117 0.039 Uiso 1 1 calc R U . . .
C39 C -0.0428(5) 0.2424(3) 0.1001(3) 0.0575(15) Uani 1 1 d . . . . .
H39A H -0.0311 0.2228 0.0468 0.086 Uiso 1 1 calc R U . . .
H39B H -0.1207 0.2469 0.0967 0.086 Uiso 1 1 calc R U . . .
H39C H -0.0106 0.2044 0.1445 0.086 Uiso 1 1 calc R U . . .
C40 C -0.0513(5) 0.3869(3) 0.0573(3) 0.0594(13) Uani 1 1 d . . . . .
H40A H -0.0472 0.3716 0.0008 0.089 Uiso 1 1 calc R U . . .
H40B H -0.0189 0.4405 0.0705 0.089 Uiso 1 1 calc R U . . .
H40C H -0.1273 0.3884 0.0609 0.089 Uiso 1 1 calc R U . . .
C41 C 0.1926(3) 0.4807(2) 0.1741(2) 0.0210(6) Uani 1 1 d . . . . .
H41 H 0.1410 0.5229 0.1709 0.025 Uiso 1 1 calc R U . . .
C42 C 0.2764(3) 0.4795(2) 0.1375(2) 0.0220(6) Uani 1 1 d . . . . .
H42 H 0.2954 0.5207 0.1034 0.026 Uiso 1 1 calc R U . . .
C43 C 0.4151(3) 0.38140(18) 0.1176(2) 0.0208(6) Uani 1 1 d . . . . .
C44 C 0.3806(3) 0.3396(2) 0.0413(2) 0.0277(7) Uani 1 1 d . . . . .
C45 C 0.2627(3) 0.3245(2) 0.0026(2) 0.0351(9) Uani 1 1 d . . . . .
H45 H 0.2226 0.3254 0.0481 0.042 Uiso 1 1 calc R U . . .
C46 C 0.2406(5) 0.2429(3) -0.0422(3) 0.0451(13) Uani 1 1 d . . . . .
H46A H 0.1623 0.2349 -0.0612 0.068 Uiso 1 1 calc R U . . .
H46B H 0.2715 0.1993 -0.0038 0.068 Uiso 1 1 calc R U . . .
H46C H 0.2737 0.2423 -0.0903 0.068 Uiso 1 1 calc R U . . .
C47 C 0.2180(4) 0.3927(3) -0.0585(3) 0.0487(11) Uani 1 1 d . . . . .
H47A H 0.2569 0.3936 -0.1034 0.073 Uiso 1 1 calc R U . . .
H47B H 0.2277 0.4446 -0.0291 0.073 Uiso 1 1 calc R U . . .
H47C H 0.1407 0.3835 -0.0822 0.073 Uiso 1 1 calc R U . . .
C48 C 0.4611(4) 0.3174(2) 0.0011(3) 0.0343(9) Uani 1 1 d . . . . .
H48 H 0.4422 0.2884 -0.0499 0.041 Uiso 1 1 calc R U . . .
C49 C 0.5683(3) 0.3368(2) 0.0341(3) 0.0371(9) Uani 1 1 d . . . . .
H49 H 0.6221 0.3189 0.0067 0.044 Uiso 1 1 calc R U . . .
C50 C 0.5986(3) 0.3816(2) 0.1061(3) 0.0324(9) Uani 1 1 d . . . . .
H50 H 0.6724 0.3961 0.1264 0.039 Uiso 1 1 calc R U . . .
C51 C 0.5211(3) 0.40616(19) 0.1499(2) 0.0221(7) Uani 1 1 d . . . . .
C52 C 0.5513(3) 0.4643(2) 0.2230(2) 0.0265(7) Uani 1 1 d . . . . .
H52 H 0.4953 0.4604 0.2566 0.032 Uiso 1 1 calc R U . . .
C53 C 0.5510(3) 0.5508(2) 0.1891(3) 0.0385(9) Uani 1 1 d . . . . .
H53A H 0.6063 0.5556 0.1566 0.058 Uiso 1 1 calc R U . . .
H53B H 0.5667 0.5891 0.2356 0.058 Uiso 1 1 calc R U . . .
H53C H 0.4797 0.5628 0.1533 0.058 Uiso 1 1 calc R U . . .
C54 C 0.6621(3) 0.4475(2) 0.2799(3) 0.0341(8) Uani 1 1 d . . . . .
H54A H 0.6664 0.3905 0.2968 0.051 Uiso 1 1 calc R U . . .
H54B H 0.6723 0.4819 0.3295 0.051 Uiso 1 1 calc R U . . .
H54C H 0.7187 0.4592 0.2500 0.051 Uiso 1 1 calc R U . . .
C55 C 0.5897(7) 0.2478(2) 0.3137(5) 0.0226(14) Uani 1 1 d . . . . .
C56 C 0.4536(3) 0.1360(2) 0.3882(3) 0.0273(8) Uani 1 1 d . . . . .
C57 C 0.3804(7) 0.2584(3) 0.4652(5) 0.0269(14) Uani 1 1 d . . . . .
C58 C 0.5016(3) 0.3770(2) 0.4084(2) 0.0235(8) Uani 1 1 d . . . . .
C59 C 0.3826(16) 0.3392(8) 0.6891(11) 0.042(3) Uani 0.67(3) 1 d D U P A 1
H59A H 0.4519 0.3092 0.7003 0.051 Uiso 0.67(3) 1 calc R U P A 1
H59B H 0.3476 0.3320 0.6293 0.051 Uiso 0.67(3) 1 calc R U P A 1
Cl5 Cl 0.4110(4) 0.4428(4) 0.7078(7) 0.0460(13) Uani 0.67(3) 1 d D U P A 1
Cl6 Cl 0.2983(5) 0.2958(4) 0.7490(6) 0.0389(11) Uani 0.67(3) 1 d D U P A 1
C59' C 0.362(3) 0.3419(16) 0.6869(19) 0.034(4) Uani 0.33(3) 1 d D U P A 2
H59C H 0.3095 0.3566 0.6347 0.041 Uiso 0.33(3) 1 calc R U P A 2
H59D H 0.4161 0.3040 0.6737 0.041 Uiso 0.33(3) 1 calc R U P A 2
Cl5' Cl 0.4253(15) 0.4288(10) 0.7386(17) 0.059(3) Uani 0.33(3) 1 d D U P A 2
Cl6' Cl 0.2959(13) 0.2991(11) 0.7599(13) 0.054(3) Uani 0.33(3) 1 d D U P A 2
N5 N 0.5238(3) 0.0939(2) 1.0084(2) 0.0411(8) Uani 0.737(9) 1 d D U P B 1
C60 C 0.6266(7) 0.1217(4) 1.0588(5) 0.0479(16) Uani 0.737(9) 1 d D U P B 1
H60 H 0.6239 0.1572 1.1036 0.058 Uiso 0.737(9) 1 calc R U P B 1
C61 C 0.7223(6) 0.1025(4) 1.0486(5) 0.0459(17) Uani 0.737(9) 1 d D U P B 1
H61 H 0.7866 0.1225 1.0844 0.055 Uiso 0.737(9) 1 calc R U P B 1
C62 C 0.7252(5) 0.0480(4) 0.9785(4) 0.0376(15) Uani 0.737(9) 1 d D U P B 1
H62 H 0.7925 0.0336 0.9665 0.045 Uiso 0.737(9) 1 calc R U P B 1
C63 C 0.6263(5) 0.0167(3) 0.9287(4) 0.0380(14) Uani 0.737(9) 1 d D U P B 1
H63 H 0.6259 -0.0194 0.8839 0.046 Uiso 0.737(9) 1 calc R U P B 1
C64 C 0.5275(7) 0.0422(7) 0.9492(7) 0.0457(17) Uani 0.737(9) 1 d D U P B 1
H64 H 0.4613 0.0203 0.9181 0.055 Uiso 0.737(9) 1 calc R U P B 1
N5' N 0.7175(10) 0.1416(9) 1.0812(8) 0.037(3) Uani 0.263(9) 1 d D U P B 2
C60' C 0.5999(15) 0.1372(11) 1.0694(12) 0.051(3) Uani 0.263(9) 1 d D U P B 2
H60' H 0.5704 0.1675 1.1078 0.061 Uiso 0.263(9) 1 calc R U P B 2
C61' C 0.5238(3) 0.0939(2) 1.0084(2) 0.0411(8) Uani 0.263(9) 1 d D U P B 2
H61' H 0.4502 0.0970 1.0117 0.049 Uiso 0.263(9) 1 calc R U P B 2
C62' C 0.547(2) 0.046(2) 0.9427(18) 0.047(3) Uani 0.263(9) 1 d D U P B 2
H62' H 0.4932 0.0248 0.8980 0.057 Uiso 0.263(9) 1 calc R U P B 2
C63' C 0.6645(19) 0.0340(13) 0.9528(14) 0.054(3) Uani 0.263(9) 1 d D U P B 2
H63' H 0.6955 -0.0020 0.9198 0.065 Uiso 0.263(9) 1 calc R U P B 2
C64' C 0.7278(18) 0.0847(15) 1.0203(14) 0.049(3) Uani 0.263(9) 1 d D U P B 2
H64' H 0.8026 0.0755 1.0239 0.058 Uiso 0.263(9) 1 calc R U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C57 2.013(8) . ?
W1 C56 2.017(4) . ?
W1 C58 2.031(3) . ?
W1 C55 2.039(8) . ?
W1 Si1 2.464(2) . ?
W1 Si2 2.4707(19) . ?
Cl1 Si1 2.1292(19) . ?
Cl2 Si1 2.134(2) . ?
Cl3 Si2 2.111(2) . ?
Cl4 Si2 2.1226(19) . ?
Si1 C1 1.996(3) . ?
Si2 C28 1.983(3) . ?
O55 C55 1.154(9) . ?
O56 C56 1.158(4) . ?
O57 C57 1.145(10) . ?
O58 C58 1.154(4) . ?
N1 C1 1.360(4) . ?
N1 C14 1.377(4) . ?
N1 C2 1.473(4) . ?
N2 C1 1.361(4) . ?
N2 C15 1.390(4) . ?
N2 C16 1.467(4) . ?
N3 C28 1.372(4) . ?
N3 C41 1.385(4) . ?
N3 C29 1.460(4) . ?
N4 C28 1.365(4) . ?
N4 C42 1.388(4) . ?
N4 C43 1.459(4) . ?
C2 C3 1.399(5) . ?
C2 C10 1.405(5) . ?
C3 C7 1.395(5) . ?
C3 C4 1.518(5) . ?
C4 C6 1.534(5) . ?
C4 C5 1.543(5) . ?
C4 H4 1.0000 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.389(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.381(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.395(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.524(5) . ?
C11 C12 1.526(5) . ?
C11 C13 1.541(5) . ?
C11 H11 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.337(5) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C24 1.390(5) . ?
C16 C17 1.392(5) . ?
C17 C21 1.397(6) . ?
C17 C18 1.520(6) . ?
C18 C20 1.523(6) . ?
C18 C19 1.538(8) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.363(7) . ?
C21 H21 0.9500 . ?
C22 C23 1.374(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.415(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.502(6) . ?
C25 C26 1.540(6) . ?
C25 C27 1.541(5) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C29 C37 1.398(5) . ?
C29 C30 1.400(5) . ?
C30 C34 1.395(5) . ?
C30 C31 1.514(5) . ?
C31 C33 1.533(5) . ?
C31 C32 1.551(6) . ?
C31 H31 1.0000 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.376(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.378(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.393(5) . ?
C36 H36 0.9500 . ?
C37 C38 1.521(5) . ?
C38 C39 1.525(6) . ?
C38 C40 1.526(6) . ?
C38 H38 1.0000 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.340(5) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C51 1.391(5) . ?
C43 C44 1.414(5) . ?
C44 C48 1.391(5) . ?
C44 C45 1.506(5) . ?
C45 C47 1.532(6) . ?
C45 C46 1.533(5) . ?
C45 H45 1.0000 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 C49 1.381(6) . ?
C48 H48 0.9500 . ?
C49 C50 1.377(6) . ?
C49 H49 0.9500 . ?
C50 C51 1.407(5) . ?
C50 H50 0.9500 . ?
C51 C52 1.520(5) . ?
C52 C54 1.526(5) . ?
C52 C53 1.535(5) . ?
C52 H52 1.0000 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C59 Cl5 1.762(11) . ?
C59 Cl6 1.769(10) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C59' Cl6' 1.767(19) . ?
C59' Cl5' 1.768(19) . ?
C59' H59C 0.9900 . ?
C59' H59D 0.9900 . ?
N5 C64 1.307(10) . ?
N5 C60 1.450(9) . ?
C60 C61 1.304(10) . ?
C60 H60 0.9500 . ?
C61 C62 1.473(9) . ?
C61 H61 0.9500 . ?
C62 C63 1.429(7) . ?
C62 H62 0.9500 . ?
C63 C64 1.435(10) . ?
C63 H63 0.9500 . ?
C64 H64 0.9500 . ?
N5' C64' 1.406(18) . ?
N5' C60' 1.462(19) . ?
C60' C61' 1.417(18) . ?
C60' H60' 0.9500 . ?
C61' C62' 1.42(2) . ?
C61' H61' 0.9500 . ?
C62' C63' 1.48(2) . ?
C62' H62' 0.9500 . ?
C63' C64' 1.475(19) . ?
C63' H63' 0.9500 . ?
C64' H64' 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
C57 W1 C56 82.92(17) . . ?
C57 W1 C58 87.03(18) . . ?
C56 W1 C58 169.94(16) . . ?
C57 W1 C55 176.7(4) . . ?
C56 W1 C55 94.64(14) . . ?
C58 W1 C55 95.40(15) . . ?
C57 W1 Si1 93.4(2) . . ?
C56 W1 Si1 98.56(11) . . ?
C58 W1 Si1 82.31(10) . . ?
C55 W1 Si1 89.2(2) . . ?
C57 W1 Si2 89.7(2) . . ?
C56 W1 Si2 83.63(11) . . ?
C58 W1 Si2 96.03(10) . . ?
C55 W1 Si2 87.8(2) . . ?
Si1 W1 Si2 176.41(7) . . ?
C1 Si1 Cl1 97.70(12) . . ?
C1 Si1 Cl2 99.55(13) . . ?
Cl1 Si1 Cl2 96.73(7) . . ?
C1 Si1 W1 126.15(11) . . ?
Cl1 Si1 W1 116.67(8) . . ?
Cl2 Si1 W1 114.80(8) . . ?
C28 Si2 Cl3 100.02(12) . . ?
C28 Si2 Cl4 99.77(12) . . ?
Cl3 Si2 Cl4 97.87(8) . . ?
C28 Si2 W1 123.96(11) . . ?
Cl3 Si2 W1 115.44(8) . . ?
