# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_t268mcsqma
_database_code_depnum_ccdc_archive 'CCDC 1960676'
loop_
_audit_author_name
_audit_author_address
'Awal Noor'
;University of Bayreuth
Germany
;
_audit_update_record             
;
2019-10-22 deposited with the CCDC.	2020-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H86 Cl4 N4 W2'
_chemical_formula_weight         1420.87

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'
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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

loop_
_symmetry_equiv_pos_as_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                   25.9780(9)
_cell_length_b                   26.9280(9)
_cell_length_c                   11.7290(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.866(4)
_cell_angle_gamma                90.00
_cell_volume                     7851.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    11835
_cell_measurement_2theta_min     2.23
_cell_measurement_2theta_max     49.37

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2856
_exptl_absorpt_coefficient_mu    3.096
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5944
_exptl_absorpt_correction_T_max  0.8082
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  STOE-IPDSII
_diffrn_measurement_method       Omega-Scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24750
_diffrn_reflns_av_R_equivalents  0.1379
_diffrn_reflns_av_sigmaI/netI    0.2108
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.11
_diffrn_reflns_theta_max         24.61
_reflns_number_total             6605
_reflns_number_gt                3021
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       X-AREA-STOE
_computing_cell_refinement       X-AREA-STOE
_computing_data_reduction        X-AREA-STOE
_computing_structure_solution    SIR-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.,SQUEEZE
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0411P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6605
_refine_ls_number_parameters     344
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1262
_refine_ls_R_factor_gt           0.0521
_refine_ls_wR_factor_ref         0.1184
_refine_ls_wR_factor_gt          0.1030
_refine_ls_goodness_of_fit_ref   0.706
_refine_ls_restrained_S_all      0.706
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.77386(2) 0.28500(2) 0.53318(5) 0.04051(15) Uani 1 1 d . . .
Cl1 Cl 0.70610(14) 0.34371(11) 0.4789(3) 0.0547(9) Uani 1 1 d . . .
Cl2 Cl 0.86180(13) 0.26079(11) 0.5711(3) 0.0550(8) Uani 1 1 d . . .
N1 N 0.7721(4) 0.2722(3) 0.6970(9) 0.043(3) Uani 1 1 d . . .
N2 N 0.7835(3) 0.2986(3) 0.3507(8) 0.036(2) Uani 1 1 d . . .
C1 C 0.8121(5) 0.2966(4) 0.7991(10) 0.036(3) Uani 1 1 d . . .
C2 C 0.8025(5) 0.3453(4) 0.8291(10) 0.038(3) Uani 1 1 d . . .
C3 C 0.8445(5) 0.3677(4) 0.9172(10) 0.042(3) Uani 1 1 d . . .
H3 H 0.8402 0.4011 0.9385 0.050 Uiso 1 1 calc R . .
C4 C 0.8902(5) 0.3443(5) 0.9726(10) 0.044(3) Uani 1 1 d . . .
H4 H 0.9181 0.3613 1.0298 0.053 Uiso 1 1 calc R . .
C5 C 0.8966(5) 0.2949(5) 0.9457(10) 0.045(3) Uani 1 1 d . . .
H5 H 0.9286 0.2780 0.9876 0.054 Uiso 1 1 calc R . .
C6 C 0.8577(5) 0.2698(4) 0.8595(10) 0.040(3) Uani 1 1 d . . .
C7 C 0.8657(5) 0.2155(5) 0.8353(10) 0.048(3) Uani 1 1 d . . .
H7 H 0.8405 0.2069 0.7556 0.058 Uiso 1 1 calc R . .
C8 C 0.9226(5) 0.2029(5) 0.8334(11) 0.064(4) Uani 1 1 d . . .
H8A H 0.9340 0.2264 0.7818 0.097 Uiso 1 1 calc R . .
H8B H 0.9233 0.1691 0.8028 0.097 Uiso 1 1 calc R . .
H8C H 0.9471 0.2050 0.9144 0.097 Uiso 1 1 calc R . .
C9 C 0.8517(6) 0.1822(5) 0.9296(12) 0.058(4) Uani 1 1 d . . .
H9A H 0.8756 0.1904 1.0087 0.087 Uiso 1 1 calc R . .
H9B H 0.8565 0.1472 0.9117 0.087 Uiso 1 1 calc R . .
H9C H 0.8143 0.1879 0.9281 0.087 Uiso 1 1 calc R . .
C10 C 0.7512(5) 0.3737(4) 0.7751(11) 0.046(3) Uani 1 1 d . . .
H10 H 0.7264 0.3518 0.7147 0.055 Uiso 1 1 calc R . .
C11 C 0.7227(6) 0.3885(5) 0.8653(12) 0.062(4) Uani 1 1 d . . .
H11A H 0.7167 0.3590 0.9086 0.093 Uiso 1 1 calc R . .
H11B H 0.6881 0.4038 0.8243 0.093 Uiso 1 1 calc R . .
H11C H 0.7449 0.4124 0.9217 0.093 Uiso 1 1 calc R . .
C12 C 0.7605(6) 0.4205(4) 0.7122(11) 0.056(4) Uani 1 1 d . . .
H12A H 0.7779 0.4456 0.7714 0.084 Uiso 1 1 calc R . .
H12B H 0.7259 0.4333 0.6625 0.084 Uiso 1 1 calc R . .
H12C H 0.7837 0.4129 0.6619 0.084 Uiso 1 1 calc R . .
C13 C 0.7627(5) 0.2617(4) 0.2721(10) 0.039(3) Uani 1 1 d . . .
C14 C 0.7750(5) 0.2569(4) 0.1628(10) 0.037(3) Uani 1 1 d . . .
H14 H 0.7612 0.2301 0.1102 0.045 Uiso 1 1 calc R . .
C15 C 0.8075(4) 0.2919(4) 0.1352(9) 0.043(3) Uani 1 1 d . . .
H15 H 0.8171 0.2891 0.0632 0.051 Uiso 1 1 calc R . .
C16 C 0.8266(4) 0.3317(4) 0.2109(10) 0.042(3) Uani 1 1 d . . .
H16 H 0.8482 0.3566 0.1904 0.050 Uiso 1 1 calc R . .
C17 C 0.8134(4) 0.3342(4) 0.3169(9) 0.033(3) Uani 1 1 d . . .
C18 C 0.8315(4) 0.3784(4) 0.3960(9) 0.032(3) Uani 1 1 d . . .
C19 C 0.7975(5) 0.4190(4) 0.3907(10) 0.034(3) Uani 1 1 d . . .
C20 C 0.8173(4) 0.4597(3) 0.4640(9) 0.030(3) Uani 1 1 d . . .
H20 H 0.7942 0.4873 0.4614 0.037 Uiso 1 1 calc R . .
C21 C 0.8691(5) 0.4616(3) 0.5405(9) 0.035(3) Uani 1 1 d . . .
C22 C 0.9030(5) 0.4222(4) 0.5392(9) 0.035(3) Uani 1 1 d . . .
H22 H 0.9392 0.4236 0.5884 0.042 Uiso 1 1 calc R . .
C23 C 0.8858(4) 0.3800(4) 0.4673(9) 0.035(3) Uani 1 1 d . . .
C24 C 0.9276(4) 0.3417(4) 0.4636(10) 0.036(3) Uani 1 1 d . . .
H24 H 0.9083 0.3103 0.4310 0.043 Uiso 1 1 calc R . .
C25 C 0.9588(5) 0.3582(4) 0.3798(11) 0.053(3) Uani 1 1 d . . .
H25A H 0.9341 0.3625 0.2995 0.079 Uiso 1 1 calc R . .
H25B H 0.9858 0.3330 0.3779 0.079 Uiso 1 1 calc R . .
H25C H 0.9768 0.3898 0.4075 0.079 Uiso 1 1 calc R . .
C26 C 0.9670(4) 0.3297(4) 0.5871(10) 0.045(3) Uani 1 1 d . . .
H26A H 0.9895 0.3588 0.6171 0.068 Uiso 1 1 calc R . .
H26B H 0.9900 0.3017 0.5798 0.068 Uiso 1 1 calc R . .
H26C H 0.9466 0.3210 0.6426 0.068 Uiso 1 1 calc R . .
C27 C 0.8881(4) 0.5062(4) 0.6218(9) 0.035(3) Uani 1 1 d . . .
H27 H 0.8583 0.5311 0.6036 0.042 Uiso 1 1 calc R . .
C28 C 0.9362(4) 0.5303(3) 0.5993(9) 0.033(3) Uani 1 1 d . . .
H28A H 0.9671 0.5078 0.6240 0.049 Uiso 1 1 calc R . .
H28B H 0.9444 0.5612 0.6450 0.049 Uiso 1 1 calc R . .
H28C H 0.9285 0.5376 0.5142 0.049 Uiso 1 1 calc R . .
C29 C 0.9001(5) 0.4914(5) 0.7539(10) 0.058(4) Uani 1 1 d . . .
H29A H 0.9273 0.4651 0.7725 0.088 Uiso 1 1 calc R . .
H29B H 0.8671 0.4794 0.7688 0.088 Uiso 1 1 calc R . .
H29C H 0.9136 0.5204 0.8043 0.088 Uiso 1 1 calc R . .
C30 C 0.7430(5) 0.4214(4) 0.2975(10) 0.042(3) Uani 1 1 d . . .
H30 H 0.7288 0.3867 0.2853 0.050 Uiso 1 1 calc R . .
C31 C 0.7014(5) 0.4522(4) 0.3329(12) 0.050(3) Uani 1 1 d . . .
H31A H 0.7120 0.4873 0.3375 0.075 Uiso 1 1 calc R . .
H31B H 0.6990 0.4412 0.4108 0.075 Uiso 1 1 calc R . .
H31C H 0.6664 0.4482 0.2733 0.075 Uiso 1 1 calc R . .
C32 C 0.7492(5) 0.4389(4) 0.1792(10) 0.045(3) Uani 1 1 d . . .
H32A H 0.7136 0.4417 0.1209 0.068 Uiso 1 1 calc R . .
H32B H 0.7709 0.4149 0.1506 0.068 Uiso 1 1 calc R . .
H32C H 0.7670 0.4713 0.1897 0.068 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 1.965(9) . ?
W1 N2 2.255(9) . ?
W1 W1 2.2660(11) 7_656 ?
W1 Cl2 2.292(3) . ?
W1 Cl1 2.314(3) . ?
N1 C13 1.404(13) 7_656 ?
N1 C1 1.491(14) . ?
N2 C13 1.356(13) . ?
N2 C17 1.365(13) . ?
C1 C6 1.391(15) . ?
C1 C2 1.401(15) . ?
C2 C3 1.401(16) . ?
C2 C10 1.509(16) . ?
C3 C4 1.336(16) . ?
C4 C5 1.387(16) . ?
C5 C6 1.383(15) . ?
C6 C7 1.516(17) . ?
C7 C8 1.523(16) . ?
C7 C9 1.545(17) . ?
C10 C11 1.510(17) . ?
C10 C12 1.514(16) . ?
C13 N1 1.404(13) 7_656 ?
C13 C14 1.414(15) . ?
C14 C15 1.365(14) . ?
C15 C16 1.387(15) . ?
C16 C17 1.383(14) . ?
C17 C18 1.499(14) . ?
C18 C19 1.396(14) . ?
