# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_bigcella_a
_database_code_depnum_ccdc_archive 'CCDC 1432626'
_audit_update_record             
;
2015-10-21 deposited with the CCDC.
2016-02-12 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT971_bigcella_a          
;
PROBLEM: Check Calcd Residual Density  0.87A From      W1       7.08 eA-3  
RESPONSE: There is residual density localized around a very heavy region of the complex.
Also one or both of the THF co-ligand may have multiple positions (disorder). However, this wasn't succesfully resolved.  
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        W2(DippF)2Cl4Li
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H70 Cl4 N4 W2, C16 H32 Li O4'
_chemical_formula_sum            'C66 H102 Cl4 Li N4 O4 W2'
_chemical_formula_weight         1531.94

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'
Cl Cl 0.1484 0.1585 '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'
W W -0.8490 6.8722 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   23.7527(9)
_cell_length_b                   12.0648(5)
_cell_length_c                   25.9809(14)
_cell_angle_alpha                90
_cell_angle_beta                 113.0650(10)
_cell_angle_gamma                90
_cell_volume                     6850.2(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_F_000             3108
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    3.559
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5875
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   'Bruker APEXII sadabs'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed tube'
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       'Bruker CMOS'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            71366
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_av_R_equivalents  0.1140
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.864
_diffrn_reflns_theta_max         24.177
_diffrn_reflns_theta_full        24.177
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             5451
_reflns_number_gt                4689
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEXII'
_computing_cell_refinement       'Bruker APEXII'
_computing_data_reduction        'Bruker APEXII SAINT'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXP-2014/7 (Sheldrick, 2014)'
_computing_publication_material  ?
_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)+(0.0410P)²+632.5916P] 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         5451
_refine_ls_number_parameters     354
_refine_ls_number_restraints     361
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.1015
_refine_ls_wR_factor_ref         0.2153
_refine_ls_wR_factor_gt          0.2071
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_restrained_S_all      1.215
_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 0.49813(3) 0.47176(6) 0.54117(3) 0.0276(2) Uani 1 1 d . U . . .
Cl2 Cl 0.5210(2) 0.2859(4) 0.5669(2) 0.0519(14) Uani 1 1 d . U . . .
Cl1 Cl 0.4685(2) 0.6479(4) 0.5642(2) 0.0513(13) Uani 1 1 d . U . . .
N2 N 0.5938(5) 0.5843(11) 0.5024(5) 0.019(2) Uani 1 1 d . U . . .
N1 N 0.5938(5) 0.5004(10) 0.5829(5) 0.023(3) Uani 1 1 d . U . . .
C13 C 0.6210(6) 0.5530(10) 0.5550(6) 0.023(3) Uani 1 1 d . U . . .
H13A H 0.6632 0.5698 0.5740 0.028 Uiso 1 1 calc R U . . .
C7 C 0.6262(6) 0.6671(13) 0.4845(6) 0.020(3) Uani 1 1 d . U . . .
C8 C 0.6493(7) 0.6396(14) 0.4441(7) 0.027(3) Uani 1 1 d . U . . .
C11 C 0.6652(7) 0.8509(14) 0.4898(7) 0.031(3) Uani 1 1 d . U . . .
H11A H 0.6716 0.9229 0.5059 0.037 Uiso 1 1 calc R U . . .
C9 C 0.6807(7) 0.7222(14) 0.4285(7) 0.029(3) Uani 1 1 d . U . . .
H9A H 0.6973 0.7057 0.4016 0.035 Uiso 1 1 calc R U . . .
C12 C 0.6327(6) 0.7737(13) 0.5066(6) 0.024(3) Uani 1 1 d . U . . .
C1 C 0.6351(7) 0.4576(17) 0.6373(7) 0.039(3) Uani 1 1 d . U . . .
C10 C 0.6880(7) 0.8257(14) 0.4509(7) 0.030(3) Uani 1 1 d . U . . .
H10A H 0.7091 0.8805 0.4393 0.036 Uiso 1 1 calc R U . . .
C121 C 0.6070(7) 0.8159(12) 0.5496(7) 0.034(3) Uani 1 1 d . U . . .
H12A H 0.5804 0.7546 0.5531 0.041 Uiso 1 1 calc R U . . .
C21 C 0.6746(8) 0.3046(14) 0.5869(9) 0.052(4) Uani 1 1 d . U . . .
H21A H 0.6400 0.3352 0.5537 0.063 Uiso 1 1 calc R U . . .
C2 C 0.6724(8) 0.3669(18) 0.6375(9) 0.048(4) Uani 1 1 d . U . . .
C81 C 0.6424(9) 0.5236(18) 0.4196(9) 0.051(4) Uani 1 1 d . U . . .
H81A H 0.6137 0.4810 0.4319 0.061 Uiso 1 1 calc R U . . .
C123 C 0.6598(8) 0.8256(19) 0.6083(8) 0.047(5) Uani 1 1 d . U . . .
H12B H 0.6842 0.7574 0.6166 0.071 Uiso 1 1 calc R U . . .
H12C H 0.6859 0.8888 0.6087 0.071 Uiso 1 1 calc R U . . .
H12D H 0.6426 0.8366 0.6366 0.071 Uiso 1 1 calc R U . . .
C6 C 0.6369(9) 0.5059(18) 0.6863(7) 0.048(4) Uani 1 1 d . U . . .
C61 C 0.5982(10) 0.605(2) 0.6868(8) 0.057(4) Uani 1 1 d . U . . .
H61A H 0.5799 0.6366 0.6483 0.069 Uiso 1 1 calc R U . . .
C122 C 0.5672(8) 0.9126(17) 0.5322(9) 0.046(4) Uani 1 1 d . U . . .
H12E H 0.5354 0.8995 0.4949 0.069 Uiso 1 1 calc R U . . .
H12F H 0.5480 0.9255 0.5589 0.069 Uiso 1 1 calc R U . . .
H12G H 0.5914 0.9777 0.5311 0.069 Uiso 1 1 calc R U . . .
C23 C 0.6654(10) 0.1862(19) 0.5842(11) 0.067(6) Uani 1 1 d . U . . .
H23A H 0.6680 0.1574 0.5499 0.101 Uiso 1 1 calc R U . . .
H23B H 0.6970 0.1513 0.6168 0.101 Uiso 1 1 calc R U . . .
H23C H 0.6250 0.1695 0.5840 0.101 Uiso 1 1 calc R U . . .
C22 C 0.7329(12) 0.341(2) 0.5796(14) 0.085(8) Uani 1 1 d . U . . .
H22A H 0.7363 0.4216 0.5818 0.128 Uiso 1 1 calc R U . . .
H22B H 0.7686 0.3075 0.6092 0.128 Uiso 1 1 calc R U . . .
H22C H 0.7310 0.3158 0.5430 0.128 Uiso 1 1 calc R U . . .
C5 C 0.6781(10) 0.464(2) 0.7375(9) 0.069(5) Uani 1 1 d . U . . .
H5A H 0.6820 0.4984 0.7716 0.083 Uiso 1 1 calc R U . . .
C3 C 0.7116(10) 0.324(2) 0.6900(10) 0.070(5) Uani 1 1 d . U . . .
H3A H 0.7368 0.2621 0.6919 0.084 Uiso 1 1 calc R U . . .
C4 C 0.7130(11) 0.373(2) 0.7375(11) 0.074(6) Uani 1 1 d . U . . .
H4A H 0.7392 0.3426 0.7724 0.089 Uiso 1 1 calc R U . . .
C63 C 0.5469(12) 0.563(2) 0.7032(11) 0.080(7) Uani 1 1 d . U . . .
H63A H 0.5209 0.6253 0.7039 0.119 Uiso 1 1 calc R U . . .
H63B H 0.5224 0.5080 0.6758 0.119 Uiso 1 1 calc R U . . .
H63C H 0.5646 0.5288 0.7403 0.119 Uiso 1 1 calc R U . . .
