#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:34:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179336 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/33/4323319.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_4323319
loop_
_publ_author_name
'F. Albert Cotton'
'Evgeny V. Dikarev'
'N. Nawar'
'Wai-Yeung Wong'
_publ_section_title
;
 W2Cl4(NR2)2(PR'3)2 Molecules. 4. A New Synthetic Route to Products with a
 Staggered Conformation. Preparations and Characterizations of
 W2Cl4(NR2)2(PR'3)2 (R = Et, Bu, Hex; R'3= Me3, Et2H) and an Intermediate
 Complex W2Cl4(NEt2)2(NHEt2)2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              559
_journal_page_last               566
_journal_paper_doi               10.1021/ic9610694
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'C22 H54 Cl4 N2 P2 W2'
_chemical_formula_structural     W2Cl4(NBu2)2(PMe3)2
_chemical_formula_sum            'C22 H54 Cl4 N2 P2 W2'
_chemical_formula_weight         918.11
_chemical_melting_point          ?
_chemical_name_common
;
 cis,cis-Tetrachloro-bis(dibutylamido)-bis(trimethyl-
 phosphine) ditungsten(III)
;
_chemical_name_systematic
; 
 1,1,2,2-Tetrachloro-1,2-bis(dibutylamido)-(cis,cis)-
 1,2-bis(trimethylphosphine) ditungsten(III) 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                95.66(3)
_cell_angle_beta                 97.99(4)
_cell_angle_gamma                91.26(3)
_cell_formula_units_Z            4
_cell_length_a                   12.162(6)
_cell_length_b                   14.955(4)
_cell_length_c                   18.82(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      14.33
_cell_measurement_theta_min      11.26
_cell_volume                     3371(3)
_computing_cell_refinement       'CAD4 EXPRESS'
_computing_data_collection       'CAD4 V5 (Enraf-Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms, 1993)'
_computing_molecular_graphics    'SHELXTL V.5 (Siemens, 1994)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9879
_diffrn_reflns_theta_max         22.95
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.244
_exptl_absorpt_correction_T_max  0.9995
_exptl_absorpt_correction_T_min  0.3085
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.809
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate-shaped
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.526
_refine_diff_density_min         -3.266
_refine_diff_density_rms         0.327
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.059
_refine_ls_goodness_of_fit_obs   1.037
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         9356
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.067
_refine_ls_restrained_S_obs      1.039
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_obs          0.0576
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1194P)²+12.5977P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1709
_refine_ls_wR_factor_obs         0.1473
_reflns_number_observed          7435
_reflns_number_total             9357
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ic9610694_4.cif
_cod_data_source_block           W2Cl4(NBu2)2(PMe3)2
_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 1715 2011-07-08 13:25:40Z 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^)+(0.1194P)^2^+12.5977P] 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^)+(0.1194P)^2^+12.5977P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323319
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.30077(5) 0.08619(3) 0.18585(3) 0.0215(2) Uani 1 d . .
W2 W 0.30641(5) 0.22794(3) 0.24853(3) 0.0213(2) Uani 1 d . .
P1 P 0.1287(3) 0.0209(2) 0.2266(2) 0.0309(9) Uani 1 d . .
P2 P 0.5046(3) 0.2269(2) 0.3106(2) 0.0294(9) Uani 1 d . .
Cl1 Cl 0.4733(3) 0.0677(2) 0.1400(2) 0.0346(9) Uani 1 d . .
Cl2 Cl 0.3725(3) -0.0173(2) 0.2713(2) 0.0317(8) Uani 1 d . .
Cl3 Cl 0.2859(3) 0.2055(2) 0.3719(2) 0.0369(9) Uani 1 d . .
Cl4 Cl 0.1192(3) 0.2772(2) 0.2389(2) 0.0357(9) Uani 1 d . .
N1 N 0.2127(9) 0.1020(8) 0.0961(6) 0.028(3) Uani 1 d . .
N2 N 0.3585(10) 0.3078(7) 0.1837(6) 0.024(3) Uani 1 d . .
C1 C -0.0043(13) 0.0610(12) 0.1910(10) 0.046(4) Uani 1 d . .
H1A H -0.0080(13) 0.0633(12) 0.1389(10) 0.069 Uiso 1 calc R .
H1B H -0.0139(13) 0.1213(12) 0.2143(10) 0.069 Uiso 1 calc R .
H1C H -0.0635(13) 0.0201(12) 0.2004(10) 0.069 Uiso 1 calc R .
C2 C 0.1209(15) 0.0209(12) 0.3216(9) 0.045(4) Uani 1 d . .