Cl4 Si2 W1 115.48(8) . . ?
C1 N1 C14 110.5(3) . . ?
C1 N1 C2 128.9(3) . . ?
C14 N1 C2 120.1(3) . . ?
C1 N2 C15 110.4(3) . . ?
C1 N2 C16 129.0(3) . . ?
C15 N2 C16 119.7(3) . . ?
C28 N3 C41 110.8(3) . . ?
C28 N3 C29 129.9(3) . . ?
C41 N3 C29 118.9(3) . . ?
C28 N4 C42 110.8(3) . . ?
C28 N4 C43 127.9(3) . . ?
C42 N4 C43 120.4(3) . . ?
N1 C1 N2 104.7(3) . . ?
N1 C1 Si1 126.0(2) . . ?
N2 C1 Si1 128.8(2) . . ?
C3 C2 C10 123.7(3) . . ?
C3 C2 N1 119.2(3) . . ?
C10 C2 N1 116.7(3) . . ?
C7 C3 C2 116.9(3) . . ?
C7 C3 C4 120.6(3) . . ?
C2 C3 C4 122.3(3) . . ?
C3 C4 C6 114.5(3) . . ?
C3 C4 C5 109.6(3) . . ?
C6 C4 C5 107.5(3) . . ?
C3 C4 H4 108.3 . . ?
C6 C4 H4 108.3 . . ?
C5 C4 H4 108.3 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 C3 120.7(3) . . ?
C8 C7 H7 119.7 . . ?
C3 C7 H7 119.7 . . ?
C9 C8 C7 120.8(3) . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C8 C9 C10 121.1(3) . . ?
C8 C9 H9 119.4 . . ?
C10 C9 H9 119.4 . . ?
C9 C10 C2 116.6(3) . . ?
C9 C10 C11 120.2(3) . . ?
C2 C10 C11 123.1(3) . . ?
C10 C11 C12 113.5(3) . . ?
C10 C11 C13 110.3(3) . . ?
C12 C11 C13 109.1(3) . . ?
C10 C11 H11 107.9 . . ?
C12 C11 H11 107.9 . . ?
C13 C11 H11 107.9 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 N1 107.7(3) . . ?
C15 C14 H14 126.2 . . ?
N1 C14 H14 126.2 . . ?
C14 C15 N2 106.7(3) . . ?
C14 C15 H15 126.6 . . ?
N2 C15 H15 126.6 . . ?
C24 C16 C17 124.4(3) . . ?
C24 C16 N2 118.4(3) . . ?
C17 C16 N2 117.1(3) . . ?
C16 C17 C21 117.0(4) . . ?
C16 C17 C18 123.2(3) . . ?
C21 C17 C18 119.8(4) . . ?
C17 C18 C20 110.1(4) . . ?
C17 C18 C19 112.2(4) . . ?
C20 C18 C19 109.5(4) . . ?
C17 C18 H18 108.3 . . ?
C20 C18 H18 108.3 . . ?
C19 C18 H18 108.3 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C17 120.7(4) . . ?
C22 C21 H21 119.7 . . ?
C17 C21 H21 119.7 . . ?
C21 C22 C23 121.2(4) . . ?
C21 C22 H22 119.4 . . ?
C23 C22 H22 119.4 . . ?
C22 C23 C24 121.2(4) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 H23 119.4 . . ?
C16 C24 C23 115.4(4) . . ?
C16 C24 C25 122.2(3) . . ?
C23 C24 C25 122.3(3) . . ?
C24 C25 C26 112.1(4) . . ?
C24 C25 C27 112.9(3) . . ?
C26 C25 C27 108.8(3) . . ?
C24 C25 H25 107.6 . . ?
C26 C25 H25 107.6 . . ?
C27 C25 H25 107.6 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N4 C28 N3 104.1(3) . . ?
N4 C28 Si2 126.6(2) . . ?
N3 C28 Si2 128.5(2) . . ?
C37 C29 C30 123.8(3) . . ?
C37 C29 N3 117.7(3) . . ?
C30 C29 N3 118.1(3) . . ?
C34 C30 C29 116.4(3) . . ?
C34 C30 C31 121.2(3) . . ?
C29 C30 C31 122.4(3) . . ?
C30 C31 C33 113.2(3) . . ?
C30 C31 C32 110.1(3) . . ?
C33 C31 C32 108.5(3) . . ?
C30 C31 H31 108.3 . . ?
C33 C31 H31 108.3 . . ?
C32 C31 H31 108.3 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 C30 121.2(4) . . ?
C35 C34 H34 119.4 . . ?
C30 C34 H34 119.4 . . ?
C34 C35 C36 120.8(3) . . ?
C34 C35 H35 119.6 . . ?
C36 C35 H35 119.6 . . ?
C35 C36 C37 121.0(4) . . ?
C35 C36 H36 119.5 . . ?
C37 C36 H36 119.5 . . ?
C36 C37 C29 116.8(3) . . ?
C36 C37 C38 121.3(3) . . ?
C29 C37 C38 121.9(3) . . ?
C37 C38 C39 112.3(3) . . ?
C37 C38 C40 110.7(3) . . ?
C39 C38 C40 109.2(4) . . ?
C37 C38 H38 108.2 . . ?
C39 C38 H38 108.2 . . ?
C40 C38 H38 108.2 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 N3 107.1(3) . . ?
C42 C41 H41 126.5 . . ?
N3 C41 H41 126.5 . . ?
C41 C42 N4 107.2(3) . . ?
C41 C42 H42 126.4 . . ?
N4 C42 H42 126.4 . . ?
C51 C43 C44 123.9(3) . . ?
C51 C43 N4 119.4(3) . . ?
C44 C43 N4 116.3(3) . . ?
C48 C44 C43 116.3(3) . . ?
C48 C44 C45 121.5(3) . . ?
C43 C44 C45 122.1(3) . . ?
C44 C45 C47 109.8(3) . . ?
C44 C45 C46 113.8(4) . . ?
C47 C45 C46 109.4(3) . . ?
C44 C45 H45 107.9 . . ?
C47 C45 H45 107.9 . . ?
C46 C45 H45 107.9 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C49 C48 C44 121.1(4) . . ?
C49 C48 H48 119.5 . . ?
C44 C48 H48 119.5 . . ?
C50 C49 C48 121.3(3) . . ?
C50 C49 H49 119.4 . . ?
C48 C49 H49 119.4 . . ?
C49 C50 C51 120.6(4) . . ?
C49 C50 H50 119.7 . . ?
C51 C50 H50 119.7 . . ?
C43 C51 C50 116.6(3) . . ?
C43 C51 C52 122.3(3) . . ?
C50 C51 C52 120.8(3) . . ?
C51 C52 C54 113.6(3) . . ?
C51 C52 C53 108.7(3) . . ?
C54 C52 C53 108.6(3) . . ?
C51 C52 H52 108.6 . . ?
C54 C52 H52 108.6 . . ?
C53 C52 H52 108.6 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C52 C54 H54A 109.5 . . ?
C52 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C52 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
O55 C55 W1 178.2(7) . . ?
O56 C56 W1 173.8(3) . . ?
O57 C57 W1 176.7(6) . . ?
O58 C58 W1 174.8(3) . . ?
Cl5 C59 Cl6 115.0(8) . . ?
Cl5 C59 H59A 108.5 . . ?
Cl6 C59 H59A 108.5 . . ?
Cl5 C59 H59B 108.5 . . ?
Cl6 C59 H59B 108.5 . . ?
H59A C59 H59B 107.5 . . ?
Cl6' C59' Cl5' 103.4(15) . . ?
Cl6' C59' H59C 111.1 . . ?
Cl5' C59' H59C 111.1 . . ?
Cl6' C59' H59D 111.1 . . ?
Cl5' C59' H59D 111.1 . . ?
H59C C59' H59D 109.1 . . ?
C64 N5 C60 117.0(6) . . ?
C61 C60 N5 126.2(7) . . ?
C61 C60 H60 116.9 . . ?
N5 C60 H60 116.9 . . ?
C60 C61 C62 116.4(7) . . ?
C60 C61 H61 121.8 . . ?
C62 C61 H61 121.8 . . ?
C63 C62 C61 119.6(6) . . ?
C63 C62 H62 120.2 . . ?
C61 C62 H62 120.2 . . ?
C62 C63 C64 117.3(6) . . ?
C62 C63 H63 121.4 . . ?
C64 C63 H63 121.4 . . ?
N5 C64 C63 123.5(7) . . ?
N5 C64 H64 118.2 . . ?
C63 C64 H64 118.3 . . ?
C64' N5' C60' 97.6(16) . . ?
C61' C60' N5' 128.9(16) . . ?
C61' C60' H60' 115.6 . . ?
N5' C60' H60' 115.6 . . ?
C60' C61' C62' 126.5(13) . . ?
C60' C61' H61' 116.8 . . ?
C62' C61' H61' 116.8 . . ?
C61' C62' C63' 111.7(18) . . ?
C61' C62' H62' 124.1 . . ?
C63' C62' H62' 124.1 . . ?
C64' C63' C62' 111.5(17) . . ?
C64' C63' H63' 124.2 . . ?
C62' C63' H63' 124.2 . . ?
N5' C64' C63' 142.8(19) . . ?
N5' C64' H64' 108.6 . . ?
C63' C64' H64' 108.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14 N1 C1 N2 -1.1(4) . . . . ?
C2 N1 C1 N2 -172.5(3) . . . . ?
C14 N1 C1 Si1 -173.8(3) . . . . ?
C2 N1 C1 Si1 14.8(5) . . . . ?
C15 N2 C1 N1 0.9(4) . . . . ?
C16 N2 C1 N1 170.1(3) . . . . ?
C15 N2 C1 Si1 173.4(3) . . . . ?
C16 N2 C1 Si1 -17.5(5) . . . . ?
C1 N1 C2 C3 -99.0(4) . . . . ?
C14 N1 C2 C3 90.3(4) . . . . ?
C1 N1 C2 C10 88.0(4) . . . . ?
C14 N1 C2 C10 -82.7(4) . . . . ?
C10 C2 C3 C7 -4.2(5) . . . . ?
N1 C2 C3 C7 -176.6(3) . . . . ?
C10 C2 C3 C4 170.7(3) . . . . ?
N1 C2 C3 C4 -1.7(4) . . . . ?
C7 C3 C4 C6 -32.0(5) . . . . ?
C2 C3 C4 C6 153.3(3) . . . . ?
C7 C3 C4 C5 88.9(5) . . . . ?
C2 C3 C4 C5 -85.8(5) . . . . ?
C2 C3 C7 C8 2.1(5) . . . . ?
C4 C3 C7 C8 -172.9(3) . . . . ?
C3 C7 C8 C9 0.5(5) . . . . ?
C7 C8 C9 C10 -1.2(5) . . . . ?
C8 C9 C10 C2 -0.7(5) . . . . ?
C8 C9 C10 C11 176.3(3) . . . . ?
C3 C2 C10 C9 3.5(5) . . . . ?
N1 C2 C10 C9 176.2(3) . . . . ?
C3 C2 C10 C11 -173.5(3) . . . . ?
N1 C2 C10 C11 -0.8(4) . . . . ?
C9 C10 C11 C12 39.0(4) . . . . ?
C2 C10 C11 C12 -144.1(3) . . . . ?
C9 C10 C11 C13 -83.8(4) . . . . ?
C2 C10 C11 C13 93.1(4) . . . . ?
C1 N1 C14 C15 0.8(4) . . . . ?
C2 N1 C14 C15 173.1(3) . . . . ?
N1 C14 C15 N2 -0.2(4) . . . . ?
C1 N2 C15 C14 -0.5(4) . . . . ?
C16 N2 C15 C14 -170.8(3) . . . . ?
C1 N2 C16 C24 93.9(4) . . . . ?
C15 N2 C16 C24 -97.8(4) . . . . ?
C1 N2 C16 C17 -88.7(4) . . . . ?
C15 N2 C16 C17 79.5(4) . . . . ?
C24 C16 C17 C21 -2.4(5) . . . . ?
N2 C16 C17 C21 -179.6(3) . . . . ?
C24 C16 C17 C18 177.4(3) . . . . ?
N2 C16 C17 C18 0.2(5) . . . . ?
C16 C17 C18 C20 -111.4(4) . . . . ?
C21 C17 C18 C20 68.4(5) . . . . ?
C16 C17 C18 C19 126.3(4) . . . . ?
C21 C17 C18 C19 -53.9(5) . . . . ?
C16 C17 C21 C22 1.5(6) . . . . ?
C18 C17 C21 C22 -178.4(4) . . . . ?
C17 C21 C22 C23 0.7(7) . . . . ?
C21 C22 C23 C24 -2.1(6) . . . . ?
C17 C16 C24 C23 1.1(5) . . . . ?
N2 C16 C24 C23 178.3(3) . . . . ?
C17 C16 C24 C25 -177.4(3) . . . . ?
N2 C16 C24 C25 -0.3(5) . . . . ?
C22 C23 C24 C16 1.1(5) . . . . ?
C22 C23 C24 C25 179.7(4) . . . . ?
C16 C24 C25 C26 79.5(4) . . . . ?
C23 C24 C25 C26 -98.9(4) . . . . ?
C16 C24 C25 C27 -157.2(3) . . . . ?
C23 C24 C25 C27 24.4(5) . . . . ?
C42 N4 C28 N3 -0.6(3) . . . . ?
C43 N4 C28 N3 -169.4(3) . . . . ?
C42 N4 C28 Si2 -171.1(2) . . . . ?
C43 N4 C28 Si2 20.1(5) . . . . ?
C41 N3 C28 N4 0.6(3) . . . . ?
C29 N3 C28 N4 173.0(3) . . . . ?
C41 N3 C28 Si2 170.9(2) . . . . ?
C29 N3 C28 Si2 -16.7(5) . . . . ?
C28 N3 C29 C37 -85.8(4) . . . . ?
C41 N3 C29 C37 86.1(4) . . . . ?
C28 N3 C29 C30 100.9(4) . . . . ?
C41 N3 C29 C30 -87.2(4) . . . . ?
C37 C29 C30 C34 1.4(5) . . . . ?
N3 C29 C30 C34 174.3(3) . . . . ?
C37 C29 C30 C31 -176.8(3) . . . . ?
N3 C29 C30 C31 -4.0(5) . . . . ?
C34 C30 C31 C33 34.6(5) . . . . ?
C29 C30 C31 C33 -147.2(3) . . . . ?
C34 C30 C31 C32 -87.0(4) . . . . ?
C29 C30 C31 C32 91.2(4) . . . . ?
C29 C30 C34 C35 -0.1(5) . . . . ?
C31 C30 C34 C35 178.1(3) . . . . ?
C30 C34 C35 C36 -0.7(6) . . . . ?
C34 C35 C36 C37 0.2(6) . . . . ?