C62 C 0.6339(14) 0.695(2) 0.7278(11) 0.090(8) Uani 1 1 d . U . . .
H62A H 0.6063 0.7569 0.7261 0.135 Uiso 1 1 calc R U . . .
H62B H 0.6511 0.6652 0.7658 0.135 Uiso 1 1 calc R U . . .
H62C H 0.6671 0.7222 0.7176 0.135 Uiso 1 1 calc R U . . .
C83 C 0.6167(17) 0.527(3) 0.3584(12) 0.111(10) Uani 1 1 d . U . . .
H83A H 0.5777 0.5671 0.3450 0.167 Uiso 1 1 calc R U . . .
H83B H 0.6453 0.5654 0.3456 0.167 Uiso 1 1 calc R U . . .
H83C H 0.6100 0.4514 0.3436 0.167 Uiso 1 1 calc R U . . .
C82 C 0.7011(15) 0.463(3) 0.4382(16) 0.122(11) Uani 1 1 d . U . . .
H82A H 0.7193 0.4593 0.4791 0.183 Uiso 1 1 calc R U . . .
H82B H 0.6938 0.3876 0.4228 0.183 Uiso 1 1 calc R U . . .
H82C H 0.7291 0.5015 0.4248 0.183 Uiso 1 1 calc R U . . .
Li1 Li 0.5000 0.029(5) 0.7500 0.064(7) Uani 1 2 d S TU P . .
O4 O 0.4708(7) -0.0604(14) 0.6830(6) 0.067(4) Uani 1 1 d D U . . .
C400 C 0.4983(10) -0.086(2) 0.6442(10) 0.117(9) Uani 1 1 d D U . . .
H40A H 0.5120 -0.1637 0.6468 0.141 Uiso 1 1 calc R U . . .
H40B H 0.5325 -0.0352 0.6479 0.141 Uiso 1 1 calc R U . . .
C401 C 0.4397(14) -0.062(4) 0.5901(10) 0.142(12) Uani 1 1 d D U . . .
H40C H 0.4313 0.0181 0.5845 0.171 Uiso 1 1 calc R U . . .
H40D H 0.4436 -0.0939 0.5565 0.171 Uiso 1 1 calc R U . . .
C402 C 0.3933(11) -0.118(3) 0.6025(10) 0.094(8) Uani 1 1 d D U . . .
H40E H 0.3794 -0.1860 0.5796 0.113 Uiso 1 1 calc R U . . .
H40F H 0.3576 -0.0691 0.5954 0.113 Uiso 1 1 calc R U . . .
C403 C 0.4254(12) -0.147(2) 0.6662(10) 0.105(8) Uani 1 1 d D U . . .
H40G H 0.3970 -0.1418 0.6856 0.127 Uiso 1 1 calc R U . . .
H40H H 0.4443 -0.2219 0.6723 0.127 Uiso 1 1 calc R U . . .
O3 O 0.5721(8) 0.1044(16) 0.7479(8) 0.087(5) Uani 1 1 d D U . . .
C300 C 0.6211(13) 0.145(3) 0.7967(9) 0.145(7) Uani 1 1 d D U . . .
H30A H 0.6167 0.1217 0.8314 0.174 Uiso 1 1 calc R U . . .
H30B H 0.6241 0.2270 0.7961 0.174 Uiso 1 1 calc R U . . .
C301 C 0.6772(13) 0.088(4) 0.7903(15) 0.182(11) Uani 1 1 d D U . . .
H30C H 0.7129 0.1384 0.8013 0.219 Uiso 1 1 calc R U . . .
H30D H 0.6891 0.0190 0.8126 0.219 Uiso 1 1 calc R U . . .
C302 C 0.6526(16) 0.065(4) 0.7306(16) 0.182(11) Uani 1 1 d D U . . .
H30E H 0.6414 -0.0142 0.7231 0.219 Uiso 1 1 calc R U . . .
H30F H 0.6822 0.0848 0.7140 0.219 Uiso 1 1 calc R U . . .
C303 C 0.5932(14) 0.143(2) 0.7070(9) 0.145(7) Uani 1 1 d D U . . .
H30G H 0.6031 0.2228 0.7103 0.174 Uiso 1 1 calc R U . . .
H30H H 0.5653 0.1240 0.6683 0.174 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 N1 2.128(12) . ?
W1 N2 2.139(11) 5_666 ?
W1 W1 2.2794(13) 5_666 ?
W1 Cl2 2.342(5) . ?
W1 Cl1 2.388(6) . ?
N2 C13 1.318(18) . ?
N2 C7 1.443(18) . ?
N2 W1 2.139(11) 5_666 ?
N1 C13 1.308(19) . ?
N1 C1 1.46(2) . ?
C13 H13A 0.9500 . ?
C7 C12 1.39(2) . ?
C7 C8 1.40(2) . ?
C8 C9 1.40(2) . ?
C8 C81 1.52(3) . ?
C11 C10 1.35(2) . ?
C11 C12 1.38(2) . ?
C11 H11A 0.9500 . ?
C9 C10 1.36(2) . ?
C9 H9A 0.9500 . ?
C12 C121 1.55(2) . ?
C1 C6 1.39(3) . ?
C1 C2 1.41(3) . ?
C10 H10A 0.9500 . ?
C121 C122 1.46(2) . ?
C121 C123 1.55(2) . ?
C121 H12A 1.0000 . ?
C21 C23 1.44(3) . ?
C21 C2 1.53(3) . ?
C21 C22 1.53(3) . ?
C21 H21A 1.0000 . ?
C2 C3 1.41(3) . ?
C81 C83 1.47(3) . ?
C81 C82 1.48(4) . ?
C81 H81A 1.0000 . ?
C123 H12B 0.9800 . ?
C123 H12C 0.9800 . ?
C123 H12D 0.9800 . ?
C6 C5 1.40(3) . ?
C6 C61 1.51(3) . ?
C61 C63 1.52(3) . ?
C61 C62 1.53(3) . ?
C61 H61A 1.0000 . ?
C122 H12E 0.9800 . ?
C122 H12F 0.9800 . ?
C122 H12G 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C5 C4 1.38(4) . ?
C5 H5A 0.9500 . ?
C3 C4 1.36(4) . ?
C3 H3A 0.9500 . ?
C4 H4A 0.9500 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
Li1 O4 1.93(4) . ?
Li1 O4 1.94(4) 2_656 ?
Li1 O3 1.96(3) 2_656 ?
Li1 O3 1.96(3) . ?
O4 C400 1.431(17) . ?
O4 C403 1.442(17) . ?
C400 C401 1.57(3) . ?
C400 H40A 0.9900 . ?
C400 H40B 0.9900 . ?
C401 C402 1.43(3) . ?
C401 H40C 0.9900 . ?
C401 H40D 0.9900 . ?
C402 C403 1.57(3) . ?
C402 H40E 0.9900 . ?
C402 H40F 0.9900 . ?
C403 H40G 0.9900 . ?
C403 H40H 0.9900 . ?
O3 C303 1.419(17) . ?
O3 C300 1.430(18) . ?
C300 C301 1.57(3) . ?
C300 H30A 0.9900 . ?
C300 H30B 0.9900 . ?
C301 C302 1.45(3) . ?
C301 H30C 0.9900 . ?
C301 H30D 0.9900 . ?
C302 C303 1.60(3) . ?
C302 H30E 0.9900 . ?
C302 H30F 0.9900 . ?
C303 H30G 0.9900 . ?
C303 H30H 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
N1 W1 N2 170.6(5) . 5_666 ?
N1 W1 W1 90.2(3) . 5_666 ?
N2 W1 W1 90.3(3) 5_666 5_666 ?
N1 W1 Cl2 85.9(4) . . ?
N2 W1 Cl2 85.6(4) 5_666 . ?
W1 W1 Cl2 117.65(16) 5_666 . ?
N1 W1 Cl1 95.1(4) . . ?
N2 W1 Cl1 94.2(4) 5_666 . ?
