#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:14:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179318 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/15/4321564.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_4321564
loop_
_publ_author_name
'F. Albert Cotton'
'Evgeny V. Dikarev'
'Jiande Gu'
'Santiago Herrero'
'Barbara Modec'
_publ_section_title
;
 Alkylpyridine Complexes of Tungsten(II) and Chromium(II). First
 Rotational Isomers of W2X4L4 Molecules with D2 hand D2 Symmetries
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5407
_journal_page_last               5411
_journal_paper_doi               10.1021/ic000555v
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety
;
 W2 Cl4 (N C5 H4 C (C H3)3)4, O C (C H3)2
;
_chemical_formula_structural     (D2)-W2Cl4(4-t-Bu-py)4,(CH3)2CO
_chemical_formula_sum            'C39 H58 Cl4 N4 O W2'
_chemical_formula_weight         1108.39
_chemical_melting_point          ?
_chemical_name_systematic
; 
 Bis(trans-dichloro-bis(4-tert-butylpyridine))-di-tungsten (II),
 D2 isomer, acetone solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 103.21(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.970(5)
_cell_length_b                   10.227(1)
_cell_length_c                   28.962(2)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.05
_cell_volume                     9507.1(19)
_computing_cell_refinement       'MADNES (Enraf-Nonius, 1989)'
_computing_data_collection       'MADNES (Enraf-Nonius, 1989)'
_computing_data_reduction        'PROCOR (Kabsch, 1988)'
_computing_molecular_graphics    'SHELXTL V.5 (Siemens, 1994)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL V.5 (Siemens, 1994)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST area detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            18324
_diffrn_reflns_theta_max         22.51
_diffrn_reflns_theta_min         2.26
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    5.092
_exptl_absorpt_correction_T_max  0.602
_exptl_absorpt_correction_T_min  0.475
_exptl_absorpt_correction_type   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             4352
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.844
_refine_diff_density_min         -1.554
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.134
_refine_ls_goodness_of_fit_obs   1.125
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         5940
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.145
_refine_ls_restrained_S_obs      1.123
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_obs          0.0457
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0421P)²+337.3920P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1235
_refine_ls_wR_factor_obs         0.1143
_reflns_number_observed          5342
_reflns_number_total             5940
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000555v_5.cif
_cod_data_source_block           W2Cl4(4-t-Bu-py)4,(CH3)2CO_(1c,(CH3)2CO)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+337.3920P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+337.3920P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        9507(2)
_cod_database_code               4321564
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'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
W1 W 0.105011(13) 0.86718(4) 0.062728(15) 0.0234(2) Uani 1 d . .
W2 W 0.133308(13) 1.05178(4) 0.09940(2) 0.0254(2) Uani 1 d . .
Cl1 Cl 0.03320(8) 0.8827(3) 0.06419(10) 0.0348(7) Uani 1 d . .
Cl2 Cl 0.16174(9) 0.7484(3) 0.04381(10) 0.0356(7) Uani 1 d . .
Cl3 Cl 0.08051(9) 1.1384(3) 0.13577(10) 0.0361(7) Uani 1 d . .
Cl4 Cl 0.20051(8) 1.0650(3) 0.08151(10) 0.0377(7) Uani 1 d . .
N1 N 0.0900(3) 0.9304(8) -0.0117(3) 0.026(2) Uani 1 d . .
N2 N 0.1064(3) 0.7382(8) 0.1232(3) 0.029(2) Uani 1 d . .
N3 N 0.1110(3) 1.2009(9) 0.0461(3) 0.029(2) Uani 1 d . .
N4 N 0.1660(3) 0.9666(9) 0.1672(3) 0.033(2) Uani 1 d . .
C1 C 0.0527(3) 0.9109(11) -0.0407(4) 0.031(3) Uani 1 d . .
H1 H 0.0313(3) 0.8790(11) -0.0273(4) 0.038 Uiso 1 calc R .