C35 C36 C37 C29 1.0(5) . . . . ?
C35 C36 C37 C38 -177.8(3) . . . . ?
C30 C29 C37 C36 -1.9(5) . . . . ?
N3 C29 C37 C36 -174.7(3) . . . . ?
C30 C29 C37 C38 176.9(3) . . . . ?
N3 C29 C37 C38 4.1(5) . . . . ?
C36 C37 C38 C39 -42.5(5) . . . . ?
C29 C37 C38 C39 138.8(4) . . . . ?
C36 C37 C38 C40 79.9(5) . . . . ?
C29 C37 C38 C40 -98.8(4) . . . . ?
C28 N3 C41 C42 -0.4(4) . . . . ?
C29 N3 C41 C42 -173.8(3) . . . . ?
N3 C41 C42 N4 0.0(4) . . . . ?
C28 N4 C42 C41 0.3(4) . . . . ?
C43 N4 C42 C41 170.1(3) . . . . ?
C28 N4 C43 C51 -104.4(4) . . . . ?
C42 N4 C43 C51 87.7(4) . . . . ?
C28 N4 C43 C44 82.1(4) . . . . ?
C42 N4 C43 C44 -85.8(4) . . . . ?
C51 C43 C44 C48 5.2(5) . . . . ?
N4 C43 C44 C48 178.3(3) . . . . ?
C51 C43 C44 C45 -171.0(3) . . . . ?
N4 C43 C44 C45 2.2(5) . . . . ?
C48 C44 C45 C47 -83.2(4) . . . . ?
C43 C44 C45 C47 92.7(4) . . . . ?
C48 C44 C45 C46 39.7(5) . . . . ?
C43 C44 C45 C46 -144.3(4) . . . . ?
C43 C44 C48 C49 -1.0(5) . . . . ?
C45 C44 C48 C49 175.2(4) . . . . ?
C44 C48 C49 C50 -2.7(6) . . . . ?
C48 C49 C50 C51 2.6(6) . . . . ?
C44 C43 C51 C50 -5.3(5) . . . . ?
N4 C43 C51 C50 -178.3(3) . . . . ?
C44 C43 C51 C52 168.2(3) . . . . ?
N4 C43 C51 C52 -4.8(5) . . . . ?
C49 C50 C51 C43 1.3(5) . . . . ?
C49 C50 C51 C52 -172.2(3) . . . . ?
C43 C51 C52 C54 146.0(3) . . . . ?
C50 C51 C52 C54 -40.8(4) . . . . ?
C43 C51 C52 C53 -93.0(4) . . . . ?
C50 C51 C52 C53 80.2(4) . . . . ?
C64 N5 C60 C61 2.9(10) . . . . ?
N5 C60 C61 C62 0.6(10) . . . . ?
C60 C61 C62 C63 -2.6(9) . . . . ?
C61 C62 C63 C64 1.3(9) . . . . ?
C60 N5 C64 C63 -4.4(13) . . . . ?
C62 C63 C64 N5 2.4(13) . . . . ?
C64' N5' C60' C61' -5.6(18) . . . . ?
N5' C60' C61' C62' -2(2) . . . . ?
C60' C61' C62' C63' 10(3) . . . . ?
C61' C62' C63' C64' -9(3) . . . . ?
C60' N5' C64' C63' 6(4) . . . . ?
C62' C63' C64' N5' 1(5) . . . . ?

_refine_diff_density_max         0.765
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.053

####################################################################### 
# 
# 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_Compound_4Cr
_database_code_depnum_ccdc_archive 'CCDC 1514802'
_audit_update_record             
;
2016-11-03 deposited with the CCDC.
2017-05-22 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         'C58 H72 Cl4 Cr N4 O4 Si2, 2(C H2 Cl2)'
_chemical_formula_sum            'C45 H57 Cl6 Cr0.75 N3 O3 Si1.50'
_chemical_formula_weight         981.77

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   12.434(2)
_cell_length_b                   48.155(4)
_cell_length_c                   16.728(2)
_cell_angle_alpha                90
_cell_angle_beta                 105.65(3)
_cell_angle_gamma                90
_cell_volume                     9645(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9904
_cell_measurement_theta_min      2.2225
_cell_measurement_theta_max      24.8235

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_F_000             4104
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.595
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4066
_exptl_absorpt_correction_T_max  0.4286
_exptl_absorpt_process_details   SADABS-2016/1
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'BRUKER Rotating Anode'
_diffrn_measurement_device_type  'Bruker Smart APEX II Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            142790
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_k_max       55
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.333
_diffrn_reflns_theta_max         25.062
_diffrn_reflns_theta_full        25.062
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.970
_reflns_number_total             16579
_reflns_number_gt                12672
_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 v2012.2'
_computing_cell_refinement       'SAINT V8.30C'
_computing_data_reduction        'SAINT V8.30C'
_computing_structure_solution    
'SHELXT (G.M.Sheldrick,Acta Cryst.(2015)A71,3-8)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'
_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)+(0.0339P)²+13.6765P] 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         16579
_refine_ls_number_parameters     1121
_refine_ls_number_restraints     81
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0430
_refine_ls_wR_factor_ref         0.0983
_refine_ls_wR_factor_gt          0.0887
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Cr1 Cr 0.04481(3) 0.33082(2) 0.07576(3) 0.01376(10) Uani 1 1 d . . . . .
Cr2 Cr 0.5000 0.5000 0.5000 0.01630(15) Uani 1 2 d S . P . .
Cl1 Cl 0.34367(6) 0.30815(2) 0.17884(4) 0.02205(16) Uani 1 1 d . . . . .
Cl2 Cl 0.17577(6) 0.30921(2) 0.29405(4) 0.02032(16) Uani 1 1 d . . . . .
Cl3 Cl -0.09484(6) 0.35850(2) -0.13982(4) 0.01998(16) Uani 1 1 d . . . . .
Cl4 Cl -0.25375(6) 0.34911(2) -0.02092(4) 0.02248(16) Uani 1 1 d . . . . .
Cl5 Cl 0.74189(8) 0.52301(2) 0.67083(6) 0.0545(3) Uani 1 1 d . . . . .
Cl6 Cl 0.52529(10) 0.51042(2) 0.72841(5) 0.0524(3) Uani 1 1 d . . . . .
Cl7 Cl 0.86924(8) 0.31787(2) 0.44879(5) 0.0462(2) Uani 1 1 d . . . . .
Cl8 Cl 0.95335(7) 0.26913(2) 0.37957(6) 0.0394(2) Uani 1 1 d . . . . .
Cl9 Cl 0.27200(7) 0.36808(2) 0.76682(6) 0.0397(2) Uani 1 1 d . . . . .
Cl10 Cl 0.06492(8) 0.39876(3) 0.72242(9) 0.0771(4) Uani 1 1 d . . . . .
Si1 Si 0.20033(6) 0.33051(2) 0.18884(4) 0.01413(16) Uani 1 1 d . . . . .
Si2 Si -0.10655(6) 0.33199(2) -0.04028(4) 0.01372(16) Uani 1 1 d . . . . .
Si3 Si 0.60186(7) 0.49667(2) 0.63688(5) 0.02367(19) Uani 1 1 d . . . . .
O1 O -0.01244(18) 0.39083(5) 0.09857(15) 0.0349(6) Uani 1 1 d . . . . .
O2 O 0.19514(17) 0.33778(4) -0.03933(12) 0.0233(5) Uani 1 1 d . . . . .
O3 O 0.05486(19) 0.26819(5) 0.08984(13) 0.0328(5) Uani 1 1 d . . . . .
O4 O -0.11012(18) 0.32463(5) 0.18536(13) 0.0336(5) Uani 1 1 d . . . . .
O5 O 0.7160(2) 0.50753(5) 0.4532(2) 0.0597(8) Uani 1 1 d . . . . .
O6 O 0.49669(18) 0.43884(5) 0.45828(13) 0.0298(5) Uani 1 1 d . . . . .
N1 N 0.33580(18) 0.38295(5) 0.21242(13) 0.0154(5) Uani 1 1 d . . . . .
N2 N 0.27200(18) 0.37603(5) 0.31822(13) 0.0155(5) Uani 1 1 d . . . . .
N3 N -0.25566(17) 0.28223(4) -0.09914(13) 0.0127(5) Uani 1 1 d . . . . .
N4 N -0.11942(17) 0.28339(4) -0.15619(13) 0.0132(5) Uani 1 1 d . . . . .
N5 N 0.7650(2) 0.44982(5) 0.68819(15) 0.0247(6) Uani 1 1 d . . . . .
N6 N 0.6202(2) 0.44302(5) 0.73335(15) 0.0223(6) Uani 1 1 d . . . . .
C1 C 0.2785(2) 0.36400(6) 0.24577(16) 0.0145(6) Uani 1 1 d . . . . .
C2 C 0.3624(2) 0.40599(6) 0.26260(17) 0.0203(6) Uani 1 1 d . . . . .
H2 H 0.4018 0.4219 0.2524 0.024 Uiso 1 1 calc R U . . .
C3 C 0.3228(2) 0.40181(6) 0.32798(17) 0.0197(6) Uani 1 1 d . . . . .
H3 H 0.3285 0.4142 0.3730 0.024 Uiso 1 1 calc R U . . .
C4 C 0.3792(2) 0.38028(6) 0.13974(17) 0.0181(6) Uani 1 1 d . . . . .
C5 C 0.3231(2) 0.39434(6) 0.06749(17) 0.0197(6) Uani 1 1 d . . . . .
C6 C 0.3720(3) 0.39301(6) 0.00175(18) 0.0232(7) Uani 1 1 d . . . . .
H6 H 0.3361 0.4020 -0.0490 0.028 Uiso 1 1 calc R U . . .
C7 C 0.4706(3) 0.37911(6) 0.00810(18) 0.0272(7) Uani 1 1 d . . . . .
H7 H 0.5006 0.3780 -0.0384 0.033 Uiso 1 1 calc R U . . .
C8 C 0.5261(3) 0.36665(6) 0.08246(19) 0.0263(7) Uani 1 1 d . . . . .
H8 H 0.5950 0.3574 0.0867 0.032 Uiso 1 1 calc R U . . .
C9 C 0.4832(2) 0.36738(6) 0.15103(18) 0.0200(6) Uani 1 1 d . . . . .
C10 C 0.2207(2) 0.41206(6) 0.06188(18) 0.0236(7) Uani 1 1 d . . . . .
H10 H 0.1875 0.4063 0.1076 0.028 Uiso 1 1 calc R U . . .
C11 C 0.1314(3) 0.40912(7) -0.01985(19) 0.0338(8) Uani 1 1 d . . . . .
H11A H 0.0646 0.4194 -0.0171 0.051 Uiso 1 1 calc R U . . .
H11B H 0.1125 0.3895 -0.0303 0.051 Uiso 1 1 calc R U . . .
H11C H 0.1594 0.4166 -0.0649 0.051 Uiso 1 1 calc R U . . .
C12 C 0.2530(3) 0.44278(6) 0.0743(2) 0.0341(8) Uani 1 1 d . . . . .
H12A H 0.3094 0.4452 0.1275 0.051 Uiso 1 1 calc R U . . .
H12B H 0.1868 0.4538 0.0742 0.051 Uiso 1 1 calc R U . . .
H12C H 0.2836 0.4490 0.0291 0.051 Uiso 1 1 calc R U . . .
C13 C 0.5521(2) 0.35728(6) 0.23551(18) 0.0245(7) Uani 1 1 d . . . . .
H13 H 0.4994 0.3522 0.2690 0.029 Uiso 1 1 calc R U . . .
C14 C 0.6233(3) 0.33195(7) 0.2311(2) 0.0324(8) Uani 1 1 d . . . . .
H14A H 0.6607 0.3257 0.2874 0.049 Uiso 1 1 calc R U . . .
H14B H 0.6794 0.3368 0.2021 0.049 Uiso 1 1 calc R U . . .
H14C H 0.5756 0.3170 0.2009 0.049 Uiso 1 1 calc R U . . .
C15 C 0.6272(3) 0.38067(7) 0.2808(2) 0.0362(8) Uani 1 1 d . . . . .
H15A H 0.6730 0.3739 0.3344 0.054 Uiso 1 1 calc R U . . .
H15B H 0.5810 0.3962 0.2899 0.054 Uiso 1 1 calc R U . . .
H15C H 0.6759 0.3870 0.2471 0.054 Uiso 1 1 calc R U . . .
C16 C 0.2309(2) 0.36550(6) 0.38594(16) 0.0171(6) Uani 1 1 d . . . . .
C17 C 0.3020(2) 0.34832(6) 0.44495(17) 0.0190(6) Uani 1 1 d . . . . .
C18 C 0.2670(3) 0.34184(6) 0.51485(17) 0.0231(7) Uani 1 1 d . . . . .
H18 H 0.3129 0.3304 0.5567 0.028 Uiso 1 1 calc R U . . .
C19 C 0.1672(3) 0.35158(6) 0.52500(18) 0.0244(7) Uani 1 1 d . . . . .
H19 H 0.1457 0.3470 0.5737 0.029 Uiso 1 1 calc R U . . .
C20 C 0.0991(3) 0.36785(6) 0.46521(19) 0.0255(7) Uani 1 1 d . . . . .
H20 H 0.0299 0.3741 0.4726 0.031 Uiso 1 1 calc R U . . .
C21 C 0.1292(2) 0.37544(6) 0.39351(17) 0.0203(6) Uani 1 1 d . . . . .
C22 C 0.4108(2) 0.33674(6) 0.43254(18) 0.0248(7) Uani 1 1 d . . . . .
H22 H 0.4010 0.3353 0.3713 0.030 Uiso 1 1 calc R U . . .
C23 C 0.4358(3) 0.30764(7) 0.4685(2) 0.0332(8) Uani 1 1 d . . . . .
H23A H 0.4513 0.3085 0.5291 0.050 Uiso 1 1 calc R U . . .
H23B H 0.5011 0.3001 0.4536 0.050 Uiso 1 1 calc R U . . .
H23C H 0.3712 0.2956 0.4460 0.050 Uiso 1 1 calc R U . . .
C24 C 0.5108(3) 0.35584(8) 0.4676(2) 0.0408(9) Uani 1 1 d . . . . .
H24A H 0.5238 0.3574 0.5279 0.061 Uiso 1 1 calc R U . . .
H24B H 0.4952 0.3743 0.4423 0.061 Uiso 1 1 calc R U . . .
H24C H 0.5773 0.3481 0.4552 0.061 Uiso 1 1 calc R U . . .
C25 C 0.0543(2) 0.39426(7) 0.32936(19) 0.0277(7) Uani 1 1 d . . . . .
H25 H 0.0833 0.3945 0.2791 0.033 Uiso 1 1 calc R U . . .
C26 C 0.0569(3) 0.42421(7) 0.3625(2) 0.0396(9) Uani 1 1 d . . . . .