W1 W1 Cl1 95.33(14) 5_666 . ?
Cl2 W1 Cl1 147.0(2) . . ?
C13 N2 C7 115.2(11) . . ?
C13 N2 W1 116.2(9) . 5_666 ?
C7 N2 W1 127.6(9) . 5_666 ?
C13 N1 C1 114.7(12) . . ?
C13 N1 W1 117.2(9) . . ?
C1 N1 W1 127.7(10) . . ?
N1 C13 N2 124.5(13) . . ?
N1 C13 H13A 117.8 . . ?
N2 C13 H13A 117.8 . . ?
C12 C7 C8 120.9(14) . . ?
C12 C7 N2 119.7(13) . . ?
C8 C7 N2 119.4(14) . . ?
C9 C8 C7 117.3(15) . . ?
C9 C8 C81 121.2(15) . . ?
C7 C8 C81 121.4(14) . . ?
C10 C11 C12 121.2(17) . . ?
C10 C11 H11A 119.4 . . ?
C12 C11 H11A 119.4 . . ?
C10 C9 C8 121.6(16) . . ?
C10 C9 H9A 119.2 . . ?
C8 C9 H9A 119.2 . . ?
C11 C12 C7 118.6(15) . . ?
C11 C12 C121 115.4(14) . . ?
C7 C12 C121 125.9(14) . . ?
C6 C1 C2 122.1(17) . . ?
C6 C1 N1 120.5(18) . . ?
C2 C1 N1 117.4(17) . . ?
C11 C10 C9 120.3(16) . . ?
C11 C10 H10A 119.8 . . ?
C9 C10 H10A 119.8 . . ?
C122 C121 C123 114.9(15) . . ?
C122 C121 C12 115.4(15) . . ?
C123 C121 C12 109.8(13) . . ?
C122 C121 H12A 105.2 . . ?
C123 C121 H12A 105.2 . . ?
C12 C121 H12A 105.2 . . ?
C23 C21 C2 118(2) . . ?
C23 C21 C22 113.7(19) . . ?
C2 C21 C22 107.7(18) . . ?
C23 C21 H21A 105.4 . . ?
C2 C21 H21A 105.4 . . ?
C22 C21 H21A 105.4 . . ?
C1 C2 C3 118(2) . . ?
C1 C2 C21 127.6(16) . . ?
C3 C2 C21 115(2) . . ?
C83 C81 C82 108(2) . . ?
C83 C81 C8 111(2) . . ?
C82 C81 C8 112.7(19) . . ?
C83 C81 H81A 108.4 . . ?
C82 C81 H81A 108.4 . . ?
C8 C81 H81A 108.4 . . ?
C121 C123 H12B 109.5 . . ?
C121 C123 H12C 109.5 . . ?
H12B C123 H12C 109.5 . . ?
C121 C123 H12D 109.5 . . ?
H12B C123 H12D 109.5 . . ?
H12C C123 H12D 109.5 . . ?
C1 C6 C5 119(2) . . ?
C1 C6 C61 122.8(17) . . ?
C5 C6 C61 119(2) . . ?
C6 C61 C63 107(2) . . ?
C6 C61 C62 114(2) . . ?
C63 C61 C62 109(2) . . ?
C6 C61 H61A 108.9 . . ?
C63 C61 H61A 108.9 . . ?
C62 C61 H61A 108.9 . . ?
C121 C122 H12E 109.5 . . ?
C121 C122 H12F 109.5 . . ?
H12E C122 H12F 109.5 . . ?
C121 C122 H12G 109.5 . . ?
H12E C122 H12G 109.5 . . ?
H12F C122 H12G 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C4 C5 C6 119(2) . . ?
C4 C5 H5A 120.5 . . ?
C6 C5 H5A 120.5 . . ?
C4 C3 C2 120(3) . . ?
C4 C3 H3A 120.2 . . ?
C2 C3 H3A 120.2 . . ?
C3 C4 C5 123(2) . . ?
C3 C4 H4A 118.5 . . ?
C5 C4 H4A 118.5 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C81 C83 H83A 109.5 . . ?
C81 C83 H83B 109.5 . . ?
H83A C83 H83B 109.5 . . ?
C81 C83 H83C 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
O4 Li1 O4 112(3) . 2_656 ?
O4 Li1 O3 105.9(8) . 2_656 ?
O4 Li1 O3 104.1(7) 2_656 2_656 ?
O4 Li1 O3 104.1(7) . . ?
O4 Li1 O3 105.9(8) 2_656 . ?
O3 Li1 O3 125(3) 2_656 . ?
C400 O4 C403 97.2(14) . . ?
C400 O4 Li1 130.6(13) . . ?
C403 O4 Li1 129.8(16) . . ?
O4 C400 C401 95.9(16) . . ?
O4 C400 H40A 112.6 . . ?
C401 C400 H40A 112.6 . . ?
O4 C400 H40B 112.6 . . ?
C401 C400 H40B 112.6 . . ?
H40A C400 H40B 110.1 . . ?
C402 C401 C400 101.9(14) . . ?
C402 C401 H40C 111.4 . . ?
C400 C401 H40C 111.4 . . ?
C402 C401 H40D 111.4 . . ?
C400 C401 H40D 111.4 . . ?
H40C C401 H40D 109.3 . . ?
C401 C402 C403 104.0(12) . . ?
C401 C402 H40E 110.9 . . ?
C403 C402 H40E 110.9 . . ?
C401 C402 H40F 110.9 . . ?
C403 C402 H40F 110.9 . . ?
H40E C402 H40F 109.0 . . ?
O4 C403 C402 98.8(15) . . ?
O4 C403 H40G 112.0 . . ?
C402 C403 H40G 112.0 . . ?
O4 C403 H40H 112.0 . . ?
C402 C403 H40H 112.0 . . ?
H40G C403 H40H 109.7 . . ?
C303 O3 C300 98.5(15) . . ?
C303 O3 Li1 137.8(15) . . ?
C300 O3 Li1 123.5(16) . . ?
O3 C300 C301 100.7(18) . . ?
O3 C300 H30A 111.6 . . ?
C301 C300 H30A 111.6 . . ?
O3 C300 H30B 111.6 . . ?
C301 C300 H30B 111.6 . . ?
H30A C300 H30B 109.4 . . ?
C302 C301 C300 101.2(13) . . ?
C302 C301 H30C 111.5 . . ?
C300 C301 H30C 111.5 . . ?
C302 C301 H30D 111.5 . . ?
C300 C301 H30D 111.5 . . ?
H30C C301 H30D 109.4 . . ?
C301 C302 C303 102.9(16) . . ?
C301 C302 H30E 111.2 . . ?
C303 C302 H30E 111.2 . . ?
C301 C302 H30F 111.2 . . ?
C303 C302 H30F 111.2 . . ?
H30E C302 H30F 109.1 . . ?
O3 C303 C302 92.2(17) . . ?
O3 C303 H30G 113.3 . . ?
C302 C303 H30G 113.3 . . ?
O3 C303 H30H 113.3 . . ?
C302 C303 H30H 113.3 . . ?
H30G C303 H30H 110.6 . . ?

_refine_diff_density_max         7.456
_refine_diff_density_min         -3.690
_refine_diff_density_rms         0.265

####################################################################### 
# 
# 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_basic_a
_database_code_depnum_ccdc_archive 'CCDC 1432627'
_audit_update_record             
;
2015-10-21 deposited with the CCDC.
2016-02-12 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_THETM01_basic_a             
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: This was the best crystal provided by the experimentalist. The resulting data is less than ideal. However another sample isn't availible at present.
;
_vrf_PLAT602_basic_a             
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info 
RESPONSE: This I'm not sure about. I've looked over the space filling diagrams in XP and used analytical software (Platon) and I don't see gaping voids. I'm more than happy to revist.