H2A H 0.1907(15) -0.0002(12) 0.3459(9) 0.068 Uiso 1 calc R .
H2B H 0.0592(15) -0.0191(12) 0.3283(9) 0.068 Uiso 1 calc R .
H2C H 0.1088(15) 0.0821(12) 0.3422(9) 0.068 Uiso 1 calc R .
C3 C 0.1142(16) -0.0965(10) 0.1921(10) 0.050(5) Uani 1 d . .
H3A H 0.1825(16) -0.1269(10) 0.2079(10) 0.074 Uiso 1 calc R .
H3B H 0.1005(16) -0.1018(10) 0.1393(10) 0.074 Uiso 1 calc R .
H3C H 0.0516(16) -0.1246(10) 0.2103(10) 0.074 Uiso 1 calc R .
C4 C 0.5533(14) 0.1333(10) 0.3603(9) 0.041(4) Uani 1 d . .
H4A H 0.5433(14) 0.0774(10) 0.3280(9) 0.061 Uiso 1 calc R .
H4B H 0.5105(14) 0.1286(10) 0.4003(9) 0.061 Uiso 1 calc R .
H4C H 0.6322(14) 0.1437(10) 0.3794(9) 0.061 Uiso 1 calc R .
C5 C 0.5305(15) 0.3192(11) 0.3792(10) 0.050(5) Uani 1 d . .
H5A H 0.4766(15) 0.3162(11) 0.4131(10) 0.076 Uiso 1 calc R .
H5B H 0.5233(15) 0.3758(11) 0.3571(10) 0.076 Uiso 1 calc R .
H5C H 0.6059(15) 0.3163(11) 0.4050(10) 0.076 Uiso 1 calc R .
C6 C 0.6116(12) 0.2465(12) 0.2559(10) 0.046(5) Uani 1 d . .
H6A H 0.6061(12) 0.1992(12) 0.2155(10) 0.069 Uiso 1 calc R .
H6B H 0.6847(12) 0.2456(12) 0.2852(10) 0.069 Uiso 1 calc R .
H6C H 0.6021(12) 0.3051(12) 0.2373(10) 0.069 Uiso 1 calc R .
C7 C 0.1631(12) 0.1775(9) 0.0601(8) 0.027(3) Uani 1 d . .
H7A H 0.2094(12) 0.1922(9) 0.0232(8) 0.033 Uiso 1 calc R .
H7B H 0.1668(12) 0.2306(9) 0.0962(8) 0.033 Uiso 1 calc R .
C8 C 0.0429(14) 0.1627(11) 0.0236(10) 0.044(4) Uani 1 d . .
H8A H 0.0380(14) 0.1097(11) -0.0128(10) 0.053 Uiso 1 calc R 1
H8B H -0.0047(14) 0.1496(11) 0.0602(10) 0.053 Uiso 1 calc R 1
C9 C -0.0006(17) 0.2428(12) -0.0127(11) 0.059(5) Uani 1 d . 1
H9A H 0.0267(17) 0.2401(12) -0.0600(11) 0.070 Uiso 1 calc R 1
H9B H -0.0825(17) 0.2348(12) -0.0227(11) 0.070 Uiso 1 calc R 1
C10 C 0.0252(47) 0.3354(32) 0.0236(28) 0.069(9) Uiso 0.46(4) d P 1
H10A H -0.0093(47) 0.3792(32) -0.0073(28) 0.104 Uiso 0.46(4) calc PR 1
H10B H 0.1058(47) 0.3467(32) 0.0322(28) 0.104 Uiso 0.46(4) calc PR 1
H10C H -0.0041(47) 0.3414(32) 0.0697(28) 0.104 Uiso 0.46(4) calc PR 1
C91 C -0.0006(17) 0.2428(12) -0.0127(11) 0.990 Uiso 0.00 d P 2
C101 C -0.0315(40) 0.3122(29) 0.0444(23) 0.069(9) Uiso 0.54(4) d P 2
H10D H -0.0600(40) 0.3649(29) 0.0217(23) 0.104 Uiso 0.54(4) calc PR 2
H10E H 0.0343(40) 0.3303(29) 0.0796(23) 0.104 Uiso 0.54(4) calc PR 2
H10F H -0.0889(40) 0.2865(29) 0.0689(23) 0.104 Uiso 0.54(4) calc PR 2
C11 C 0.2066(12) 0.0154(9) 0.0488(9) 0.032(4) Uani 1 d . .
