#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:17:09 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179916 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/11/7021116.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_7021116
loop_
_publ_author_name
'Dolci, Sara'
'Marchetti, Fabio'
'Pampaloni, Guido'
'Zacchini, Stefano'
_publ_section_title
;
 A crystallographic and spectroscopic study on the reactions of WCl6 with
 carbonyl compounds.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5635
_journal_page_last               5648
_journal_paper_doi               10.1039/c2dt32771f
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C10 H19 Cl6 N2 O2 W'
_chemical_formula_weight         595.82
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   19.219(4)
_cell_length_b                   29.661(6)
_cell_length_c                   13.226(3)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.4515
_cell_measurement_theta_min      2.228
_cell_volume                     7540(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            72771
_diffrn_reflns_theta_full        25.66
_diffrn_reflns_theta_max         25.66
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    6.981
_exptl_absorpt_correction_T_max  0.5419
_exptl_absorpt_correction_T_min  0.3505
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_diffrn    2.100
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4560
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.981
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         7274
_refine_ls_number_restraints     342
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0279
_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)+(0.0246P)²+23.1337P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0668
_reflns_number_gt                6189
_reflns_number_total             7274
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32771f.txt
_cod_data_source_block           fm230112_PNMA
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7021116
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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_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 0.181881(9) 0.490354(7) 0.787508(13) 0.02857(6) Uani 1 1 d . . .
W2 W 0.168301(15) 0.2500 0.28167(2) 0.03439(8) Uani 1 2 d S . .
W3 W 0.381645(15) 0.2500 0.81472(2) 0.02984(8) Uani 1 2 d S . .
Cl1 Cl 0.13158(7) 0.48829(6) 0.62968(9) 0.0536(4) Uani 1 1 d . . .
Cl2 Cl 0.27079(6) 0.53638(5) 0.72858(9) 0.0396(3) Uani 1 1 d . . .
Cl3 Cl 0.24811(7) 0.42682(5) 0.74877(12) 0.0531(4) Uani 1 1 d . . .
Cl4 Cl 0.22868(6) 0.49036(5) 0.94793(9) 0.0376(3) Uani 1 1 d . . .
Cl5 Cl 0.09281(6) 0.44289(5) 0.84381(9) 0.0393(3) Uani 1 1 d . . .
Cl6 Cl 0.11744(6) 0.55357(5) 0.83022(10) 0.0416(3) Uani 1 1 d . . .
Cl7 Cl 0.27524(11) 0.2500 0.36413(16) 0.0602(6) Uani 1 2 d S . .
Cl8 Cl 0.11076(10) 0.2500 0.43726(13) 0.0453(5) Uani 1 2 d S . .
Cl9 Cl 0.16734(8) 0.32752(5) 0.28298(11) 0.0519(4) Uani 1 1 d . . .
Cl10 Cl 0.06145(10) 0.2500 0.19838(13) 0.0421(4) Uani 1 2 d S . .
Cl11 Cl 0.22492(10) 0.2500 0.12670(14) 0.0464(5) Uani 1 2 d S . .
Cl12 Cl 0.50006(10) 0.2500 0.77679(16) 0.0497(5) Uani 1 2 d S . .
Cl13 Cl 0.35647(9) 0.2500 0.64324(14) 0.0447(5) Uani 1 2 d S . .
Cl14 Cl 0.38290(11) 0.32788(5) 0.81310(16) 0.0729(5) Uani 1 1 d . . .
Cl15 Cl 0.40807(14) 0.2500 0.98518(17) 0.0744(8) Uani 1 2 d S . .
Cl16 Cl 0.26412(11) 0.2500 0.85033(17) 0.0630(6) Uani 1 2 d S . .
C11 C 0.1328(3) 0.37198(17) 0.5287(4) 0.0360(11) Uani 1 1 d U . .
C12 C 0.0953(3) 0.3448(2) 0.6069(4) 0.0486(14) Uani 1 1 d U . .
H12A H 0.0648 0.3219 0.5753 0.058 Uiso 1 1 calc R . .
H12B H 0.0670 0.3643 0.6516 0.058 Uiso 1 1 calc R . .
C13 C 0.1545(4) 0.3229(2) 0.6647(5) 0.0673(18) Uani 1 1 d U . .
H13A H 0.1600 0.3370 0.7320 0.081 Uiso 1 1 calc R . .
H13B H 0.1455 0.2903 0.6740 0.081 Uiso 1 1 calc R . .
C14 C 0.2186(3) 0.3301(2) 0.6017(5) 0.0533(15) Uani 1 1 d U . .
H14A H 0.2581 0.3400 0.6444 0.064 Uiso 1 1 calc R . .
H14B H 0.2318 0.3020 0.5660 0.064 Uiso 1 1 calc R . .
C15 C 0.2493(3) 0.3864(2) 0.4656(5) 0.0548(16) Uani 1 1 d U . .
H15A H 0.2960 0.3753 0.4818 0.082 Uiso 1 1 calc R . .
H15B H 0.2476 0.4191 0.4757 0.082 Uiso 1 1 calc R . .
H15C H 0.2384 0.3793 0.3949 0.082 Uiso 1 1 calc R . .
O1 O 0.10477(19) 0.39909(13) 0.4663(3) 0.0424(9) Uani 1 1 d U . .
H1 H 0.0628 0.4029 0.4819 0.064 Uiso 1 1 calc R . .
N1 N 0.1993(2) 0.36499(15) 0.5304(3) 0.0401(10) Uani 1 1 d U . .
C21 C 0.4459(3) 0.37595(17) 0.0867(4) 0.0367(11) Uani 1 1 d U . .
C22 C 0.4779(3) 0.3440(2) 0.1602(5) 0.0499(14) Uani 1 1 d U . .