C2 C 0.0436(3) 0.9335(11) -0.0877(4) 0.032(3) Uani 1 d . .
H2 H 0.0164(3) 0.9172(11) -0.1055(4) 0.039 Uiso 1 calc R .
C3 C 0.0733(4) 0.9803(11) -0.1105(4) 0.033(3) Uani 1 d . .
C4 C 0.1131(4) 1.0032(12) -0.0801(4) 0.037(3) Uani 1 d . .
H4 H 0.1350(4) 1.0360(12) -0.0927(4) 0.044 Uiso 1 calc R .
C5 C 0.1196(3) 0.9777(13) -0.0329(4) 0.040(3) Uani 1 d . .
H5 H 0.1462(3) 0.9938(13) -0.0137(4) 0.049 Uiso 1 calc R .
C6 C 0.0633(4) 1.0034(13) -0.1634(4) 0.043(3) Uani 1 d D 1
C7 C 0.0631(13) 0.8717(25) -0.1889(13) 0.078(12) Uiso 0.50 d PD 1
H7A H 0.0568(13) 0.8858(25) -0.2229(13) 0.116 Uiso 0.50 calc PR 1
H7B H 0.0422(13) 0.8149(25) -0.1808(13) 0.116 Uiso 0.50 calc PR 1
H7C H 0.0903(13) 0.8311(25) -0.1790(13) 0.116 Uiso 0.50 calc PR 1
C8 C 0.0969(8) 1.0895(29) -0.1777(11) 0.049(7) Uiso 0.50 d PD 1
H8A H 0.0898(8) 1.1029(29) -0.2118(11) 0.073 Uiso 0.50 calc PR 1
H8B H 0.1237(8) 1.0463(29) -0.1686(11) 0.073 Uiso 0.50 calc PR 1
H8C H 0.0982(8) 1.1733(29) -0.1618(11) 0.073 Uiso 0.50 calc PR 1
C9 C 0.0208(8) 1.0733(30) -0.1769(11) 0.050(8) Uiso 0.50 d PD 1
H9A H 0.0136(8) 1.0895(30) -0.2108(11) 0.075 Uiso 0.50 calc PR 1
H9B H 0.0225(8) 1.1559(30) -0.1600(11) 0.075 Uiso 0.50 calc PR 1
H9C H -0.0003(8) 1.0187(30) -0.1682(11) 0.075 Uiso 0.50 calc PR 1
C7X C 0.0465(11) 0.8690(23) -0.1868(12) 0.065(10) Uiso 0.500(6) d PD 2
H7X1 H 0.0396(11) 0.8782(23) -0.2211(12) 0.098 Uiso 0.50 calc PR 2
H7X2 H 0.0219(11) 0.8436(23) -0.1761(12) 0.098 Uiso 0.50 calc PR 2
H7X3 H 0.0679(11) 0.8026(23) -0.1777(12) 0.098 Uiso 0.50 calc PR 2
C8X C 0.1021(9) 1.0321(41) -0.1837(15) 0.094(14) Uiso 0.50 d PD 2
H8X1 H 0.0935(9) 1.0459(41) -0.2177(15) 0.140 Uiso 0.50 calc PR 2
H8X2 H 0.1211(9) 0.9585(41) -0.1773(15) 0.140 Uiso 0.50 calc PR 2
H8X3 H 0.1161(9) 1.1100(41) -0.1687(15) 0.140 Uiso 0.50 calc PR 2
C9X C 0.0313(10) 1.1111(31) -0.1796(14) 0.075(13) Uiso 0.50 d PD 2
H9X1 H 0.0264(10) 1.1209(31) -0.2138(14) 0.112 Uiso 0.50 calc PR 2
H9X2 H 0.0418(10) 1.1927(31) -0.1644(14) 0.112 Uiso 0.50 calc PR 2
H9X3 H 0.0055(10) 1.0883(31) -0.1710(14) 0.112 Uiso 0.50 calc PR 2
C10 C 0.0920(4) 0.7784(12) 0.1602(4) 0.037(3) Uani 1 d . .