H11A H 0.1275(12) -0.0041(9) 0.0352(9) 0.038 Uiso 1 calc R .
H11B H 0.2437(12) -0.0308(9) 0.0769(9) 0.038 Uiso 1 calc R .
C12 C 0.2589(13) 0.0190(9) -0.0194(8) 0.030(3) Uani 1 d . .
H12A H 0.3347(13) 0.0467(9) -0.0068(8) 0.036 Uiso 1 calc R .
H12B H 0.2147(13) 0.0576(9) -0.0516(8) 0.036 Uiso 1 calc R .
C13 C 0.2654(12) -0.0742(9) -0.0594(8) 0.029(3) Uani 1 d . .
H13A H 0.1893(12) -0.1016(9) -0.0703(8) 0.035 Uiso 1 calc R .
H13B H 0.2917(12) -0.0668(9) -0.1060(8) 0.035 Uiso 1 calc R .
C14 C 0.3394(16) -0.1389(12) -0.0207(10) 0.050(5) Uani 1 d . .
H14A H 0.3374(16) -0.1962(12) -0.0510(10) 0.076 Uiso 1 calc R .
H14B H 0.3131(16) -0.1486(12) 0.0249(10) 0.076 Uiso 1 calc R .
H14C H 0.4157(16) -0.1138(12) -0.0109(10) 0.076 Uiso 1 calc R .
C15 C 0.3916(11) 0.2979(8) 0.1115(7) 0.021(3) Uani 1 d . .
H15A H 0.3285(11) 0.3153(8) 0.0771(7) 0.025 Uiso 1 calc R .
H15B H 0.4031(11) 0.2334(8) 0.0987(7) 0.025 Uiso 1 calc R .
C16 C 0.4937(13) 0.3499(9) 0.0993(7) 0.029(3) Uani 1 d . .
H16A H 0.4915(13) 0.4124(9) 0.1218(7) 0.035 Uiso 1 calc R .
H16B H 0.5604(13) 0.3226(9) 0.1234(7) 0.035 Uiso 1 calc R .
C17 C 0.5033(13) 0.3515(10) 0.0221(8) 0.033(4) Uani 1 d . .
H17A H 0.4387(13) 0.3824(10) -0.0010(8) 0.040 Uiso 1 calc R .
H17B H 0.4995(13) 0.2888(10) -0.0008(8) 0.040 Uiso 1 calc R .
C18 C 0.6092(14) 0.3978(11) 0.0069(10) 0.045(4) Uani 1 d . .
H18A H 0.6087(14) 0.3958(11) -0.0454(10) 0.067 Uiso 1 calc R .
H18B H 0.6739(14) 0.3667(11) 0.0282(10) 0.067 Uiso 1 calc R .
H18C H 0.6130(14) 0.4605(11) 0.0280(10) 0.067 Uiso 1 calc R .
C19 C 0.3587(14) 0.4020(9) 0.2159(8) 0.033(4) Uani 1 d . .
H19A H 0.4358(14) 0.4275(9) 0.2232(8) 0.040 Uiso 1 calc R .
H19B H 0.3339(14) 0.4029(9) 0.2639(8) 0.040 Uiso 1 calc R .
C20 C 0.2832(13) 0.4624(9) 0.1694(9) 0.033(4) Uani 1 d . .
H20A H 0.3083(13) 0.4630(9) 0.1217(9) 0.040 Uiso 1 calc R .
H20B H 0.2059(13) 0.4376(9) 0.1619(9) 0.040 Uiso 1 calc R .
C21 C 0.2870(14) 0.5573(10) 0.2061(10) 0.041(4) Uani 1 d . .
H21A H 0.2642(14) 0.5557(10) 0.2545(10) 0.049 Uiso 1 calc R .
H21B H 0.3645(14) 0.5817(10) 0.2129(10) 0.049 Uiso 1 calc R .
C22 C 0.2134(17) 0.6195(12) 0.1646(11) 0.058(5) Uani 1 d . .
H22A H 0.2194(17) 0.6797(12) 0.1910(11) 0.087 Uiso 1 calc R .
H22B H 0.1361(17) 0.5967(12) 0.1587(11) 0.087 Uiso 1 calc R .
H22C H 0.2365(17) 0.6227(12) 0.1171(11) 0.087 Uiso 1 calc R .
W3 W 0.34500(4) 0.32093(3) 0.71114(3) 0.0192(2) Uani 1 d . .
W4 W 0.15346(4) 0.31114(3) 0.67879(3) 0.0217(2) Uani 1 d . .