H26A H 0.1330 0.4316 0.3737 0.059 Uiso 1 1 calc R U . . .
H26B H 0.0332 0.4242 0.4138 0.059 Uiso 1 1 calc R U . . .
H26C H 0.0061 0.4359 0.3209 0.059 Uiso 1 1 calc R U . . .
C27 C -0.0656(3) 0.38366(7) 0.3034(2) 0.0342(8) Uani 1 1 d . . . . .
H27A H -0.0974 0.3845 0.3510 0.051 Uiso 1 1 calc R U . . .
H27B H -0.0665 0.3644 0.2844 0.051 Uiso 1 1 calc R U . . .
H27C H -0.1100 0.3952 0.2583 0.051 Uiso 1 1 calc R U . . .
C28 C -0.1685(2) 0.29842(6) -0.10594(15) 0.0135(6) Uani 1 1 d . . . . .
C29 C -0.2606(2) 0.25822(6) -0.14433(16) 0.0154(6) Uani 1 1 d . . . . .
H29 H -0.3145 0.2439 -0.1498 0.019 Uiso 1 1 calc R U . . .
C30 C -0.1756(2) 0.25871(6) -0.17916(16) 0.0165(6) Uani 1 1 d . . . . .
H30 H -0.1574 0.2447 -0.2133 0.020 Uiso 1 1 calc R U . . .
C31 C -0.3506(2) 0.28987(5) -0.06782(16) 0.0135(6) Uani 1 1 d . . . . .
C32 C -0.4389(2) 0.30368(6) -0.12279(16) 0.0169(6) Uani 1 1 d . . . . .
C33 C -0.5300(2) 0.31064(6) -0.09399(18) 0.0208(7) Uani 1 1 d . . . . .
H33 H -0.5908 0.3205 -0.1292 0.025 Uiso 1 1 calc R U . . .
C34 C -0.5336(2) 0.30345(6) -0.01498(18) 0.0214(7) Uani 1 1 d . . . . .
H34 H -0.5955 0.3089 0.0045 0.026 Uiso 1 1 calc R U . . .
C35 C -0.4479(2) 0.28833(6) 0.03587(17) 0.0199(6) Uani 1 1 d . . . . .
H35 H -0.4535 0.2827 0.0890 0.024 Uiso 1 1 calc R U . . .
C36 C -0.3535(2) 0.28115(6) 0.01128(16) 0.0159(6) Uani 1 1 d . . . . .
C37 C -0.4393(2) 0.31029(6) -0.21169(17) 0.0229(7) Uani 1 1 d . . . . .
H37 H -0.3687 0.3027 -0.2208 0.027 Uiso 1 1 calc R U . . .
C38 C -0.5362(3) 0.29573(9) -0.2720(2) 0.0503(11) Uani 1 1 d . . . . .
H38A H -0.6068 0.3029 -0.2651 0.075 Uiso 1 1 calc R U . . .
H38B H -0.5317 0.2757 -0.2609 0.075 Uiso 1 1 calc R U . . .
H38C H -0.5327 0.2991 -0.3290 0.075 Uiso 1 1 calc R U . . .
C39 C -0.4407(3) 0.34154(7) -0.2284(2) 0.0404(9) Uani 1 1 d . . . . .
H39A H -0.3728 0.3500 -0.1929 0.061 Uiso 1 1 calc R U . . .
H39B H -0.5063 0.3499 -0.2160 0.061 Uiso 1 1 calc R U . . .
H39C H -0.4439 0.3448 -0.2868 0.061 Uiso 1 1 calc R U . . .
C40 C -0.2605(2) 0.26364(6) 0.06650(17) 0.0217(7) Uani 1 1 d . . . . .
H40 H -0.1883 0.2689 0.0551 0.026 Uiso 1 1 calc R U . . .
C41 C -0.2494(3) 0.26799(7) 0.15879(18) 0.0288(7) Uani 1 1 d . . . . .
H41A H -0.1794 0.2597 0.1915 0.043 Uiso 1 1 calc R U . . .
H41B H -0.3125 0.2592 0.1735 0.043 Uiso 1 1 calc R U . . .
H41C H -0.2492 0.2879 0.1706 0.043 Uiso 1 1 calc R U . . .
C42 C -0.2814(3) 0.23275(6) 0.04729(19) 0.0328(8) Uani 1 1 d . . . . .
H42A H -0.3525 0.2273 0.0575 0.049 Uiso 1 1 calc R U . . .
H42B H -0.2207 0.2218 0.0831 0.049 Uiso 1 1 calc R U . . .
H42C H -0.2845 0.2293 -0.0110 0.049 Uiso 1 1 calc R U . . .
C43 C -0.0327(2) 0.29181(6) -0.19534(16) 0.0146(6) Uani 1 1 d . . . . .
C44 C 0.0744(2) 0.28068(6) -0.16589(16) 0.0168(6) Uani 1 1 d . . . . .
C45 C 0.1524(2) 0.28795(6) -0.20855(17) 0.0203(6) Uani 1 1 d . . . . .
H45 H 0.2271 0.2815 -0.1888 0.024 Uiso 1 1 calc R U . . .
C46 C 0.1232(2) 0.30422(6) -0.27870(18) 0.0232(7) Uani 1 1 d . . . . .
H46 H 0.1779 0.3090 -0.3065 0.028 Uiso 1 1 calc R U . . .
C47 C 0.0151(2) 0.31359(6) -0.30893(17) 0.0211(7) Uani 1 1 d . . . . .
H47 H -0.0042 0.3243 -0.3585 0.025 Uiso 1 1 calc R U . . .
C48 C -0.0661(2) 0.30770(6) -0.26827(16) 0.0173(6) Uani 1 1 d . . . . .
C49 C 0.1054(2) 0.25892(6) -0.09825(17) 0.0202(6) Uani 1 1 d . . . . .
H49 H 0.0445 0.2579 -0.0696 0.024 Uiso 1 1 calc R U . . .
C50 C 0.1137(3) 0.23053(6) -0.1391(2) 0.0275(7) Uani 1 1 d . . . . .
H50A H 0.1374 0.2164 -0.0958 0.041 Uiso 1 1 calc R U . . .
H50B H 0.1684 0.2317 -0.1716 0.041 Uiso 1 1 calc R U . . .
H50C H 0.0405 0.2255 -0.1757 0.041 Uiso 1 1 calc R U . . .
C51 C 0.2153(2) 0.26485(6) -0.03348(18) 0.0234(7) Uani 1 1 d . . . . .
H51A H 0.2272 0.2510 0.0109 0.035 Uiso 1 1 calc R U . . .
H51B H 0.2126 0.2834 -0.0101 0.035 Uiso 1 1 calc R U . . .
H51C H 0.2769 0.2640 -0.0596 0.035 Uiso 1 1 calc R U . . .
C52 C -0.1866(2) 0.31653(6) -0.30570(17) 0.0214(7) Uani 1 1 d . . . . .
H52 H -0.2232 0.3181 -0.2595 0.026 Uiso 1 1 calc R U . . .
C53 C -0.2494(3) 0.29426(7) -0.36615(18) 0.0304(8) Uani 1 1 d . . . . .
H53A H -0.2477 0.2766 -0.3365 0.046 Uiso 1 1 calc R U . . .
H53B H -0.2135 0.2918 -0.4111 0.046 Uiso 1 1 calc R U . . .
H53C H -0.3271 0.3001 -0.3894 0.046 Uiso 1 1 calc R U . . .
C54 C -0.1972(3) 0.34451(6) -0.34966(18) 0.0249(7) Uani 1 1 d . . . . .
H54A H -0.1485 0.3581 -0.3136 0.037 Uiso 1 1 calc R U . . .
H54B H -0.2748 0.3509 -0.3623 0.037 Uiso 1 1 calc R U . . .
H54C H -0.1751 0.3426 -0.4014 0.037 Uiso 1 1 calc R U . . .
C55 C 0.0140(2) 0.36864(7) 0.08663(18) 0.0229(7) Uani 1 1 d . . . . .
C56 C 0.1389(2) 0.33524(6) 0.00464(17) 0.0173(6) Uani 1 1 d . . . . .
C57 C 0.0544(2) 0.29195(7) 0.08144(17) 0.0199(7) Uani 1 1 d . . . . .
C58 C -0.0502(2) 0.32669(6) 0.14326(17) 0.0211(7) Uani 1 1 d . . . . .
C59 C 0.6677(2) 0.46199(6) 0.69230(17) 0.0211(7) Uani 1 1 d . . . . .
C60 C 0.7778(3) 0.42423(6) 0.7267(2) 0.0293(8) Uani 1 1 d . . . . .
H60 H 0.8392 0.4119 0.7324 0.035 Uiso 1 1 calc R U . . .
C61 C 0.6884(3) 0.41994(6) 0.75445(19) 0.0283(7) Uani 1 1 d . . . . .
H61 H 0.6740 0.4040 0.7834 0.034 Uiso 1 1 calc R U . . .
C62 C 0.8553(3) 0.46155(7) 0.6584(2) 0.0310(8) Uani 1 1 d . . . . .
C63 C 0.9356(3) 0.47752(7) 0.7157(2) 0.0397(9) Uani 1 1 d . . . . .
C64 C 1.0248(3) 0.48709(8) 0.6884(3) 0.0513(10) Uani 1 1 d . . . . .
H64 H 1.0810 0.4980 0.7246 0.062 Uiso 1 1 calc R U . . .
C65 C 1.0334(3) 0.48110(8) 0.6106(3) 0.0499(10) Uani 1 1 d . . . . .
H65 H 1.0950 0.4881 0.5934 0.060 Uiso 1 1 calc R U . . .
C66 C 0.9547(3) 0.46511(8) 0.5564(2) 0.0446(10) Uani 1 1 d . . . . .
H66 H 0.9632 0.4613 0.5027 0.054 Uiso 1 1 calc R U . . .
C67 C 0.8618(3) 0.45432(7) 0.5791(2) 0.0320(8) Uani 1 1 d . . . . .
C68 C 0.9283(3) 0.48384(8) 0.8035(2) 0.0473(10) Uani 1 1 d . . . . .
H68 H 0.8475 0.4834 0.8026 0.057 Uiso 1 1 calc R U . . .
C69 C 0.9873(4) 0.46152(10) 0.8629(3) 0.0723(14) Uani 1 1 d . . . . .
H69A H 0.9810 0.4656 0.9188 0.108 Uiso 1 1 calc R U . . .
H69B H 1.0663 0.4610 0.8635 0.108 Uiso 1 1 calc R U . . .
H69C H 0.9529 0.4435 0.8448 0.108 Uiso 1 1 calc R U . . .
C70 C 0.9749(4) 0.51226(9) 0.8373(3) 0.0618(12) Uani 1 1 d . . . . .
H70A H 0.9621 0.5152 0.8919 0.093 Uiso 1 1 calc R U . . .
H70B H 0.9371 0.5269 0.7991 0.093 Uiso 1 1 calc R U . . .
H70C H 1.0552 0.5129 0.8424 0.093 Uiso 1 1 calc R U . . .
C71 C 0.7792(3) 0.43536(7) 0.5222(2) 0.0346(8) Uani 1 1 d . . . . .
H71 H 0.7066 0.4369 0.5369 0.042 Uiso 1 1 calc R U . . .
C72 C 0.8182(4) 0.40511(8) 0.5353(2) 0.0584(12) Uani 1 1 d . . . . .
H72A H 0.8221 0.3995 0.5923 0.088 Uiso 1 1 calc R U . . .
H72B H 0.8922 0.4034 0.5257 0.088 Uiso 1 1 calc R U . . .
H72C H 0.7652 0.3932 0.4962 0.088 Uiso 1 1 calc R U . . .
C73 C 0.7571(4) 0.44159(8) 0.4297(2) 0.0482(10) Uani 1 1 d . . . . .
H73A H 0.8232 0.4367 0.4114 0.072 Uiso 1 1 calc R U . . .
H73B H 0.7411 0.4614 0.4199 0.072 Uiso 1 1 calc R U . . .
H73C H 0.6930 0.4307 0.3984 0.072 Uiso 1 1 calc R U . . .
C74 C 0.5246(3) 0.44631(6) 0.76759(18) 0.0238(7) Uani 1 1 d . . . . .
C75 C 0.4172(3) 0.44006(6) 0.71875(19) 0.0252(7) Uani 1 1 d . . . . .
C76 C 0.3305(3) 0.44338(7) 0.7562(2) 0.0328(8) Uani 1 1 d . . . . .
H76 H 0.2558 0.4399 0.7248 0.039 Uiso 1 1 calc R U . . .
C77 C 0.3511(3) 0.45167(7) 0.8382(2) 0.0395(9) Uani 1 1 d . . . . .
H77 H 0.2907 0.4541 0.8622 0.047 Uiso 1 1 calc R U . . .
C78 C 0.4583(3) 0.45648(7) 0.8850(2) 0.0377(9) Uani 1 1 d . . . . .
H78 H 0.4713 0.4616 0.9416 0.045 Uiso 1 1 calc R U . . .
C79 C 0.5487(3) 0.45397(6) 0.85094(19) 0.0296(7) Uani 1 1 d . . . . .
C80 C 0.3955(3) 0.42983(6) 0.63031(19) 0.0295(8) Uani 1 1 d . . . . .
H80 H 0.4335 0.4430 0.6004 0.035 Uiso 1 1 calc R U . . .
C81 C 0.2714(3) 0.42914(7) 0.5828(2) 0.0422(9) Uani 1 1 d . . . . .
H81A H 0.2366 0.4469 0.5900 0.063 Uiso 1 1 calc R U . . .
H81B H 0.2342 0.4141 0.6044 0.063 Uiso 1 1 calc R U . . .
H81C H 0.2640 0.4260 0.5237 0.063 Uiso 1 1 calc R U . . .
C82 C 0.4435(3) 0.40097(7) 0.6246(2) 0.0405(9) Uani 1 1 d . . . . .
H82A H 0.4122 0.3878 0.6570 0.061 Uiso 1 1 calc R U . . .
H82B H 0.5249 0.4015 0.6468 0.061 Uiso 1 1 calc R U . . .
H82C H 0.4243 0.3950 0.5665 0.061 Uiso 1 1 calc R U . . .
C83 C 0.6667(3) 0.45938(7) 0.9045(2) 0.0366(8) Uani 1 1 d . . . . .
H83 H 0.7159 0.4617 0.8665 0.044 Uiso 1 1 calc R U . . .
C84 C 0.7114(3) 0.43470(8) 0.9617(2) 0.0487(10) Uani 1 1 d . . . . .
H84A H 0.6647 0.4319 0.9998 0.073 Uiso 1 1 calc R U . . .
H84B H 0.7884 0.4385 0.9938 0.073 Uiso 1 1 calc R U . . .