H10 H 0.0849(4) 0.8671(12) 0.1618(4) 0.044 Uiso 1 calc R .
C11 C 0.0868(4) 0.6963(11) 0.1966(4) 0.037(3) Uani 1 d . .
H11 H 0.0782(4) 0.7311(11) 0.2228(4) 0.044 Uiso 1 calc R .
C12 C 0.0941(4) 0.5654(11) 0.1945(5) 0.039(3) Uani 1 d . .
C13 C 0.1080(4) 0.5232(12) 0.1557(4) 0.047(3) Uani 1 d . .
H13 H 0.1136(4) 0.4340(12) 0.1525(4) 0.056 Uiso 1 calc R .
C14 C 0.1137(4) 0.6102(11) 0.1216(4) 0.034(3) Uani 1 d . .
H14 H 0.1233(4) 0.5777(11) 0.0956(4) 0.041 Uiso 1 calc R .
C15 C 0.0864(4) 0.4676(11) 0.2324(4) 0.040(3) Uani 1 d D 3
C16 C 0.1240(7) 0.3766(26) 0.2477(10) 0.025(8) Uiso 0.50 d PD 3
H16A H 0.1299(7) 0.3346(26) 0.2200(10) 0.037 Uiso 0.50 calc PR 3
H16B H 0.1177(7) 0.3106(26) 0.2691(10) 0.037 Uiso 0.50 calc PR 3
H16C H 0.1480(7) 0.4270(26) 0.2637(10) 0.037 Uiso 0.50 calc PR 3
C17 C 0.0474(6) 0.3881(24) 0.2092(9) 0.024(7) Uiso 0.50 d PD 3
H17A H 0.0238(6) 0.4467(24) 0.1996(9) 0.035 Uiso 0.50 calc PR 3
H17B H 0.0415(6) 0.3249(24) 0.2318(9) 0.035 Uiso 0.50 calc PR 3
H17C H 0.0523(6) 0.3426(24) 0.1816(9) 0.035 Uiso 0.50 calc PR 3
C18 C 0.0758(9) 0.5363(23) 0.2751(8) 0.037(7) Uiso 0.50 d PD 3
H18A H 0.0520(9) 0.5932(23) 0.2644(8) 0.055 Uiso 0.50 calc PR 3
H18B H 0.0995(9) 0.5878(23) 0.2914(8) 0.055 Uiso 0.50 calc PR 3
H18C H 0.0693(9) 0.4714(23) 0.2967(8) 0.055 Uiso 0.50 calc PR 3
C16X C 0.1190(10) 0.3548(33) 0.2386(15) 0.071(17) Uiso 0.500(6) d PD 4
H16D H 0.1469(10) 0.3911(33) 0.2474(15) 0.107 Uiso 0.50 calc PR 4
H16E H 0.1157(10) 0.3072(33) 0.2090(15) 0.107 Uiso 0.50 calc PR 4
H16F H 0.1147(10) 0.2958(33) 0.2633(15) 0.107 Uiso 0.50 calc PR 4
C17X C 0.0430(7) 0.4117(35) 0.2187(13) 0.062(13) Uiso 0.50 d PD 4
H17D H 0.0393(7) 0.3671(35) 0.1885(13) 0.093 Uiso 0.50 calc PR 4
H17E H 0.0228(7) 0.4819(35) 0.2161(13) 0.093 Uiso 0.50 calc PR 4
H17F H 0.0391(7) 0.3502(35) 0.2428(13) 0.093 Uiso 0.50 calc PR 4
C18X C 0.0927(10) 0.5389(25) 0.2805(8) 0.044(8) Uiso 0.50 d PD 4
H18D H 0.1207(10) 0.5747(25) 0.2891(8) 0.067 Uiso 0.50 calc PR 4
H18E H 0.0888(10) 0.4775(25) 0.3047(8) 0.067 Uiso 0.50 calc PR 4
H18F H 0.0726(10) 0.6092(25) 0.2780(8) 0.067 Uiso 0.50 calc PR 4
C19 C 0.0707(3) 1.2044(10) 0.0221(4) 0.030(3) Uani 1 d . .