P3 P 0.3587(3) 0.2035(2) 0.7991(2) 0.0266(8) Uani 1 d . .
C23 C 0.4999(13) 0.2013(10) 0.8367(8) 0.035(4) Uani 1 d . .
H23A H 0.5459(13) 0.1930(10) 0.7979(8) 0.053 Uiso 1 calc R .
H23B H 0.5103(13) 0.1515(10) 0.8669(8) 0.053 Uiso 1 calc R .
H23C H 0.5219(13) 0.2582(10) 0.8662(8) 0.053 Uiso 1 calc R .
C24 C 0.2899(13) 0.2192(10) 0.8790(8) 0.035(4) Uani 1 d . .
H24A H 0.2095(13) 0.2214(10) 0.8644(8) 0.052 Uiso 1 calc R .
H24B H 0.3173(13) 0.2756(10) 0.9074(8) 0.052 Uiso 1 calc R .
H24C H 0.3057(13) 0.1689(10) 0.9081(8) 0.052 Uiso 1 calc R .
C25 C 0.3249(17) 0.0866(9) 0.7646(10) 0.048(5) Uani 1 d . .
H25A H 0.2470(17) 0.0806(9) 0.7423(10) 0.072 Uiso 1 calc R .
H25B H 0.3366(17) 0.0487(9) 0.8044(10) 0.072 Uiso 1 calc R .
H25C H 0.3728(17) 0.0677(9) 0.7285(10) 0.072 Uiso 1 calc R .
P4 P 0.1172(4) 0.4721(3) 0.7188(3) 0.0387(10) Uani 1 d D 3
C26 C -0.0295(14) 0.4835(12) 0.6990(11) 0.055(5) Uani 1 d D 3
H26A H -0.0567(14) 0.4515(12) 0.6517(11) 0.082 Uiso 1 calc R 3
H26B H -0.0460(14) 0.5473(12) 0.6987(11) 0.082 Uiso 1 calc R 3
H26C H -0.0662(14) 0.4578(12) 0.7359(11) 0.082 Uiso 1 calc R 3
C27 C 0.1548(32) 0.5321(31) 0.8046(20) 0.051(7) Uiso 0.50(7) d PD 3
H27A H 0.2350(32) 0.5289(31) 0.8193(20) 0.077 Uiso 0.50(7) calc PR 3
H27B H 0.1149(32) 0.5057(31) 0.8398(20) 0.077 Uiso 0.50(7) calc PR 3
H27C H 0.1352(32) 0.5951(31) 0.8025(20) 0.077 Uiso 0.50(7) calc PR 3
C28 C 0.1607(29) 0.5559(28) 0.6582(29) 0.053(7) Uiso 0.50(7) d PD 3
H28A H 0.1440(29) 0.5302(28) 0.6077(29) 0.080 Uiso 0.50(7) calc PR 3
H28B H 0.2407(29) 0.5696(28) 0.6702(29) 0.080 Uiso 0.50(7) calc PR 3
H28C H 0.1201(29) 0.6112(28) 0.6651(29) 0.080 Uiso 0.50(7) calc PR 3
P41 P 0.1172(4) 0.4721(3) 0.7188(3) 0.990 Uiso 0.00 d PD 4
C261 C -0.0295(14) 0.4835(12) 0.6990(11) 0.990(2) Uiso 0.000(2) d PD 4
C271 C 0.1325(32) 0.5042(35) 0.8164(15) 0.051(7) Uiso 0.50(7) d PD 4
H27D H 0.2108(32) 0.5017(35) 0.8370(15) 0.077 Uiso 0.50(7) calc PR 4
H27E H 0.0877(32) 0.4626(35) 0.8386(15) 0.077 Uiso 0.50(7) calc PR 4
H27F H 0.1072(32) 0.5655(35) 0.8255(15) 0.077 Uiso 0.50(7) calc PR 4
C281 C 0.1760(27) 0.5704(23) 0.6874(32) 0.053(7) Uiso 0.50(7) d PD 4
H28D H 0.2572(27) 0.5694(23) 0.6964(32) 0.080 Uiso 0.50(7) calc PR 4
H28E H 0.1511(27) 0.6247(23) 0.7132(32) 0.080 Uiso 0.50(7) calc PR 4
H28F H 0.1515(27) 0.5705(23) 0.6356(32) 0.080 Uiso 0.50(7) calc PR 4
Cl5 Cl 0.4188(3) 0.4524(2) 0.6676(2) 0.0329(9) Uani 1 d . .
Cl6 Cl 0.3912(3) 0.4087(2) 0.8271(2) 0.0337(9) Uani 1 d . .