C18 C23 1.415(15) . ?
C19 C20 1.394(14) . ?
C19 C30 1.519(15) . ?
C20 C21 1.386(15) . ?
C21 C22 1.381(14) . ?
C21 C27 1.524(13) . ?
C22 C23 1.409(14) . ?
C23 C24 1.508(14) . ?
C24 C25 1.512(15) . ?
C24 C26 1.546(15) . ?
C27 C28 1.496(14) . ?
C27 C29 1.541(15) . ?
C30 C31 1.512(16) . ?
C30 C32 1.518(16) . ?

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 175.1(4) . . ?
N1 W1 W1 91.4(2) . 7_656 ?
N2 W1 W1 90.5(2) . 7_656 ?
N1 W1 Cl2 93.7(3) . . ?
N2 W1 Cl2 81.5(2) . . ?
W1 W1 Cl2 104.20(9) 7_656 . ?
N1 W1 Cl1 99.1(3) . . ?
N2 W1 Cl1 85.0(2) . . ?
W1 W1 Cl1 100.21(9) 7_656 . ?
Cl2 W1 Cl1 152.09(11) . . ?
C13 N1 C1 115.4(9) 7_656 . ?
C13 N1 W1 124.5(7) 7_656 . ?
C1 N1 W1 120.0(7) . . ?
C13 N2 C17 117.7(9) . . ?
C13 N2 W1 113.3(7) . . ?
C17 N2 W1 128.3(7) . . ?
C6 C1 C2 123.0(11) . . ?
C6 C1 N1 118.2(9) . . ?
C2 C1 N1 118.8(11) . . ?
C1 C2 C3 115.6(11) . . ?
C1 C2 C10 124.7(11) . . ?
C3 C2 C10 119.7(10) . . ?
C4 C3 C2 123.2(11) . . ?
C3 C4 C5 119.4(11) . . ?
C6 C5 C4 121.6(12) . . ?
C5 C6 C1 117.0(10) . . ?
C5 C6 C7 119.8(11) . . ?
C1 C6 C7 123.2(10) . . ?
C6 C7 C8 113.8(11) . . ?
C6 C7 C9 110.6(10) . . ?
C8 C7 C9 108.1(11) . . ?
C2 C10 C11 113.1(10) . . ?
C2 C10 C12 112.3(10) . . ?
C11 C10 C12 107.6(11) . . ?
N2 C13 N1 117.3(10) . 7_656 ?
N2 C13 C14 122.2(10) . . ?
N1 C13 C14 120.5(10) 7_656 . ?
C15 C14 C13 118.0(10) . . ?
C14 C15 C16 120.8(10) . . ?
C17 C16 C15 118.5(11) . . ?
N2 C17 C16 122.5(10) . . ?
N2 C17 C18 118.8(9) . . ?
C16 C17 C18 118.7(10) . . ?
C19 C18 C23 120.8(10) . . ?
C19 C18 C17 121.0(10) . . ?
C23 C18 C17 118.0(9) . . ?
C20 C19 C18 118.2(10) . . ?
C20 C19 C30 120.7(10) . . ?
C18 C19 C30 120.7(10) . . ?
C21 C20 C19 122.8(10) . . ?
C22 C21 C20 117.9(9) . . ?
C22 C21 C27 121.4(10) . . ?
C20 C21 C27 120.7(9) . . ?
C21 C22 C23 122.2(10) . . ?
C22 C23 C18 117.9(10) . . ?
C22 C23 C24 117.5(10) . . ?
C18 C23 C24 124.4(9) . . ?
C23 C24 C25 110.2(9) . . ?
C23 C24 C26 113.8(9) . . ?
C25 C24 C26 109.6(9) . . ?
C28 C27 C21 111.5(9) . . ?
C28 C27 C29 110.7(9) . . ?
C21 C27 C29 111.1(9) . . ?
C31 C30 C32 110.7(9) . . ?
C31 C30 C19 114.6(10) . . ?
C32 C30 C19 110.3(10) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        24.61
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.308
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.163

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.018 1102 491 ' '
2 0.500 0.500 -0.017 1102 491 ' '
_platon_squeeze_details          
;
;

_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_t471apapabsorption
_database_code_depnum_ccdc_archive 'CCDC 1960677'
loop_
_audit_author_name
_audit_author_address
'Awal Noor'
;University of Bayreuth
Germany
;
_audit_update_record             
;
2019-10-22 deposited with the CCDC.	2020-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C88 H110 K2 N4 W2'
_chemical_formula_weight         1669.70

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   14.9690(5)
_cell_length_b                   11.8000(4)
_cell_length_c                   23.3070(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.463(3)
_cell_angle_gamma                90.00
_cell_volume                     4113.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    35501
_cell_measurement_2theta_min     3.17
_cell_measurement_t2heta_max     56.02

_exptl_crystal_description       Block
_exptl_crystal_colour            Purple?
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1704
_exptl_absorpt_coefficient_mu    2.940
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.3882
_exptl_absorpt_correction_T_max  0.7348
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  STOE-IPDS-II
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            65003
_diffrn_reflns_av_R_equivalents  0.0841
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.59
_diffrn_reflns_theta_max         27.85
_reflns_number_total             9638
_reflns_number_gt                7417
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       STOE-XAREA
_computing_cell_refinement       STOE-XAREA
_computing_data_reduction        STOE-XAREA
_computing_structure_solution    Sir-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0834P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    Constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9638
_refine_ls_number_parameters     431
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_ref         0.1299
_refine_ls_wR_factor_gt          0.1218
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.068613(14) -0.011687(14) 0.518456(9) 0.03773(8) Uani 1 1 d . . .
K1 K -0.09070(14) -0.1155(2) 0.61481(10) 0.0947(6) Uani 1 1 d . . .
N1 N -0.0927(3) -0.1665(3) 0.48317(18) 0.0332(9) Uani 1 1 d . . .
C1 C -0.0250(4) -0.2376(4) 0.5037(2) 0.0362(11) Uani 1 1 d . . .
C2 C -0.0430(4) -0.3553(4) 0.5111(3) 0.0434(12) Uani 1 1 d . . .
H2 H 0.0031 -0.4036 0.5263 0.052 Uiso 1 1 calc R . .
C3 C -0.1240(4) -0.3990(4) 0.4971(3) 0.0474(13) Uani 1 1 d . . .
H3 H -0.1361 -0.4769 0.5037 0.057 Uiso 1 1 calc R . .
C4 C -0.1915(4) -0.3270(4) 0.4724(3) 0.0435(12) Uani 1 1 d . . .
H4 H -0.2487 -0.3563 0.4612 0.052 Uiso 1 1 calc R . .
C5 C -0.1724(4) -0.2154(4) 0.4650(2) 0.0382(11) Uani 1 1 d . . .
C6 C -0.2355(3) -0.1428(4) 0.4292(2) 0.0372(10) Uani 1 1 d . . .
C7 C -0.3075(4) -0.0865(4) 0.4519(2) 0.0402(11) Uani 1 1 d . . .
C8 C -0.3661(4) -0.0268(5) 0.4147(2) 0.0467(13) Uani 1 1 d . . .
H8 H -0.4140 0.0142 0.4302 0.056 Uiso 1 1 calc R . .
C9 C -0.3563(4) -0.0254(5) 0.3558(3) 0.0472(13) Uani 1 1 d . . .
C10 C -0.2833(4) -0.0819(5) 0.3346(3) 0.0479(13) Uani 1 1 d . . .
H10 H -0.2748 -0.0804 0.2944 0.058 Uiso 1 1 calc R . .
C11 C -0.2229(4) -0.1400(4) 0.3698(2) 0.0421(11) Uani 1 1 d . . .
C12 C -0.1439(4) -0.2019(5) 0.3443(3) 0.0507(14) Uani 1 1 d . . .
H12 H -0.0965 -0.2115 0.3754 0.061 Uiso 1 1 calc R . .
N2 N 0.0530(3) -0.1876(3) 0.51793(19) 0.0352(9) Uani 1 1 d . . .
C13 C -0.1036(5) -0.1369(7) 0.2956(3) 0.070(2) Uani 1 1 d . . .
H13A H -0.0500 -0.1763 0.2834 0.105 Uiso 1 1 calc R . .
H13B H -0.0875 -0.0604 0.3087 0.105 Uiso 1 1 calc R . .
H13C H -0.1473 -0.1320 0.2632 0.105 Uiso 1 1 calc R . .
C14 C -0.1725(5) -0.3196(6) 0.3237(3) 0.0639(18) Uani 1 1 d . . .
H14A H -0.2226 -0.3128 0.2955 0.096 Uiso 1 1 calc R . .
H14B H -0.1910 -0.3646 0.3565 0.096 Uiso 1 1 calc R . .
H14C H -0.1222 -0.3570 0.3059 0.096 Uiso 1 1 calc R . .
C15 C -0.4222(5) 0.0359(6) 0.3155(3) 0.0585(16) Uani 1 1 d . . .
H15 H -0.3937 0.0437 0.2776 0.070 Uiso 1 1 calc R . .
C16 C -0.5062(6) -0.0340(8) 0.3058(4) 0.078(2) Uani 1 1 d . . .
H16A H -0.4900 -0.1122 0.2966 0.117 Uiso 1 1 calc R . .
H16B H -0.5425 -0.0018 0.2738 0.117 Uiso 1 1 calc R . .
H16C H -0.5405 -0.0332 0.3407 0.117 Uiso 1 1 calc R . .
C17 C -0.4448(5) 0.1538(6) 0.3358(3) 0.070(2) Uani 1 1 d . . .
H17A H -0.4782 0.1486 0.3710 0.105 Uiso 1 1 calc R . .
H17B H -0.4813 0.1927 0.3060 0.105 Uiso 1 1 calc R . .
H17C H -0.3894 0.1965 0.3437 0.105 Uiso 1 1 calc R . .
C18 C -0.3243(4) -0.0915(5) 0.5157(2) 0.0465(13) Uani 1 1 d . . .
H18 H -0.2664 -0.1117 0.5361 0.056 Uiso 1 1 calc R . .
C19 C -0.3543(5) 0.0212(5) 0.5396(3) 0.0532(14) Uani 1 1 d . . .
H19A H -0.3115 0.0804 0.5301 0.080 Uiso 1 1 calc R . .
H19B H -0.3574 0.0156 0.5814 0.080 Uiso 1 1 calc R . .
H19C H -0.4135 0.0405 0.5228 0.080 Uiso 1 1 calc R . .
C20 C -0.3910(5) -0.1838(6) 0.5284(3) 0.0617(17) Uani 1 1 d . . .
H20A H -0.4485 -0.1667 0.5087 0.092 Uiso 1 1 calc R . .
H20B H -0.3987 -0.1876 0.5699 0.092 Uiso 1 1 calc R . .
H20C H -0.3687 -0.2568 0.5149 0.092 Uiso 1 1 calc R . .
C21 C 0.1318(3) -0.2576(4) 0.5220(2) 0.0368(10) Uani 1 1 d . . .
C22 C 0.1687(4) -0.2905(4) 0.5754(2) 0.0411(11) Uani 1 1 d . . .
C23 C 0.2489(4) -0.3501(4) 0.5776(3) 0.0471(13) Uani 1 1 d . . .
H23 H 0.2750 -0.3719 0.6138 0.057 Uiso 1 1 calc R . .