H19 H 0.0527(3) 1.1392(10) 0.0286(4) 0.035 Uiso 1 calc R .
C20 C 0.0543(3) 1.2983(10) -0.0114(4) 0.030(3) Uani 1 d . .
H20 H 0.0258(3) 1.2961(10) -0.0263(4) 0.036 Uiso 1 calc R .
C21 C 0.0794(4) 1.3956(10) -0.0232(4) 0.030(3) Uani 1 d . .
C22 C 0.1208(4) 1.3942(11) 0.0029(4) 0.039(3) Uani 1 d . .
H22 H 0.1392(4) 1.4597(11) -0.0023(4) 0.047 Uiso 1 calc R .
C23 C 0.1348(4) 1.2988(11) 0.0359(4) 0.040(3) Uani 1 d . .
H23 H 0.1628(4) 1.3020(11) 0.0524(4) 0.048 Uiso 1 calc R .
C24 C 0.0625(4) 1.4938(12) -0.0614(4) 0.038(3) Uani 1 d . .
C25 C 0.0270(5) 1.5689(15) -0.0475(6) 0.065(4) Uani 1 d . .
H25A H 0.0158(5) 1.6327(15) -0.0719(6) 0.098 Uiso 1 calc R .
H25B H 0.0375(5) 1.6133(15) -0.0176(6) 0.098 Uiso 1 calc R .
H25C H 0.0052(5) 1.5082(15) -0.0442(6) 0.098 Uiso 1 calc R .
C26 C 0.0954(4) 1.5866(14) -0.0714(5) 0.054(4) Uani 1 d . .
H26A H 0.0826(4) 1.6473(14) -0.0963(5) 0.082 Uiso 1 calc R .
H26B H 0.1169(4) 1.5369(14) -0.0816(5) 0.082 Uiso 1 calc R .
H26C H 0.1077(4) 1.6349(14) -0.0428(5) 0.082 Uiso 1 calc R .
C27 C 0.0438(6) 1.4198(16) -0.1068(5) 0.072(5) Uani 1 d . .
H27A H 0.0327(6) 1.4816(16) -0.1319(5) 0.108 Uiso 1 calc R .
H27B H 0.0215(6) 1.3636(16) -0.1016(5) 0.108 Uiso 1 calc R .
H27C H 0.0652(6) 1.3670(16) -0.1158(5) 0.108 Uiso 1 calc R .
C28 C 0.1928(3) 0.8676(11) 0.1682(4) 0.035(3) Uani 1 d . .
H28 H 0.1965(3) 0.8344(11) 0.1392(4) 0.041 Uiso 1 calc R .
C29 C 0.2151(4) 0.8120(12) 0.2093(4) 0.037(3) Uani 1 d . .
H29 H 0.2333(4) 0.7423(12) 0.2078(4) 0.045 Uiso 1 calc R .
C30 C 0.2110(4) 0.8580(12) 0.2533(4) 0.039(3) Uani 1 d . .
C31 C 0.1840(4) 0.9628(12) 0.2527(4) 0.040(3) Uani 1 d . .
H31 H 0.1807(4) 1.0002(12) 0.2812(4) 0.048 Uiso 1 calc R .
C32 C 0.1621(4) 1.0115(11) 0.2098(4) 0.037(3) Uani 1 d . .
H32 H 0.1433(4) 1.0803(11) 0.2102(4) 0.044 Uiso 1 calc R .