Cl7 Cl 0.0642(3) 0.2997(3) 0.7848(2) 0.0432(10) Uani 1 d . .
Cl8 Cl 0.0977(3) 0.1558(2) 0.6526(2) 0.0355(9) Uani 1 d . .
N3 N 0.3948(9) 0.2389(7) 0.6395(6) 0.024(3) Uani 1 d U .
N4 N 0.1337(10) 0.3384(8) 0.5794(7) 0.030(3) Uani 1 d . .
C29 C 0.3466(12) 0.1785(9) 0.5767(8) 0.029(3) Uani 1 d . .
H29A H 0.3646(12) 0.2040(9) 0.5329(8) 0.034 Uiso 1 calc R .
H29B H 0.2648(12) 0.1778(9) 0.5745(8) 0.034 Uiso 1 calc R .
C30 C 0.3833(16) 0.0816(10) 0.5737(9) 0.045(5) Uani 1 d . .
H30A H 0.4646(16) 0.0809(10) 0.5733(9) 0.054 Uiso 1 calc R .
H30B H 0.3671(16) 0.0554(10) 0.6175(9) 0.054 Uiso 1 calc R .
C31 C 0.3251(16) 0.0242(11) 0.5074(9) 0.046(4) Uani 1 d . .
H31A H 0.3358(16) 0.0537(11) 0.4639(9) 0.055 Uiso 1 calc R .
H31B H 0.3604(16) -0.0348(11) 0.5038(9) 0.055 Uiso 1 calc R .
C32 C 0.2048(17) 0.0093(12) 0.5084(10) 0.054(5) Uani 1 d . .
H32A H 0.1723(17) -0.0280(12) 0.4645(10) 0.081 Uiso 1 calc R .
H32B H 0.1689(17) 0.0673(12) 0.5108(10) 0.081 Uiso 1 calc R .
H32C H 0.1936(17) -0.0213(12) 0.5507(10) 0.081 Uiso 1 calc R .
C33 C 0.5213(12) 0.2381(10) 0.6512(8) 0.028(3) Uani 1 d . .
H33A H 0.5500(12) 0.2804(10) 0.6939(8) 0.033 Uiso 1 calc R .
H33B H 0.5446(12) 0.1772(10) 0.6615(8) 0.033 Uiso 1 calc R .
C34 C 0.5722(13) 0.2639(10) 0.5874(8) 0.035(4) Uani 1 d . .
H34A H 0.5353(13) 0.3172(10) 0.5693(8) 0.042 Uiso 1 calc R .
H34B H 0.5600(13) 0.2139(10) 0.5483(8) 0.042 Uiso 1 calc R .
C35 C 0.6961(15) 0.2851(11) 0.6073(10) 0.049(5) Uani 1 d . .
H35A H 0.7257(15) 0.3047(11) 0.5647(10) 0.058 Uiso 1 calc R .
H35B H 0.7076(15) 0.3357(11) 0.6459(10) 0.058 Uiso 1 calc R .
C36 C 0.7592(16) 0.2085(13) 0.6320(12) 0.061(6) Uani 1 d . .
H36A H 0.8381(16) 0.2264(13) 0.6439(12) 0.092 Uiso 1 calc R .
H36B H 0.7498(16) 0.1585(13) 0.5936(12) 0.092 Uiso 1 calc R .
H36C H 0.7317(16) 0.1895(13) 0.6749(12) 0.092 Uiso 1 calc R .
C37 C 0.0177(11) 0.3197(10) 0.5434(8) 0.030(3) Uani 1 d . .
H37A H -0.0129(11) 0.3759(10) 0.5266(8) 0.036 Uiso 1 calc R .
H37B H -0.0280(11) 0.3000(10) 0.5790(8) 0.036 Uiso 1 calc R .
C38 C 0.0090(12) 0.2487(9) 0.4804(8) 0.030(3) Uani 1 d . .
H38A H 0.0398(12) 0.1926(9) 0.4974(8) 0.036 Uiso 1 calc R .
H38B H 0.0549(12) 0.2684(9) 0.4449(8) 0.036 Uiso 1 calc R .
C39 C -0.1083(13) 0.2287(11) 0.4431(9) 0.043(4) Uani 1 d . .
H39A H -0.1525(13) 0.2015(11) 0.4764(9) 0.051 Uiso 1 calc R .
H39B H -0.1427(13) 0.2857(11) 0.4309(9) 0.051 Uiso 1 calc R .
C40 C -0.1111(14) 0.1660(12) 0.3757(10) 0.049(5) Uani 1 d . .