;
_vrf_PLAT213_basic_a             
;
PROBLEM: Atom C7              has ADP max/min Ratio .....        4.4 oblate
RESPONSE: C7 is affected by a nearby metal center (this message is copied for similar entries ignore where appropriate) 
;
_vrf_PLAT342_basic_a             
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0442 Ang.  
RESPONSE: This was the best crystal provided by the experimentalist. The resulting data is less than ideal. However another sample isn't availible at present.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        W2(DippF)2K2
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C116 H176 K4 N8 O4 W4'
_chemical_formula_weight         2638.44

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'
K K 0.2009 0.2494 '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'
W W -0.8490 6.8722 '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'

_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                   10.879(2)
_cell_length_b                   13.364(3)
_cell_length_c                   23.272(5)
_cell_angle_alpha                96.119(6)
_cell_angle_beta                 99.340(6)
_cell_angle_gamma                105.700(6)
_cell_volume                     3173.6(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_F_000             1326
_exptl_transmission_factor_min   0.5817
_exptl_transmission_factor_max   0.7446
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    3.791
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'Bruker SadAbs'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Mo sealed tube'
_diffrn_measurement_device_type  'D8 quest'
_diffrn_measurement_method       'phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28893
_diffrn_reflns_av_unetI/netI     0.0740
_diffrn_reflns_av_R_equivalents  0.0971
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.388
_diffrn_reflns_theta_max         20.841
_diffrn_reflns_theta_full        20.841
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measured_fraction_theta_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_point_group_measured_fraction_full 0.966
_reflns_number_total             6451
_reflns_number_gt                4600
_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       'Apex II Bruker 2015'
_computing_cell_refinement       'Apex II Bruker 2015'
_computing_data_reduction        'Apex II Bruker 2015'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Apex II Bruker 2015'
_computing_publication_material  ?
_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)+(0.1196P)²+135.4914P] 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         6451
_refine_ls_number_parameters     603
_refine_ls_number_restraints     661
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0740
_refine_ls_wR_factor_ref         0.2446
_refine_ls_wR_factor_gt          0.2002
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_restrained_S_all      1.070
_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 0.35480(9) 0.38467(8) 0.21956(4) 0.0215(4) Uani 1 1 d . U . . .
W2 W 0.57733(9) 0.38380(8) 0.24767(4) 0.0216(4) Uani 1 1 d . U . . .
K1 K 1.0120(6) 0.3666(5) 0.2253(2) 0.0388(16) Uani 1 1 d . U . . .
K2 K 0.4494(7) 0.6721(6) 0.2177(3) 0.0605(19) Uani 1 1 d . U . . .
N1 N 0.5619(16) 0.3997(15) 0.3359(7) 0.017(3) Uani 1 1 d . U . . .
C1 C 0.448(2) 0.403(2) 0.3529(10) 0.023(5) Uani 1 1 d . U . . .
H1 H 0.4411 0.4086 0.3932 0.028 Uiso 1 1 calc R U . . .
N2 N 0.3444(17) 0.3995(15) 0.3101(8) 0.019(3) Uani 1 1 d . U . . .
N3 N 0.3706(16) 0.3629(15) 0.1304(7) 0.016(3) Uani 1 1 d . U . . .
C2 C 0.486(2) 0.359(2) 0.1158(10) 0.023(5) Uani 1 1 d . U . . .
H2 H 0.4922 0.3500 0.0754 0.028 Uiso 1 1 calc R U . . .
N4 N 0.5920(17) 0.3681(15) 0.1576(8) 0.020(4) Uani 1 1 d . U . . .
C3 C 0.658(2) 0.385(2) 0.3839(10) 0.0250(18) Uani 1 1 d . U . . .
C4 C 0.674(2) 0.286(2) 0.3775(11) 0.033(5) Uani 1 1 d . U . . .
C5 C 0.601(3) 0.200(2) 0.3230(11) 0.041(5) Uani 1 1 d . U . . .
H5 H 0.5054 0.1909 0.3202 0.050 Uiso 1 1 calc R U . . .
C6 C 0.622(4) 0.095(3) 0.3296(13) 0.063(8) Uani 1 1 d . U . . .
H6A H 0.5716 0.0435 0.2950 0.095 Uiso 1 1 calc R U . . .
H6B H 0.5934 0.0725 0.3651 0.095 Uiso 1 1 calc R U . . .
H6C H 0.7148 0.1016 0.3329 0.095 Uiso 1 1 calc R U . . .
C7 C 0.637(3) 0.243(2) 0.2671(11) 0.041(6) Uani 1 1 d . U . . .
H7A H 0.7320 0.2687 0.2723 0.062 Uiso 1 1 calc R U . . .
H7B H 0.5996 0.3005 0.2603 0.062 Uiso 1 1 calc R U . . .
H7C H 0.6025 0.1862 0.2331 0.062 Uiso 1 1 calc R U . . .
C8 C 0.757(3) 0.268(3) 0.4262(12) 0.051(7) Uani 1 1 d . U . . .
H8 H 0.7690 0.2008 0.4268 0.061 Uiso 1 1 calc R U . . .
C9 C 0.819(3) 0.347(3) 0.4726(12) 0.043(6) Uani 1 1 d . U . . .
H9 H 0.8744 0.3323 0.5044 0.052 Uiso 1 1 calc R U . . .
C10 C 0.808(3) 0.444(3) 0.4758(11) 0.044(6) Uani 1 1 d . U . . .
H10 H 0.8547 0.4958 0.5088 0.053 Uiso 1 1 calc R U . . .
C11 C 0.724(2) 0.468(2) 0.4294(11) 0.038(5) Uani 1 1 d . U . . .
C12 C 0.716(3) 0.578(2) 0.4321(12) 0.042(5) Uani 1 1 d . U . . .
H12 H 0.6467 0.5777 0.3980 0.050 Uiso 1 1 calc R U . . .
C13 C 0.673(3) 0.614(3) 0.4882(13) 0.066(8) Uani 1 1 d . U . . .
H13A H 0.7303 0.6029 0.5227 0.099 Uiso 1 1 calc R U . . .
H13B H 0.5831 0.5725 0.4871 0.099 Uiso 1 1 calc R U . . .
H13C H 0.6789 0.6884 0.4908 0.099 Uiso 1 1 calc R U . . .
C14 C 0.840(3) 0.650(2) 0.4242(13) 0.048(6) Uani 1 1 d . U . . .
H14A H 0.9109 0.6498 0.4561 0.072 Uiso 1 1 calc R U . . .
H14B H 0.8323 0.7215 0.4251 0.072 Uiso 1 1 calc R U . . .
H14C H 0.8593 0.6265 0.3862 0.072 Uiso 1 1 calc R U . . .
C15 C 0.233(2) 0.402(2) 0.3317(10) 0.0250(18) Uani 1 1 d . U . . .
C16 C 0.144(2) 0.312(2) 0.3377(10) 0.027(4) Uani 1 1 d . U . . .
C17 C 0.169(3) 0.204(2) 0.3265(12) 0.043(5) Uani 1 1 d . U . . .
H17 H 0.2375 0.2137 0.3018 0.052 Uiso 1 1 calc R U . . .
C18 C 0.051(3) 0.118(3) 0.2904(15) 0.062(8) Uani 1 1 d . U . . .
H18A H 0.0756 0.0526 0.2827 0.094 Uiso 1 1 calc R U . . .
H18B H 0.0222 0.1392 0.2529 0.094 Uiso 1 1 calc R U . . .
H18C H -0.0192 0.1052 0.3125 0.094 Uiso 1 1 calc R U . . .
C19 C 0.229(3) 0.176(3) 0.3836(13) 0.056(8) Uani 1 1 d . U . . .
H19A H 0.1630 0.1567 0.4075 0.084 Uiso 1 1 calc R U . . .
H19B H 0.3006 0.2370 0.4054 0.084 Uiso 1 1 calc R U . . .
H19C H 0.2636 0.1168 0.3748 0.084 Uiso 1 1 calc R U . . .
C20 C 0.029(2) 0.316(2) 0.3553(10) 0.031(4) Uani 1 1 d . U . . .