H84C H 0.7097 0.4179 0.9283 0.073 Uiso 1 1 calc R U . . .
C85 C 0.6735(4) 0.48615(8) 0.9548(2) 0.0542(11) Uani 1 1 d . . . . .
H85A H 0.7520 0.4908 0.9801 0.081 Uiso 1 1 calc R U . . .
H85B H 0.6354 0.4835 0.9984 0.081 Uiso 1 1 calc R U . . .
H85C H 0.6376 0.5013 0.9180 0.081 Uiso 1 1 calc R U . . .
C86 C 0.6335(3) 0.50463(6) 0.4707(2) 0.0303(8) Uani 1 1 d . . . . .
C87 C 0.4994(2) 0.46220(7) 0.47477(17) 0.0210(7) Uani 1 1 d . . . . .
C88 C 0.6648(4) 0.46227(11) 0.1971(3) 0.0605(13) Uani 0.9119(19) 1 d D U P A 1
H88A H 0.6612 0.4819 0.1794 0.073 Uiso 0.9119(19) 1 calc R U P A 1
H88B H 0.6587 0.4617 0.2549 0.073 Uiso 0.9119(19) 1 calc R U P A 1
Cl11 Cl 0.78990(10) 0.44859(3) 0.19404(10) 0.0811(5) Uani 0.9119(19) 1 d D U P
A 1
Cl12 Cl 0.55093(8) 0.44392(2) 0.13190(6) 0.0417(3) Uani 0.9119(19) 1 d D U P A
1
C88' C 0.645(4) 0.4519(11) 0.188(3) 0.082(4) Uani 0.0881(19) 1 d D U P A 2
H88C H 0.5713 0.4531 0.2008 0.099 Uiso 0.0881(19) 1 calc R U P A 2
H88D H 0.6464 0.4364 0.1496 0.099 Uiso 0.0881(19) 1 calc R U P A 2
Cl21 Cl 0.7571(12) 0.4530(3) 0.2737(10) 0.086(3) Uani 0.0881(19) 1 d D U P A 2
Cl22 Cl 0.6953(15) 0.4844(4) 0.1601(12) 0.105(4) Uani 0.0881(19) 1 d D U P A 2
C89 C 0.9384(3) 0.30530(7) 0.3777(2) 0.0444(10) Uani 1 1 d . . . . .
H89A H 0.8964 0.3111 0.3211 0.053 Uiso 1 1 calc R U . . .
H89B H 1.0134 0.3139 0.3899 0.053 Uiso 1 1 calc R U . . .
C90 C 0.1441(3) 0.37420(7) 0.7891(2) 0.0330(8) Uani 1 1 d . . . . .
H90A H 0.1017 0.3566 0.7840 0.040 Uiso 1 1 calc R U . . .
H90B H 0.1583 0.3808 0.8471 0.040 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
Cr1 C58 1.852(3) . ?
Cr1 C57 1.876(3) . ?
Cr1 C55 1.880(3) . ?
Cr1 C56 1.892(3) . ?
Cr1 Si2 2.3113(12) . ?
Cr1 Si1 2.3118(12) . ?
Cr2 C86 1.866(3) 3_666 ?
Cr2 C86 1.866(3) . ?
Cr2 C87 1.868(3) 3_666 ?
Cr2 C87 1.868(3) . ?
Cr2 Si3 2.3039(11) 3_666 ?
Cr2 Si3 2.3039(11) . ?
Cl1 Si1 2.1272(10) . ?
Cl2 Si1 2.1291(10) . ?
Cl3 Si2 2.1341(10) . ?
Cl4 Si2 2.1105(10) . ?
Cl5 Si3 2.1048(13) . ?
Cl6 Si3 2.1157(13) . ?
Cl7 C89 1.753(3) . ?
Cl8 C89 1.751(4) . ?
Cl9 C90 1.753(3) . ?
Cl10 C90 1.738(3) . ?
Si1 C1 1.988(3) . ?
Si2 C28 1.989(3) . ?
Si3 C59 1.977(3) . ?
O1 C55 1.151(4) . ?
O2 C56 1.150(3) . ?
O3 C57 1.153(3) . ?
O4 C58 1.159(3) . ?
O5 C86 1.149(4) . ?
O6 C87 1.156(3) . ?
N1 C1 1.366(3) . ?
N1 C2 1.377(3) . ?
N1 C4 1.463(3) . ?
N2 C1 1.365(3) . ?
N2 C3 1.383(4) . ?
N2 C16 1.454(3) . ?
N3 C28 1.365(3) . ?
N3 C29 1.374(3) . ?
N3 C31 1.462(3) . ?
N4 C28 1.371(3) . ?
N4 C30 1.380(3) . ?
N4 C43 1.462(3) . ?
N5 C59 1.362(4) . ?
N5 C60 1.380(4) . ?
N5 C62 1.460(4) . ?
N6 C59 1.369(4) . ?
N6 C61 1.385(4) . ?
N6 C74 1.460(4) . ?
C2 C3 1.330(4) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 C5 1.397(4) . ?
C4 C9 1.401(4) . ?
C5 C6 1.394(4) . ?
C5 C10 1.514(4) . ?
C6 C7 1.375(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.386(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.390(4) . ?
C8 H8 0.9500 . ?
C9 C13 1.521(4) . ?
C10 C11 1.518(4) . ?
C10 C12 1.533(4) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.521(4) . ?
C13 C15 1.527(4) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C21 1.389(4) . ?
C16 C17 1.404(4) . ?
C17 C18 1.389(4) . ?
C17 C22 1.528(4) . ?
C18 C19 1.378(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.370(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.398(4) . ?
C20 H20 0.9500 . ?
C21 C25 1.517(4) . ?
C22 C23 1.524(4) . ?
C22 C24 1.531(4) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C27 1.524(4) . ?
C25 C26 1.542(5) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C29 C30 1.337(4) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C32 1.396(4) . ?
C31 C36 1.398(4) . ?
C32 C33 1.386(4) . ?
C32 C37 1.520(4) . ?
C33 C34 1.379(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.379(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.388(4) . ?
C35 H35 0.9500 . ?
C36 C40 1.525(4) . ?
C37 C38 1.519(4) . ?
C37 C39 1.530(4) . ?
C37 H37 1.0000 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C41 1.527(4) . ?
C40 C42 1.529(4) . ?
C40 H40 1.0000 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.397(4) . ?
C43 C48 1.405(4) . ?
C44 C45 1.394(4) . ?
C44 C49 1.514(4) . ?
C45 C46 1.376(4) . ?
C45 H45 0.9500 . ?
C46 C47 1.378(4) . ?
C46 H46 0.9500 . ?
C47 C48 1.391(4) . ?
C47 H47 0.9500 . ?
C48 C52 1.521(4) . ?
C49 C51 1.525(4) . ?
C49 C50 1.544(4) . ?
C49 H49 1.0000 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 C54 1.523(4) . ?
C52 C53 1.535(4) . ?
C52 H52 1.0000 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C60 C61 1.332(4) . ?
C60 H60 0.9500 . ?
C61 H61 0.9500 . ?
C62 C67 1.395(5) . ?
C62 C63 1.411(5) . ?
C63 C64 1.386(5) . ?
C63 C68 1.527(5) . ?
C64 C65 1.366(6) . ?
C64 H64 0.9500 . ?
C65 C66 1.375(5) . ?
C65 H65 0.9500 . ?
C66 C67 1.409(5) . ?
C66 H66 0.9500 . ?
C67 C71 1.505(5) . ?
C68 C69 1.513(5) . ?
C68 C70 1.534(5) . ?
C68 H68 1.0000 . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C71 C73 1.527(5) . ?
C71 C72 1.532(5) . ?
C71 H71 1.0000 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 C79 1.394(4) . ?
C74 C75 1.398(4) . ?
C75 C76 1.394(4) . ?
C75 C80 1.513(4) . ?
C76 C77 1.384(5) . ?
C76 H76 0.9500 . ?
C77 C78 1.371(5) . ?
C77 H77 0.9500 . ?
C78 C79 1.395(5) . ?
C78 H78 0.9500 . ?
C79 C83 1.521(5) . ?
C80 C82 1.526(5) . ?
C80 C81 1.534(5) . ?
C80 H80 1.0000 . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 C85 1.529(5) . ?
C83 C84 1.534(5) . ?
C83 H83 1.0000 . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C88 Cl11 1.703(6) . ?
C88 Cl12 1.772(4) . ?
C88 H88A 0.9900 . ?
C88 H88B 0.9900 . ?
C88' Cl21 1.71(2) . ?
C88' Cl22 1.80(2) . ?
C88' H88C 0.9900 . ?
C88' H88D 0.9900 . ?
Cl21 Cl22 2.39(2) . ?
C89 H89A 0.9900 . ?
C89 H89B 0.9900 . ?
C90 H90A 0.9900 . ?
C90 H90B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C58 Cr1 C57 84.51(12) . . ?
C58 Cr1 C55 82.23(13) . . ?
C57 Cr1 C55 166.73(12) . . ?
C58 Cr1 C56 178.63(12) . . ?
C57 Cr1 C56 95.87(12) . . ?
C55 Cr1 C56 97.40(12) . . ?
C58 Cr1 Si2 90.33(9) . . ?
C57 Cr1 Si2 95.34(9) . . ?
C55 Cr1 Si2 85.21(9) . . ?
C56 Cr1 Si2 88.33(8) . . ?
C58 Cr1 Si1 91.77(9) . . ?
C57 Cr1 Si1 85.66(9) . . ?
C55 Cr1 Si1 94.28(9) . . ?
C56 Cr1 Si1 89.57(8) . . ?
Si2 Cr1 Si1 177.76(3) . . ?
C86 Cr2 C86 180.00(18) 3_666 . ?
C86 Cr2 C87 90.38(13) 3_666 3_666 ?
C86 Cr2 C87 89.62(13) . 3_666 ?
C86 Cr2 C87 89.62(13) 3_666 . ?
C86 Cr2 C87 90.38(13) . . ?
C87 Cr2 C87 180.00(17) 3_666 . ?
C86 Cr2 Si3 88.85(11) 3_666 3_666 ?
C86 Cr2 Si3 91.15(11) . 3_666 ?
C87 Cr2 Si3 97.13(9) 3_666 3_666 ?
C87 Cr2 Si3 82.87(9) . 3_666 ?
C86 Cr2 Si3 91.15(11) 3_666 . ?
C86 Cr2 Si3 88.85(11) . . ?
C87 Cr2 Si3 82.86(9) 3_666 . ?
C87 Cr2 Si3 97.13(9) . . ?
Si3 Cr2 Si3 180.0 3_666 . ?
C1 Si1 Cl1 97.87(8) . . ?
C1 Si1 Cl2 98.94(8) . . ?
Cl1 Si1 Cl2 97.54(5) . . ?
C1 Si1 Cr1 125.41(8) . . ?
Cl1 Si1 Cr1 118.20(4) . . ?
Cl2 Si1 Cr1 113.87(4) . . ?
C28 Si2 Cl4 100.35(8) . . ?
C28 Si2 Cl3 98.81(8) . . ?
Cl4 Si2 Cl3 97.50(5) . . ?
C28 Si2 Cr1 123.38(8) . . ?
Cl4 Si2 Cr1 115.09(4) . . ?
Cl3 Si2 Cr1 117.28(4) . . ?
C59 Si3 Cl5 100.07(10) . . ?
C59 Si3 Cl6 97.78(9) . . ?
Cl5 Si3 Cl6 96.72(6) . . ?
C59 Si3 Cr2 124.88(9) . . ?
Cl5 Si3 Cr2 114.78(5) . . ?
Cl6 Si3 Cr2 117.61(5) . . ?
C1 N1 C2 110.8(2) . . ?
C1 N1 C4 129.1(2) . . ?
C2 N1 C4 119.7(2) . . ?
C1 N2 C3 110.6(2) . . ?
C1 N2 C16 131.4(2) . . ?
C3 N2 C16 117.8(2) . . ?
C28 N3 C29 110.7(2) . . ?
C28 N3 C31 128.5(2) . . ?
C29 N3 C31 119.2(2) . . ?
C28 N4 C30 110.5(2) . . ?
C28 N4 C43 129.2(2) . . ?
C30 N4 C43 119.6(2) . . ?
C59 N5 C60 110.7(2) . . ?
C59 N5 C62 128.8(2) . . ?
C60 N5 C62 120.1(3) . . ?
C59 N6 C61 110.2(2) . . ?
C59 N6 C74 129.2(2) . . ?
C61 N6 C74 119.6(2) . . ?
N2 C1 N1 104.0(2) . . ?
N2 C1 Si1 129.1(2) . . ?
N1 C1 Si1 125.99(19) . . ?
C3 C2 N1 107.3(2) . . ?
C3 C2 H2 126.3 . . ?
N1 C2 H2 126.3 . . ?
C2 C3 N2 107.3(2) . . ?
C2 C3 H3 126.4 . . ?
N2 C3 H3 126.4 . . ?
C5 C4 C9 124.0(3) . . ?
C5 C4 N1 117.8(2) . . ?
C9 C4 N1 117.5(2) . . ?
C6 C5 C4 116.0(3) . . ?
C6 C5 C10 121.0(3) . . ?
C4 C5 C10 122.8(3) . . ?
C7 C6 C5 122.1(3) . . ?
C7 C6 H6 119.0 . . ?
C5 C6 H6 119.0 . . ?
C6 C7 C8 119.9(3) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?
C7 C8 C9 121.4(3) . . ?
C7 C8 H8 119.3 . . ?
C9 C8 H8 119.3 . . ?
C8 C9 C4 116.5(3) . . ?
C8 C9 C13 120.9(3) . . ?
C4 C9 C13 122.4(2) . . ?
C5 C10 C11 113.7(3) . . ?
C5 C10 C12 110.5(2) . . ?
C11 C10 C12 108.3(3) . . ?
C5 C10 H10 108.1 . . ?
C11 C10 H10 108.1 . . ?
C12 C10 H10 108.1 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C9 113.6(3) . . ?
C14 C13 C15 109.2(3) . . ?
C9 C13 C15 109.9(3) . . ?
C14 C13 H13 108.0 . . ?
C9 C13 H13 108.0 . . ?
C15 C13 H13 108.0 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C16 C17 123.8(3) . . ?
C21 C16 N2 118.1(2) . . ?
C17 C16 N2 117.7(2) . . ?
C18 C17 C16 116.3(3) . . ?
C18 C17 C22 121.5(3) . . ?
C16 C17 C22 122.2(2) . . ?
C19 C18 C17 121.6(3) . . ?
C19 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
C20 C19 C18 120.3(3) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C19 C20 C21 121.3(3) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C16 C21 C20 116.7(3) . . ?
C16 C21 C25 122.8(3) . . ?
C20 C21 C25 120.5(3) . . ?
C23 C22 C17 112.1(3) . . ?