H40A H -0.1882(14) 0.1545(12) 0.3530(10) 0.073 Uiso 1 calc R .
H40B H -0.0783(14) 0.1092(12) 0.3878(10) 0.073 Uiso 1 calc R .
H40C H -0.0686(14) 0.1933(12) 0.3424(10) 0.073 Uiso 1 calc R .
C41 C 0.2088(13) 0.3665(10) 0.5315(9) 0.036(4) Uani 1 d . .
H41A H 0.2233(13) 0.3132(10) 0.4990(9) 0.043 Uiso 1 calc R 5
H41B H 0.2804(13) 0.3866(10) 0.5612(9) 0.043 Uiso 1 calc R 5
C42 C 0.1709(17) 0.4403(14) 0.4856(11) 0.062(6) Uani 1 d D 5
H42A H 0.1629(17) 0.4965(14) 0.5167(11) 0.075 Uiso 1 calc R 5
H42B H 0.0978(17) 0.4231(14) 0.4567(11) 0.075 Uiso 1 calc R 5
C43 C 0.2637(19) 0.4563(16) 0.4320(12) 0.042(5) Uiso 0.72(2) d PD 5
H43A H 0.2787(19) 0.3981(16) 0.4060(12) 0.051 Uiso 0.72(2) calc PR 5
H43B H 0.2338(19) 0.4966(16) 0.3958(12) 0.051 Uiso 0.72(2) calc PR 5
C44 C 0.3661(24) 0.4957(20) 0.4722(17) 0.070(8) Uiso 0.72(2) d PD 5
H44A H 0.4199(24) 0.5044(20) 0.4390(17) 0.105 Uiso 0.72(2) calc PR 5
H44B H 0.3964(24) 0.4554(20) 0.5075(17) 0.105 Uiso 0.72(2) calc PR 5
H44C H 0.3516(24) 0.5538(20) 0.4973(17) 0.105 Uiso 0.72(2) calc PR 5
C421 C 0.1709(17) 0.4403(14) 0.4856(11) 0.990 Uiso 0.00 d PD 6
C431 C 0.2615(41) 0.5135(30) 0.4725(30) 0.042(5) Uiso 0.28(2) d PD 6
H43C H 0.2244(41) 0.5674(30) 0.4556(30) 0.051 Uiso 0.28(2) calc PR 6
H43D H 0.3112(41) 0.5320(30) 0.5181(30) 0.051 Uiso 0.28(2) calc PR 6
C441 C 0.3265(54) 0.4736(46) 0.4179(38) 0.070(8) Uiso 0.28(2) d PD 6
H44D H 0.3826(54) 0.5179(46) 0.4093(38) 0.105 Uiso 0.28(2) calc PR 6
H44E H 0.2769(54) 0.4558(46) 0.3728(38) 0.105 Uiso 0.28(2) calc PR 6
H44F H 0.3634(54) 0.4206(46) 0.4351(38) 0.105 Uiso 0.28(2) calc PR 6
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'
W W -0.8490 6.8722 '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'
P P 0.1023 0.0942 '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'
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 W2 103.0(4) . . y
N1 W1 Cl1 96.7(4) . . y
W2 W1 Cl1 107.70(10) . . y
N1 W1 Cl2 147.5(4) . . y
W2 W1 Cl2 107.32(10) . . y
Cl1 W1 Cl2 85.12(13) . . y
N1 W1 P1 88.3(3) . . y
W2 W1 P1 99.00(10) . . y
Cl1 W1 P1 150.84(13) . . y
Cl2 W1 P1 75.75(13) . . y
N2 W2 W1 104.5(3) . . y
N2 W2 Cl4 96.8(4) . . y
W1 W2 Cl4 107.00(10) . . y
N2 W2 Cl3 146.7(3) . . y
W1 W2 Cl3 106.51(10) . . y
Cl4 W2 Cl3 85.65(15) . . y
N2 W2 P2 87.9(4) . . y
W1 W2 P2 97.36(10) . . y
Cl4 W2 P2 153.07(14) . . y
Cl3 W2 P2 76.40(14) . . y
C1 P1 C2 103.5(9) . . n
C1 P1 C3 101.1(9) . . n
C2 P1 C3 104.3(8) . . n
C1 P1 W1 118.0(6) . . n
C2 P1 W1 119.8(6) . . n