C33 C 0.2349(5) 0.7943(15) 0.2996(5) 0.060(4) Uani 1 d D 5
C34 C 0.2152(12) 0.8209(40) 0.3408(11) 0.044(8) Uiso 0.40 d PD 5
H34A H 0.1862(12) 0.7937(40) 0.3327(11) 0.066 Uiso 0.40 calc PR 5
H34B H 0.2167(12) 0.9137(40) 0.3480(11) 0.066 Uiso 0.40 calc PR 5
H34C H 0.2299(12) 0.7724(40) 0.3684(11) 0.066 Uiso 0.40 calc PR 5
C35 C 0.2803(9) 0.8345(46) 0.3098(17) 0.072(17) Uiso 0.40 d PD 5
H35A H 0.2915(9) 0.8155(46) 0.2823(17) 0.108 Uiso 0.40 calc PR 5
H35B H 0.2958(9) 0.7861(46) 0.3369(17) 0.108 Uiso 0.40 calc PR 5
H35C H 0.2826(9) 0.9274(46) 0.3165(17) 0.108 Uiso 0.40 calc PR 5
C36 C 0.2332(11) 0.6410(21) 0.2907(13) 0.036(9) Uiso 0.40 d PD 5
H36A H 0.2457(11) 0.6208(21) 0.2643(13) 0.053 Uiso 0.40 calc PR 5
H36B H 0.2044(11) 0.6119(21) 0.2834(13) 0.053 Uiso 0.40 calc PR 5
H36C H 0.2485(11) 0.5965(21) 0.3189(13) 0.053 Uiso 0.40 calc PR 5
C34X C 0.2303(13) 0.8685(39) 0.3431(12) 0.065(12) Uiso 0.400(7) d PD 6
H34D H 0.2459(13) 0.8244(39) 0.3713(12) 0.098 Uiso 0.40 calc PR 6
H34E H 0.2011(13) 0.8722(39) 0.3441(12) 0.098 Uiso 0.40 calc PR 6
H34F H 0.2409(13) 0.9566(39) 0.3420(12) 0.098 Uiso 0.40 calc PR 6
C35X C 0.2820(7) 0.7998(38) 0.2984(15) 0.044(10) Uiso 0.40 d PD 6
H35D H 0.2863(7) 0.7529(38) 0.2708(15) 0.066 Uiso 0.40 calc PR 6
H35E H 0.2985(7) 0.7596(38) 0.3269(15) 0.066 Uiso 0.40 calc PR 6
H35F H 0.2905(7) 0.8902(38) 0.2968(15) 0.066 Uiso 0.40 calc PR 6
C36X C 0.2233(13) 0.6488(25) 0.3017(15) 0.054(12) Uiso 0.40 d PD 6
H36D H 0.2267(13) 0.6052(25) 0.2731(15) 0.081 Uiso 0.40 calc PR 6
H36E H 0.1946(13) 0.6414(25) 0.3042(15) 0.081 Uiso 0.40 calc PR 6
H36F H 0.2414(13) 0.6083(25) 0.3291(15) 0.081 Uiso 0.40 calc PR 6
C34Y C 0.2042(17) 0.7545(68) 0.3286(24) 0.056(19) Uiso 0.200(7) d PD 7
H34G H 0.2191(17) 0.7142(68) 0.3579(24) 0.084 Uiso 0.20 calc PR 7
H34H H 0.1844(17) 0.6926(68) 0.3107(24) 0.084 Uiso 0.20 calc PR 7
H34I H 0.1895(17) 0.8312(68) 0.3358(24) 0.084 Uiso 0.20 calc PR 7
C35Y C 0.2636(21) 0.9036(57) 0.3264(26) 0.080(25) Uiso 0.20 d PD 7
H35G H 0.2834(21) 0.9296(57) 0.3079(26) 0.120 Uiso 0.20 calc PR 7
H35H H 0.2786(21) 0.8710(57) 0.3570(26) 0.120 Uiso 0.20 calc PR 7