C24 C 0.2911(4) -0.3778(5) 0.5284(3) 0.0513(14) Uani 1 1 d . . .
H24 H 0.3466 -0.4169 0.5307 0.062 Uiso 1 1 calc R . .
C25 C 0.2523(4) -0.3486(5) 0.4753(3) 0.0513(14) Uani 1 1 d . . .
H25 H 0.2812 -0.3691 0.4413 0.062 Uiso 1 1 calc R . .
C26 C 0.1715(4) -0.2898(4) 0.4710(2) 0.0428(12) Uani 1 1 d . . .
C27 C 0.1288(4) -0.2651(5) 0.4122(3) 0.0498(13) Uani 1 1 d . . .
H27 H 0.0787 -0.2106 0.4175 0.060 Uiso 1 1 calc R . .
C28 C 0.1925(6) -0.2107(7) 0.3714(3) 0.0693(19) Uani 1 1 d . . .
H28A H 0.2146 -0.1389 0.3877 0.104 Uiso 1 1 calc R . .
H28B H 0.1611 -0.1964 0.3344 0.104 Uiso 1 1 calc R . .
H28C H 0.2431 -0.2617 0.3658 0.104 Uiso 1 1 calc R . .
C29 C 0.0881(5) -0.3737(5) 0.3850(3) 0.0619(17) Uani 1 1 d . . .
H29A H 0.1358 -0.4287 0.3788 0.093 Uiso 1 1 calc R . .
H29B H 0.0576 -0.3551 0.3482 0.093 Uiso 1 1 calc R . .
H29C H 0.0450 -0.4064 0.4109 0.093 Uiso 1 1 calc R . .
C30 C 0.1217(4) -0.2642(5) 0.6303(3) 0.0500(13) Uani 1 1 d . . .
H30 H 0.0676 -0.2175 0.6199 0.060 Uiso 1 1 calc R . .
C31 C 0.1796(7) -0.1975(9) 0.6731(4) 0.093(3) Uani 1 1 d . . .
H31A H 0.2286 -0.2456 0.6881 0.140 Uiso 1 1 calc R . .
H31B H 0.1434 -0.1727 0.7049 0.140 Uiso 1 1 calc R . .
H31C H 0.2042 -0.1311 0.6541 0.140 Uiso 1 1 calc R . .
C32 C 0.0903(8) -0.3738(8) 0.6583(4) 0.103(4) Uani 1 1 d . . .
H32A H 0.0554 -0.4187 0.6299 0.155 Uiso 1 1 calc R . .
H32B H 0.0529 -0.3553 0.6905 0.155 Uiso 1 1 calc R . .
H32C H 0.1424 -0.4176 0.6723 0.155 Uiso 1 1 calc R . .
C33 C -0.1219(10) -0.2045(17) 0.7440(7) 0.140(6) Uani 1 1 d . . .
H33 H -0.0668 -0.2193 0.7644 0.168 Uiso 1 1 calc R . .
C34 C -0.1618(11) -0.1013(18) 0.7489(6) 0.143(5) Uani 1 1 d . . .
H34 H -0.1365 -0.0452 0.7739 0.172 Uiso 1 1 calc R . .
C35 C -0.2388(8) -0.0800(14) 0.7172(5) 0.122(4) Uani 1 1 d . . .
H35 H -0.2661 -0.0074 0.7193 0.147 Uiso 1 1 calc R . .
C36 C -0.2762(6) -0.1592(11) 0.6835(4) 0.096(3) Uani 1 1 d . . .
H36 H -0.3293 -0.1420 0.6614 0.116 Uiso 1 1 calc R . .
C37 C -0.2390(9) -0.2667(11) 0.6800(7) 0.137(5) Uani 1 1 d . . .
H37 H -0.2669 -0.3249 0.6575 0.165 Uiso 1 1 calc R . .
C38 C -0.1598(11) -0.2845(15) 0.7109(9) 0.177(8) Uani 1 1 d . . .
H38 H -0.1313 -0.3562 0.7084 0.212 Uiso 1 1 calc R . .
C39 C 0.0477(5) 0.0112(7) 0.8393(3) 0.119(5) Uani 1 1 d G . .
H39 H 0.0698 0.0579 0.8099 0.143 Uiso 1 1 calc R . .
C40 C -0.0146(5) 0.0539(4) 0.8762(3) 0.100(3) Uani 1 1 d G . .
H40 H -0.0350 0.1298 0.8721 0.120 Uiso 1 1 calc R . .
C41 C -0.0469(4) -0.0144(5) 0.9193(3) 0.089(3) Uani 1 1 d G . .
H41 H -0.0895 0.0148 0.9445 0.107 Uiso 1 1 calc R . .
C42 C -0.0171(5) -0.1255(5) 0.9253(3) 0.094(3) Uani 1 1 d G . .
H42 H -0.0392 -0.1722 0.9547 0.113 Uiso 1 1 calc R . .
C43 C 0.0451(5) -0.1683(5) 0.8884(3) 0.096(3) Uani 1 1 d G . .
H43 H 0.0655 -0.2442 0.8925 0.115 Uiso 1 1 calc R . .
C44 C 0.0775(4) -0.0999(8) 0.8454(3) 0.125(5) Uani 1 1 d G . .
H44 H 0.1200 -0.1291 0.8201 0.150 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 N2 2.089(4) . ?
W1 N1 2.133(4) 3_556 ?
W1 W1 2.2099(4) 3_556 ?
W1 K1 3.478(2) 3_556 ?
W1 K1 3.563(2) . ?
K1 N1 3.125(5) . ?
K1 C1 3.158(6) . ?
K1 C38 3.203(15) . ?
K1 C33 3.243(13) . ?
K1 C37 3.273(13) . ?
K1 N2 3.297(5) . ?
K1 C36 3.305(10) . ?
K1 C34 3.349(14) . ?
K1 C35 3.354(11) . ?
K1 W1 3.478(2) 3_556 ?
N1 C5 1.377(7) . ?
N1 C1 1.384(6) . ?
N1 W1 2.133(4) 3_556 ?
C1 N2 1.338(7) . ?
C1 C2 1.426(6) . ?
C2 C3 1.346(8) . ?
C3 C4 1.424(8) . ?
C4 C5 1.359(7) . ?
C5 C6 1.502(7) . ?
C6 C7 1.390(7) . ?
C6 C11 1.404(7) . ?
C7 C8 1.397(7) . ?
C7 C18 1.519(8) . ?
C8 C9 1.386(8) . ?
C9 C10 1.389(8) . ?
C9 C15 1.517(9) . ?
C10 C11 1.378(8) . ?
C11 C12 1.532(8) . ?
C12 C13 1.516(9) . ?
C12 C14 1.524(9) . ?
N2 C21 1.440(6) . ?
C15 C17 1.513(10) . ?
C15 C16 1.513(12) . ?
C18 C19 1.517(8) . ?
C18 C20 1.515(9) . ?
C21 C22 1.396(7) . ?
C21 C26 1.404(8) . ?
C22 C23 1.390(7) . ?
C22 C30 1.519(8) . ?
C23 C24 1.371(9) . ?
C24 C25 1.388(9) . ?
C25 C26 1.395(8) . ?
C26 C27 1.514(8) . ?
C27 C28 1.517(9) . ?
C27 C29 1.543(8) . ?
C30 C31 1.514(10) . ?
C30 C32 1.531(10) . ?
C33 C38 1.33(2) . ?
C33 C34 1.36(2) . ?
C34 C35 1.365(19) . ?
C35 C36 1.329(16) . ?
C36 C37 1.389(16) . ?
C37 C38 1.376(19) . ?
C39 C40 1.3900 . ?
C39 C44 1.3900 . ?
C40 C41 1.3900 . ?
C41 C42 1.3900 . ?
C42 C43 1.3900 . ?
C43 C44 1.3900 . ?

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
N2 W1 N1 176.38(16) . 3_556 ?
N2 W1 W1 91.14(11) . 3_556 ?
N1 W1 W1 91.42(11) 3_556 3_556 ?
N2 W1 K1 116.01(13) . 3_556 ?
N1 W1 K1 62.37(12) 3_556 3_556 ?
W1 W1 K1 73.80(4) 3_556 3_556 ?
N2 W1 K1 65.44(13) . . ?
N1 W1 K1 117.91(12) 3_556 . ?
W1 W1 K1 69.64(4) 3_556 . ?
K1 W1 K1 143.44(2) 3_556 . ?
N1 K1 C1 25.45(11) . . ?
N1 K1 C38 125.2(4) . . ?
C1 K1 C38 114.2(4) . . ?
N1 K1 C33 148.7(4) . . ?
C1 K1 C33 132.6(4) . . ?
C38 K1 C33 23.8(4) . . ?
N1 K1 C37 111.9(3) . . ?
C1 K1 C37 111.9(3) . . ?
C38 K1 C37 24.5(3) . . ?
C33 K1 C37 42.6(4) . . ?
N1 K1 N2 42.00(11) . . ?
C1 K1 N2 23.80(12) . . ?
C38 K1 N2 123.9(4) . . ?
C33 K1 N2 132.6(4) . . ?
C37 K1 N2 130.8(3) . . ?
N1 K1 C36 118.2(2) . . ?
C1 K1 C36 128.6(3) . . ?
C38 K1 C36 42.3(3) . . ?
C33 K1 C36 48.8(3) . . ?
C37 K1 C36 24.4(3) . . ?
N2 K1 C36 151.4(3) . . ?
N1 K1 C34 159.4(3) . . ?
C1 K1 C34 155.7(4) . . ?
C38 K1 C34 41.7(5) . . ?
C33 K1 C34 23.8(4) . . ?
C37 K1 C34 49.0(4) . . ?
N2 K1 C34 153.5(3) . . ?
C36 K1 C34 41.2(3) . . ?
N1 K1 C35 138.1(3) . . ?
C1 K1 C35 151.6(3) . . ?
C38 K1 C35 48.5(5) . . ?
C33 K1 C35 41.7(4) . . ?
C37 K1 C35 41.8(4) . . ?
N2 K1 C35 172.2(3) . . ?
C36 K1 C35 23.0(3) . . ?
C34 K1 C35 23.5(3) . . ?
N1 K1 W1 37.21(7) . 3_556 ?
C1 K1 W1 54.51(9) . 3_556 ?
C38 K1 W1 159.9(4) . 3_556 ?
C33 K1 W1 172.9(4) . 3_556 ?
C37 K1 W1 137.9(2) . 3_556 ?
N2 K1 W1 53.83(7) . 3_556 ?
C36 K1 W1 127.88(19) . 3_556 ?
C34 K1 W1 149.1(4) . 3_556 ?
C35 K1 W1 132.3(3) . 3_556 ?
N1 K1 W1 54.94(8) . . ?
C1 K1 W1 53.08(10) . . ?
C38 K1 W1 154.1(3) . . ?
C33 K1 W1 145.5(3) . . ?
C37 K1 W1 165.0(3) . . ?
N2 K1 W1 35.19(7) . . ?
C36 K1 W1 163.4(2) . . ?
C34 K1 W1 145.0(3) . . ?
C35 K1 W1 152.5(3) . . ?
W1 K1 W1 36.56(2) 3_556 . ?
C5 N1 C1 117.6(4) . . ?
C5 N1 W1 123.6(3) . 3_556 ?