C23 C22 C24 110.1(3) . . ?
C17 C22 C24 112.7(3) . . ?
C23 C22 H22 107.2 . . ?
C17 C22 H22 107.2 . . ?
C24 C22 H22 107.2 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 C27 111.6(3) . . ?
C21 C25 C26 110.8(3) . . ?
C27 C25 C26 109.8(3) . . ?
C21 C25 H25 108.2 . . ?
C27 C25 H25 108.2 . . ?
C26 C25 H25 108.2 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N3 C28 N4 104.2(2) . . ?
N3 C28 Si2 128.03(19) . . ?
N4 C28 Si2 126.70(19) . . ?
C30 C29 N3 107.6(2) . . ?
C30 C29 H29 126.2 . . ?
N3 C29 H29 126.2 . . ?
C29 C30 N4 107.1(2) . . ?
C29 C30 H30 126.4 . . ?
N4 C30 H30 126.4 . . ?
C32 C31 C36 123.4(2) . . ?
C32 C31 N3 116.8(2) . . ?
C36 C31 N3 119.5(2) . . ?
C33 C32 C31 117.2(2) . . ?
C33 C32 C37 120.2(3) . . ?
C31 C32 C37 122.6(2) . . ?
C34 C33 C32 120.9(3) . . ?
C34 C33 H33 119.5 . . ?
C32 C33 H33 119.5 . . ?
C33 C34 C35 120.3(3) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
C34 C35 C36 121.6(3) . . ?
C34 C35 H35 119.2 . . ?
C36 C35 H35 119.2 . . ?
C35 C36 C31 116.4(3) . . ?
C35 C36 C40 121.4(2) . . ?
C31 C36 C40 122.1(2) . . ?
C38 C37 C32 110.2(2) . . ?
C38 C37 C39 111.4(3) . . ?
C32 C37 C39 112.4(3) . . ?
C38 C37 H37 107.5 . . ?
C32 C37 H37 107.5 . . ?
C39 C37 H37 107.5 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C36 C40 C41 112.6(2) . . ?
C36 C40 C42 110.6(2) . . ?
C41 C40 C42 108.0(2) . . ?
C36 C40 H40 108.5 . . ?
C41 C40 H40 108.5 . . ?
C42 C40 H40 108.5 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 C48 123.1(2) . . ?
C44 C43 N4 119.0(2) . . ?
C48 C43 N4 117.4(2) . . ?
C45 C44 C43 116.9(3) . . ?
C45 C44 C49 119.0(2) . . ?
C43 C44 C49 123.7(2) . . ?
C46 C45 C44 121.3(3) . . ?
C46 C45 H45 119.3 . . ?
C44 C45 H45 119.3 . . ?
C45 C46 C47 120.4(3) . . ?
C45 C46 H46 119.8 . . ?
C47 C46 H46 119.8 . . ?
C46 C47 C48 121.2(3) . . ?
C46 C47 H47 119.4 . . ?
C48 C47 H47 119.4 . . ?
C47 C48 C43 116.9(3) . . ?
C47 C48 C52 120.4(2) . . ?
C43 C48 C52 122.5(2) . . ?
C44 C49 C51 113.6(2) . . ?
C44 C49 C50 108.5(2) . . ?
C51 C49 C50 109.0(2) . . ?
C44 C49 H49 108.6 . . ?
C51 C49 H49 108.6 . . ?
C50 C49 H49 108.6 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C49 C51 H51A 109.5 . . ?
C49 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C49 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C48 C52 C54 113.2(2) . . ?
C48 C52 C53 110.2(2) . . ?
C54 C52 C53 109.7(2) . . ?
C48 C52 H52 107.9 . . ?
C54 C52 H52 107.9 . . ?
C53 C52 H52 107.9 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C52 C54 H54A 109.5 . . ?
C52 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C52 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
O1 C55 Cr1 172.4(3) . . ?
O2 C56 Cr1 179.2(3) . . ?
O3 C57 Cr1 174.0(2) . . ?
O4 C58 Cr1 178.7(3) . . ?
N5 C59 N6 104.3(2) . . ?
N5 C59 Si3 126.9(2) . . ?
N6 C59 Si3 128.2(2) . . ?
C61 C60 N5 107.4(3) . . ?
C61 C60 H60 126.3 . . ?
N5 C60 H60 126.3 . . ?
C60 C61 N6 107.4(3) . . ?
C60 C61 H61 126.3 . . ?
N6 C61 H61 126.3 . . ?
C67 C62 C63 124.7(3) . . ?
C67 C62 N5 118.4(3) . . ?
C63 C62 N5 116.6(3) . . ?
C64 C63 C62 116.1(3) . . ?
C64 C63 C68 120.7(3) . . ?
C62 C63 C68 123.2(3) . . ?
C65 C64 C63 121.2(4) . . ?
C65 C64 H64 119.4 . . ?
C63 C64 H64 119.4 . . ?
C64 C65 C66 121.5(4) . . ?
C64 C65 H65 119.3 . . ?
C66 C65 H65 119.3 . . ?
C65 C66 C67 121.2(4) . . ?
C65 C66 H66 119.4 . . ?
C67 C66 H66 119.4 . . ?
C62 C67 C66 115.2(3) . . ?
C62 C67 C71 123.2(3) . . ?
C66 C67 C71 121.5(3) . . ?
C69 C68 C63 110.3(4) . . ?
C69 C68 C70 108.9(3) . . ?
C63 C68 C70 114.7(3) . . ?
C69 C68 H68 107.6 . . ?
C63 C68 H68 107.6 . . ?
C70 C68 H68 107.6 . . ?
C68 C69 H69A 109.5 . . ?
C68 C69 H69B 109.5 . . ?
H69A C69 H69B 109.5 . . ?
C68 C69 H69C 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C68 C70 H70A 109.5 . . ?
C68 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C68 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C67 C71 C73 115.2(3) . . ?
C67 C71 C72 110.5(3) . . ?
C73 C71 C72 107.1(3) . . ?
C67 C71 H71 107.9 . . ?
C73 C71 H71 107.9 . . ?
C72 C71 H71 107.9 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C71 C73 H73A 109.5 . . ?
C71 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C71 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C79 C74 C75 123.7(3) . . ?
C79 C74 N6 116.3(3) . . ?
C75 C74 N6 119.9(3) . . ?
C76 C75 C74 116.5(3) . . ?
C76 C75 C80 121.4(3) . . ?
C74 C75 C80 122.1(3) . . ?
C77 C76 C75 121.3(3) . . ?
C77 C76 H76 119.4 . . ?
C75 C76 H76 119.4 . . ?
C78 C77 C76 120.4(3) . . ?
C78 C77 H77 119.8 . . ?
C76 C77 H77 119.8 . . ?
C77 C78 C79 121.3(3) . . ?
C77 C78 H78 119.4 . . ?
C79 C78 H78 119.4 . . ?
C74 C79 C78 116.8(3) . . ?
C74 C79 C83 123.2(3) . . ?
C78 C79 C83 120.0(3) . . ?
C75 C80 C82 112.8(3) . . ?
C75 C80 C81 113.7(3) . . ?
C82 C80 C81 107.7(3) . . ?
C75 C80 H80 107.4 . . ?
C82 C80 H80 107.4 . . ?
C81 C80 H80 107.4 . . ?
C80 C81 H81A 109.5 . . ?
C80 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
C80 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C80 C82 H82A 109.5 . . ?
C80 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C80 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C79 C83 C85 111.7(3) . . ?
C79 C83 C84 111.4(3) . . ?
C85 C83 C84 110.7(3) . . ?
C79 C83 H83 107.6 . . ?
C85 C83 H83 107.6 . . ?
C84 C83 H83 107.6 . . ?
C83 C84 H84A 109.5 . . ?
C83 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
C83 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
C83 C85 H85A 109.5 . . ?
C83 C85 H85B 109.5 . . ?
H85A C85 H85B 109.5 . . ?
C83 C85 H85C 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
O5 C86 Cr2 179.5(4) . . ?
O6 C87 Cr2 178.6(3) . . ?
Cl11 C88 Cl12 111.9(3) . . ?
Cl11 C88 H88A 109.2 . . ?
Cl12 C88 H88A 109.2 . . ?
Cl11 C88 H88B 109.2 . . ?
Cl12 C88 H88B 109.2 . . ?
H88A C88 H88B 107.9 . . ?
Cl21 C88' Cl22 85.6(13) . . ?
Cl21 C88' H88C 114.4 . . ?
Cl22 C88' H88C 114.4 . . ?
Cl21 C88' H88D 114.4 . . ?
Cl22 C88' H88D 114.4 . . ?
H88C C88' H88D 111.5 . . ?
C88' Cl21 Cl22 48.7(9) . . ?
C88' Cl22 Cl21 45.6(8) . . ?
Cl8 C89 Cl7 113.58(19) . . ?
Cl8 C89 H89A 108.8 . . ?
Cl7 C89 H89A 108.8 . . ?
Cl8 C89 H89B 108.8 . . ?
Cl7 C89 H89B 108.8 . . ?
H89A C89 H89B 107.7 . . ?
Cl10 C90 Cl9 111.58(18) . . ?
Cl10 C90 H90A 109.3 . . ?
Cl9 C90 H90A 109.3 . . ?
Cl10 C90 H90B 109.3 . . ?
Cl9 C90 H90B 109.3 . . ?
H90A C90 H90B 108.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N2 C1 N1 0.8(3) . . . . ?
C16 N2 C1 N1 -173.4(3) . . . . ?
C3 N2 C1 Si1 -168.7(2) . . . . ?
C16 N2 C1 Si1 17.1(4) . . . . ?
C2 N1 C1 N2 -0.7(3) . . . . ?
C4 N1 C1 N2 172.3(2) . . . . ?
C2 N1 C1 Si1 169.2(2) . . . . ?
C4 N1 C1 Si1 -17.8(4) . . . . ?
C1 N1 C2 C3 0.3(3) . . . . ?
C4 N1 C2 C3 -173.4(2) . . . . ?
N1 C2 C3 N2 0.2(3) . . . . ?
C1 N2 C3 C2 -0.7(3) . . . . ?
C16 N2 C3 C2 174.4(2) . . . . ?
C1 N1 C4 C5 106.0(3) . . . . ?
C2 N1 C4 C5 -81.6(3) . . . . ?
C1 N1 C4 C9 -83.5(3) . . . . ?
C2 N1 C4 C9 88.9(3) . . . . ?
C9 C4 C5 C6 5.4(4) . . . . ?
N1 C4 C5 C6 175.2(2) . . . . ?
C9 C4 C5 C10 -169.6(3) . . . . ?
N1 C4 C5 C10 0.2(4) . . . . ?
C4 C5 C6 C7 -1.1(4) . . . . ?
C10 C5 C6 C7 174.0(3) . . . . ?
C5 C6 C7 C8 -2.1(5) . . . . ?
C6 C7 C8 C9 1.3(5) . . . . ?
C7 C8 C9 C4 2.6(4) . . . . ?
C7 C8 C9 C13 -171.3(3) . . . . ?
C5 C4 C9 C8 -6.1(4) . . . . ?
N1 C4 C9 C8 -176.0(2) . . . . ?
C5 C4 C9 C13 167.6(3) . . . . ?
N1 C4 C9 C13 -2.2(4) . . . . ?
C6 C5 C10 C11 45.2(4) . . . . ?
C4 C5 C10 C11 -140.0(3) . . . . ?
C6 C5 C10 C12 -76.8(3) . . . . ?
C4 C5 C10 C12 98.0(3) . . . . ?
C8 C9 C13 C14 -37.5(4) . . . . ?
C4 C9 C13 C14 149.0(3) . . . . ?
C8 C9 C13 C15 85.2(3) . . . . ?
C4 C9 C13 C15 -88.3(3) . . . . ?
C1 N2 C16 C21 -106.6(3) . . . . ?
C3 N2 C16 C21 79.5(3) . . . . ?
C1 N2 C16 C17 80.4(4) . . . . ?
C3 N2 C16 C17 -93.5(3) . . . . ?
C21 C16 C17 C18 -1.4(4) . . . . ?
N2 C16 C17 C18 171.2(2) . . . . ?
C21 C16 C17 C22 177.2(3) . . . . ?
N2 C16 C17 C22 -10.3(4) . . . . ?
C16 C17 C18 C19 0.6(4) . . . . ?
C22 C17 C18 C19 -178.0(3) . . . . ?
C17 C18 C19 C20 0.7(5) . . . . ?
C18 C19 C20 C21 -1.2(5) . . . . ?
C17 C16 C21 C20 0.9(4) . . . . ?
N2 C16 C21 C20 -171.7(2) . . . . ?
C17 C16 C21 C25 179.3(3) . . . . ?
N2 C16 C21 C25 6.7(4) . . . . ?
C19 C20 C21 C16 0.5(4) . . . . ?
C19 C20 C21 C25 -178.0(3) . . . . ?
C18 C17 C22 C23 33.5(4) . . . . ?
C16 C17 C22 C23 -145.0(3) . . . . ?
C18 C17 C22 C24 -91.3(3) . . . . ?
C16 C17 C22 C24 90.2(3) . . . . ?
C16 C21 C25 C27 130.1(3) . . . . ?
C20 C21 C25 C27 -51.5(4) . . . . ?
C16 C21 C25 C26 -107.1(3) . . . . ?
C20 C21 C25 C26 71.2(4) . . . . ?
C29 N3 C28 N4 -0.6(3) . . . . ?
C31 N3 C28 N4 -166.0(2) . . . . ?
C29 N3 C28 Si2 -169.01(19) . . . . ?
C31 N3 C28 Si2 25.5(4) . . . . ?
C30 N4 C28 N3 0.0(3) . . . . ?
C43 N4 C28 N3 170.0(2) . . . . ?
C30 N4 C28 Si2 168.64(19) . . . . ?
C43 N4 C28 Si2 -21.4(4) . . . . ?
C28 N3 C29 C30 1.0(3) . . . . ?
C31 N3 C29 C30 167.9(2) . . . . ?
N3 C29 C30 N4 -0.9(3) . . . . ?
C28 N4 C30 C29 0.6(3) . . . . ?
C43 N4 C30 C29 -170.5(2) . . . . ?
C28 N3 C31 C32 81.2(3) . . . . ?
C29 N3 C31 C32 -83.2(3) . . . . ?
C28 N3 C31 C36 -104.2(3) . . . . ?
C29 N3 C31 C36 91.4(3) . . . . ?
C36 C31 C32 C33 4.7(4) . . . . ?
N3 C31 C32 C33 179.1(2) . . . . ?
C36 C31 C32 C37 -173.4(3) . . . . ?
N3 C31 C32 C37 1.0(4) . . . . ?
C31 C32 C33 C34 -1.7(4) . . . . ?
C37 C32 C33 C34 176.5(3) . . . . ?
