#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:19:44 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180257 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/43/7114378.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7114378
loop_
_publ_author_name
'Gibson, Vernon C.'
'Redshaw, Carl'
'Elsegood, Mark R. J.'
_publ_section_title
;
 Novel tungsten calix[8]arene complexesElectronic supplementary
 information (ESI) available: selected spectroscopic data. See
 http://www.rsc.org/suppdata/cc/b2/b201777f/
;
_journal_issue                   11
_journal_name_full               'Chemical Communications'
_journal_page_first              1200
_journal_paper_doi               10.1039/b201777f
_journal_year                    2002
_chemical_formula_sum            'C96 H124 Cl24 O10 W4'
_chemical_formula_weight         3024.15
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.937(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.9255(8)
_cell_length_b                   24.9463(14)
_cell_length_c                   18.0215(10)
_cell_measurement_reflns_used    28055
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      29.45
_cell_measurement_theta_min      3.10
_cell_volume                     5956.2(6)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6884
_diffrn_reflns_av_R_equivalents  0.0943
_diffrn_reflns_av_sigmaI/netI    0.0663
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36959
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.438
_exptl_absorpt_correction_T_max  0.809
_exptl_absorpt_correction_T_min  0.777
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2968
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         5.845
_refine_diff_density_min         -4.124
_refine_diff_density_rms         0.428
_refine_ls_extinction_coef       0.0037(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.538
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     753
_refine_ls_number_reflns         8539
_refine_ls_number_restraints     451
_refine_ls_restrained_S_all      1.505
_refine_ls_R_factor_all          0.1449
_refine_ls_R_factor_gt           0.1256
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3664
_refine_ls_wR_factor_ref         0.3744
_reflns_number_gt                6438
_reflns_number_total             8539
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b201777f.txt
_cod_data_source_block           4.4C2H4Cl2.2H2O
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7114378
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'
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 0.0391(12) 0.7321(6) 0.5505(5) 0.0287(16) Uani 0.56(5) 1 d PDU A 1
Cl1 Cl 0.063(3) 0.7457(14) 0.6842(9) 0.060(6) Uani 0.56(5) 1 d PDU A 1
Cl2 Cl 0.2062(16) 0.7526(13) 0.570(2) 0.060(5) Uani 0.56(5) 1 d PDU A 1
Cl3 Cl 0.084(2) 0.6446(8) 0.5841(15) 0.046(5) Uani 0.56(5) 1 d PDU A 1
Cl4 Cl 0.001(2) 0.8229(7) 0.5290(15) 0.051(5) Uani 0.56(5) 1 d PDU A 1
W1X W 0.0176(14) 0.7405(5) 0.5515(6) 0.0229(17) Uani 0.44(5) 1 d PDU A 2
Cl1X Cl 0.044(4) 0.7582(13) 0.6847(10) 0.046(6) Uani 0.44(5) 1 d PDU A 2
Cl2X Cl 0.1843(19) 0.7585(14) 0.566(3) 0.047(5) Uani 0.44(5) 1 d PDU A 2
Cl3X Cl 0.062(3) 0.6536(8) 0.590(2) 0.046(6) Uani 0.44(5) 1 d PDU A 2
Cl4X Cl -0.019(3) 0.8312(8) 0.525(2) 0.054(6) Uani 0.44(5) 1 d PDU A 2
W2 W -0.21776(11) 0.51538(5) 0.52655(7) 0.0709(6) Uani 1 1 d U . .
Cl5 Cl -0.1656(14) 0.4597(4) 0.4447(7) 0.163(5) Uani 1 1 d U . .
Cl6 Cl -0.1770(7) 0.5853(3) 0.4614(5) 0.086(2) Uani 1 1 d U . .
Cl7 Cl -0.0524(6) 0.5179(4) 0.6130(8) 0.109(3) Uani 1 1 d U . .
Cl8 Cl -0.3760(10) 0.5124(4) 0.4413(6) 0.130(4) Uani 1 1 d U . .
O1 O 0.0084(11) 0.7167(6) 0.4503(7) 0.037(3) Uani 1 1 d . . .
O2 O -0.1026(12) 0.7196(6) 0.5374(8) 0.044(4) Uani 1 1 d . . .
O3 O -0.2538(13) 0.5610(6) 0.5952(9) 0.052(4) Uani 1 1 d . . .
O4 O -0.2366(12) 0.4550(6) 0.5782(9) 0.051(4) Uani 1 1 d . . .
C1 C -0.0472(15) 0.6870(8) 0.3850(11) 0.037(5) Uani 1 1 d . A .
C2 C 0.0004(17) 0.6473(8) 0.3590(10) 0.037(5) Uani 1 1 d . . .
C3 C -0.0582(19) 0.6151(9) 0.3013(13) 0.049(6) Uani 1 1 d . A .
H3 H -0.0267 0.5870 0.2819 0.059 Uiso 1 1 calc R . .
C4 C -0.161(2) 0.6219(9) 0.2700(11) 0.054(7) Uani 1 1 d . . .
C5 C -0.2027(18) 0.6685(9) 0.2950(12) 0.050(6) Uani 1 1 d . A .
H5 H -0.2715 0.6771 0.2698 0.059 Uiso 1 1 calc R . .
C6 C -0.1498(19) 0.6999(8) 0.3515(13) 0.045(5) Uani 1 1 d . . .