C1 N1 W1 118.8(3) . 3_556 ?
C5 N1 K1 110.7(3) . . ?
C1 N1 K1 78.6(3) . . ?
W1 N1 K1 80.42(13) 3_556 . ?
N2 C1 N1 115.9(4) . . ?
N2 C1 C2 124.5(5) . . ?
N1 C1 C2 119.6(5) . . ?
N2 C1 K1 83.9(3) . . ?
N1 C1 K1 76.0(3) . . ?
C2 C1 K1 106.1(4) . . ?
C3 C2 C1 121.1(5) . . ?
C2 C3 C4 119.1(5) . . ?
C5 C4 C3 118.7(5) . . ?
C4 C5 N1 123.5(5) . . ?
C4 C5 C6 119.5(5) . . ?
N1 C5 C6 116.6(4) . . ?
C7 C6 C11 120.2(5) . . ?
C7 C6 C5 122.7(5) . . ?
C11 C6 C5 117.0(5) . . ?
C6 C7 C8 118.8(5) . . ?
C6 C7 C18 121.2(5) . . ?
C8 C7 C18 120.0(5) . . ?
C9 C8 C7 122.0(5) . . ?
C8 C9 C10 117.7(5) . . ?
C8 C9 C15 121.7(5) . . ?
C10 C9 C15 120.5(5) . . ?
C11 C10 C9 122.1(5) . . ?
C10 C11 C6 119.1(5) . . ?
C10 C11 C12 120.2(5) . . ?
C6 C11 C12 120.6(5) . . ?
C13 C12 C14 109.9(6) . . ?
C13 C12 C11 112.8(5) . . ?
C14 C12 C11 110.3(5) . . ?
C1 N2 C21 117.9(4) . . ?
C1 N2 W1 122.4(3) . . ?
C21 N2 W1 118.6(3) . . ?
C1 N2 K1 72.3(3) . . ?
C21 N2 K1 131.3(3) . . ?
W1 N2 K1 79.37(13) . . ?
C17 C15 C16 110.6(6) . . ?
C17 C15 C9 113.1(6) . . ?
C16 C15 C9 110.3(6) . . ?
C19 C18 C20 110.5(5) . . ?
C19 C18 C7 113.0(5) . . ?
C20 C18 C7 110.9(5) . . ?
C22 C21 C26 121.0(5) . . ?
C22 C21 N2 120.6(5) . . ?
C26 C21 N2 118.3(5) . . ?
C23 C22 C21 118.7(5) . . ?
C23 C22 C30 120.3(5) . . ?
C21 C22 C30 121.0(5) . . ?
C24 C23 C22 121.2(6) . . ?
C23 C24 C25 119.7(5) . . ?
C24 C25 C26 121.1(6) . . ?
C25 C26 C21 118.0(5) . . ?
C25 C26 C27 119.5(5) . . ?
C21 C26 C27 122.5(5) . . ?
C26 C27 C28 113.3(6) . . ?
C26 C27 C29 110.8(5) . . ?
C28 C27 C29 110.1(5) . . ?
C31 C30 C22 112.9(6) . . ?
C31 C30 C32 109.6(7) . . ?
C22 C30 C32 110.3(5) . . ?
C38 C33 C34 120.3(14) . . ?
C38 C33 K1 76.4(10) . . ?
C34 C33 K1 82.5(8) . . ?
C33 C34 C35 118.9(15) . . ?
C33 C34 K1 73.7(8) . . ?
C35 C34 K1 78.4(7) . . ?
C36 C35 C34 120.9(15) . . ?
C36 C35 K1 76.5(6) . . ?
C34 C35 K1 78.1(8) . . ?
C35 C36 C37 121.1(11) . . ?
C35 C36 K1 80.5(7) . . ?
C37 C36 K1 76.5(7) . . ?
C38 C37 C36 116.6(14) . . ?
C38 C37 K1 74.9(9) . . ?
C36 C37 K1 79.1(7) . . ?
C33 C38 C37 122.0(16) . . ?
C33 C38 K1 79.7(9) . . ?
C37 C38 K1 80.6(8) . . ?
C40 C39 C44 120.0 . . ?
C39 C40 C41 120.0 . . ?
C42 C41 C40 120.0 . . ?
C41 C42 C43 120.0 . . ?
C42 C43 C44 120.0 . . ?
C43 C44 C39 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        27.85
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         2.584
_refine_diff_density_min         -1.787
_refine_diff_density_rms         0.139
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1960678'
loop_
_audit_author_name
_audit_author_address
'Awal Noor'
;University of Bayreuth
Germany
;
_audit_update_record             
;
2019-10-22 deposited with the CCDC.	2020-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C99.97 H156.95 K2 N8 O11.96 W2, 2 (C6D6) '
_chemical_formula_sum            'C99.97 H156.95 K2 N8 O11.96 W2'
_chemical_formula_weight         2108.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
K K 0.2009 0.2494 '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           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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+1/2, -z'

_cell_length_a                   13.358(5)
_cell_length_b                   24.830(5)
_cell_length_c                   17.125(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 93.678(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     5668(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    16566
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      24.895

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_F_000             2189
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.042
_exptl_absorpt_coefficient_mu    2.156
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8257
_exptl_absorpt_correction_T_max  0.9581
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  STOE-STADIVARI
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24629
_diffrn_reflns_av_unetI/netI     0.0957
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.159
_diffrn_reflns_theta_max         24.750
_diffrn_reflns_theta_full        24.750
_chemical_absolute_configuration -
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             14747
_reflns_number_gt                10611
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.952
_reflns_Friedel_fraction_max     0.994
_reflns_Friedel_fraction_full    0.994

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       STOE-XAREA
_computing_cell_refinement       STOE-XAREA
_computing_data_reduction        STOE-XAREA
_computing_structure_solution    SIR-97
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1160P)²+26.1994P] 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     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.0062(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(3)
_refine_ls_number_reflns         14747
_refine_ls_number_parameters     1123
_refine_ls_number_restraints     349
_refine_ls_R_factor_all          0.1214
_refine_ls_R_factor_gt           0.0858
_refine_ls_wR_factor_ref         0.2335
_refine_ls_wR_factor_gt          0.2061
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.008
_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 0.48394(8) 0.26848(4) 0.27752(6) 0.0560(3) Uani 1 1 d . U . . .
W2 W 0.44323(8) 0.18336(4) 0.24719(6) 0.0550(3) Uani 1 1 d . U . . .
K3 K 0.7758(4) 0.1521(2) 0.6474(4) 0.0600(14) Uani 1 1 d . . . . .
K4 K 1.1637(5) 0.2951(3) 0.8733(4) 0.0678(16) Uani 1 1 d . . . . .
N3 N 0.3630(12) 0.1786(11) 0.3493(10) 0.045(4) Uani 1 1 d . . . . .
O1 O 0.6984(14) 0.1472(10) 0.4943(11) 0.073(6) Uani 1 1 d . . . . .
C33 C 0.3161(14) 0.0855(8) 0.3117(12) 0.034(4) Uani 1 1 d . U . . .
N4 N 0.3927(14) 0.2679(12) 0.3767(10) 0.049(4) Uani 1 1 d . U . . .
O2 O 0.5696(13) 0.1548(10) 0.6176(12) 0.079(6) Uani 1 1 d . . . . .
C51 C 0.306(2) 0.2162(11) 0.4667(14) 0.052(6) Uani 1 1 d . . . . .
H51 H 0.300958 0.246657 0.499899 0.063 Uiso 1 1 calc R U . . .
N1 N 0.5751(16) 0.2789(8) 0.1711(13) 0.056(6) Uani 1 1 d . U . . .
O11 O 0.9715(16) 0.3464(9) 0.8865(14) 0.084(6) Uani 1 1 d . U . . .
O3 O 0.7716(19) 0.0659(10) 0.7536(15) 0.088(7) Uani 1 1 d . . . . .
C19 C 0.604(2) 0.2425(14) 0.0468(15) 0.068(8) Uani 1 1 d . . . . .
H19 H 0.595361 0.214545 0.009083 0.081 Uiso 1 1 calc R U . . .
C48 C 0.3142(19) 0.1320(10) 0.3690(16) 0.050(6) Uani 1 1 d . . . . .
C17 C 0.650(2) 0.3289(14) 0.0830(17) 0.064(7) Uani 1 1 d . U . . .
H17 H 0.677770 0.362054 0.067641 0.077 Uiso 1 1 calc R U . . .
N2 N 0.5222(14) 0.1893(11) 0.1480(13) 0.060(5) Uani 1 1 d . U . . .
C49 C 0.263(2) 0.1261(12) 0.4321(16) 0.057(6) Uani 1 1 d . U . . .
H49 H 0.226605 0.093864 0.439630 0.069 Uiso 1 1 calc R U . . .
C54 C 0.272(2) 0.3372(10) 0.3887(15) 0.055(6) Uani 1 1 d . . . . .
O7 O 1.0993(13) 0.1879(9) 0.8583(11) 0.067(4) Uani 1 1 d . U . . .
C1 C 0.6378(17) 0.3641(10) 0.2173(15) 0.050(6) Uani 1 1 d . U . . .
C58 C 0.428(2) 0.3402(11) 0.4693(18) 0.064(7) Uani 1 1 d . . . . .
O5 O 0.7978(15) 0.2346(9) 0.7638(14) 0.079(6) Uani 1 1 d . . . . .
C34 C 0.386(2) 0.0495(13) 0.3155(19) 0.071(8) Uani 1 1 d . . . . .
C53 C 0.369(3) 0.3150(11) 0.4150(18) 0.068(9) Uani 1 1 d . . . . .
O6 O 0.9153(16) 0.2396(9) 0.6311(13) 0.079(6) Uani 1 1 d . . . . .
N6 N 0.6376(18) 0.1512(14) 0.7816(16) 0.084(8) Uani 1 1 d . . . . .
C92 C 1.330(3) 0.2957(16) 1.046(2) 0.087(10) Uani 1 1 d . U . . .
H92A H 1.349166 0.302829 1.101487 0.104 Uiso 1 1 calc R U . . .
H92B H 1.353760 0.259067 1.033210 0.104 Uiso 1 1 calc R U . . .
C62 C 0.2043(19) 0.3122(11) 0.3280(16) 0.059(6) Uani 1 1 d . . . . .
H62 H 0.243787 0.283905 0.302083 0.070 Uiso 1 1 calc R U . . .
N7 N 1.0257(17) 0.2509(10) 0.9874(15) 0.070(6) Uani 1 1 d . U . . .
C28 C 0.385(2) 0.1640(17) -0.0581(14) 0.088(12) Uani 1 1 d . . . . .
H28A H 0.320593 0.181306 -0.072612 0.132 Uiso 1 1 calc R U . . .
H28B H 0.439308 0.190281 -0.061775 0.132 Uiso 1 1 calc R U . . .
H28C H 0.395418 0.133922 -0.093773 0.132 Uiso 1 1 calc R U . . .
O8 O 1.1931(16) 0.2322(9) 0.7360(13) 0.074(10) Uani 0.96(7) 1 d . U P . .
C22 C 0.649(2) 0.1173(13) 0.119(2) 0.073(9) Uani 1 1 d . . . . .
C24 C 0.603(3) 0.0488(12) 0.0273(18) 0.071(8) Uani 1 1 d . U . . .