H20 H -0.0317 0.2529 0.3608 0.037 Uiso 1 1 calc R U . . .
C21 C 0.004(2) 0.411(2) 0.3647(11) 0.037(6) Uani 1 1 d . U . . .
H21 H -0.0779 0.4130 0.3738 0.044 Uiso 1 1 calc R U . . .
C22 C 0.089(2) 0.499(2) 0.3613(10) 0.031(4) Uani 1 1 d . U . . .
H22 H 0.0684 0.5635 0.3703 0.037 Uiso 1 1 calc R U . . .
C23 C 0.208(2) 0.504(2) 0.3452(10) 0.028(4) Uani 1 1 d . U . . .
C24 C 0.309(2) 0.604(2) 0.3439(12) 0.042(5) Uani 1 1 d . U . . .
H24 H 0.3752 0.5867 0.3226 0.050 Uiso 1 1 calc R U . . .
C25 C 0.251(3) 0.681(3) 0.3117(14) 0.056(6) Uani 1 1 d . U . . .
H25A H 0.3210 0.7454 0.3120 0.084 Uiso 1 1 calc R U . . .
H25B H 0.2109 0.6481 0.2709 0.084 Uiso 1 1 calc R U . . .
H25C H 0.1855 0.6983 0.3318 0.084 Uiso 1 1 calc R U . . .
C26 C 0.378(3) 0.660(3) 0.4067(13) 0.059(7) Uani 1 1 d . U . . .
H26A H 0.3203 0.6921 0.4250 0.088 Uiso 1 1 calc R U . . .
H26B H 0.4577 0.7149 0.4048 0.088 Uiso 1 1 calc R U . . .
H26C H 0.4016 0.6088 0.4302 0.088 Uiso 1 1 calc R U . . .
C27 C 0.273(2) 0.354(2) 0.0772(10) 0.0250(18) Uani 1 1 d . U . . .
C28 C 0.191(3) 0.249(2) 0.0562(12) 0.044(5) Uani 1 1 d . U . . .
C29 C 0.195(3) 0.149(3) 0.0819(14) 0.058(6) Uani 1 1 d . U . . .
H29 H 0.2600 0.1714 0.1201 0.070 Uiso 1 1 calc R U . . .
C30 C 0.065(3) 0.088(3) 0.0960(18) 0.081(10) Uani 1 1 d . U . . .
H30A H 0.0498 0.1268 0.1311 0.121 Uiso 1 1 calc R U . . .
H30B H 0.0679 0.0182 0.1033 0.121 Uiso 1 1 calc R U . . .
H30C H -0.0056 0.0819 0.0625 0.121 Uiso 1 1 calc R U . . .
C31 C 0.247(4) 0.079(3) 0.0416(16) 0.079(9) Uani 1 1 d . U . . .
H31A H 0.1924 0.0626 0.0021 0.119 Uiso 1 1 calc R U . . .
H31B H 0.2461 0.0142 0.0575 0.119 Uiso 1 1 calc R U . . .
H31C H 0.3369 0.1169 0.0395 0.119 Uiso 1 1 calc R U . . .
C32 C 0.098(3) 0.243(3) 0.0033(13) 0.059(7) Uani 1 1 d . U . . .
H32 H 0.0390 0.1765 -0.0148 0.070 Uiso 1 1 calc R U . . .
C33 C 0.094(3) 0.325(3) -0.0203(15) 0.063(7) Uani 1 1 d . U . . .
H33 H 0.0306 0.3168 -0.0549 0.076 Uiso 1 1 calc R U . . .
C34 C 0.171(3) 0.417(3) 0.0000(13) 0.057(6) Uani 1 1 d . U . . .
H34 H 0.1662 0.4743 -0.0201 0.068 Uiso 1 1 calc R U . . .
C35 C 0.260(3) 0.431(3) 0.0515(12) 0.044(5) Uani 1 1 d . U . . .
C36 C 0.342(3) 0.539(3) 0.0749(14) 0.054(5) Uani 1 1 d . U . . .
H36 H 0.3908 0.5355 0.1144 0.065 Uiso 1 1 calc R U . . .
C37 C 0.265(3) 0.617(3) 0.0873(14) 0.060(6) Uani 1 1 d . U . . .
H37A H 0.3253 0.6872 0.1027 0.090 Uiso 1 1 calc R U . . .
H37B H 0.2073 0.6195 0.0507 0.090 Uiso 1 1 calc R U . . .
H37C H 0.2122 0.5938 0.1166 0.090 Uiso 1 1 calc R U . . .
C38 C 0.451(4) 0.591(3) 0.0399(19) 0.088(9) Uani 1 1 d . U . . .
H38A H 0.5174 0.5540 0.0429 0.132 Uiso 1 1 calc R U . . .
H38B H 0.4912 0.6654 0.0570 0.132 Uiso 1 1 calc R U . . .
H38C H 0.4110 0.5855 -0.0017 0.132 Uiso 1 1 calc R U . . .
C39 C 0.707(2) 0.379(2) 0.1391(10) 0.0250(18) Uani 1 1 d . U . . .
C40 C 0.736(2) 0.293(2) 0.1063(10) 0.030(4) Uani 1 1 d . U . . .
C41 C 0.637(3) 0.186(2) 0.0890(12) 0.044(5) Uani 1 1 d . U . . .
H41 H 0.5575 0.1872 0.1051 0.052 Uiso 1 1 calc R U . . .
C42 C 0.694(3) 0.106(3) 0.1161(14) 0.057(7) Uani 1 1 d . U . . .
H42A H 0.7693 0.1005 0.0989 0.086 Uiso 1 1 calc R U . . .
H42B H 0.6283 0.0369 0.1081 0.086 Uiso 1 1 calc R U . . .
H42C H 0.7227 0.1284 0.1588 0.086 Uiso 1 1 calc R U . . .
C43 C 0.598(3) 0.156(3) 0.0218(13) 0.057(7) Uani 1 1 d . U . . .
H43A H 0.5697 0.2118 0.0049 0.085 Uiso 1 1 calc R U . . .
H43B H 0.5263 0.0899 0.0115 0.085 Uiso 1 1 calc R U . . .
H43C H 0.6729 0.1461 0.0060 0.085 Uiso 1 1 calc R U . . .
C44 C 0.855(2) 0.316(2) 0.0882(10) 0.032(5) Uani 1 1 d . U . . .
H44 H 0.8736 0.2615 0.0647 0.038 Uiso 1 1 calc R U . . .
C45 C 0.943(2) 0.409(2) 0.1019(11) 0.032(4) Uani 1 1 d . U . . .
H45 H 1.0215 0.4208 0.0876 0.039 Uiso 1 1 calc R U . . .
C46 C 0.920(2) 0.491(2) 0.1372(10) 0.032(4) Uani 1 1 d . U . . .
H46 H 0.9842 0.5576 0.1480 0.038 Uiso 1 1 calc R U . . .
C47 C 0.803(2) 0.472(2) 0.1564(11) 0.032(4) Uani 1 1 d . U . . .
C48 C 0.780(3) 0.561(2) 0.1962(12) 0.039(4) Uani 1 1 d . U . . .
H48 H 0.6985 0.5729 0.1753 0.047 Uiso 1 1 calc R U . . .
C49 C 0.884(3) 0.668(2) 0.2080(14) 0.055(7) Uani 1 1 d . U . . .
H49A H 0.9612 0.6644 0.2351 0.082 Uiso 1 1 calc R U . . .
H49B H 0.8496 0.7217 0.2257 0.082 Uiso 1 1 calc R U . . .
H49C H 0.9079 0.6860 0.1708 0.082 Uiso 1 1 calc R U . . .
C50 C 0.749(2) 0.525(2) 0.2557(10) 0.027(5) Uani 1 1 d . U . . .
H50A H 0.7347 0.5829 0.2806 0.041 Uiso 1 1 calc R U . . .