C7 C -0.229(3) 0.5826(11) 0.2031(16) 0.080(7) Uani 1 1 d DU A .
C8 C -0.200(4) 0.583(2) 0.140(2) 0.111(12) Uani 0.82(5) 1 d PDU A 1
H8A H -0.1357 0.5638 0.1510 0.167 Uiso 0.82(5) 1 calc PR A 1
H8B H -0.1915 0.6200 0.1256 0.167 Uiso 0.82(5) 1 calc PR A 1
H8C H -0.2512 0.5652 0.0975 0.167 Uiso 0.82(5) 1 calc PR A 1
C9 C -0.328(3) 0.589(2) 0.181(3) 0.109(12) Uani 0.82(5) 1 d PDU A 1
H9A H -0.3468 0.6199 0.1458 0.163 Uiso 0.82(5) 1 calc PR A 1
H9B H -0.3495 0.5961 0.2276 0.163 Uiso 0.82(5) 1 calc PR A 1
H9C H -0.3614 0.5568 0.1550 0.163 Uiso 0.82(5) 1 calc PR A 1
C10 C -0.206(3) 0.5259(12) 0.241(3) 0.093(14) Uani 0.82(5) 1 d PDU A 1
H10A H -0.1325 0.5211 0.2625 0.139 Uiso 0.82(5) 1 calc PR A 1
H10B H -0.2337 0.4984 0.2015 0.139 Uiso 0.82(5) 1 calc PR A 1
H10C H -0.2363 0.5226 0.2831 0.139 Uiso 0.82(5) 1 calc PR A 1
C8X C -0.248(13) 0.611(5) 0.138(5) 0.09(2) Uani 0.18(5) 1 d PDU A 2
H8D H -0.1849 0.6168 0.1259 0.142 Uiso 0.18(5) 1 calc PR A 2
H8E H -0.2771 0.6455 0.1454 0.142 Uiso 0.18(5) 1 calc PR A 2
H8F H -0.2957 0.5913 0.0954 0.142 Uiso 0.18(5) 1 calc PR A 2
C9X C -0.318(7) 0.567(7) 0.208(10) 0.10(2) Uani 0.18(5) 1 d PDU A 2
H9D H -0.3690 0.5939 0.1853 0.147 Uiso 0.18(5) 1 calc PR A 2
H9E H -0.3129 0.5617 0.2634 0.147 Uiso 0.18(5) 1 calc PR A 2
H9F H -0.3370 0.5327 0.1805 0.147 Uiso 0.18(5) 1 calc PR A 2
C10X C -0.175(11) 0.531(5) 0.187(9) 0.09(2) Uani 0.18(5) 1 d PDU A 2
H10D H -0.1043 0.5388 0.1925 0.136 Uiso 0.18(5) 1 calc PR A 2
H10E H -0.2091 0.5175 0.1347 0.136 Uiso 0.18(5) 1 calc PR A 2
H10F H -0.1774 0.5029 0.2255 0.136 Uiso 0.18(5) 1 calc PR A 2
C11 C -0.1983(19) 0.7469(9) 0.3796(12) 0.044(5) Uani 1 1 d . A .
H11A H -0.2458 0.7655 0.3346 0.053 Uiso 1 1 calc R . .
H11B H -0.1459 0.7728 0.4079 0.053 Uiso 1 1 calc R . .
C12 C -0.2004(15) 0.7107(8) 0.5107(11) 0.032(4) Uani 1 1 d . A .
C13 C -0.2560(18) 0.7249(8) 0.4349(12) 0.040(5) Uani 1 1 d . . .
C14 C -0.3588(18) 0.7147(10) 0.4108(12) 0.050(6) Uani 1 1 d . A .
H14 H -0.3971 0.7245 0.3592 0.060 Uiso 1 1 calc R . .
C15 C -0.4063(18) 0.6920(10) 0.4561(16) 0.060(7) Uani 1 1 d . . .
C16 C -0.3440(18) 0.6750(8) 0.5391(13) 0.043(5) Uani 1 1 d . A .
H16 H -0.3763 0.6585 0.5726 0.052 Uiso 1 1 calc R . .
C17 C -0.2454(14) 0.6832(7) 0.5636(12) 0.031(4) Uani 1 1 d . . .
C18 C -0.5197(19) 0.6804(11) 0.4315(13) 0.077(7) Uani 1 1 d DU A .