H24 H 0.621088 0.016877 0.001159 0.085 Uiso 1 1 calc R U . . .
O9 O 1.3624(18) 0.3181(10) 0.9173(15) 0.090(7) Uani 1 1 d . U . . .
O10 O 1.2233(15) 0.2976(10) 1.0334(14) 0.082(6) Uani 1 1 d . U . . .
C36 C 0.308(2) -0.0008(10) 0.2027(19) 0.064(7) Uani 1 1 d . . . . .
C68 C 0.540(2) 0.1398(16) 0.5437(16) 0.078(9) Uani 1 1 d . . . . .
H68A H 0.468343 0.148431 0.532974 0.093 Uiso 1 1 calc R U . . .
H68B H 0.548496 0.100358 0.538263 0.093 Uiso 1 1 calc R U . . .
C23 C 0.674(2) 0.0722(15) 0.0864(18) 0.076(9) Uani 1 1 d . . . . .
H23 H 0.736166 0.055181 0.100489 0.092 Uiso 1 1 calc R U . . .
C35 C 0.387(3) 0.0068(14) 0.254(2) 0.093(11) Uani 1 1 d . . . . .
H35 H 0.443835 -0.015734 0.252006 0.111 Uiso 1 1 calc R U . . .
C38 C 0.227(2) 0.0761(12) 0.2594(17) 0.066(7) Uani 1 1 d . . . . .
C70 C 0.533(2) 0.1630(15) 0.7516(18) 0.084(10) Uani 1 1 d . . . . .
H70A H 0.524968 0.202440 0.745108 0.101 Uiso 1 1 calc R U . . .
H70B H 0.486096 0.150665 0.790045 0.101 Uiso 1 1 calc R U . . .
C52 C 0.355(2) 0.2223(10) 0.4002(18) 0.051(7) Uani 1 1 d . . . . .
C2 C 0.568(3) 0.4086(13) 0.2283(16) 0.078(9) Uani 1 1 d . . . . .
C94 C 1.066(2) 0.2658(17) 1.062(2) 0.089(9) Uani 1 1 d . U . . .
H94A H 1.031813 0.244720 1.101842 0.107 Uiso 1 1 calc R U . . .
H94B H 1.050761 0.304252 1.070924 0.107 Uiso 1 1 calc R U . . .
C21 C 0.550(2) 0.1415(12) 0.1089(19) 0.061(8) Uani 1 1 d . . . . .
C18 C 0.649(3) 0.2885(14) 0.0312(18) 0.086(10) Uani 1 1 d . U . . .
H18 H 0.681397 0.292644 -0.016387 0.103 Uiso 1 1 calc R U . . .
C65 C 0.861(2) 0.1438(15) 0.445(2) 0.081(9) Uani 1 1 d . U . . .
H65A H 0.851841 0.104563 0.436711 0.098 Uiso 1 1 calc R U . . .
H65B H 0.901564 0.157561 0.402992 0.098 Uiso 1 1 calc R U . . .
O4 O 0.9188(19) 0.0669(11) 0.6381(18) 0.109(9) Uani 1 1 d . U . . .
C63 C 0.163(3) 0.3523(14) 0.261(2) 0.087(10) Uani 1 1 d . . . . .
H63A H 0.118445 0.332684 0.223534 0.131 Uiso 1 1 calc R U . . .
H63B H 0.125306 0.381416 0.284803 0.131 Uiso 1 1 calc R U . . .
H63C H 0.219138 0.367514 0.234802 0.131 Uiso 1 1 calc R U . . .
O12 O 1.119(2) 0.3951(12) 0.8024(18) 0.112(9) Uani 1 1 d . U . . .
C27 C 0.385(2) 0.1425(13) 0.0274(19) 0.071(8) Uani 1 1 d . . . . .
H27 H 0.372566 0.172626 0.064412 0.086 Uiso 1 1 calc R U . . .
C77 C 0.965(3) 0.2035(15) 0.514(2) 0.092(10) Uani 1 1 d . U . . .
H77A H 0.917376 0.227936 0.484982 0.110 Uiso 1 1 calc R U . . .
H77B H 1.023773 0.198782 0.482969 0.110 Uiso 1 1 calc R U . . .
C31 C 0.8010(17) 0.1718(15) 0.138(2) 0.081(10) Uani 1 1 d . . . . .
H31A H 0.766658 0.198151 0.103230 0.121 Uiso 1 1 calc R U . . .
H31B H 0.847216 0.190530 0.175660 0.121 Uiso 1 1 calc R U . . .
H31C H 0.838699 0.146594 0.107184 0.121 Uiso 1 1 calc R U . . .
C8 C 0.832(2) 0.2916(19) 0.335(2) 0.104(13) Uani 1 1 d . . . . .
H8A H 0.777111 0.281814 0.367078 0.156 Uiso 1 1 calc R U . . .
H8B H 0.874857 0.260092 0.327792 0.156 Uiso 1 1 calc R U . . .
H8C H 0.872175 0.320398 0.360564 0.156 Uiso 1 1 calc R U . . .
C82 C 0.674(2) 0.1966(13) 0.8385(18) 0.076(9) Uani 1 1 d . . . . .
H82A H 0.618928 0.205124 0.872850 0.092 Uiso 1 1 calc R U . . .
H82B H 0.731160 0.183055 0.872212 0.092 Uiso 1 1 calc R U . . .
C37 C 0.218(2) 0.0330(15) 0.214(2) 0.085(10) Uani 1 1 d . . . . .
H37 H 0.155231 0.023723 0.189031 0.102 Uiso 1 1 calc R U . . .
C71 C 0.638(2) 0.0985(15) 0.818(2) 0.079(8) Uani 1 1 d . . . . .
H71A H 0.606985 0.101712 0.869437 0.095 Uiso 1 1 calc R U . . .
H71B H 0.595079 0.073858 0.785176 0.095 Uiso 1 1 calc R U . . .
C7 C 0.7905(19) 0.3108(16) 0.257(2) 0.083(10) Uani 1 1 d . . . . .
H7 H 0.752535 0.280474 0.230289 0.100 Uiso 1 1 calc R U . . .
C16 C 0.614(2) 0.3272(13) 0.1551(18) 0.061(7) Uani 1 1 d . U . . .
C76 C 0.994(2) 0.1098(14) 0.5336(18) 0.080(9) Uani 1 1 d . U . . .
H76A H 1.018595 0.099109 0.482549 0.096 Uiso 1 1 calc R U . . .
H76B H 1.051413 0.123384 0.567185 0.096 Uiso 1 1 calc R U . . .
C55 C 0.245(2) 0.3848(12) 0.425(2) 0.080(10) Uani 1 1 d . U . . .
H55 H 0.181306 0.399976 0.411012 0.096 Uiso 1 1 calc R U . . .
C96 C 0.922(3) 0.3326(14) 0.961(2) 0.082(9) Uani 1 1 d . U . . .
H96A H 0.960890 0.348233 1.006293 0.098 Uiso 1 1 calc R U . . .
H96B H 0.853381 0.347668 0.958672 0.098 Uiso 1 1 calc R U . . .
C30 C 0.723(3) 0.1407(16) 0.182(2) 0.089(10) Uani 1 1 d . U . . .
H30 H 0.687056 0.166815 0.214750 0.107 Uiso 1 1 calc R U . . .
C45 C 0.489(2) 0.0706(14) 0.355(2) 0.089(10) Uani 1 1 d D U . . .
H45 H 0.477804 0.091530 0.403615 0.107 Uiso 1 1 calc R U . . .
C56 C 0.302(2) 0.4093(12) 0.478(2) 0.082(10) Uani 1 1 d . . . . .
H56 H 0.278545 0.441482 0.500512 0.098 Uiso 1 1 calc R U . . .
C25 C 0.514(2) 0.0707(11) 0.009(2) 0.068(8) Uani 1 1 d . U . . .
H25 H 0.471451 0.055304 -0.031467 0.081 Uiso 1 1 calc R U . . .
C97 C 0.977(3) 0.4051(14) 0.884(2) 0.084(9) Uani 1 1 d . U . . .
H97A H 1.021653 0.419373 0.927518 0.100 Uiso 1 1 calc R U . . .
H97B H 0.910226 0.421718 0.885234 0.100 Uiso 1 1 calc R U . . .
C5 C 0.754(3) 0.4054(17) 0.314(3) 0.101(11) Uani 1 1 d . U . . .
H5 H 0.819622 0.404437 0.339554 0.121 Uiso 1 1 calc R U . . .
C80 C 0.833(2) 0.2842(11) 0.733(2) 0.070(8) Uani 1 1 d . . . . .
H80A H 0.843686 0.311109 0.774965 0.084 Uiso 1 1 calc R U . . .
H80B H 0.782972 0.298614 0.692990 0.084 Uiso 1 1 calc R U . . .
C91 C 1.379(2) 0.3339(12) 0.9987(17) 0.066(7) Uani 1 1 d . U . . .
H91A H 1.451564 0.334761 1.013826 0.079 Uiso 1 1 calc R U . . .
H91B H 1.350988 0.370313 1.006596 0.079 Uiso 1 1 calc R U . . .
C50 C 0.262(2) 0.1686(13) 0.4893(17) 0.076(9) Uani 1 1 d . . . . .
H50 H 0.234484 0.164312 0.538606 0.091 Uiso 1 1 calc R U . . .
C81 C 0.704(2) 0.2459(13) 0.8014(18) 0.078(8) Uani 1 1 d . . . . .
H81A H 0.714368 0.274853 0.840768 0.094 Uiso 1 1 calc R U . . .
H81B H 0.651013 0.257689 0.761741 0.094 Uiso 1 1 calc R U . . .
C29 C 0.300(3) 0.1010(17) 0.028(3) 0.100(12) Uani 1 1 d . . . . .
H29A H 0.235909 0.118668 0.013682 0.150 Uiso 1 1 calc R U . . .
H29B H 0.311835 0.072559 -0.010271 0.150 Uiso 1 1 calc R U . . .
H29C H 0.298457 0.085189 0.080104 0.150 Uiso 1 1 calc R U . . .
C79 C 0.929(2) 0.2733(16) 0.6963(18) 0.083(9) Uani 1 1 d . . . . .
H79A H 0.958738 0.307792 0.680228 0.099 Uiso 1 1 calc R U . . .
H79B H 0.976854 0.256183 0.735405 0.099 Uiso 1 1 calc R U . . .
C26 C 0.483(2) 0.1163(12) 0.049(2) 0.070(8) Uani 1 1 d . . . . .
C59 C 0.530(3) 0.3184(14) 0.4912(18) 0.075(9) Uani 1 1 d . . . . .
H59 H 0.534690 0.283079 0.463573 0.091 Uiso 1 1 calc R U . . .
C84 C 1.007(2) 0.1725(12) 0.8960(17) 0.076(8) Uani 1 1 d . . . . .
H84A H 0.999357 0.132824 0.895815 0.091 Uiso 1 1 calc R U . . .
H84B H 0.947591 0.188590 0.867721 0.091 Uiso 1 1 calc R U . . .
C85 C 1.101(3) 0.1574(14) 0.7880(18) 0.080(9) Uani 1 1 d . . . . .
H85A H 1.040069 0.164432 0.753304 0.096 Uiso 1 1 calc R U . . .