C32 C33 C34 C35 -2.2(4) . . . . ?
C33 C34 C35 C36 3.4(4) . . . . ?
C34 C35 C36 C31 -0.5(4) . . . . ?
C34 C35 C36 C40 -178.0(3) . . . . ?
C32 C31 C36 C35 -3.6(4) . . . . ?
N3 C31 C36 C35 -177.8(2) . . . . ?
C32 C31 C36 C40 173.9(3) . . . . ?
N3 C31 C36 C40 -0.4(4) . . . . ?
C33 C32 C37 C38 -59.8(4) . . . . ?
C31 C32 C37 C38 118.2(3) . . . . ?
C33 C32 C37 C39 65.1(4) . . . . ?
C31 C32 C37 C39 -116.8(3) . . . . ?
C35 C36 C40 C41 -30.2(4) . . . . ?
C31 C36 C40 C41 152.4(3) . . . . ?
C35 C36 C40 C42 90.8(3) . . . . ?
C31 C36 C40 C42 -86.6(3) . . . . ?
C28 N4 C43 C44 108.9(3) . . . . ?
C30 N4 C43 C44 -81.9(3) . . . . ?
C28 N4 C43 C48 -79.8(3) . . . . ?
C30 N4 C43 C48 89.4(3) . . . . ?
C48 C43 C44 C45 5.3(4) . . . . ?
N4 C43 C44 C45 176.0(2) . . . . ?
C48 C43 C44 C49 -167.1(3) . . . . ?
N4 C43 C44 C49 3.7(4) . . . . ?
C43 C44 C45 C46 -3.1(4) . . . . ?
C49 C44 C45 C46 169.7(3) . . . . ?
C44 C45 C46 C47 -0.5(4) . . . . ?
C45 C46 C47 C48 2.1(4) . . . . ?
C46 C47 C48 C43 0.0(4) . . . . ?
C46 C47 C48 C52 -175.8(3) . . . . ?
C44 C43 C48 C47 -3.8(4) . . . . ?
N4 C43 C48 C47 -174.7(2) . . . . ?
C44 C43 C48 C52 171.9(3) . . . . ?
N4 C43 C48 C52 1.0(4) . . . . ?
C45 C44 C49 C51 52.3(3) . . . . ?
C43 C44 C49 C51 -135.5(3) . . . . ?
C45 C44 C49 C50 -69.1(3) . . . . ?
C43 C44 C49 C50 103.1(3) . . . . ?
C47 C48 C52 C54 -36.6(4) . . . . ?
C43 C48 C52 C54 147.8(3) . . . . ?
C47 C48 C52 C53 86.7(3) . . . . ?
C43 C48 C52 C53 -88.9(3) . . . . ?
C60 N5 C59 N6 -0.8(3) . . . . ?
C62 N5 C59 N6 -173.4(3) . . . . ?
C60 N5 C59 Si3 -173.0(2) . . . . ?
C62 N5 C59 Si3 14.4(4) . . . . ?
C61 N6 C59 N5 0.7(3) . . . . ?
C74 N6 C59 N5 169.0(3) . . . . ?
C61 N6 C59 Si3 172.7(2) . . . . ?
C74 N6 C59 Si3 -19.0(4) . . . . ?
C59 N5 C60 C61 0.7(4) . . . . ?
C62 N5 C60 C61 174.0(3) . . . . ?
N5 C60 C61 N6 -0.3(4) . . . . ?
C59 N6 C61 C60 -0.3(4) . . . . ?
C74 N6 C61 C60 -169.9(3) . . . . ?
C59 N5 C62 C67 -101.6(4) . . . . ?
C60 N5 C62 C67 86.4(4) . . . . ?
C59 N5 C62 C63 84.0(4) . . . . ?
C60 N5 C62 C63 -88.0(4) . . . . ?
C67 C62 C63 C64 2.0(5) . . . . ?
N5 C62 C63 C64 176.0(3) . . . . ?
C67 C62 C63 C68 -177.0(3) . . . . ?
N5 C62 C63 C68 -2.9(5) . . . . ?
C62 C63 C64 C65 -0.3(6) . . . . ?
C68 C63 C64 C65 178.7(4) . . . . ?
C63 C64 C65 C66 -0.8(6) . . . . ?
C64 C65 C66 C67 0.2(6) . . . . ?
C63 C62 C67 C66 -2.5(5) . . . . ?
N5 C62 C67 C66 -176.4(3) . . . . ?
C63 C62 C67 C71 175.0(3) . . . . ?
N5 C62 C67 C71 1.0(5) . . . . ?
C65 C66 C67 C62 1.3(5) . . . . ?
C65 C66 C67 C71 -176.2(3) . . . . ?
C64 C63 C68 C69 -89.0(4) . . . . ?
C62 C63 C68 C69 89.9(4) . . . . ?
C64 C63 C68 C70 34.4(5) . . . . ?
C62 C63 C68 C70 -146.8(4) . . . . ?
C62 C67 C71 C73 147.8(3) . . . . ?
C66 C67 C71 C73 -34.9(4) . . . . ?
C62 C67 C71 C72 -90.6(4) . . . . ?
C66 C67 C71 C72 86.7(4) . . . . ?
C59 N6 C74 C79 -93.3(4) . . . . ?
C61 N6 C74 C79 74.1(4) . . . . ?
C59 N6 C74 C75 90.9(4) . . . . ?
C61 N6 C74 C75 -101.7(3) . . . . ?
C79 C74 C75 C76 3.6(4) . . . . ?
N6 C74 C75 C76 179.2(3) . . . . ?
C79 C74 C75 C80 -175.5(3) . . . . ?
N6 C74 C75 C80 0.0(4) . . . . ?
C74 C75 C76 C77 -1.8(5) . . . . ?
C80 C75 C76 C77 177.4(3) . . . . ?
C75 C76 C77 C78 -0.9(5) . . . . ?
C76 C77 C78 C79 1.9(5) . . . . ?
C75 C74 C79 C78 -2.7(5) . . . . ?
N6 C74 C79 C78 -178.4(3) . . . . ?
C75 C74 C79 C83 177.0(3) . . . . ?
N6 C74 C79 C83 1.3(4) . . . . ?
C77 C78 C79 C74 -0.2(5) . . . . ?
C77 C78 C79 C83 -179.9(3) . . . . ?
C76 C75 C80 C82 -111.9(3) . . . . ?
C74 C75 C80 C82 67.2(4) . . . . ?
C76 C75 C80 C81 11.2(4) . . . . ?
C74 C75 C80 C81 -169.7(3) . . . . ?
C74 C79 C83 C85 133.6(3) . . . . ?
C78 C79 C83 C85 -46.8(4) . . . . ?
C74 C79 C83 C84 -102.1(4) . . . . ?
C78 C79 C83 C84 77.5(4) . . . . ?

_refine_diff_density_max         0.594
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.064

####################################################################### 
# 
# 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_Compound_6W
_database_code_depnum_ccdc_archive 'CCDC 1514799'
_audit_update_record             
;
2016-11-15 deposited with the CCDC.
2017-05-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C32 H36 N2 O5 W), 0.5(C14 H16), 2(C7 H8)'
_chemical_formula_sum            'C42.50 H48 N2 O5 W'
_chemical_formula_weight         850.68

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      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                   12.193(2)
_cell_length_b                   13.362(2)
_cell_length_c                   14.396(3)
_cell_angle_alpha                105.95(2)
_cell_angle_beta                 105.03(2)
_cell_angle_gamma                110.55(2)
_cell_volume                     1939.8(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9497
_cell_measurement_theta_min      2.492
_cell_measurement_theta_max      32.216

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_F_000             862
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    3.023
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  0.7995
_exptl_absorpt_correction_T_max  0.9092
_exptl_absorpt_process_details   SADABS-2012/1

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'rotating anode'
_diffrn_measurement_device_type  'Smart APEX II Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            60979
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.602
_diffrn_reflns_theta_max         33.443
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             13473
_reflns_number_gt                12566
_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 v2012.2'
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_reduction        'SAINT V7.68A'
_computing_structure_solution    'SHELXS-2012 (Sheldrick, 2012)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'

_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)+(0.0266P)²+0.8367P] 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         13473
_refine_ls_number_parameters     562
_refine_ls_number_restraints     636
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0211
_refine_ls_wR_factor_ref         0.0494
_refine_ls_wR_factor_gt          0.0486
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.30359(2) 0.24748(2) 0.23665(2) 0.01488(2) Uani 1 1 d . . . . .
O1 O 0.13450(17) -0.02340(13) 0.08690(13) 0.0433(4) Uani 1 1 d . . . . .
N1 N 0.31329(12) 0.15330(11) 0.51274(10) 0.0144(2) Uani 1 1 d . . . . .
C1 C 0.21241(14) 0.17376(13) 0.49919(11) 0.0149(2) Uani 1 1 d . . . . .
H1 H 0.1630 0.1680 0.5406 0.018 Uiso 1 1 calc R U . . .
O2 O 0.55649(12) 0.21842(12) 0.27441(11) 0.0267(3) Uani 1 1 d . . . . .
N2 N 0.19230(12) 0.20388(11) 0.41722(10) 0.0141(2) Uani 1 1 d . . . . .
C2 C 0.35756(14) 0.17096(13) 0.43608(12) 0.0162(3) Uani 1 1 d . . . . .
H2 H 0.4290 0.1620 0.4282 0.019 Uiso 1 1 calc R U . . .
O3 O 0.36372(13) 0.31604(12) 0.05664(10) 0.0273(3) Uani 1 1 d . . . . .
C3 C 0.28302(14) 0.20333(13) 0.37303(11) 0.0146(2) Uani 1 1 d . . . . .
O4 O 0.47142(12) 0.51240(11) 0.40006(10) 0.0249(2) Uani 1 1 d . . . . .
C4 C 0.36044(14) 0.11177(13) 0.58934(11) 0.0152(3) Uani 1 1 d . . . . .
O5 O 0.06271(14) 0.29504(15) 0.16571(12) 0.0351(3) Uani 1 1 d . . . . .
C5 C 0.32247(14) -0.00838(13) 0.55592(11) 0.0159(3) Uani 1 1 d . . . . .
C6 C 0.36902(15) -0.04711(14) 0.63075(12) 0.0191(3) Uani 1 1 d . . . . .
H6 H 0.3465 -0.1279 0.6105 0.023 Uiso 1 1 calc R U . . .
C7 C 0.44776(16) 0.03045(15) 0.73434(13) 0.0210(3) Uani 1 1 d . . . . .
H7 H 0.4779 0.0024 0.7844 0.025 Uiso 1 1 calc R U . . .
C8 C 0.48240(16) 0.14847(14) 0.76480(12) 0.0200(3) Uani 1 1 d . . . . .
H8 H 0.5360 0.2006 0.8359 0.024 Uiso 1 1 calc R U . . .
C9 C 0.44015(14) 0.19259(13) 0.69312(12) 0.0164(3) Uani 1 1 d . . . . .
C10 C 0.23401(15) -0.09616(13) 0.44385(12) 0.0182(3) Uani 1 1 d . . . . .
H10 H 0.2068 -0.0531 0.4032 0.022 Uiso 1 1 calc R U . . .
C11 C 0.11412(17) -0.18960(16) 0.44066(14) 0.0265(3) Uani 1 1 d . . . . .
H11A H 0.0562 -0.2413 0.3673 0.040 Uiso 1 1 calc R U . . .
H11B H 0.0713 -0.1517 0.4755 0.040 Uiso 1 1 calc R U . . .
H11C H 0.1382 -0.2355 0.4771 0.040 Uiso 1 1 calc R U . . .
C12 C 0.30378(19) -0.15306(18) 0.39130(15) 0.0313(4) Uani 1 1 d . . . . .
H12A H 0.3298 -0.1971 0.4291 0.047 Uiso 1 1 calc R U . . .
H12B H 0.3794 -0.0923 0.3931 0.047 Uiso 1 1 calc R U . . .
H12C H 0.2468 -0.2062 0.3181 0.047 Uiso 1 1 calc R U . . .
C13 C 0.47962(15) 0.32249(14) 0.72938(12) 0.0192(3) Uani 1 1 d . . . . .
H13 H 0.4450 0.3375 0.6664 0.023 Uiso 1 1 calc R U . . .
C14 C 0.62507(16) 0.39332(15) 0.77681(14) 0.0250(3) Uani 1 1 d . . . . .
H14A H 0.6587 0.3682 0.7247 0.038 Uiso 1 1 calc R U . . .
H14B H 0.6612 0.3805 0.8391 0.038 Uiso 1 1 calc R U . . .
H14C H 0.6484 0.4766 0.7969 0.038 Uiso 1 1 calc R U . . .
C15 C 0.42373(19) 0.36185(17) 0.80786(16) 0.0305(4) Uani 1 1 d . . . . .
H15A H 0.3305 0.3176 0.7751 0.046 Uiso 1 1 calc R U . . .
H15B H 0.4487 0.4454 0.8285 0.046 Uiso 1 1 calc R U . . .
H15C H 0.4561 0.3477 0.8703 0.046 Uiso 1 1 calc R U . . .
C16 C 0.08428(13) 0.22458(13) 0.37900(11) 0.0149(3) Uani 1 1 d . . . . .
C17 C -0.03065(14) 0.12858(14) 0.30373(12) 0.0171(3) Uani 1 1 d . . . . .
C18 C -0.13580(15) 0.14958(15) 0.27161(13) 0.0210(3) Uani 1 1 d . . . . .
H18 H -0.2155 0.0866 0.2213 0.025 Uiso 1 1 calc R U . . .
C19 C -0.12562(16) 0.26054(16) 0.31187(14) 0.0237(3) Uani 1 1 d . . . . .
H19 H -0.1985 0.2728 0.2895 0.028 Uiso 1 1 calc R U . . .
C20 C -0.01046(16) 0.35373(15) 0.38434(13) 0.0207(3) Uani 1 1 d . . . . .
H20 H -0.0050 0.4295 0.4107 0.025 Uiso 1 1 calc R U . . .
C21 C 0.09799(14) 0.33819(14) 0.41938(12) 0.0164(3) Uani 1 1 d . . . . .
C22 C 0.22484(15) 0.44061(14) 0.49796(12) 0.0186(3) Uani 1 1 d . . . . .
H22 H 0.2935 0.4181 0.4915 0.022 Uiso 1 1 calc R U . . .
C23 C 0.25029(18) 0.55073(16) 0.47578(15) 0.0262(3) Uani 1 1 d . . . . .
H23A H 0.2313 0.5302 0.4007 0.039 Uiso 1 1 calc R U . . .
H23B H 0.3400 0.6080 0.5168 0.039 Uiso 1 1 calc R U . . .
H23C H 0.1959 0.5843 0.4957 0.039 Uiso 1 1 calc R U . . .