H35I H 0.2469(21) 0.9784(57) 0.3309(26) 0.120 Uiso 0.20 calc PR 7
C36Y C 0.2639(20) 0.6785(51) 0.2944(27) 0.075(24) Uiso 0.20 d PD 7
H36G H 0.2833(20) 0.7060(51) 0.2757(27) 0.113 Uiso 0.20 calc PR 7
H36H H 0.2473(20) 0.6061(51) 0.2787(27) 0.113 Uiso 0.20 calc PR 7
H36I H 0.2793(20) 0.6510(51) 0.3255(27) 0.113 Uiso 0.20 calc PR 7
O1 O 0.1803(10) 0.8361(26) -0.1421(10) 0.096(9) Uiso 0.50 d PD 8
C37 C 0.2014(10) 0.7663(28) -0.1125(10) 0.044(8) Uiso 0.50 d PD 8
C38 C 0.1996(16) 0.6336(35) -0.1090(19) 0.117(18) Uiso 0.50 d PD 8
H38A H 0.1863(16) 0.5972(35) -0.1397(19) 0.176 Uiso 0.50 calc PR 8
H38B H 0.1837(16) 0.6102(35) -0.0859(19) 0.176 Uiso 0.50 calc PR 8
H38C H 0.2277(16) 0.5989(35) -0.0991(19) 0.176 Uiso 0.50 calc PR 8
C39 C 0.2211(12) 0.8381(41) -0.0680(11) 0.081(11) Uiso 0.50 d PD 8
H39A H 0.2207(12) 0.9312(41) -0.0744(11) 0.122 Uiso 0.50 calc PR 8
H39B H 0.2497(12) 0.8091(41) -0.0569(11) 0.122 Uiso 0.50 calc PR 8
H39C H 0.2058(12) 0.8204(41) -0.0438(11) 0.122 Uiso 0.50 calc PR 8
O1X O 0.1994(16) 0.8301(39) -0.1487(14) 0.160(18) Uiso 0.50 d PD 9
C37X C 0.1991(30) 0.7387(45) -0.1229(19) 0.188(43) Uiso 0.50 d PD 9
C38X C 0.1964(13) 0.6101(33) -0.1346(16) 0.088(12) Uiso 0.50 d PD 9
H38D H 0.1867(13) 0.6012(33) -0.1687(16) 0.132 Uiso 0.50 calc PR 9
H38E H 0.1770(13) 0.5673(33) -0.1189(16) 0.132 Uiso 0.50 calc PR 9
H38F H 0.2237(13) 0.5699(33) -0.1245(16) 0.132 Uiso 0.50 calc PR 9
C39X C 0.2138(17) 0.7699(50) -0.0710(14) 0.123(18) Uiso 0.50 d PD 9
H39D H 0.2146(17) 0.8639(50) -0.0666(14) 0.184 Uiso 0.50 calc PR 9
H39E H 0.2415(17) 0.7341(50) -0.0593(14) 0.184 Uiso 0.50 calc PR 9
H39F H 0.1949(17) 0.7316(50) -0.0537(14) 0.184 Uiso 0.50 calc PR 9
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
_geom_angle_publ_flag
N2 W1 N1 157.4(3) . . y
N2 W1 W2 101.4(2) . . y
N1 W1 W2 101.0(2) . . y
N2 W1 Cl1 82.2(2) . . y
N1 W1 Cl1 89.8(2) . . y
W2 W1 Cl1 103.95(7) . . y
N2 W1 Cl2 90.2(2) . . y
N1 W1 Cl2 86.4(2) . . y
W2 W1 Cl2 105.73(7) . . y
Cl1 W1 Cl2 150.27(10) . . y
N3 W2 N4 158.6(3) . . y
N3 W2 W1 102.5(2) . . y
N4 W2 W1 98.9(2) . . y
N3 W2 Cl4 89.2(2) . . y
N4 W2 Cl4 85.7(3) . . y
W1 W2 Cl4 104.39(8) . . y