H85B H 1.104913 0.118316 0.799445 0.096 Uiso 1 1 calc R U . . .
C88 C 1.285(3) 0.3074(15) 0.6869(19) 0.087(10) Uani 1 1 d . . . . .
H88A H 1.224903 0.320204 0.655278 0.105 Uiso 1 1 calc R U . . .
H88B H 1.343596 0.315276 0.656255 0.105 Uiso 1 1 calc R U . . .
C9 C 0.869(3) 0.324(2) 0.213(2) 0.117(15) Uani 1 1 d . . . . .
H9A H 0.842912 0.336775 0.161865 0.176 Uiso 1 1 calc R U . . .
H9B H 0.908370 0.352616 0.240034 0.176 Uiso 1 1 calc R U . . .
H9C H 0.911052 0.292310 0.207261 0.176 Uiso 1 1 calc R U . . .
C57 C 0.403(3) 0.3882(14) 0.5028(18) 0.089(11) Uani 1 1 d . . . . .
H57 H 0.447370 0.406607 0.539445 0.107 Uiso 1 1 calc R U . . .
C72 C 0.736(3) 0.0752(16) 0.831(2) 0.098(11) Uani 1 1 d . . . . .
H72A H 0.733175 0.040967 0.860442 0.117 Uiso 1 1 calc R U . . .
H72B H 0.781839 0.100266 0.861265 0.117 Uiso 1 1 calc R U . . .
C69 C 0.508(2) 0.1355(14) 0.6738(19) 0.080(9) Uani 1 1 d . . . . .
H69A H 0.518063 0.096115 0.679801 0.096 Uiso 1 1 calc R U . . .
H69B H 0.437298 0.142129 0.656804 0.096 Uiso 1 1 calc R U . . .
C95 C 0.918(2) 0.2727(17) 0.968(2) 0.093(9) Uani 1 1 d . U . . .
H95A H 0.890026 0.256713 0.918454 0.112 Uiso 1 1 calc R U . . .
H95B H 0.874372 0.262650 1.010174 0.112 Uiso 1 1 calc R U . . .
N5 N 0.917(2) 0.1525(13) 0.522(2) 0.101(9) Uani 1 1 d . . . . .
N8 N 1.294(2) 0.3401(14) 0.755(2) 0.100(9) Uani 1 1 d . U . . .
C60 C 0.617(2) 0.3540(18) 0.464(2) 0.102(13) Uani 1 1 d . U . . .
H60A H 0.605782 0.361809 0.408333 0.153 Uiso 1 1 calc R U . . .
H60B H 0.619164 0.387815 0.493871 0.153 Uiso 1 1 calc R U . . .
H60C H 0.680660 0.334822 0.473761 0.153 Uiso 1 1 calc R U . . .
C39 C 0.142(3) 0.1146(16) 0.256(2) 0.090(10) Uani 1 1 d . U . . .
H39 H 0.165419 0.147116 0.286178 0.108 Uiso 1 1 calc R U . . .
C13 C 0.469(3) 0.4155(19) 0.186(2) 0.103(11) Uani 1 1 d D U . . .
H13 H 0.451275 0.379852 0.161481 0.124 Uiso 1 1 calc R U . . .
C75 C 0.950(3) 0.0642(15) 0.570(3) 0.117(15) Uani 1 1 d . U . . .
H75A H 0.892759 0.052273 0.534615 0.141 Uiso 1 1 calc R U . . .
H75B H 1.000447 0.034870 0.570698 0.141 Uiso 1 1 calc R U . . .
C90 C 1.418(3) 0.3491(17) 0.868(2) 0.104(11) Uani 1 1 d . U . . .
H90A H 1.490446 0.344882 0.881372 0.125 Uiso 1 1 calc R U . . .
H90B H 1.400221 0.387699 0.872341 0.125 Uiso 1 1 calc R U . . .
C78 C 0.998(3) 0.229(2) 0.589(3) 0.110(13) Uani 1 1 d . U . . .
H78A H 1.044707 0.205400 0.619824 0.132 Uiso 1 1 calc R U . . .
H78B H 1.032977 0.263504 0.579250 0.132 Uiso 1 1 calc R U . . .
C67 C 0.6024(19) 0.1689(11) 0.4836(18) 0.065(8) Uani 1 1 d . . . . .
H67A H 0.573978 0.162226 0.429697 0.077 Uiso 1 1 calc R U . . .
H67B H 0.603667 0.208163 0.493369 0.077 Uiso 1 1 calc R U . . .
C74 C 0.886(3) 0.0202(18) 0.672(3) 0.112(13) Uani 1 1 d . U . . .
H74A H 0.941471 -0.006145 0.677111 0.134 Uiso 1 1 calc R U . . .
H74B H 0.831116 0.004128 0.637466 0.134 Uiso 1 1 calc R U . . .
C64 C 0.112(2) 0.2830(14) 0.363(2) 0.095(12) Uani 1 1 d . . . . .
H64A H 0.069362 0.267073 0.320537 0.143 Uiso 1 1 calc R U . . .
H64B H 0.136653 0.254509 0.399120 0.143 Uiso 1 1 calc R U . . .
H64C H 0.073263 0.309155 0.391449 0.143 Uiso 1 1 calc R U . . .
C89 C 1.393(3) 0.3303(18) 0.788(3) 0.107(12) Uani 1 1 d . U . . .
H89A H 1.440697 0.347338 0.753262 0.128 Uiso 1 1 calc R U . . .
H89B H 1.405344 0.290993 0.786610 0.128 Uiso 1 1 calc R U . . .
C86 C 1.199(2) 0.178(2) 0.7493(17) 0.093(11) Uani 1 1 d . . . . .
H86A H 1.258781 0.169728 0.784434 0.112 Uiso 1 1 calc R U . . .
H86B H 1.206053 0.158745 0.699163 0.112 Uiso 1 1 calc R U . . .
C4 C 0.695(4) 0.4474(19) 0.323(3) 0.119(13) Uani 1 1 d D U . . .
C47 C 0.541(2) 0.1083(13) 0.292(2) 0.077(8) Uani 1 1 d D U . . .
H47A H 0.556215 0.085965 0.246271 0.093 Uiso 1 1 calc R U . . .
H47B H 0.606138 0.121750 0.315843 0.093 Uiso 1 1 calc R U . . .
C20 C 0.569(2) 0.2375(11) 0.1205(19) 0.064(9) Uani 1 1 d . . . . .
C12 C 0.752(5) 0.538(3) 0.358(5) 0.19(2) Uani 1 1 d . U . . .
H12A H 0.773766 0.561139 0.402509 0.291 Uiso 1 1 calc R U . . .
H12B H 0.806997 0.535682 0.322310 0.291 Uiso 1 1 calc R U . . .
H12C H 0.693282 0.554211 0.329874 0.291 Uiso 1 1 calc R U . . .
C66 C 0.759(2) 0.1707(15) 0.4384(16) 0.077(10) Uani 1 1 d . . . . .
H66A H 0.766941 0.209809 0.448401 0.092 Uiso 1 1 calc R U . . .
H66B H 0.727906 0.165707 0.385000 0.092 Uiso 1 1 calc R U . . .
C73 C 0.848(3) 0.0321(16) 0.752(2) 0.094(10) Uani 1 1 d . U . . .
H73A H 0.828017 -0.002397 0.775066 0.113 Uiso 1 1 calc R U . . .
H73B H 0.904418 0.046833 0.785228 0.113 Uiso 1 1 calc R U . . .
C42 C 0.305(3) -0.0467(14) 0.144(2) 0.083(9) Uani 1 1 d . U . . .
H42 H 0.240558 -0.043672 0.111450 0.100 Uiso 1 1 calc R U . . .
C6 C 0.718(3) 0.3596(15) 0.2627(17) 0.077(9) Uani 1 1 d . . . . .
C41 C 0.048(3) 0.0923(19) 0.297(3) 0.116(13) Uani 1 1 d . U . . .
H41A H -0.006147 0.119174 0.292747 0.174 Uiso 1 1 calc R U . . .
H41B H 0.024462 0.058996 0.270784 0.174 Uiso 1 1 calc R U . . .
H41C H 0.066334 0.084964 0.351954 0.174 Uiso 1 1 calc R U . . .
C83 C 1.018(3) 0.1933(15) 0.979(2) 0.088(10) Uani 1 1 d . . . . .
H83A H 0.959238 0.180930 1.006779 0.105 Uiso 1 1 calc R U . . .
H83B H 1.078362 0.176751 1.005613 0.105 Uiso 1 1 calc R U . . .
C46 C 0.566(3) 0.0246(17) 0.373(3) 0.121(17) Uani 1 1 d . . . . .
H46A H 0.628196 0.039715 0.397657 0.181 Uiso 1 1 calc R U . . .
H46B H 0.537812 -0.001237 0.409171 0.181 Uiso 1 1 calc R U . . .
H46C H 0.580342 0.006275 0.324591 0.181 Uiso 1 1 calc R U . . .
C44 C 0.301(3) -0.1005(17) 0.190(3) 0.108(12) Uani 1 1 d . U . . .
H44A H 0.246877 -0.098723 0.225746 0.162 Uiso 1 1 calc R U . . .
H44B H 0.288883 -0.130411 0.153330 0.162 Uiso 1 1 calc R U . . .
H44C H 0.365201 -0.106175 0.220147 0.162 Uiso 1 1 calc R U . . .
C15 C 0.476(4) 0.456(2) 0.116(3) 0.130(15) Uani 1 1 d . U . . .
H15A H 0.410055 0.460330 0.088348 0.195 Uiso 1 1 calc R U . . .
H15B H 0.499137 0.491417 0.136312 0.195 Uiso 1 1 calc R U . . .
H15C H 0.524014 0.442738 0.079451 0.195 Uiso 1 1 calc R U . . .
C99 C 1.169(3) 0.409(2) 0.722(3) 0.125(15) Uani 1 1 d . U . . .
H99A H 1.139611 0.386001 0.679095 0.150 Uiso 1 1 calc R U . . .
H99B H 1.159578 0.446975 0.708247 0.150 Uiso 1 1 calc R U . . .
C32 C 0.776(3) 0.1002(18) 0.236(2) 0.104(13) Uani 1 1 d . . . . .
H32A H 0.725987 0.080397 0.264106 0.156 Uiso 1 1 calc R U . . .
H32B H 0.813525 0.074992 0.205019 0.156 Uiso 1 1 calc R U . . .
H32C H 0.822043 0.118927 0.273495 0.156 Uiso 1 1 calc R U . . .
C10 C 0.730(5) 0.491(2) 0.382(4) 0.159(16) Uani 1 1 d D U . . .
H10 H 0.790288 0.476240 0.413880 0.191 Uiso 1 1 calc R U . . .
C40 C 0.107(3) 0.1347(17) 0.172(2) 0.099(11) Uani 1 1 d . U . . .
H40A H 0.050716 0.159842 0.175505 0.149 Uiso 1 1 calc R U . . .
H40B H 0.162585 0.153076 0.148645 0.149 Uiso 1 1 calc R U . . .
H40C H 0.085286 0.103902 0.139418 0.149 Uiso 1 1 calc R U . . .
C93 C 1.176(2) 0.2580(15) 1.077(2) 0.087(9) Uani 1 1 d . U . . .
H93A H 1.195315 0.262120 1.133451 0.104 Uiso 1 1 calc R U . . .