C3 P1 W1 107.8(6) . . n
C5 P2 C6 101.5(9) . . n
C5 P2 C4 101.4(8) . . n
C6 P2 C4 104.4(8) . . n
C5 P2 W2 109.9(6) . . n
C6 P2 W2 116.1(5) . . n
C4 P2 W2 120.9(5) . . n
C7 N1 C11 114.1(11) . . n
C7 N1 W1 136.9(10) . . n
C11 N1 W1 108.5(9) . . n
C15 N2 C19 113.9(10) . . n
C15 N2 W2 136.3(8) . . n
C19 N2 W2 109.7(9) . . n
N1 C7 C8 116.4(11) . . n
C91 C8 C7 112.8(14) . . n
C9 C8 C7 112.8(14) . . n
C10 C9 C8 120.1(24) . . n
C8 C91 C101 108.4(23) . . n
N1 C11 C12 114.9(11) . . n
C11 C12 C13 112.1(11) . . n
C14 C13 C12 116.2(13) . . n
N2 C15 C16 118.2(11) . . n
C17 C16 C15 112.8(12) . . n
C16 C17 C18 114.9(13) . . n
N2 C19 C20 113.5(12) . . n
C21 C20 C19 110.5(13) . . n
C22 C21 C20 113.4(15) . . n
N3 W3 W4 102.4(3) . . y
N3 W3 Cl5 94.6(3) . . y
W4 W3 Cl5 109.45(10) . . y
N3 W3 Cl6 146.8(3) . . y
W4 W3 Cl6 109.70(10) . . y
Cl5 W3 Cl6 82.91(13) . . y
N3 W3 P3 91.1(3) . . y
W4 W3 P3 97.46(10) . . y
Cl5 W3 P3 150.52(13) . . y
Cl6 W3 P3 76.72(13) . . y
N4 W4 W3 103.2(4) . . y
N4 W4 Cl8 95.8(4) . . y
W3 W4 Cl8 108.22(10) . . y
N4 W4 Cl7 145.4(4) . . y
W3 W4 Cl7 109.78(11) . . y
Cl8 W4 Cl7 83.52(15) . . y
N4 W4 P4 89.8(4) . . y
W3 W4 P4 96.88(11) . . y
Cl8 W4 P4 152.17(14) . . y
Cl7 W4 P4 76.7(2) . . y
N4 W4 P41 89.8(4) . . y
W3 W4 P41 96.88(11) . . y
Cl8 W4 P41 152.17(14) . . y
Cl7 W4 P41 76.7(2) . . y
C23 P3 C24 102.2(8) . . n
C23 P3 C25 103.1(8) . . n
C24 P3 C25 103.8(8) . . n
C23 P3 W3 106.9(5) . . n
C24 P3 W3 119.9(5) . . n
C25 P3 W3 118.6(6) . . n
C27 P4 C26 104.7(14) . . n
C27 P4 C28 101.2(15) . . n
C26 P4 C28 97.7(13) . . n
C27 P4 W4 128.4(15) . . n
C26 P4 W4 106.1(6) . . n
C28 P4 W4 114.3(16) . . n
C261 P41 C281 104.3(14) . . n
C261 P41 C271 98.2(13) . . n
C281 P41 C271 101.6(15) . . n
C261 P41 W4 106.1(6) . . n
C281 P41 W4 126.0(15) . . n
C271 P41 W4 116.7(16) . . n
C29 N3 C33 111.9(11) . . n
C29 N3 W3 138.2(9) . . n
C33 N3 W3 109.9(8) . . n
C41 N4 C37 113.6(12) . . n
C41 N4 W4 134.0(10) . . n
C37 N4 W4 112.2(9) . . n
N3 C29 C30 116.7(12) . . n
C31 C30 C29 112.2(13) . . n
C32 C31 C30 113.4(16) . . n
C34 C33 N3 113.1(12) . . n
C33 C34 C35 111.4(13) . . n
C36 C35 C34 113.5(14) . . n
N4 C37 C38 113.0(12) . . n
C37 C38 C39 113.7(13) . . n
C40 C39 C38 111.6(14) . . n
N4 C41 C421 116.9(14) . . n
N4 C41 C42 116.9(14) . . n
C41 C42 C43 108.6(17) . . n
C44 C43 C42 111.2(19) . . n
C41 C421 C431 118.1(27) . . n
C441 C431 C421 108.6(28) . . 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 N1 1.908(11) . y
W1 W2 2.3169(11) . y