C19 C -0.578(3) 0.695(2) 0.350(2) 0.078(13) Uani 0.52(4) 1 d PDU A 1
H19A H -0.5493 0.6764 0.3139 0.117 Uiso 0.52(4) 1 calc PR A 1
H19B H -0.5760 0.7335 0.3432 0.117 Uiso 0.52(4) 1 calc PR A 1
H19C H -0.6487 0.6832 0.3399 0.117 Uiso 0.52(4) 1 calc PR A 1
C20 C -0.533(5) 0.611(2) 0.441(3) 0.098(18) Uani 0.52(4) 1 d PDU A 1
H20A H -0.5047 0.5917 0.4049 0.147 Uiso 0.52(4) 1 calc PR A 1
H20B H -0.6052 0.6017 0.4282 0.147 Uiso 0.52(4) 1 calc PR A 1
H20C H -0.4980 0.5996 0.4945 0.147 Uiso 0.52(4) 1 calc PR A 1
C21 C -0.565(3) 0.706(2) 0.487(2) 0.071(11) Uani 0.52(4) 1 d PDU A 1
H21A H -0.5282 0.6946 0.5406 0.106 Uiso 0.52(4) 1 calc PR A 1
H21B H -0.6359 0.6954 0.4748 0.106 Uiso 0.52(4) 1 calc PR A 1
H21C H -0.5607 0.7451 0.4835 0.106 Uiso 0.52(4) 1 calc PR A 1
C19X C -0.577(3) 0.7311(17) 0.420(4) 0.077(13) Uani 0.48(4) 1 d PDU A 2
H19D H -0.5476 0.7565 0.3916 0.116 Uiso 0.48(4) 1 calc PR A 2
H19E H -0.5741 0.7462 0.4708 0.116 Uiso 0.48(4) 1 calc PR A 2
H19F H -0.6475 0.7241 0.3898 0.116 Uiso 0.48(4) 1 calc PR A 2
C20X C -0.534(4) 0.652(2) 0.339(3) 0.082(15) Uani 0.48(4) 1 d PDU A 2
H20D H -0.4944 0.6188 0.3452 0.123 Uiso 0.48(4) 1 calc PR A 2
H20E H -0.5093 0.6774 0.3073 0.123 Uiso 0.48(4) 1 calc PR A 2
H20F H -0.6051 0.6441 0.3129 0.123 Uiso 0.48(4) 1 calc PR A 2
C21X C -0.553(5) 0.640(2) 0.477(3) 0.091(16) Uani 0.48(4) 1 d PDU A 2
H21D H -0.5195 0.6055 0.4745 0.137 Uiso 0.48(4) 1 calc PR A 2
H21E H -0.6264 0.6350 0.4559 0.137 Uiso 0.48(4) 1 calc PR A 2
H21F H -0.5358 0.6512 0.5317 0.137 Uiso 0.48(4) 1 calc PR A 2
C22 C -0.1766(17) 0.6659(9) 0.6388(13) 0.044(5) Uani 1 1 d . A .
H22A H -0.1462 0.6980 0.6694 0.053 Uiso 1 1 calc R . .
H22B H -0.1213 0.6447 0.6295 0.053 Uiso 1 1 calc R . .
C23 C -0.2661(19) 0.5823(8) 0.6601(12) 0.044(5) Uani 1 1 d . A .
C24 C -0.2272(17) 0.6321(8) 0.6872(12) 0.041(5) Uani 1 1 d . . .
C25 C -0.237(2) 0.6524(10) 0.7532(15) 0.064(7) Uani 1 1 d . A .
H25 H -0.2135 0.6875 0.7696 0.077 Uiso 1 1 calc R . .
C26 C -0.284(2) 0.6208(10) 0.7986(15) 0.059(7) Uani 1 1 d . . .
C27 C -0.3161(18) 0.5700(10) 0.7755(13) 0.050(6) Uani 1 1 d . A .
H27 H -0.3423 0.5481 0.8079 0.059 Uiso 1 1 calc R . .
C28 C -0.3105(17) 0.5499(8) 0.7043(13) 0.043(5) Uani 1 1 d . . .
C29 C -0.294(3) 0.6437(13) 0.8766(18) 0.085(10) Uani 1 1 d . A .
C30 C -0.179(3) 0.6475(15) 0.9380(16) 0.088(10) Uani 1 1 d . . .
H30A H -0.1505 0.6114 0.9489 0.132 Uiso 1 1 calc R A .
H30B H -0.1812 0.6642 0.9867 0.132 Uiso 1 1 calc R . .
H30C H -0.1370 0.6692 0.9149 0.132 Uiso 1 1 calc R . .
C31 C -0.337(3) 0.6979(12) 0.8603(16) 0.076(8) Uani 1 1 d . . .
H31A H -0.3405 0.7143 0.9088 0.114 Uiso 1 1 calc R A .
H31B H -0.4048 0.6958 0.8228 0.114 Uiso 1 1 calc R . .
H31C H -0.2937 0.7197 0.8384 0.114 Uiso 1 1 calc R . .
C32 C -0.360(2) 0.6115(13) 0.9114(15) 0.076(9) Uani 1 1 d . . .
H32A H -0.3323 0.5752 0.9224 0.115 Uiso 1 1 calc R A .
H32B H -0.4283 0.6097 0.8746 0.115 Uiso 1 1 calc R . .
H32C H -0.3619 0.6284 0.9600 0.115 Uiso 1 1 calc R . .
C33 C -0.3513(19) 0.4928(8) 0.6764(14) 0.048(6) Uani 1 1 d . A .
H33A H -0.4080 0.4847 0.6968 0.058 Uiso 1 1 calc R . .
H33B H -0.3784 0.4929 0.6187 0.058 Uiso 1 1 calc R . .
C34 C -0.2222(16) 0.4297(7) 0.6479(11) 0.034(5) Uani 1 1 d U A .
C35 C -0.2741(17) 0.4486(7) 0.7011(13) 0.040(5) Uani 1 1 d . . .
C36 C -0.261(2) 0.4238(9) 0.7680(13) 0.052(6) Uani 1 1 d . A .
H36 H -0.2965 0.4359 0.8019 0.063 Uiso 1 1 calc R . .
C37 C -0.1975(18) 0.3817(10) 0.7898(13) 0.049(6) Uani 1 1 d . . .
C38 C -0.1496(19) 0.3616(9) 0.7362(13) 0.049(6) Uani 1 1 d . A .