H50B H 0.6703 0.4644 0.2473 0.041 Uiso 1 1 calc R U . . .
H50C H 0.8224 0.5047 0.2762 0.041 Uiso 1 1 calc R U . . .
C51 C 0.657(3) 0.813(4) 0.3388(19) 0.091(9) Uani 1 1 d . U . . .
H51A H 0.6894 0.8338 0.3815 0.137 Uiso 1 1 calc R U . . .
H51B H 0.5722 0.8255 0.3280 0.137 Uiso 1 1 calc R U . . .
H51C H 0.6479 0.7381 0.3278 0.137 Uiso 1 1 calc R U . . .
C52 C 0.754(4) 0.879(4) 0.306(2) 0.122(16) Uani 1 1 d . U . . .
H52A H 0.7641 0.9548 0.3142 0.146 Uiso 1 1 calc R U . . .
H52B H 0.8408 0.8662 0.3140 0.146 Uiso 1 1 calc R U . . .
O2 O 0.681(2) 0.831(2) 0.2479(13) 0.090(6) Uani 1 1 d . U . . .
C53 C 0.756(4) 0.889(4) 0.211(2) 0.099(10) Uani 1 1 d . U . . .
H53A H 0.7527 0.9623 0.2168 0.119 Uiso 1 1 calc R U . . .
H53B H 0.8485 0.8900 0.2230 0.119 Uiso 1 1 calc R U . . .
C54 C 0.709(4) 0.843(4) 0.151(2) 0.105(12) Uani 1 1 d . U . . .
H54A H 0.7043 0.7685 0.1465 0.158 Uiso 1 1 calc R U . . .
H54B H 0.7678 0.8794 0.1273 0.158 Uiso 1 1 calc R U . . .
H54C H 0.6218 0.8504 0.1384 0.158 Uiso 1 1 calc R U . . .
O1 O 0.344(2) 0.8320(19) 0.1959(11) 0.079(5) Uani 1 1 d D U . . .
C100 C 0.210(3) 0.809(3) 0.187(2) 0.114(13) Uani 1 1 d D U . . .
H10A H 0.1710 0.7481 0.2057 0.137 Uiso 1 1 calc R U . . .
H10B H 0.1695 0.7951 0.1446 0.137 Uiso 1 1 calc R U . . .
C101 C 0.194(4) 0.908(4) 0.217(3) 0.17(2) Uani 1 1 d D U . . .
H10C H 0.1863 0.9032 0.2583 0.199 Uiso 1 1 calc R U . . .
H10D H 0.1157 0.9233 0.1960 0.199 Uiso 1 1 calc R U . . .
C102 C 0.323(5) 0.995(3) 0.213(3) 0.16(2) Uani 1 1 d D U . . .
H10E H 0.3045 1.0433 0.1856 0.190 Uiso 1 1 calc R U . . .
H10F H 0.3668 1.0369 0.2523 0.190 Uiso 1 1 calc R U . . .
C103 C 0.407(4) 0.933(3) 0.190(2) 0.103(11) Uani 1 1 d D U . . .
H10G H 0.4108 0.9400 0.1487 0.124 Uiso 1 1 calc R U . . .
H10H H 0.4961 0.9572 0.2144 0.124 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 N3 2.105(17) . ?
W1 N2 2.119(17) . ?
W1 W2 2.4067(13) . ?
W1 K1 3.697(6) 1_455 ?
W1 K2 3.705(8) . ?
W2 N1 2.081(17) . ?
W2 N4 2.121(18) . ?
W2 C50 2.23(3) . ?
K1 C46 2.98(2) . ?
K1 C45 3.00(2) . ?
K1 C16 3.03(2) 1_655 ?
K1 C15 3.06(2) 1_655 ?
K1 C20 3.16(2) 1_655 ?
K1 C23 3.25(2) 1_655 ?
K1 C21 3.26(3) 1_655 ?
K1 C44 3.27(2) . ?
K1 C47 3.28(2) . ?
K1 C22 3.32(2) 1_655 ?
K1 W1 3.697(6) 1_655 ?
K2 O1 2.74(2) . ?
K2 O2 2.75(3) . ?
K2 C37 3.24(3) . ?
K2 C25 3.33(3) . ?
K2 C51 3.33(4) . ?
K2 C36 3.45(3) . ?
N1 C1 1.37(3) . ?
N1 C3 1.46(3) . ?
C1 N2 1.36(3) . ?
C1 H1 0.9500 . ?
N2 C15 1.39(3) . ?
N3 C2 1.37(3) . ?
N3 C27 1.46(3) . ?
C2 N4 1.35(3) . ?
C2 H2 0.9500 . ?
N4 C39 1.36(3) . ?
C3 C4 1.38(4) . ?
C3 C11 1.39(4) . ?
C4 C8 1.41(4) . ?
C4 C5 1.56(4) . ?
C5 C6 1.50(4) . ?
C5 C7 1.54(4) . ?
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 1.37(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.32(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.42(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.49(4) . ?
C12 C14 1.49(4) . ?
C12 C13 1.53(4) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.36(4) . ?
C15 C23 1.47(4) . ?
C15 K1 3.06(2) 1_455 ?
C16 C20 1.40(3) . ?
C16 C17 1.54(4) . ?
C16 K1 3.03(2) 1_455 ?
C17 C19 1.51(4) . ?
C17 C18 1.53(4) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.38(4) . ?
C20 K1 3.16(2) 1_455 ?
C20 H20 0.9500 . ?
C21 C22 1.30(4) . ?
C21 K1 3.26(3) 1_455 ?
C21 H21 0.9500 . ?
C22 C23 1.40(3) . ?
C22 K1 3.32(2) 1_455 ?
C22 H22 0.9500 . ?
C23 C24 1.49(4) . ?
C23 K1 3.25(2) 1_455 ?
C24 C26 1.54(4) . ?
C24 C25 1.54(4) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C35 1.28(4) . ?
C27 C28 1.42(4) . ?
C28 C32 1.44(4) . ?
C28 C29 1.53(4) . ?
C29 C31 1.53(4) . ?
C29 C30 1.54(5) . ?
C29 H29 1.0000 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.29(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.27(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.37(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.48(4) . ?
C36 C37 1.53(4) . ?
C36 C38 1.59(5) . ?
C36 H36 1.0000 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C47 1.36(4) . ?
C39 C40 1.45(3) . ?
C40 C44 1.39(3) . ?
C40 C41 1.51(4) . ?
C41 C42 1.52(4) . ?
C41 C43 1.53(4) . ?
C41 H41 1.0000 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C45 1.32(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.39(4) . ?
C45 H45 0.9500 . ?
C46 C47 1.39(3) . ?
C46 H46 0.9500 . ?
C47 C48 1.53(4) . ?
C48 C49 1.53(4) . ?
C48 C50 1.57(4) . ?
C48 H48 1.0000 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 C52 1.54(6) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 O2 1.43(5) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
O2 C53 1.42(5) . ?
C53 C54 1.42(6) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
O1 C103 1.37(3) . ?
O1 C100 1.39(3) . ?
C100 C101 1.49(4) . ?
C100 H10A 0.9900 . ?
C100 H10B 0.9900 . ?
C101 C102 1.59(7) . ?
C101 H10C 0.9900 . ?
C101 H10D 0.9900 . ?
C102 C103 1.50(4) . ?
C102 H10E 0.9900 . ?
C102 H10F 0.9900 . ?
C103 H10G 0.9900 . ?
C103 H10H 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
N3 W1 N2 176.6(6) . . ?
N3 W1 W2 89.2(4) . . ?
N2 W1 W2 88.4(5) . . ?
N3 W1 K1 108.2(5) . 1_455 ?
N2 W1 K1 73.9(5) . 1_455 ?
W2 W1 K1 161.41(10) . 1_455 ?
N3 W1 K2 88.2(5) . . ?
N2 W1 K2 94.4(5) . . ?
W2 W1 K2 92.93(11) . . ?