H93B H 1.195395 0.221587 1.060270 0.104 Uiso 1 1 calc R U . . .
C61 C 0.548(3) 0.3070(18) 0.576(3) 0.108(13) Uani 1 1 d . U . . .
H61A H 0.616268 0.292801 0.586256 0.162 Uiso 1 1 calc R U . . .
H61B H 0.541056 0.340358 0.605955 0.162 Uiso 1 1 calc R U . . .
H61C H 0.499461 0.280421 0.592379 0.162 Uiso 1 1 calc R U . . .
C3 C 0.616(4) 0.453(2) 0.279(3) 0.118(14) Uani 1 1 d . U . . .
H3 H 0.584416 0.487382 0.276644 0.141 Uiso 1 1 calc R U . . .
C87 C 1.277(4) 0.252(2) 0.692(4) 0.14(3) Uani 0.97(12) 1 d . U P . .
H87A H 1.340646 0.237545 0.717056 0.162 Uiso 0.97(12) 1 calc R U P . .
H87B H 1.269892 0.236840 0.638261 0.162 Uiso 0.97(12) 1 calc R U P . .
C98 C 1.028(3) 0.4160(16) 0.795(2) 0.096(10) Uani 1 1 d . U . . .
H98A H 0.986793 0.398079 0.752685 0.115 Uiso 1 1 calc R U . . .
H98B H 1.030556 0.455066 0.783953 0.115 Uiso 1 1 calc R U . . .
C43 C 0.383(4) -0.047(2) 0.091(3) 0.127(15) Uani 1 1 d . U . . .
H43A H 0.374631 -0.077553 0.055312 0.190 Uiso 1 1 calc R U . . .
H43B H 0.379152 -0.013214 0.059772 0.190 Uiso 1 1 calc R U . . .
H43C H 0.448230 -0.048665 0.119792 0.190 Uiso 1 1 calc R U . . .
C100 C 1.278(3) 0.3959(18) 0.739(3) 0.110(13) Uani 1 1 d . U . . .
H10A H 1.315542 0.405925 0.692541 0.132 Uiso 1 1 calc R U . . .
H10B H 1.305310 0.417628 0.783631 0.132 Uiso 1 1 calc R U . . .
C14 C 0.378(3) 0.434(2) 0.229(3) 0.139(17) Uani 1 1 d D U . . .
H14A H 0.319318 0.436167 0.192503 0.209 Uiso 1 1 calc R U . . .
H14B H 0.365524 0.407126 0.270088 0.209 Uiso 1 1 calc R U . . .
H14C H 0.392082 0.468756 0.253518 0.209 Uiso 1 1 calc R U . . .
C11 C 0.635(6) 0.504(3) 0.448(5) 0.21(3) Uani 1 1 d . U . . .
H11A H 0.612241 0.469816 0.469978 0.322 Uiso 1 1 calc R U . . .
H11B H 0.660978 0.527459 0.489976 0.322 Uiso 1 1 calc R U . . .
H11C H 0.577666 0.521396 0.419100 0.322 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 N4 2.154(17) . ?
W1 W2 2.2353(14) . ?
W1 N1 2.27(2) . ?
W2 N2 2.06(2) . ?
W2 N3 2.112(17) . ?
W2 C47 2.38(3) . ?
K3 O1 2.76(2) . ?
K3 O2 2.770(19) . ?
K3 O3 2.81(2) . ?
K3 O5 2.86(2) . ?
K3 O4 2.86(3) . ?
K3 O6 2.89(2) . ?
K3 N5 2.95(4) . ?
K3 N6 3.04(3) . ?
K3 C75 3.51(3) . ?
K3 C68 3.53(3) . ?
K4 O9 2.77(2) . ?
K4 O7 2.80(2) . ?
K4 O10 2.81(2) . ?
K4 O12 2.81(3) . ?
K4 O8 2.87(2) . ?
K4 O11 2.89(2) . ?
K4 N8 2.97(4) . ?
K4 N7 2.98(3) . ?
N3 C48 1.38(3) . ?
N3 C52 1.40(4) . ?
O1 C67 1.39(3) . ?
O1 C66 1.42(3) . ?
C33 C34 1.29(3) . ?
C33 C38 1.46(3) . ?
C33 C48 1.52(3) . ?
N4 C52 1.31(4) . ?
N4 C53 1.39(4) . ?
O2 C68 1.35(3) . ?
O2 C69 1.39(3) . ?
C51 C52 1.36(4) . ?
C51 C50 1.38(4) . ?
N1 C16 1.34(3) . ?
N1 C20 1.34(3) . ?
O11 C97 1.46(4) . ?
O11 C96 1.51(4) . ?
O3 C73 1.32(4) . ?
O3 C72 1.46(5) . ?
C19 C18 1.33(4) . ?
C19 C20 1.38(4) . ?
C48 C49 1.32(4) . ?
C17 C18 1.34(4) . ?
C17 C16 1.35(4) . ?
N2 C21 1.42(4) . ?
N2 C20 1.45(4) . ?
C49 C50 1.44(4) . ?
C54 C55 1.40(4) . ?
C54 C53 1.45(4) . ?
C54 C62 1.47(4) . ?
O7 C85 1.42(4) . ?
O7 C84 1.48(4) . ?
C1 C6 1.29(4) . ?
C1 C16 1.43(4) . ?
C1 C2 1.47(4) . ?
C58 C53 1.34(4) . ?
C58 C57 1.37(4) . ?
C58 C59 1.49(4) . ?
O5 C80 1.43(3) . ?
O5 C81 1.47(3) . ?
C34 C35 1.49(5) . ?
C34 C45 1.59(4) . ?
O6 C78 1.37(4) . ?
O6 C79 1.40(3) . ?
N6 C71 1.45(4) . ?
N6 C70 1.48(4) . ?
N6 C82 1.55(4) . ?
C92 C91 1.43(5) . ?
C92 O10 1.43(4) . ?
C62 C64 1.58(4) . ?
C62 C63 1.59(4) . ?
N7 C94 1.41(4) . ?
N7 C83 1.44(4) . ?
N7 C95 1.55(4) . ?
C28 C27 1.56(4) . ?
O8 C86 1.37(5) . ?
O8 C87 1.48(6) . ?
C22 C23 1.31(4) . ?
C22 C21 1.45(4) . ?
C22 C30 1.54(4) . ?
C24 C25 1.32(4) . ?
C24 C23 1.46(4) . ?
O9 C90 1.39(4) . ?
O9 C91 1.45(4) . ?
O10 C93 1.41(4) . ?
C36 C35 1.35(4) . ?
C36 C37 1.48(4) . ?
C36 C42 1.52(4) . ?
C68 C67 1.54(4) . ?
C38 C37 1.32(4) . ?
C38 C39 1.48(4) . ?
C70 C69 1.52(4) . ?
C2 C13 1.47(5) . ?
C2 C3 1.52(6) . ?
C94 C93 1.48(4) . ?
C21 C26 1.46(4) . ?
C65 N5 1.49(4) . ?
C65 C66 1.51(4) . ?
O4 C75 1.27(5) . ?
O4 C74 1.38(5) . ?
O12 C98 1.33(4) . ?
O12 C99 1.60(6) . ?
C27 C26 1.49(4) . ?
C27 C29 1.53(5) . ?
C77 N5 1.42(4) . ?
C77 C78 1.48(5) . ?
C31 C30 1.53(5) . ?
C8 C7 1.49(5) . ?
C82 C81 1.45(4) . ?
C71 C72 1.45(5) . ?
C7 C9 1.36(5) . ?
C7 C6 1.56(5) . ?
C76 C75 1.44(5) . ?
C76 N5 1.48(4) . ?
C55 C56 1.29(5) . ?
C96 C95 1.49(5) . ?
C30 C32 1.50(5) . ?
C45 C46 1.55(5) . ?
C45 C47 1.62(2) . ?
C56 C57 1.49(5) . ?
C25 C26 1.40(4) . ?
C97 C98 1.72(5) . ?
C5 C4 1.33(6) . ?
C5 C6 1.50(5) . ?
C80 C79 1.49(4) . ?
C59 C61 1.49(5) . ?
C59 C60 1.55(5) . ?
C84 C83 1.51(4) . ?
C85 C86 1.59(5) . ?
C88 C87 1.39(6) . ?
C88 N8 1.43(4) . ?
N8 C89 1.42(5) . ?
N8 C100 1.43(5) . ?
C39 C40 1.56(5) . ?
C39 C41 1.58(5) . ?
C13 C14 1.53(2) . ?
C13 C15 1.57(6) . ?
C90 C89 1.46(5) . ?
C74 C73 1.52(6) . ?
C4 C3 1.27(6) . ?
C4 C10 1.53(2) . ?
C12 C10 1.30(8) . ?
C42 C43 1.42(6) . ?
C42 C44 1.56(5) . ?
C99 C100 1.50(6) . ?
C10 C11 1.78(9) . ?

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
N4 W1 W2 92.0(7) . . ?
N4 W1 N1 173.6(10) . . ?
W2 W1 N1 93.2(5) . . ?
N2 W2 N3 179.1(12) . . ?
N2 W2 W1 89.7(7) . . ?
N3 W2 W1 89.4(7) . . ?
N2 W2 C47 91.2(10) . . ?
N3 W2 C47 89.3(10) . . ?
W1 W2 C47 123.0(8) . . ?
O1 K3 O2 61.2(6) . . ?
O1 K3 O3 124.0(7) . . ?
O2 K3 O3 94.3(7) . . ?
O1 K3 O5 135.2(7) . . ?
O2 K3 O5 99.6(7) . . ?
O3 K3 O5 95.7(7) . . ?
O1 K3 O4 97.2(8) . . ?
O2 K3 O4 131.8(8) . . ?
O3 K3 O4 60.9(8) . . ?
O5 K3 O4 121.9(8) . . ?
O1 K3 O6 98.4(6) . . ?
O2 K3 O6 127.2(7) . . ?
O3 K3 O6 132.5(7) . . ?
O5 K3 O6 59.4(6) . . ?
O4 K3 O6 96.5(7) . . ?
O1 K3 N5 61.7(7) . . ?
O2 K3 N5 122.8(8) . . ?
O3 K3 N5 120.9(9) . . ?
O5 K3 N5 117.6(8) . . ?
O4 K3 N5 60.1(9) . . ?
O6 K3 N5 58.7(8) . . ?
O1 K3 N6 120.6(6) . . ?
O2 K3 N6 59.6(6) . . ?
O3 K3 N6 57.7(8) . . ?
O5 K3 N6 61.2(7) . . ?
O4 K3 N6 118.4(8) . . ?
O6 K3 N6 120.4(8) . . ?
N5 K3 N6 177.6(8) . . ?
O1 K3 C75 80.3(10) . . ?
O2 K3 C75 128.3(10) . . ?
O3 K3 C75 79.2(9) . . ?
O5 K3 C75 131.9(10) . . ?
O4 K3 C75 19.7(10) . . ?
O6 K3 C75 89.1(9) . . ?
N5 K3 C75 42.0(9) . . ?
N6 K3 C75 136.9(9) . . ?
O1 K3 C68 41.4(6) . . ?
O2 K3 C68 20.7(7) . . ?
O3 K3 C68 101.8(8) . . ?
O5 K3 C68 117.5(8) . . ?