H38 H -0.1080 0.3307 0.7502 0.059 Uiso 1 1 calc R . .
C39 C -0.1607(17) 0.3841(8) 0.6680(12) 0.039(5) Uani 1 1 d . . .
C40 C -0.169(2) 0.3524(10) 0.8717(14) 0.078(6) Uani 1 1 d DU A .
C41 C -0.103(4) 0.3019(19) 0.881(3) 0.083(10) Uani 0.53(3) 1 d PDU A 1
H41A H -0.0914 0.2867 0.9330 0.125 Uiso 0.53(3) 1 calc PR A 1
H41B H -0.0377 0.3113 0.8740 0.125 Uiso 0.53(3) 1 calc PR A 1
H41C H -0.1370 0.2754 0.8415 0.125 Uiso 0.53(3) 1 calc PR A 1
C42 C -0.280(4) 0.332(2) 0.879(3) 0.085(11) Uani 0.53(3) 1 d PDU A 1
H42A H -0.2699 0.3137 0.9283 0.127 Uiso 0.53(3) 1 calc PR A 1
H42B H -0.3121 0.3080 0.8354 0.127 Uiso 0.53(3) 1 calc PR A 1
H42C H -0.3236 0.3636 0.8760 0.127 Uiso 0.53(3) 1 calc PR A 1
C43 C -0.125(5) 0.394(2) 0.937(3) 0.090(11) Uani 0.53(3) 1 d PDU A 1
H43A H -0.1083 0.3760 0.9875 0.134 Uiso 0.53(3) 1 calc PR A 1
H43B H -0.1743 0.4221 0.9335 0.134 Uiso 0.53(3) 1 calc PR A 1
H43C H -0.0631 0.4094 0.9300 0.134 Uiso 0.53(3) 1 calc PR A 1
C41X C -0.211(5) 0.2955(18) 0.861(3) 0.078(10) Uani 0.47(3) 1 d PDU A 2
H41D H -0.1953 0.2777 0.9116 0.116 Uiso 0.47(3) 1 calc PR A 2
H41E H -0.1809 0.2753 0.8269 0.116 Uiso 0.47(3) 1 calc PR A 2
H41F H -0.2845 0.2969 0.8367 0.116 Uiso 0.47(3) 1 calc PR A 2
C42X C -0.217(5) 0.386(2) 0.932(3) 0.091(12) Uani 0.47(3) 1 d PDU A 2
H42D H -0.1910 0.4229 0.9374 0.136 Uiso 0.47(3) 1 calc PR A 2
H42E H -0.1970 0.3685 0.9829 0.136 Uiso 0.47(3) 1 calc PR A 2
H42F H -0.2905 0.3866 0.9103 0.136 Uiso 0.47(3) 1 calc PR A 2
C43X C -0.053(3) 0.354(3) 0.906(3) 0.089(11) Uani 0.47(3) 1 d PDU A 2
H43D H -0.0301 0.3912 0.9123 0.134 Uiso 0.47(3) 1 calc PR A 2
H43E H -0.0229 0.3354 0.8706 0.134 Uiso 0.47(3) 1 calc PR A 2
H43F H -0.0326 0.3359 0.9568 0.134 Uiso 0.47(3) 1 calc PR A 2
C44 C -0.1112(19) 0.3622(9) 0.6077(12) 0.047(6) Uani 1 1 d . . .
H44A H -0.1445 0.3280 0.5861 0.057 Uiso 1 1 calc R . .
H44B H -0.1232 0.3880 0.5641 0.057 Uiso 1 1 calc R . .
Cl9 Cl -0.0680(16) 0.3469(6) 1.1590(9) 0.184(7) Uani 1 1 d DU . .
C45 C -0.059(4) 0.4099(13) 1.189(3) 0.187(15) Uani 1 1 d DU . .
H45A H -0.1223 0.4289 1.1617 0.224 Uiso 1 1 calc R . .
H45B H -0.0516 0.4104 1.2457 0.224 Uiso 1 1 calc R . .
C46 C 0.021(4) 0.4368(16) 1.177(3) 0.199(17) Uani 1 1 d DU . .
H46A H 0.0691 0.4099 1.1695 0.239 Uiso 1 1 calc R . .
H46B H 0.0553 0.4570 1.2252 0.239 Uiso 1 1 calc R . .
Cl10 Cl -0.006(3) 0.4789(13) 1.103(3) 0.344(18) Uani 1 1 d DU . .
Cl11 Cl 0.0369(18) 0.1175(13) 0.8130(15) 0.157(11) Uani 0.50 1 d PDU . .
C47 C 0.158(3) 0.130(2) 0.828(4) 0.16(2) Uani 0.50 1 d PDU . .
H47A H 0.1966 0.1226 0.8829 0.192 Uiso 0.50 1 calc PR . .
H47B H 0.1844 0.1059 0.7947 0.192 Uiso 0.50 1 calc PR . .
C48 C 0.174(4) 0.182(3) 0.811(6) 0.17(2) Uani 0.50 1 d PDU . .
H48A H 0.1979 0.1834 0.7642 0.208 Uiso 0.50 1 calc PR . .
H48B H 0.2271 0.1984 0.8549 0.208 Uiso 0.50 1 calc PR . .
Cl12 Cl 0.068(3) 0.2179(16) 0.793(4) 0.28(2) Uani 0.50 1 d PDU . .