K1 W1 K2 93.89(15) 1_455 . ?
N1 W2 N4 179.6(6) . . ?
N1 W2 C50 97.3(8) . . ?
N4 W2 C50 82.8(8) . . ?
N1 W2 W1 89.9(4) . . ?
N4 W2 W1 89.7(5) . . ?
C50 W2 W1 123.8(6) . . ?
C46 K1 C45 26.9(7) . . ?
C46 K1 C16 161.2(8) . 1_655 ?
C45 K1 C16 164.4(7) . 1_655 ?
C46 K1 C15 138.0(8) . 1_655 ?
C45 K1 C15 144.9(7) . 1_655 ?
C16 K1 C15 25.8(7) 1_655 1_655 ?
C46 K1 C20 147.1(7) . 1_655 ?
C45 K1 C20 169.2(6) . 1_655 ?
C16 K1 C20 25.9(6) 1_655 1_655 ?
C15 K1 C20 45.2(6) 1_655 1_655 ?
C46 K1 C23 115.6(7) . 1_655 ?
C45 K1 C23 134.2(8) . 1_655 ?
C16 K1 C23 45.7(7) 1_655 1_655 ?
C15 K1 C23 26.7(6) 1_655 1_655 ?
C20 K1 C23 51.7(7) 1_655 1_655 ?
C46 K1 C21 123.2(7) . 1_655 ?
C45 K1 C21 149.6(7) . 1_655 ?
C16 K1 C21 44.6(6) 1_655 1_655 ?
C15 K1 C21 51.7(6) 1_655 1_655 ?
C20 K1 C21 24.8(7) 1_655 1_655 ?
C23 K1 C21 42.9(6) 1_655 1_655 ?
C46 K1 C44 43.9(7) . . ?
C45 K1 C44 23.8(7) . . ?
C16 K1 C44 154.8(7) 1_655 . ?
C15 K1 C44 160.1(6) 1_655 . ?
C20 K1 C44 149.0(7) 1_655 . ?
C23 K1 C44 157.9(7) 1_655 . ?
C21 K1 C44 148.1(6) 1_655 . ?
C46 K1 C47 25.1(6) . . ?
C45 K1 C47 44.5(6) . . ?
C16 K1 C47 150.6(6) 1_655 . ?
C15 K1 C47 144.4(7) 1_655 . ?
C20 K1 C47 126.2(6) 1_655 . ?
C23 K1 C47 117.7(7) 1_655 . ?
C21 K1 C47 106.1(6) 1_655 . ?
C44 K1 C47 49.1(6) . . ?
C46 K1 C22 111.7(7) . 1_655 ?
C45 K1 C22 137.5(7) . 1_655 ?
C16 K1 C22 51.1(7) 1_655 1_655 ?
C15 K1 C22 44.6(6) 1_655 1_655 ?
C20 K1 C22 42.4(7) 1_655 1_655 ?
C23 K1 C22 24.6(6) 1_655 1_655 ?
C21 K1 C22 22.9(6) 1_655 1_655 ?
C44 K1 C22 152.3(6) . 1_655 ?
C47 K1 C22 103.2(6) . 1_655 ?
C46 K1 W1 107.7(5) . 1_655 ?
C45 K1 W1 95.3(5) . 1_655 ?
C16 K1 W1 69.8(4) 1_655 1_655 ?
C15 K1 W1 54.2(4) 1_655 1_655 ?
C20 K1 W1 95.5(4) 1_655 1_655 ?
C23 K1 W1 68.8(4) 1_655 1_655 ?
C21 K1 W1 105.7(4) 1_655 1_655 ?
C44 K1 W1 106.1(4) . 1_655 ?
C47 K1 W1 132.7(5) . 1_655 ?
C22 K1 W1 93.2(4) 1_655 1_655 ?
O1 K2 O2 84.1(7) . . ?
O1 K2 C37 69.4(8) . . ?
O2 K2 C37 123.3(9) . . ?
O1 K2 C25 73.2(8) . . ?
O2 K2 C25 113.5(9) . . ?
C37 K2 C25 105.6(8) . . ?
O1 K2 C51 93.5(9) . . ?
O2 K2 C51 41.1(10) . . ?
C37 K2 C51 159.8(10) . . ?
C25 K2 C51 78.3(9) . . ?
O1 K2 C36 94.1(7) . . ?
O2 K2 C36 120.3(9) . . ?
C37 K2 C36 26.2(7) . . ?
C25 K2 C36 123.0(8) . . ?
C51 K2 C36 158.8(9) . . ?
O1 K2 W1 141.5(5) . . ?
O2 K2 W1 134.3(6) . . ?
C37 K2 W1 86.5(6) . . ?
C25 K2 W1 85.7(6) . . ?
C51 K2 W1 113.7(8) . . ?
C36 K2 W1 70.5(5) . . ?
C1 N1 C3 112.9(17) . . ?
C1 N1 W2 121.8(14) . . ?
C3 N1 W2 124.1(13) . . ?
N2 C1 N1 118.0(19) . . ?
N2 C1 H1 121.0 . . ?
N1 C1 H1 121.0 . . ?
C1 N2 C15 113.5(18) . . ?
C1 N2 W1 121.9(14) . . ?
C15 N2 W1 124.6(14) . . ?
C2 N3 C27 110.3(17) . . ?
C2 N3 W1 120.3(14) . . ?
C27 N3 W1 129.4(13) . . ?
N4 C2 N3 121(2) . . ?
N4 C2 H2 119.4 . . ?
N3 C2 H2 119.4 . . ?
C2 N4 C39 116.6(19) . . ?
C2 N4 W2 119.4(14) . . ?
C39 N4 W2 123.5(14) . . ?
C4 C3 C11 126(2) . . ?
C4 C3 N1 114(2) . . ?
C11 C3 N1 120(2) . . ?
C3 C4 C8 114(2) . . ?
C3 C4 C5 123(2) . . ?
C8 C4 C5 123(2) . . ?
C6 C5 C7 114(2) . . ?
C6 C5 C4 113(2) . . ?
C7 C5 C4 108(2) . . ?
C6 C5 H5 107.1 . . ?
C7 C5 H5 107.1 . . ?
C4 C5 H5 107.1 . . ?
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 121(3) . . ?
C9 C8 H8 119.7 . . ?
C4 C8 H8 119.7 . . ?
C10 C9 C8 124(3) . . ?
C10 C9 H9 118.0 . . ?
C8 C9 H9 118.0 . . ?
C9 C10 C11 119(3) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
C3 C11 C10 116(3) . . ?
C3 C11 C12 125(2) . . ?
C10 C11 C12 119(2) . . ?
C11 C12 C14 110(2) . . ?
C11 C12 C13 112(3) . . ?
C14 C12 C13 113(3) . . ?
C11 C12 H12 107.2 . . ?
C14 C12 H12 107.2 . . ?
C13 C12 H12 107.2 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 N2 121(2) . . ?
C16 C15 C23 120(2) . . ?
N2 C15 C23 119(2) . . ?
C16 C15 K1 76.1(13) . 1_455 ?
N2 C15 K1 107.2(13) . 1_455 ?
C23 C15 K1 84.0(12) . 1_455 ?
C15 C16 C20 121(2) . . ?
C15 C16 C17 121(2) . . ?
C20 C16 C17 118(2) . . ?
C15 C16 K1 78.1(13) . 1_455 ?
C20 C16 K1 82.1(13) . 1_455 ?
C17 C16 K1 111.4(15) . 1_455 ?
C19 C17 C18 114(3) . . ?
C19 C17 C16 111(2) . . ?
C18 C17 C16 114(2) . . ?
C19 C17 H17 105.9 . . ?
C18 C17 H17 105.9 . . ?
C16 C17 H17 105.9 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C16 119(3) . . ?
C21 C20 K1 81.5(15) . 1_455 ?
C16 C20 K1 71.9(13) . 1_455 ?
C21 C20 H20 120.5 . . ?