N3 W2 Cl3 83.8(3) . . y
N4 W2 Cl3 90.7(3) . . y
W1 W2 Cl3 104.56(7) . . y
Cl4 W2 Cl3 151.04(10) . . y
C1 N1 C5 115.1(10) . . n
C1 N1 W1 122.8(7) . . n
C5 N1 W1 121.7(7) . . n
C10 N2 C14 115.6(10) . . n
C10 N2 W1 120.8(7) . . n
C14 N2 W1 122.3(7) . . n
C23 N3 C19 114.9(9) . . n
C23 N3 W2 124.0(7) . . n
C19 N3 W2 121.0(7) . . n
C28 N4 C32 116.0(10) . . n
C28 N4 W2 120.5(8) . . n
C32 N4 W2 123.5(7) . . n
N1 C1 C2 124.9(11) . . n
C1 C2 C3 121.4(10) . . n
C2 C3 C4 114.7(10) . . n
C2 C3 C6 121.6(11) . . n
C4 C3 C6 123.8(11) . . n
C5 C4 C3 119.9(11) . . n
N1 C5 C4 124.0(11) . . n
C3 C6 C7 109.0(17) . . n
C3 C6 C9 107.7(15) . . n
C7 C6 C9 112.6(20) . . n
C3 C6 C8 111.0(14) . . n
C7 C6 C8 107.2(20) . . n
C9 C6 C8 109.5(18) . . n
C3 C6 C9X 113.6(17) . . n
C3 C6 C8X 113.9(18) . . n
C9X C6 C8X 108.6(21) . . n
C3 C6 C7X 105.9(16) . . n
C9X C6 C7X 110.4(19) . . n
C8X C6 C7X 103.9(20) . . n
N2 C10 C11 123.5(11) . . n
C12 C11 C10 120.4(11) . . n
C11 C12 C13 116.1(11) . . n
C11 C12 C15 122.9(11) . . n
C13 C12 C15 121.0(10) . . n
C14 C13 C12 120.6(11) . . n
N2 C14 C13 123.7(10) . . n
C16 C15 C18 111.3(16) . . n
C16 C15 C17 110.2(16) . . n
C18 C15 C17 105.8(17) . . n
C16 C15 C12 110.2(14) . . n
C18 C15 C12 112.4(13) . . n
C17 C15 C12 106.8(13) . . n
C17X C15 C18X 109.8(19) . . n
C17X C15 C12 111.0(17) . . n
C18X C15 C12 109.0(14) . . n
C17X C15 C16X 109.7(19) . . n
C18X C15 C16X 107.4(18) . . n
C12 C15 C16X 109.9(18) . . n
N3 C19 C20 123.9(10) . . n
C19 C20 C21 120.8(10) . . n
C20 C21 C22 115.0(10) . . n
C20 C21 C24 121.3(10) . . n
C22 C21 C24 123.7(10) . . n
C23 C22 C21 121.0(10) . . n
N3 C23 C22 124.3(11) . . n
C21 C24 C26 113.4(10) . . n
C21 C24 C27 108.2(10) . . n
C26 C24 C27 108.2(11) . . n
C21 C24 C25 108.6(10) . . n
C26 C24 C25 111.1(11) . . n
C27 C24 C25 107.1(12) . . n
N4 C28 C29 123.6(11) . . n
C28 C29 C30 120.5(11) . . n
C31 C30 C29 116.4(10) . . n
C31 C30 C33 122.5(11) . . n
C29 C30 C33 121.1(11) . . n
C32 C31 C30 119.4(11) . . n
N4 C32 C31 124.0(11) . . n
C34 C33 C35 112.5(25) . . n
C34 C33 C30 112.8(16) . . n
C35 C33 C30 110.0(21) . . n
C34 C33 C36 107.6(22) . . n
C35 C33 C36 107.2(22) . . n