Cl13 Cl -0.383(2) 0.4680(7) 0.9649(19) 0.263(13) Uani 1 1 d DU . .
C49 C -0.470(6) 0.486(3) 1.006(6) 0.26(3) Uani 1 1 d DU . .
H49A H -0.5046 0.4515 1.0097 0.318 Uiso 1 1 calc R . .
H49B H -0.4299 0.4943 1.0606 0.318 Uiso 1 1 calc R . .
O1W O 0.1526(14) 0.1182(7) 0.6815(13) 0.078(6) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
O1 W1 O2 85.7(8) . .
O1 W1 Cl3 91.3(9) . .
O2 W1 Cl3 93.5(9) . .
O1 W1 Cl2 96.9(13) . .
O2 W1 Cl2 175.9(12) . .
Cl3 W1 Cl2 89.6(7) . .
O1 W1 Cl4 94.1(9) . .
O2 W1 Cl4 88.1(9) . .
Cl3 W1 Cl4 174.5(7) . .
Cl2 W1 Cl4 88.6(5) . .
O1 W1 Cl1 172.8(11) . .
O2 W1 Cl1 87.9(11) . .
Cl3 W1 Cl1 85.8(6) . .
Cl2 W1 Cl1 89.7(7) . .
Cl4 W1 Cl1 89.0(6) . .
O2 W1X O1 89.3(8) . .
O2 W1X Cl2X 173.0(12) . .
O1 W1X Cl2X 86.5(14) . .
O2 W1X Cl3X 85.1(11) . .
O1 W1X Cl3X 85.7(10) . .
Cl2X W1X Cl3X 89.0(8) . .
O2 W1X Cl4X 97.2(12) . .
O1 W1X Cl4X 99.5(10) . .
Cl2X W1X Cl4X 89.1(7) . .
Cl3X W1X Cl4X 174.3(10) . .
O2 W1X Cl1X 92.9(14) . .
O1 W1X Cl1X 171.0(10) . .
Cl2X W1X Cl1X 90.4(7) . .
Cl3X W1X Cl1X 85.8(6) . .
Cl4X W1X Cl1X 88.9(7) . .
O4 W2 O3 93.1(7) . .
O4 W2 Cl8 93.2(5) . .
O3 W2 Cl8 93.8(6) . .
O4 W2 Cl6 173.0(5) . .
O3 W2 Cl6 92.0(5) . .
Cl8 W2 Cl6 91.2(4) . .
O4 W2 Cl5 87.3(5) . .
O3 W2 Cl5 177.4(7) . .
Cl8 W2 Cl5 88.8(6) . .
Cl6 W2 Cl5 87.4(3) . .
O4 W2 Cl7 87.1(5) . .
O3 W2 Cl7 87.3(6) . .
Cl8 W2 Cl7 178.9(5) . .
Cl6 W2 Cl7 88.4(3) . .
Cl5 W2 Cl7 90.2(6) . .
C1 O1 W1 150.4(13) . .
C1 O1 W1X 146.4(14) . .
W1 O1 W1X 11.0(4) . .
C12 O2 W1X 165.7(15) . .
C12 O2 W1 166.3(13) . .
W1X O2 W1 8.9(5) . .
C23 O3 W2 162.6(15) . .
C34 O4 W2 147.7(13) . .
C2 C1 O1 118.2(18) . .
C2 C1 C6 124.2(19) . .
O1 C1 C6 117.6(19) . .
C1 C2 C3 117(2) . .
C1 C2 C44 122.2(18) . 3_566
C3 C2 C44 120.9(19) . 3_566
C2 C3 C4 123(2) . .
C3 C4 C5 116(2) . .
C3 C4 C7 122(2) . .
C5 C4 C7 122(2) . .
C6 C5 C4 123(2) . .
C5 C6 C1 117(2) . .
C5 C6 C11 121(2) . .
C1 C6 C11 122(2) . .
C8 C7 C8X 43(6) . .
C8 C7 C9 108(4) . .
C8X C7 C9 76(7) . .
C8 C7 C9X 127(8) . .
C8X C7 C9X 107(5) . .
C9 C7 C9X 32(7) . .
C8 C7 C10 108(4) . .
C8X C7 C10 146(7) . .
C9 C7 C10 107(4) . .
C9X C7 C10 77(8) . .
C8 C7 C10X 64(7) . .
C8X C7 C10X 105(5) . .
C9 C7 C10X 124(7) . .
C9X C7 C10X 106(4) . .
C10 C7 C10X 44(6) . .
C8 C7 C4 112(3) . .
C8X C7 C4 104(7) . .
C9 C7 C4 117(3) . .
C9X C7 C4 118(8) . .
C10 C7 C4 103(2) . .
C10X C7 C4 116(6) . .
C6 C11 C13 108.2(18) . .
O2 C12 C13 121.0(18) . .
O2 C12 C17 116.3(17) . .
C13 C12 C17 122.6(18) . .
C14 C13 C12 118.0(19) . .
C14 C13 C11 123.4(19) . .
C12 C13 C11 118(2) . .
C15 C14 C13 123(2) . .
C14 C15 C18 125(2) . .
C14 C15 C16 119(2) . .
C18 C15 C16 117(2) . .
C17 C16 C15 120(2) . .
C16 C17 C12 117.6(19) . .
C16 C17 C22 125.4(19) . .