C24 C 0.23267(18) 0.46544(16) 0.61057(13) 0.0245(3) Uani 1 1 d . . . . .
H24A H 0.3164 0.5298 0.6603 0.037 Uiso 1 1 calc R U . . .
H24B H 0.2209 0.3953 0.6244 0.037 Uiso 1 1 calc R U . . .
H24C H 0.1658 0.4870 0.6190 0.037 Uiso 1 1 calc R U . . .
C25 C -0.04099(15) 0.00716(14) 0.25988(12) 0.0197(3) Uani 1 1 d . . . . .
H25 H 0.0465 0.0155 0.2699 0.024 Uiso 1 1 calc R U . . .
C26 C -0.1253(2) -0.05944(18) 0.14250(15) 0.0339(4) Uani 1 1 d . . . . .
H26A H -0.0968 -0.0112 0.1050 0.051 Uiso 1 1 calc R U . . .
H26B H -0.2140 -0.0777 0.1317 0.051 Uiso 1 1 calc R U . . .
H26C H -0.1191 -0.1322 0.1156 0.051 Uiso 1 1 calc R U . . .
C27 C -0.09232(18) -0.06345(16) 0.32010(16) 0.0292(4) Uani 1 1 d . . . . .
H27A H -0.1783 -0.0729 0.3111 0.044 Uiso 1 1 calc R U . . .
H27B H -0.0361 -0.0220 0.3950 0.044 Uiso 1 1 calc R U . . .
H27C H -0.0953 -0.1405 0.2927 0.044 Uiso 1 1 calc R U . . .
C28 C 0.46403(16) 0.22630(14) 0.26334(12) 0.0188(3) Uani 1 1 d . . . . .
C29 C 0.19464(18) 0.07341(16) 0.14015(14) 0.0253(3) Uani 1 1 d . . . . .
C30 C 0.33861(15) 0.28974(14) 0.12106(12) 0.0193(3) Uani 1 1 d . . . . .
C31 C 0.41060(15) 0.41713(15) 0.34140(12) 0.0188(3) Uani 1 1 d . . . . .
C32 C 0.14643(16) 0.27613(16) 0.19545(13) 0.0222(3) Uani 1 1 d . . . . .
C33 C -0.1229(2) 0.30424(19) -0.07605(17) 0.0384(5) Uani 1 1 d D . . . .
H33A H -0.1871 0.2354 -0.1399 0.058 Uiso 1 1 calc R U . . .
H33B H -0.1608 0.3548 -0.0524 0.058 Uiso 1 1 calc R U . . .
H33C H -0.0927 0.2793 -0.0207 0.058 Uiso 1 1 calc R U . . .
C34 C -0.0127(2) 0.37041(17) -0.09919(14) 0.0303(4) Uani 1 1 d D . . . .
C35 C 0.1035(2) 0.3668(2) -0.06329(16) 0.0376(5) Uani 1 1 d D . . . .
H35 H 0.1127 0.3220 -0.0235 0.045 Uiso 1 1 calc R U . . .
C36 C 0.2049(2) 0.4270(2) -0.08440(18) 0.0445(6) Uani 1 1 d D . . . .
H36 H 0.2831 0.4237 -0.0588 0.053 Uiso 1 1 calc R U . . .
C37 C 0.1931(2) 0.4922(2) -0.14283(17) 0.0416(5) Uani 1 1 d D . . . .
H37 H 0.2625 0.5330 -0.1583 0.050 Uiso 1 1 calc R U . . .
C38 C 0.0788(2) 0.4975(2) -0.17866(16) 0.0363(4) Uani 1 1 d D . . . .
H38 H 0.0701 0.5426 -0.2183 0.044 Uiso 1 1 calc R U . . .
C39 C -0.0218(2) 0.43749(18) -0.15681(15) 0.0322(4) Uani 1 1 d D . . . .
H39 H -0.0994 0.4420 -0.1817 0.039 Uiso 1 1 calc R U . . .
C1C C -0.5558(11) -0.0519(9) -0.0115(7) 0.041(2) Uani 0.264(7) 1 d D U P A -1
C2C C -0.5760(14) 0.0466(13) 0.003(2) 0.026(3) Uani 0.264(7) 1 d D U P A -1
H2C H -0.6571 0.0418 -0.0022 0.031 Uiso 0.264(7) 1 calc R U P A -1
C3C C -0.4750(10) 0.1521(9) 0.0256(6) 0.0298(18) Uani 0.264(7) 1 d D U P A -1
H3C H -0.4883 0.2196 0.0366 0.036 Uiso 0.264(7) 1 calc R U P A -1
C4C C -0.3583(14) 0.1624(13) 0.0324(17) 0.034(3) Uani 0.264(7) 1 d D U P A -1
H4C H -0.2905 0.2365 0.0508 0.041 Uiso 0.264(7) 1 calc R U P A -1
C5C C -0.3389(14) 0.0640(13) 0.012(2) 0.039(3) Uani 0.264(7) 1 d D U P A -1
H5C H -0.2579 0.0693 0.0162 0.047 Uiso 0.264(7) 1 calc R U P A -1
C6C C -0.4398(16) -0.0426(15) -0.014(3) 0.042(4) Uani 0.264(7) 1 d D U P A -1
H6C H -0.4291 -0.1114 -0.0337 0.051 Uiso 0.264(7) 1 calc R U P A -1
C7C C -0.6627(19) -0.1631(15) -0.026(2) 0.066(6) Uani 0.264(7) 1 d D U P A -1
H7CA H -0.7315 -0.1958 -0.0950 0.099 Uiso 0.264(7) 1 calc R U P A -1
H7CB H -0.6954 -0.1459 0.0290 0.099 Uiso 0.264(7) 1 calc R U P A -1
H7CC H -0.6305 -0.2198 -0.0201 0.099 Uiso 0.264(7) 1 calc R U P A -1
C1B C -0.4631(10) 0.0916(11) 0.0262(7) 0.033(2) Uani 0.236(7) 1 d D U P A -2
C2B C -0.5885(15) 0.0380(13) 0.015(2) 0.028(3) Uani 0.236(7) 1 d D U P A -2
H2B H -0.6314 0.0843 0.0273 0.034 Uiso 0.236(7) 1 calc R U P A -2
C3B C -0.6535(16) -0.0813(13) -0.013(2) 0.038(3) Uani 0.236(7) 1 d D U P A -2
H3B H -0.7398 -0.1153 -0.0205 0.046 Uiso 0.236(7) 1 calc R U P A -2
C4B C -0.5932(17) -0.1509(13) -0.0300(11) 0.045(3) Uani 0.236(7) 1 d D U P A -2
H4B H -0.6363 -0.2328 -0.0498 0.054 Uiso 0.236(7) 1 calc R U P A -2
C5B C -0.4681(16) -0.0960(16) -0.0169(12) 0.051(4) Uani 0.236(7) 1 d D U P A -2
H5B H -0.4247 -0.1423 -0.0269 0.061 Uiso 0.236(7) 1 calc R U P A -2
C6B C -0.4026(14) 0.0208(16) 0.0095(10) 0.047(3) Uani 0.236(7) 1 d D U P A -2
H6B H -0.3165 0.0538 0.0165 0.056 Uiso 0.236(7) 1 calc R U P A -2
C7B C -0.3890(11) 0.2210(11) 0.0580(8) 0.050(3) Uani 0.236(7) 1 d D U P A -2
H7BA H -0.3245 0.2351 0.0279 0.074 Uiso 0.236(7) 1 calc R U P A -2
H7BB H -0.3470 0.2605 0.1349 0.074 Uiso 0.236(7) 1 calc R U P A -2
H7BC H -0.4473 0.2515 0.0320 0.074 Uiso 0.236(7) 1 calc R U P A -2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C30 1.9964(16) . ?
W1 C28 2.0282(17) . ?
W1 C31 2.0345(19) . ?
W1 C29 2.050(2) . ?
W1 C32 2.0543(17) . ?
W1 C3 2.2480(15) . ?
O1 C29 1.139(2) . ?
N1 C1 1.3291(19) . ?
N1 C2 1.3884(19) . ?
N1 C4 1.4444(18) . ?
C1 N2 1.3398(18) . ?
O2 C28 1.143(2) . ?
N2 C3 1.4129(19) . ?
N2 C16 1.4414(18) . ?
C2 C3 1.379(2) . ?
O3 C30 1.153(2) . ?
O4 C31 1.142(2) . ?
C4 C5 1.400(2) . ?
C4 C9 1.402(2) . ?
O5 C32 1.142(2) . ?
C5 C6 1.395(2) . ?
C5 C10 1.520(2) . ?
C6 C7 1.389(2) . ?
C7 C8 1.383(2) . ?
C8 C9 1.396(2) . ?
C9 C13 1.517(2) . ?
C10 C12 1.532(2) . ?
C10 C11 1.533(2) . ?
C13 C15 1.530(2) . ?
C13 C14 1.532(2) . ?
C16 C21 1.399(2) . ?
C16 C17 1.404(2) . ?
C17 C18 1.397(2) . ?
C17 C25 1.516(2) . ?
C18 C19 1.382(3) . ?
C19 C20 1.382(3) . ?
C20 C21 1.397(2) . ?
C21 C22 1.517(2) . ?
C22 C24 1.533(2) . ?
C22 C23 1.534(2) . ?
C25 C26 1.528(2) . ?
C25 C27 1.533(2) . ?
C33 C34 1.503(3) . ?
C34 C39 1.391(3) . ?
C34 C35 1.399(3) . ?
C35 C36 1.378(3) . ?
C36 C37 1.384(3) . ?
C37 C38 1.389(3) . ?
C38 C39 1.377(3) . ?
C1C C6C 1.386(12) . ?
C1C C2C 1.393(11) . ?
C1C C7C 1.512(13) . ?
C2C C3C 1.390(11) . ?
C3C C4C 1.354(11) . ?
C4C C5C 1.384(12) . ?
C5C C6C 1.385(12) . ?
C1B C2B 1.385(11) . ?
C1B C6B 1.398(11) . ?
C1B C7B 1.506(12) . ?
C2B C3B 1.387(12) . ?
C3B C4B 1.383(12) . ?
C4B C5B 1.375(12) . ?
C5B C6B 1.364(12) . ?

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
C30 W1 C28 85.70(7) . . ?
C30 W1 C31 91.02(7) . . ?
C28 W1 C31 89.36(7) . . ?
C30 W1 C29 93.14(7) . . ?
C28 W1 C29 90.47(7) . . ?
C31 W1 C29 175.81(6) . . ?
C30 W1 C32 87.02(7) . . ?
C28 W1 C32 172.70(6) . . ?
C31 W1 C32 90.23(7) . . ?
C29 W1 C32 90.47(8) . . ?
C30 W1 C3 174.73(6) . . ?
C28 W1 C3 89.31(6) . . ?
C31 W1 C3 87.23(6) . . ?
C29 W1 C3 88.59(6) . . ?
C32 W1 C3 97.95(6) . . ?
C1 N1 C2 107.78(12) . . ?
C1 N1 C4 124.98(12) . . ?
C2 N1 C4 127.10(13) . . ?
N1 C1 N2 108.34(13) . . ?
C1 N2 C3 111.24(12) . . ?
C1 N2 C16 121.39(12) . . ?
C3 N2 C16 127.23(12) . . ?
C3 C2 N1 110.28(13) . . ?
C2 C3 N2 102.37(12) . . ?
C2 C3 W1 128.66(11) . . ?
N2 C3 W1 128.96(10) . . ?
C5 C4 C9 123.25(13) . . ?
C5 C4 N1 117.86(13) . . ?
C9 C4 N1 118.88(13) . . ?
C6 C5 C4 117.18(14) . . ?
C6 C5 C10 119.64(14) . . ?
C4 C5 C10 123.18(13) . . ?
C7 C6 C5 121.10(15) . . ?
C8 C7 C6 120.14(14) . . ?
C7 C8 C9 121.36(15) . . ?
C8 C9 C4 116.96(14) . . ?
C8 C9 C13 119.93(14) . . ?
C4 C9 C13 123.11(13) . . ?
C5 C10 C12 110.63(13) . . ?
C5 C10 C11 111.34(13) . . ?
C12 C10 C11 110.51(15) . . ?
C9 C13 C15 111.16(14) . . ?
C9 C13 C14 110.81(14) . . ?
C15 C13 C14 110.79(15) . . ?
C21 C16 C17 123.18(14) . . ?
C21 C16 N2 118.86(13) . . ?
C17 C16 N2 117.95(14) . . ?
C18 C17 C16 117.01(15) . . ?
C18 C17 C25 121.34(14) . . ?
C16 C17 C25 121.65(14) . . ?
C19 C18 C17 121.02(15) . . ?
C20 C19 C18 120.58(15) . . ?
C19 C20 C21 121.02(16) . . ?
C20 C21 C16 117.16(15) . . ?
C20 C21 C22 121.09(14) . . ?
C16 C21 C22 121.75(13) . . ?
C21 C22 C24 110.61(13) . . ?
C21 C22 C23 112.34(14) . . ?
C24 C22 C23 110.79(14) . . ?
C17 C25 C26 112.44(14) . . ?
C17 C25 C27 110.47(14) . . ?
C26 C25 C27 109.63(15) . . ?
O2 C28 W1 175.43(14) . . ?
O1 C29 W1 179.7(2) . . ?
O3 C30 W1 177.40(14) . . ?
O4 C31 W1 179.51(15) . . ?
O5 C32 W1 173.57(14) . . ?
C39 C34 C35 117.4(2) . . ?
C39 C34 C33 121.54(19) . . ?
C35 C34 C33 121.05(19) . . ?
C36 C35 C34 121.4(2) . . ?
C35 C36 C37 120.1(2) . . ?
C36 C37 C38 119.3(2) . . ?
C39 C38 C37 120.1(2) . . ?
C38 C39 C34 121.57(19) . . ?
C6C C1C C2C 118.1(10) . . ?
C6C C1C C7C 124.0(12) . . ?
C2C C1C C7C 118.0(11) . . ?
C3C C2C C1C 118.7(11) . . ?
C4C C3C C2C 122.6(11) . . ?
C3C C4C C5C 119.4(11) . . ?
C4C C5C C6C 118.7(12) . . ?
C5C C6C C1C 122.0(13) . . ?
C2B C1B C6B 117.3(11) . . ?
C2B C1B C7B 123.6(11) . . ?
C6B C1B C7B 119.1(11) . . ?
C1B C2B C3B 122.1(12) . . ?
C4B C3B C2B 120.3(13) . . ?
C5B C4B C3B 116.9(12) . . ?
C6B C5B C4B 123.9(12) . . ?
C5B C6B C1B 119.5(12) . . ?

_refine_diff_density_max         2.332
_refine_diff_density_min         -1.096
_refine_diff_density_rms         0.089

_shelxl_version_number           2013-4