C30 C33 C36 106.5(16) . . n
C34X C33 C30 112.8(19) . . n
C34X C33 C36X 112.4(24) . . n
C30 C33 C36X 111.2(19) . . n
C34X C33 C35X 106.9(23) . . n
C30 C33 C35X 106.2(17) . . n
C36X C33 C35X 106.9(21) . . n
C34Y C33 C30 109.0(28) . . n
C34Y C33 C36Y 110.8(29) . . n
C30 C33 C36Y 116.3(30) . . n
C34Y C33 C35Y 109.1(29) . . n
C30 C33 C35Y 105.3(32) . . n
C36Y C33 C35Y 106.1(27) . . n
O1 C37 C38 127.9(36) . . n
O1 C37 C39 112.9(29) . . n
C38 C37 C39 116.3(32) . . n
O1X C37X C38X 127.6(47) . . n
O1X C37X C39X 114.3(37) . . n
C38X C37X C39X 116.3(37) . . n
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 2.185(9) . y
W1 N1 2.196(9) . y
W1 W2 2.2605(6) . y
W1 Cl1 2.383(3) . y
W1 Cl2 2.397(3) . y
W2 N3 2.176(9) . y
W2 N4 2.193(9) . y
W2 Cl4 2.392(3) . y
W2 Cl3 2.401(3) . y
N1 C1 1.335(14) . n
N1 C5 1.354(14) . n
N2 C10 1.333(14) . n
N2 C14 1.333(14) . n
N3 C23 1.344(14) . n
N3 C19 1.353(14) . n
N4 C28 1.338(14) . n
N4 C32 1.350(15) . n
C1 C2 1.35(2) . n
C2 C3 1.38(2) . n
C3 C4 1.42(2) . n
C3 C6 1.51(2) . n
C4 C5 1.36(2) . n
C6 C7 1.53(3) . n
C6 C9 1.54(2) . n
C6 C8 1.54(2) . n
C6 C9X 1.52(2) . n
C6 C8X 1.55(3) . n
C6 C7X 1.58(3) . n
C10 C11 1.39(2) . n
C11 C12 1.36(2) . n
C12 C13 1.38(2) . n
C12 C15 1.55(2) . n
C13 C14 1.38(2) . n
C15 C16 1.53(2) . n
C15 C18 1.53(2) . n
C15 C17 1.54(2) . n
C15 C17X 1.51(2) . n
C15 C18X 1.54(2) . n
C15 C16X 1.56(2) . n
C19 C20 1.384(15) . n
C20 C21 1.39(2) . n
C21 C22 1.40(2) . n
C21 C24 1.50(2) . n
C22 C23 1.37(2) . n
C24 C26 1.52(2) . n
C24 C27 1.52(2) . n
C24 C25 1.53(2) . n
C28 C29 1.37(2) . n
C29 C30 1.39(2) . n
C30 C31 1.39(2) . n
C30 C33 1.54(2) . n
C31 C32 1.38(2) . n
C33 C34 1.51(2) . n
C33 C35 1.51(3) . n
C33 C36 1.59(2) . n
C33 C34X 1.51(3) . n
C33 C36X 1.54(3) . n
C33 C35X 1.56(3) . n
C33 C34Y 1.51(3) . n
C33 C36Y 1.55(3) . n
C33 C35Y 1.55(3) . n
O1 C37 1.21(3) . n
C37 C38 1.36(4) . n
C37 C39 1.50(4) . n
O1X C37X 1.20(4) . n
C37X C38X 1.36(4) . n
C37X C39X 1.50(4) . n
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 W1 W2 N3 18.5(3) . . . . y
N2 W1 W2 N4 21.1(3) . . . . y
Cl1 W1 W2 Cl3 12.77(10) . . . . y
Cl2 W1 W2 Cl4 15.53(10) . . . . y