C12 C17 C22 116.9(17) . .
C21X C18 C19X 115(3) . .
C21X C18 C19 123(4) . .
C19X C18 C19 63(3) . .
C21X C18 C21 69(3) . .
C19X C18 C21 53(3) . .
C19 C18 C21 110(3) . .
C21X C18 C15 116(3) . .
C19X C18 C15 110(3) . .
C19 C18 C15 117(3) . .
C21 C18 C15 110(2) . .
C21X C18 C20 37(3) . .
C19X C18 C20 142(3) . .
C19 C18 C20 107(2) . .
C21 C18 C20 106(2) . .
C15 C18 C20 107(3) . .
C21X C18 C20X 107(2) . .
C19X C18 C20X 108(2) . .
C19 C18 C20X 45(3) . .
C21 C18 C20X 150(3) . .
C15 C18 C20X 99(3) . .
C20 C18 C20X 73(2) . .
C17 C22 C24 114.0(19) . .
O3 C23 C24 122(2) . .
O3 C23 C28 117.5(19) . .
C24 C23 C28 120.6(18) . .
C25 C24 C23 121(2) . .
C25 C24 C22 119(2) . .
C23 C24 C22 119.4(19) . .
C24 C25 C26 119(2) . .
C27 C26 C25 120(2) . .
C27 C26 C29 120(2) . .
C25 C26 C29 120(2) . .
C26 C27 C28 120(2) . .
C27 C28 C23 118(2) . .
C27 C28 C33 120.3(19) . .
C23 C28 C33 121.5(18) . .
C31 C29 C32 109(3) . .
C31 C29 C26 107(3) . .
C32 C29 C26 115(2) . .
C31 C29 C30 109(3) . .
C32 C29 C30 110(3) . .
C26 C29 C30 106(2) . .
C35 C33 C28 115(2) . .
O4 C34 C39 121.2(17) . .
O4 C34 C35 119.9(17) . .
C39 C34 C35 118.9(16) . .
C36 C35 C34 119.6(19) . .
C36 C35 C33 120.2(19) . .
C34 C35 C33 119.9(18) . .
C35 C36 C37 122(2) . .
C36 C37 C38 118(2) . .
C36 C37 C40 126(2) . .
C38 C37 C40 116(2) . .
C39 C38 C37 123(2) . .
C38 C39 C34 118(2) . .
C38 C39 C44 124(2) . .
C34 C39 C44 118.1(17) . .
C41X C40 C43X 113(3) . .
C41X C40 C41 56(3) . .
C43X C40 C41 57(4) . .
C41X C40 C43 140(3) . .
C43X C40 C43 64(3) . .
C41 C40 C43 113(3) . .
C41X C40 C37 109(3) . .
C43X C40 C37 107(3) . .
C41 C40 C37 117(2) . .
C43 C40 C37 109(3) . .
C41X C40 C42X 110(2) . .
C43X C40 C42X 108(2) . .
C41 C40 C42X 134(3) . .
C43 C40 C42X 47(3) . .
C37 C40 C42X 110(3) . .
C41X C40 C42 53(3) . .
C43X C40 C42 149(3) . .
C41 C40 C42 106(2) . .
C43 C40 C42 108(2) . .
C37 C40 C42 103(2) . .
C42X C40 C42 62(2) . .
C2 C44 C39 113.6(18) 3_566 .
C46 C45 Cl9 113(3) . .
C45 C46 Cl10 117(3) . .
C48 C47 Cl11 112(2) . .
C47 C48 Cl12 110.9(19) . .
C49 C49 Cl13 135(10) 3_467 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O1 1.766(16) .
W1 O2 1.94(2) .
W1 Cl3 2.298(10) .
W1 Cl2 2.301(11) .
W1 Cl4 2.330(10) .
W1 Cl1 2.354(11) .
W1X O2 1.70(2) .
W1X O1 1.887(17) .
W1X Cl2X 2.297(13) .
W1X Cl3X 2.302(12) .
W1X Cl4X 2.335(12) .
W1X Cl1X 2.353(13) .
W2 O4 1.831(17) .
W2 O3 1.861(16) .
W2 Cl8 2.266(11) .
W2 Cl6 2.271(7) .
W2 Cl5 2.301(9) .
W2 Cl7 2.351(10) .
O1 C1 1.40(2) .
O2 C12 1.32(2) .
O3 C23 1.34(2) .
O4 C34 1.37(2) .
C1 C2 1.35(3) .
C1 C6 1.41(3) .
C2 C3 1.37(3) .
C2 C44 1.49(3) 3_566
C3 C4 1.38(4) .
C4 C5 1.43(3) .
C4 C7 1.61(3) .
C5 C6 1.32(3) .
C6 C11 1.52(3) .
C7 C8 1.31(5) .
C7 C8X 1.32(6) .
C7 C9 1.32(5) .
C7 C9X 1.33(5) .
C7 C10 1.56(4) .
C7 C10X 1.57(5) .
C11 C13 1.56(3) .
C12 C13 1.39(3) .
C12 C17 1.46(3) .
C13 C14 1.38(3) .
C14 C15 1.33(4) .
C15 C18 1.53(3) .
C15 C16 1.54(3) .
C16 C17 1.32(3) .
C17 C22 1.46(3) .
C18 C21X 1.47(3) .
C18 C19X 1.48(3) .
C18 C19 1.48(3) .