W1 Cl1 2.388(4) . y
W1 Cl2 2.430(4) . y
W1 P1 2.535(4) . y
W2 N2 1.946(10) . y
W2 Cl4 2.396(4) . y
W2 Cl3 2.424(4) . y
W2 P2 2.529(4) . y
P1 C1 1.80(2) . n
P1 C2 1.80(2) . n
P1 C3 1.81(2) . n
P2 C5 1.79(2) . n
P2 C6 1.80(2) . n
P2 C4 1.824(15) . n
N1 C7 1.47(2) . n
N1 C11 1.49(2) . n
N2 C15 1.47(2) . n
N2 C19 1.48(2) . n
C7 C8 1.53(2) . n
C8 C91 1.51(2) . n
C8 C9 1.51(2) . n
C9 C10 1.49(5) . n
C91 C101 1.51(5) . n
C11 C12 1.51(2) . n
C12 C13 1.53(2) . n
C13 C14 1.51(2) . n
C15 C16 1.51(2) . n
C16 C17 1.48(2) . n
C17 C18 1.52(2) . n
C19 C20 1.55(2) . n
C20 C21 1.51(2) . n
C21 C22 1.50(2) . n
W3 N3 1.903(12) . y
W3 W4 2.3221(14) . y
W3 Cl5 2.406(3) . y
W3 Cl6 2.421(4) . y
W3 P3 2.523(4) . y
W4 N4 1.937(12) . y
W4 Cl8 2.389(3) . y
W4 Cl7 2.418(4) . y
W4 P4 2.518(4) . y
W4 P41 2.518(4) . y
P3 C23 1.77(2) . n
P3 C24 1.818(15) . n
P3 C25 1.821(15) . n
P4 C27 1.76(3) . n
P4 C26 1.79(2) . n
P4 C28 1.89(3) . n
P41 C261 1.79(2) . n
P41 C281 1.81(2) . n
P41 C271 1.83(3) . n
N3 C29 1.46(2) . n
N3 C33 1.52(2) . n
N4 C41 1.45(2) . n
N4 C37 1.49(2) . n
C29 C30 1.52(2) . n
C30 C31 1.52(2) . n
C31 C32 1.48(3) . n
C33 C34 1.50(2) . n
C34 C35 1.52(2) . n
C35 C36 1.47(3) . n
C37 C38 1.50(2) . n
C38 C39 1.51(2) . n
C39 C40 1.50(2) . n
C41 C421 1.51(2) . n
C41 C42 1.51(2) . n
C42 C43 1.64(3) . n
C43 C44 1.45(3) . n
C421 C431 1.60(3) . n
C431 C441 1.47(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
P1 W1 W2 P2 126.72(13) . . . . y
P1 W1 W2 N2 -143.6(4) . . . . y
P1 W1 W2 Cl3 48.78(15) . . . . y
P1 W1 W2 Cl4 -41.67(14) . . . . y
N1 W1 W2 P2 -142.9(3) . . . . y
N1 W1 W2 N2 -53.3(5) . . . . y
N1 W1 W2 Cl3 139.1(4) . . . . y
N1 W1 W2 Cl4 48.7(3) . . . . y
Cl1 W1 W2 P2 -41.40(14) . . . . y
Cl1 W1 W2 N2 48.3(4) . . . . y
Cl1 W1 W2 Cl3 -119.34(15) . . . . y
Cl1 W1 W2 Cl4 150.21(14) . . . . y
Cl2 W1 W2 P2 48.94(13) . . . . y
Cl2 W1 W2 N2 138.6(4) . . . . y
Cl2 W1 W2 Cl3 -29.00(14) . . . . y
Cl2 W1 W2 Cl4 -119.45(14) . . . . y
P3 W3 W4 P4 120.36(15) . . . . y
P3 W3 W4 N4 -148.2(4) . . . . y
P3 W3 W4 Cl7 42.09(14) . . . . y
P3 W3 W4 Cl8 -47.47(14) . . . . y
N3 W3 W4 P4 -146.9(3) . . . . y
N3 W3 W4 N4 -55.5(5) . . . . y
N3 W3 W4 Cl7 134.8(3) . . . . y
N3 W3 W4 Cl8 45.3(3) . . . . y
Cl5 W3 W4 P4 -47.4(2) . . . . y
Cl5 W3 W4 N4 44.0(4) . . . . y
Cl5 W3 W4 Cl7 -125.70(15) . . . . y
Cl5 W3 W4 Cl8 144.75(15) . . . . y
Cl6 W3 W4 P4 41.85(15) . . . . y
Cl6 W3 W4 N4 133.2(4) . . . . y
Cl6 W3 W4 Cl7 -36.42(15) . . . . y
Cl6 W3 W4 Cl8 -125.97(14) . . . . y