C16 C20 H20 120.5 . . ?
K1 C20 H20 116.9 1_455 . ?
C22 C21 C20 122(2) . . ?
C22 C21 K1 81.3(16) . 1_455 ?
C20 C21 K1 73.7(14) . 1_455 ?
C22 C21 H21 119.1 . . ?
C20 C21 H21 119.1 . . ?
K1 C21 H21 116.4 1_455 . ?
C21 C22 C23 123(3) . . ?
C21 C22 K1 75.8(16) . 1_455 ?
C23 C22 K1 75.0(14) . 1_455 ?
C21 C22 H22 118.5 . . ?
C23 C22 H22 118.5 . . ?
K1 C22 H22 121.9 1_455 . ?
C22 C23 C15 116(2) . . ?
C22 C23 C24 124(2) . . ?
C15 C23 C24 121(2) . . ?
C22 C23 K1 80.4(14) . 1_455 ?
C15 C23 K1 69.3(12) . 1_455 ?
C24 C23 K1 121.4(16) . 1_455 ?
C23 C24 C26 111(2) . . ?
C23 C24 C25 112(2) . . ?
C26 C24 C25 108(2) . . ?
C23 C24 H24 108.3 . . ?
C26 C24 H24 108.3 . . ?
C25 C24 H24 108.3 . . ?
C24 C25 K2 88.0(16) . . ?
C24 C25 H25A 109.5 . . ?
K2 C25 H25A 62.4 . . ?
C24 C25 H25B 109.5 . . ?
K2 C25 H25B 62.8 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
K2 C25 H25C 162.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C35 C27 C28 122(2) . . ?
C35 C27 N3 124(3) . . ?
C28 C27 N3 114(2) . . ?
C27 C28 C32 112(3) . . ?
C27 C28 C29 128(2) . . ?
C32 C28 C29 120(3) . . ?
C31 C29 C28 110(3) . . ?
C31 C29 C30 112(3) . . ?
C28 C29 C30 113(3) . . ?
C31 C29 H29 106.9 . . ?
C28 C29 H29 106.9 . . ?
C30 C29 H29 106.9 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 C28 122(3) . . ?
C33 C32 H32 119.2 . . ?
C28 C32 H32 119.2 . . ?
C34 C33 C32 124(4) . . ?
C34 C33 H33 118.0 . . ?
C32 C33 H33 118.0 . . ?
C33 C34 C35 119(3) . . ?
C33 C34 H34 120.7 . . ?
C35 C34 H34 120.7 . . ?
C27 C35 C34 122(3) . . ?
C27 C35 C36 121(3) . . ?
C34 C35 C36 117(3) . . ?
C35 C36 C37 114(3) . . ?
C35 C36 C38 118(3) . . ?
C37 C36 C38 109(3) . . ?
C35 C36 K2 130.9(19) . . ?
C37 C36 K2 69.3(17) . . ?
C38 C36 K2 105(2) . . ?
C35 C36 H36 105.0 . . ?
C37 C36 H36 105.0 . . ?
C38 C36 H36 105.0 . . ?
K2 C36 H36 37.7 . . ?
C36 C37 K2 84.5(17) . . ?
C36 C37 H37A 109.5 . . ?
K2 C37 H37A 58.0 . . ?
C36 C37 H37B 109.5 . . ?
K2 C37 H37B 164.6 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
K2 C37 H37C 70.2 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C47 C39 N4 119(2) . . ?
C47 C39 C40 118(2) . . ?
N4 C39 C40 123(2) . . ?
C44 C40 C39 117(2) . . ?
C44 C40 C41 122(2) . . ?
C39 C40 C41 121(2) . . ?
C40 C41 C42 109(2) . . ?
C40 C41 C43 111(2) . . ?
C42 C41 C43 111(2) . . ?
C40 C41 H41 108.8 . . ?
C42 C41 H41 108.8 . . ?
C43 C41 H41 108.8 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C45 C44 C40 124(3) . . ?
C45 C44 K1 66.6(14) . . ?
C40 C44 K1 90.8(15) . . ?
C45 C44 H44 118.2 . . ?
C40 C44 H44 118.2 . . ?
K1 C44 H44 113.9 . . ?
C44 C45 C46 120(2) . . ?
C44 C45 K1 89.6(16) . . ?
C46 C45 K1 75.8(14) . . ?
C44 C45 H45 119.8 . . ?
C46 C45 H45 119.8 . . ?
K1 C45 H45 104.7 . . ?
C47 C46 C45 118(3) . . ?
C47 C46 K1 89.6(15) . . ?
C45 C46 K1 77.3(14) . . ?
C47 C46 H46 120.8 . . ?
C45 C46 H46 120.8 . . ?
K1 C46 H46 102.8 . . ?
C39 C47 C46 122(2) . . ?
C39 C47 C48 120(2) . . ?
C46 C47 C48 118(2) . . ?
C39 C47 K1 94.2(15) . . ?
C46 C47 K1 65.3(13) . . ?
C48 C47 K1 112.5(15) . . ?
C47 C48 C49 117(2) . . ?
C47 C48 C50 111(2) . . ?
C49 C48 C50 111(2) . . ?
C47 C48 H48 105.8 . . ?
C49 C48 H48 105.8 . . ?
C50 C48 H48 105.8 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C48 C50 W2 116.1(17) . . ?
C48 C50 H50A 109.5 . . ?
W2 C50 H50A 107.7 . . ?
C48 C50 H50B 109.5 . . ?
W2 C50 H50B 7.0 . . ?
H50A C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
W2 C50 H50C 104.4 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C52 C51 K2 96(3) . . ?
C52 C51 H51A 109.5 . . ?
K2 C51 H51A 154.9 . . ?
C52 C51 H51B 109.5 . . ?
K2 C51 H51B 60.7 . . ?
H51A C51 H51B 109.5 . . ?
C52 C51 H51C 109.5 . . ?
K2 C51 H51C 59.1 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
O2 C52 C51 96(3) . . ?
O2 C52 H52A 112.6 . . ?
C51 C52 H52A 112.6 . . ?
O2 C52 H52B 112.6 . . ?
C51 C52 H52B 112.6 . . ?
H52A C52 H52B 110.1 . . ?
C52 O2 C53 102(3) . . ?
C52 O2 K2 128(3) . . ?
C53 O2 K2 130(3) . . ?
C54 C53 O2 111(4) . . ?
C54 C53 H53A 109.5 . . ?
O2 C53 H53A 109.5 . . ?
C54 C53 H53B 109.5 . . ?
O2 C53 H53B 109.5 . . ?
H53A C53 H53B 108.1 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C103 O1 C100 114(3) . . ?
C103 O1 K2 128.5(19) . . ?
C100 O1 K2 118(2) . . ?
O1 C100 C101 102(3) . . ?
O1 C100 H10A 111.4 . . ?
C101 C100 H10A 111.4 . . ?
O1 C100 H10B 111.4 . . ?
C101 C100 H10B 111.4 . . ?
H10A C100 H10B 109.2 . . ?
C100 C101 C102 103(2) . . ?
C100 C101 H10C 111.1 . . ?
C102 C101 H10C 111.1 . . ?
C100 C101 H10D 111.1 . . ?
C102 C101 H10D 111.1 . . ?
H10C C101 H10D 109.0 . . ?
C103 C102 C101 104(2) . . ?
C103 C102 H10E 110.9 . . ?
C101 C102 H10E 110.9 . . ?
C103 C102 H10F 110.9 . . ?
C101 C102 H10F 110.9 . . ?
H10E C102 H10F 108.9 . . ?
O1 C103 C102 103(3) . . ?
O1 C103 H10G 111.1 . . ?
C102 C103 H10G 111.1 . . ?
O1 C103 H10H 111.1 . . ?
C102 C103 H10H 111.1 . . ?
H10G C103 H10H 109.1 . . ?

_refine_diff_density_max         2.715
_refine_diff_density_min         -2.428
_refine_diff_density_rms         0.282