C18 C21 1.49(3) .
C18 C20 1.77(5) .
C18 C20X 1.77(5) .
C22 C24 1.53(3) .
C23 C24 1.38(3) .
C23 C28 1.41(3) .
C24 C25 1.34(3) .
C25 C26 1.43(4) .
C26 C27 1.37(3) .
C26 C29 1.57(3) .
C27 C28 1.40(3) .
C28 C33 1.56(3) .
C29 C31 1.47(4) .
C29 C32 1.49(4) .
C29 C30 1.65(5) .
C33 C35 1.51(3) .
C34 C39 1.40(3) .
C34 C35 1.45(3) .
C35 C36 1.32(3) .
C36 C37 1.35(3) .
C37 C38 1.42(3) .
C37 C40 1.58(3) .
C38 C39 1.32(3) .
C39 C44 1.56(3) .
C40 C41X 1.53(4) .
C40 C43X 1.53(4) .
C40 C41 1.54(4) .
C40 C43 1.54(4) .
C40 C42X 1.67(5) .
C40 C42 1.67(5) .
C44 C2 1.49(3) 3_566
Cl9 C45 1.66(3) .
C45 C46 1.37(6) .
C46 Cl10 1.65(3) .
Cl11 C47 1.66(3) .
C47 C48 1.37(6) .
C48 Cl12 1.66(3) .
Cl13 C49 1.66(3) .
C49 C49 1.07(14) 3_467
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O2 W1 O1 C1 -36(3) . .
Cl3 W1 O1 C1 57(3) . .
Cl2 W1 O1 C1 147(3) . .
Cl4 W1 O1 C1 -124(3) . .
Cl1 W1 O1 C1 -8(10) . .
O2 W1 O1 W1X 42(3) . .
Cl3 W1 O1 W1X 135(3) . .
Cl2 W1 O1 W1X -135(3) . .
Cl4 W1 O1 W1X -46(3) . .
Cl1 W1 O1 W1X 69(8) . .
O2 W1X O1 C1 -11(3) . .
Cl2X W1X O1 C1 163(2) . .
Cl3X W1X O1 C1 74(2) . .
Cl4X W1X O1 C1 -109(2) . .
Cl1X W1X O1 C1 93(9) . .
O2 W1X O1 W1 -131(3) . .
Cl2X W1X O1 W1 43(3) . .
Cl3X W1X O1 W1 -46(3) . .
Cl4X W1X O1 W1 132(4) . .
Cl1X W1X O1 W1 -27(8) . .
O1 W1X O2 C12 -53(6) . .
Cl2X W1X O2 C12 -106(11) . .
Cl3X W1X O2 C12 -139(6) . .
Cl4X W1X O2 C12 47(6) . .
Cl1X W1X O2 C12 136(6) . .
O1 W1X O2 W1 59(4) . .
Cl2X W1X O2 W1 5(9) . .
Cl3X W1X O2 W1 -27(4) . .
Cl4X W1X O2 W1 158(4) . .
Cl1X W1X O2 W1 -113(4) . .
O1 W1 O2 C12 -9(6) . .
Cl3 W1 O2 C12 -100(6) . .
Cl2 W1 O2 C12 120(16) . .
Cl4 W1 O2 C12 85(6) . .
Cl1 W1 O2 C12 174(6) . .
O1 W1 O2 W1X -114(4) . .
Cl3 W1 O2 W1X 155(4) . .
Cl2 W1 O2 W1X 16(15) . .
Cl4 W1 O2 W1X -20(4) . .
Cl1 W1 O2 W1X 69(4) . .
O4 W2 O3 C23 34(6) . .
Cl8 W2 O3 C23 128(5) . .
Cl6 W2 O3 C23 -141(5) . .
Cl5 W2 O3 C23 -64(14) . .
Cl7 W2 O3 C23 -53(5) . .
O3 W2 O4 C34 -44(3) . .
Cl8 W2 O4 C34 -138(3) . .
Cl6 W2 O4 C34 93(5) . .
Cl5 W2 O4 C34 133(3) . .
Cl7 W2 O4 C34 43(3) . .
W1 O1 C1 C2 -105(3) . .
W1X O1 C1 C2 -125(2) . .
W1 O1 C1 C6 74(3) . .
W1X O1 C1 C6 54(3) . .
O1 C1 C2 C3 172.6(17) . .
C6 C1 C2 C3 -6(3) . .
O1 C1 C2 C44 -6(3) . 3_566
C6 C1 C2 C44 175.0(19) . 3_566
C1 C2 C3 C4 0(3) . .
C44 C2 C3 C4 179(2) 3_566 .
C2 C3 C4 C5 7(3) . .
C2 C3 C4 C7 -179(2) . .
C3 C4 C5 C6 -8(3) . .
C7 C4 C5 C6 177(2) . .
C4 C5 C6 C1 3(3) . .
C4 C5 C6 C11 -176(2) . .
C2 C1 C6 C5 5(3) . .
O1 C1 C6 C5 -173.9(18) . .
C2 C1 C6 C11 -176.3(19) . .
O1 C1 C6 C11 5(3) . .
C3 C4 C7 C8 -59(4) . .
C5 C4 C7 C8 115(4) . .
C3 C4 C7 C8X -104(9) . .
C5 C4 C7 C8X 70(9) . .
C3 C4 C7 C9 174(4) . .