O4 K3 C68 119.0(9) . . ?
O6 K3 C68 125.3(8) . . ?
N5 K3 C68 103.0(8) . . ?
N6 K3 C68 79.3(7) . . ?
C75 K3 C68 110.3(11) . . ?
O9 K4 O7 120.2(7) . . ?
O9 K4 O10 61.5(7) . . ?
O7 K4 O10 100.1(7) . . ?
O9 K4 O12 96.1(7) . . ?
O7 K4 O12 138.1(6) . . ?
O10 K4 O12 116.2(8) . . ?
O9 K4 O8 99.0(7) . . ?
O7 K4 O8 57.7(6) . . ?
O10 K4 O8 140.0(7) . . ?
O12 K4 O8 99.4(9) . . ?
O9 K4 O11 136.8(7) . . ?
O7 K4 O11 99.0(6) . . ?
O10 K4 O11 96.4(7) . . ?
O12 K4 O11 58.7(8) . . ?
O8 K4 O11 118.3(7) . . ?
O9 K4 N8 60.9(8) . . ?
O7 K4 N8 119.0(8) . . ?
O10 K4 N8 120.9(8) . . ?
O12 K4 N8 59.4(10) . . ?
O8 K4 N8 62.0(8) . . ?
O11 K4 N8 116.9(8) . . ?
O9 K4 N7 121.3(7) . . ?
O7 K4 N7 60.7(6) . . ?
O10 K4 N7 61.1(7) . . ?
O12 K4 N7 119.1(8) . . ?
O8 K4 N7 117.3(7) . . ?
O11 K4 N7 61.4(7) . . ?
N8 K4 N7 177.8(8) . . ?
C48 N3 C52 116(2) . . ?
C48 N3 W2 121.5(18) . . ?
C52 N3 W2 122.4(19) . . ?
C67 O1 C66 109(2) . . ?
C67 O1 K3 113.2(17) . . ?
C66 O1 K3 115.1(16) . . ?
C34 C33 C38 119(2) . . ?
C34 C33 C48 122(2) . . ?
C38 C33 C48 118.0(18) . . ?
C52 N4 C53 119(2) . . ?
C52 N4 W1 120(2) . . ?
C53 N4 W1 122(2) . . ?
C68 O2 C69 114(2) . . ?
C68 O2 K3 113.0(18) . . ?
C69 O2 K3 119.2(18) . . ?
C52 C51 C50 124(3) . . ?
C16 N1 C20 124(3) . . ?
C16 N1 W1 120(2) . . ?
C20 N1 W1 114.7(15) . . ?
C97 O11 C96 106(2) . . ?
C97 O11 K4 112.7(18) . . ?
C96 O11 K4 113.9(17) . . ?
C73 O3 C72 115(3) . . ?
C73 O3 K3 115(2) . . ?
C72 O3 K3 119(2) . . ?
C18 C19 C20 117(3) . . ?
C49 C48 N3 125(3) . . ?
C49 C48 C33 118(2) . . ?
N3 C48 C33 117(2) . . ?
C18 C17 C16 127(3) . . ?
C21 N2 C20 114(2) . . ?
C21 N2 W2 119(2) . . ?
C20 N2 W2 125.7(18) . . ?
C48 C49 C50 120(3) . . ?
C55 C54 C53 116(3) . . ?
C55 C54 C62 121(3) . . ?
C53 C54 C62 124(2) . . ?
C85 O7 C84 107(2) . . ?
C85 O7 K4 124.2(18) . . ?
C84 O7 K4 117.7(16) . . ?
C6 C1 C16 122(3) . . ?
C6 C1 C2 120(3) . . ?
C16 C1 C2 118(2) . . ?
C53 C58 C57 123(3) . . ?
C53 C58 C59 120(3) . . ?
C57 C58 C59 117(3) . . ?
C80 O5 C81 108(2) . . ?
C80 O5 K3 112.1(17) . . ?
C81 O5 K3 112.8(17) . . ?
C33 C34 C35 119(3) . . ?
C33 C34 C45 114(3) . . ?
C35 C34 C45 120(3) . . ?
C58 C53 N4 125(3) . . ?
C58 C53 C54 121(3) . . ?
N4 C53 C54 114(3) . . ?
C78 O6 C79 117(3) . . ?
C78 O6 K3 117(2) . . ?
C79 O6 K3 115.2(19) . . ?
C71 N6 C70 108(3) . . ?
C71 N6 C82 113(3) . . ?
C70 N6 C82 109(3) . . ?
C71 N6 K3 110.7(18) . . ?
C70 N6 K3 109.8(19) . . ?
C82 N6 K3 106.9(17) . . ?
C91 C92 O10 112(3) . . ?
C54 C62 C64 113(2) . . ?
C54 C62 C63 115(2) . . ?
C64 C62 C63 108(2) . . ?
C94 N7 C83 112(3) . . ?
C94 N7 C95 114(3) . . ?
C83 N7 C95 105(2) . . ?
C94 N7 K4 106.4(19) . . ?
C83 N7 K4 110(2) . . ?
C95 N7 K4 109.5(19) . . ?
C86 O8 C87 112(3) . . ?
C86 O8 K4 114.2(18) . . ?
C87 O8 K4 113(3) . . ?
C23 C22 C21 124(3) . . ?
C23 C22 C30 117(3) . . ?
C21 C22 C30 118(3) . . ?
C25 C24 C23 122(3) . . ?
C90 O9 C91 113(3) . . ?
C90 O9 K4 119(2) . . ?
C91 O9 K4 113.6(18) . . ?
C93 O10 C92 112(3) . . ?
C93 O10 K4 113.2(19) . . ?
C92 O10 K4 111(2) . . ?
C35 C36 C37 116(3) . . ?
C35 C36 C42 121(3) . . ?
C37 C36 C42 122(3) . . ?
O2 C68 C67 111(3) . . ?
O2 C68 K3 46.3(13) . . ?
C67 C68 K3 78.1(15) . . ?
C22 C23 C24 118(3) . . ?
C36 C35 C34 122(3) . . ?
C37 C38 C33 122(2) . . ?
C37 C38 C39 117(3) . . ?
C33 C38 C39 121(2) . . ?
N6 C70 C69 111(2) . . ?
N4 C52 C51 125(3) . . ?
N4 C52 N3 116(2) . . ?
C51 C52 N3 120(2) . . ?
C1 C2 C13 126(3) . . ?
C1 C2 C3 112(3) . . ?
C13 C2 C3 122(3) . . ?
N7 C94 C93 116(3) . . ?
N2 C21 C22 123(2) . . ?
N2 C21 C26 122(2) . . ?
C22 C21 C26 115(3) . . ?
C19 C18 C17 119(3) . . ?
N5 C65 C66 114(3) . . ?
C75 O4 C74 118(3) . . ?
C75 O4 K3 111(3) . . ?
C74 O4 K3 111(2) . . ?
C98 O12 C99 106(3) . . ?
C98 O12 K4 123(2) . . ?
C99 O12 K4 118(3) . . ?
C26 C27 C29 110(3) . . ?
C26 C27 C28 109(3) . . ?
C29 C27 C28 106(3) . . ?
N5 C77 C78 115(3) . . ?
C81 C82 N6 115(3) . . ?
C38 C37 C36 120(3) . . ?
C72 C71 N6 114(3) . . ?
C9 C7 C8 108(3) . . ?
C9 C7 C6 110(4) . . ?
C8 C7 C6 113(3) . . ?
N1 C16 C17 112(3) . . ?
N1 C16 C1 120(3) . . ?
C17 C16 C1 126(3) . . ?
C75 C76 N5 109(3) . . ?
C56 C55 C54 124(3) . . ?
C95 C96 O11 109(3) . . ?
C32 C30 C31 110(3) . . ?
C32 C30 C22 116(3) . . ?
C31 C30 C22 106(3) . . ?
C46 C45 C34 113(3) . . ?
C46 C45 C47 105(3) . . ?
C34 C45 C47 108(3) . . ?
C55 C56 C57 121(3) . . ?
C24 C25 C26 120(3) . . ?
O11 C97 C98 102(3) . . ?
C4 C5 C6 120(4) . . ?
O5 C80 C79 108(3) . . ?
C92 C91 O9 108(3) . . ?
C51 C50 C49 115(2) . . ?
C82 C81 O5 107(2) . . ?
O6 C79 C80 112(2) . . ?
C25 C26 C21 120(3) . . ?
C25 C26 C27 121(3) . . ?
C21 C26 C27 118(3) . . ?
C61 C59 C58 114(3) . . ?
C61 C59 C60 109(3) . . ?
C58 C59 C60 114(3) . . ?
O7 C84 C83 107(2) . . ?
O7 C85 C86 104(3) . . ?
C87 C88 N8 121(4) . . ?
C58 C57 C56 115(3) . . ?
C71 C72 O3 106(3) . . ?
O2 C69 C70 110(2) . . ?
C96 C95 N7 109(3) . . ?
C77 N5 C76 110(3) . . ?
C77 N5 C65 105(3) . . ?
C76 N5 C65 109(3) . . ?
C77 N5 K3 112(2) . . ?
C76 N5 K3 112(2) . . ?
C65 N5 K3 109(2) . . ?
C89 N8 C88 105(3) . . ?
C89 N8 C100 112(3) . . ?
C88 N8 C100 112(4) . . ?
C89 N8 K4 104(3) . . ?
C88 N8 K4 109(2) . . ?
C100 N8 K4 115(3) . . ?
C38 C39 C40 115(3) . . ?
C38 C39 C41 113(3) . . ?
C40 C39 C41 109(3) . . ?
C2 C13 C14 120(3) . . ?
C2 C13 C15 111(3) . . ?
C14 C13 C15 106(4) . . ?
O4 C75 C76 122(4) . . ?
O4 C75 K3 50(2) . . ?
C76 C75 K3 88.3(18) . . ?
O9 C90 C89 107(3) . . ?
O6 C78 C77 109(3) . . ?
O1 C67 C68 105(2) . . ?
O4 C74 C73 110(4) . . ?
N8 C89 C90 117(4) . . ?
O8 C86 C85 110(3) . . ?
C3 C4 C5 120(5) . . ?
C3 C4 C10 122(5) . . ?
C5 C4 C10 118(5) . . ?
C45 C47 W2 115(2) . . ?
N1 C20 C19 121(3) . . ?
N1 C20 N2 116(2) . . ?
C19 C20 N2 123(3) . . ?
O1 C66 C65 109(3) . . ?
O3 C73 C74 117(4) . . ?
C43 C42 C36 116(3) . . ?
C43 C42 C44 112(4) . . ?
C36 C42 C44 108(3) . . ?
C1 C6 C5 121(3) . . ?
C1 C6 C7 122(3) . . ?
C5 C6 C7 117(3) . . ?
N7 C83 C84 116(3) . . ?
C100 C99 O12 104(4) . . ?
C12 C10 C4 119(6) . . ?
C12 C10 C11 103(6) . . ?
C4 C10 C11 110(5) . . ?
O10 C93 C94 107(3) . . ?
C4 C3 C2 125(4) . . ?
C88 C87 O8 115(4) . . ?
O12 C98 C97 106(3) . . ?
N8 C100 C99 112(4) . . ?

_refine_diff_density_max         2.224
_refine_diff_density_min         -1.907
_refine_diff_density_rms         0.180