C5 C4 C7 C9 -12(5) . .
C3 C4 C7 C9X 138(9) . .
C5 C4 C7 C9X -48(9) . .
C3 C4 C7 C10 56(4) . .
C5 C4 C7 C10 -130(3) . .
C3 C4 C7 C10X 11(9) . .
C5 C4 C7 C10X -175(8) . .
C5 C6 C11 C13 79(3) . .
C1 C6 C11 C13 -100(2) . .
W1X O2 C12 C13 13(7) . .
W1 O2 C12 C13 -24(7) . .
W1X O2 C12 C17 -170(5) . .
W1 O2 C12 C17 153(5) . .
O2 C12 C13 C14 -179.6(19) . .
C17 C12 C13 C14 3(3) . .
O2 C12 C13 C11 5(3) . .
C17 C12 C13 C11 -171.7(18) . .
C6 C11 C13 C14 -98(3) . .
C6 C11 C13 C12 77(2) . .
C12 C13 C14 C15 0(4) . .
C11 C13 C14 C15 174(2) . .
C13 C14 C15 C18 180(2) . .
C13 C14 C15 C16 -1(4) . .
C14 C15 C16 C17 0(3) . .
C18 C15 C16 C17 179(2) . .
C15 C16 C17 C12 3(3) . .
C15 C16 C17 C22 -176(2) . .
O2 C12 C17 C16 178.3(18) . .
C13 C12 C17 C16 -4(3) . .
O2 C12 C17 C22 -3(3) . .
C13 C12 C17 C22 174.1(19) . .
C14 C15 C18 C21X 160(4) . .
C16 C15 C18 C21X -19(4) . .
C14 C15 C18 C19X -67(4) . .
C16 C15 C18 C19X 114(3) . .
C14 C15 C18 C19 2(5) . .
C16 C15 C18 C19 -177(3) . .
C14 C15 C18 C21 -124(3) . .
C16 C15 C18 C21 57(3) . .
C14 C15 C18 C20 121(3) . .
C16 C15 C18 C20 -58(3) . .
C14 C15 C18 C20X 46(3) . .
C16 C15 C18 C20X -133(3) . .
C16 C17 C22 C24 5(3) . .
C12 C17 C22 C24 -173.6(17) . .
W2 O3 C23 C24 121(5) . .
W2 O3 C23 C28 -53(7) . .
O3 C23 C24 C25 -178(2) . .
C28 C23 C24 C25 -5(4) . .
O3 C23 C24 C22 5(3) . .
C28 C23 C24 C22 178(2) . .
C17 C22 C24 C25 -112(2) . .
C17 C22 C24 C23 65(3) . .
C23 C24 C25 C26 4(4) . .
C22 C24 C25 C26 -180(2) . .
C24 C25 C26 C27 1(4) . .
C24 C25 C26 C29 179(3) . .
C25 C26 C27 C28 -5(4) . .
C29 C26 C27 C28 177(3) . .
C26 C27 C28 C23 3(4) . .
C26 C27 C28 C33 -177(2) . .
O3 C23 C28 C27 175(2) . .
C24 C23 C28 C27 1(3) . .
O3 C23 C28 C33 -4(3) . .
C24 C23 C28 C33 -178(2) . .
C27 C26 C29 C31 -134(3) . .
C25 C26 C29 C31 49(4) . .
C27 C26 C29 C32 -13(4) . .
C25 C26 C29 C32 170(3) . .
C27 C26 C29 C30 110(3) . .
C25 C26 C29 C30 -68(4) . .
C27 C28 C33 C35 -91(2) . .
C23 C28 C33 C35 88(3) . .
W2 O4 C34 C39 -114(2) . .
W2 O4 C34 C35 68(3) . .
O4 C34 C35 C36 179(2) . .
C39 C34 C35 C36 2(3) . .
O4 C34 C35 C33 6(3) . .
C39 C34 C35 C33 -172(2) . .
C28 C33 C35 C36 89(3) . .
C28 C33 C35 C34 -97(2) . .
C34 C35 C36 C37 2(4) . .
C33 C35 C36 C37 175(2) . .
C35 C36 C37 C38 -4(4) . .
C35 C36 C37 C40 174(2) . .
C36 C37 C38 C39 3(4) . .
C40 C37 C38 C39 -175(2) . .
C37 C38 C39 C34 0(4) . .
C37 C38 C39 C44 -178(2) . .
O4 C34 C39 C38 180(2) . .
C35 C34 C39 C38 -3(3) . .
O4 C34 C39 C44 -2(3) . .
C35 C34 C39 C44 176(2) . .
C36 C37 C40 C41X 113(4) . .
C38 C37 C40 C41X -68(4) . .
C36 C37 C40 C43X -124(4) . .
C38 C37 C40 C43X 54(3) . .
C36 C37 C40 C41 174(3) . .
C38 C37 C40 C41 -7(4) . .
C36 C37 C40 C43 -56(4) . .
C38 C37 C40 C43 122(3) . .
C36 C37 C40 C42X -7(4) . .
C38 C37 C40 C42X 172(3) . .
C36 C37 C40 C42 58(3) . .
C38 C37 C40 C42 -124(3) . .
C38 C39 C44 C2 -52(3) . 3_566
C34 C39 C44 C2 130(2) . 3_566
Cl9 C45 C46 Cl10 103(5) . .
Cl11 C47 C48 Cl12 8(10) . .