H22A H 0.5130 0.3594 0.2027 0.060 Uiso 1 1 calc R . .
H22B H 0.5004 0.3184 0.1247 0.060 Uiso 1 1 calc R . .
C23 C 0.4167(3) 0.3278(2) 0.2236(5) 0.0569(16) Uani 1 1 d U . .
H23A H 0.4176 0.2946 0.2305 0.068 Uiso 1 1 calc R . .
H23B H 0.4183 0.3415 0.2919 0.068 Uiso 1 1 calc R . .
C24 C 0.3522(3) 0.3429(2) 0.1674(5) 0.0507(14) Uani 1 1 d U . .
H24A H 0.3292 0.3170 0.1339 0.061 Uiso 1 1 calc R . .
H24B H 0.3187 0.3575 0.2139 0.061 Uiso 1 1 calc R . .
C25 C 0.3326(3) 0.4011(2) 0.0279(5) 0.0563(17) Uani 1 1 d U . .
H25A H 0.2841 0.3949 0.0462 0.084 Uiso 1 1 calc R . .
H25B H 0.3403 0.3926 -0.0429 0.084 Uiso 1 1 calc R . .
H25C H 0.3422 0.4333 0.0365 0.084 Uiso 1 1 calc R . .
O2 O 0.47851(19) 0.40137(13) 0.0255(3) 0.0442(9) Uani 1 1 d U . .
N2 N 0.3787(2) 0.37510(15) 0.0927(3) 0.0363(10) Uani 1 1 d U . .
C31 C 0.0673(3) 0.3715(2) 0.0427(4) 0.0505(14) Uani 1 1 d U . .
C32 C 0.1449(3) 0.3783(2) 0.0420(5) 0.0581(16) Uani 1 1 d U . .
H32A H 0.1652 0.3713 0.1090 0.070 Uiso 1 1 calc R . .
H32B H 0.1569 0.4097 0.0236 0.070 Uiso 1 1 calc R . .
C33 C 0.1709(4) 0.3454(2) -0.0378(6) 0.0670(18) Uani 1 1 d U . .
H33A H 0.2119 0.3284 -0.0132 0.080 Uiso 1 1 calc R . .
H33B H 0.1834 0.3613 -0.1010 0.080 Uiso 1 1 calc R . .
C34 C 0.1089(4) 0.3138(2) -0.0546(6) 0.0746(19) Uani 1 1 d U . .
H34A H 0.1018 0.3081 -0.1276 0.090 Uiso 1 1 calc R . .
H34B H 0.1162 0.2847 -0.0197 0.090 Uiso 1 1 calc R . .
C35 C -0.0186(4) 0.3201(2) -0.0248(5) 0.070(2) Uani 1 1 d U . .
H35A H -0.0186 0.2934 -0.0683 0.105 Uiso 1 1 calc R . .
H35B H -0.0476 0.3436 -0.0554 0.105 Uiso 1 1 calc R . .
H35C H -0.0373 0.3122 0.0418 0.105 Uiso 1 1 calc R . .
O3 O 0.0234(2) 0.3935(2) 0.0880(3) 0.0822(16) Uani 1 1 d U . .
N3 N 0.0519(3) 0.33663(16) -0.0137(4) 0.0511(12) Uani 1 1 d U . .
C41 C 0.0631(6) 0.4954(3) 0.1833(6) 0.0297(18) Uani 0.570(5) 1 d PDU A 1
C42 C 0.0506(4) 0.4710(3) 0.2809(6) 0.0327(17) Uani 0.570(5) 1 d PDU A 1
H42A H 0.0798 0.4436 0.2856 0.039 Uiso 0.570(5) 1 calc PR A 1
H42B H 0.0011 0.4623 0.2877 0.039 Uiso 0.570(5) 1 calc PR A 1
C43 C 0.0711(11) 0.5057(4) 0.3618(9) 0.034(2) Uani 0.570(5) 1 d PDU A 1
H43A H 0.1187 0.4999 0.3871 0.041 Uiso 0.570(5) 1 calc PR A 1
H43B H 0.0383 0.5048 0.4195 0.041 Uiso 0.570(5) 1 calc PR A 1
C44 C 0.0674(5) 0.5513(3) 0.3069(6) 0.0350(18) Uani 0.570(5) 1 d PDU A 1
H44A H 0.0224 0.5665 0.3199 0.042 Uiso 0.570(5) 1 calc PR A 1
H44B H 0.1057 0.5715 0.3286 0.042 Uiso 0.570(5) 1 calc PR A 1
C45 C 0.0830(5) 0.5732(4) 0.1204(7) 0.033(2) Uani 0.570(5) 1 d PDU A 1
H45A H 0.0902 0.6029 0.1510 0.050 Uiso 0.570(5) 1 calc PR A 1
H45B H 0.0412 0.5739 0.0781 0.050 Uiso 0.570(5) 1 calc PR A 1
H45C H 0.1234 0.5654 0.0788 0.050 Uiso 0.570(5) 1 calc PR A 1
O4 O 0.0622(5) 0.4795(3) 0.0939(5) 0.044(2) Uani 0.570(5) 1 d PDU A 1
H4 H 0.0610 0.4512 0.0964 0.066 Uiso 0.570(5) 1 calc PR A 1
N4 N 0.0744(4) 0.5393(3) 0.2006(5) 0.0334(17) Uani 0.570(5) 1 d PDU A 1
C51 C 0.0605(8) 0.4793(3) 0.2101(8) 0.031(2) Uani 0.430(5) 1 d PDU A 2
C52 C 0.0611(10) 0.4995(4) 0.1046(10) 0.037(3) Uani 0.430(5) 1 d PDU A 2
H52A H 0.0140 0.4991 0.0744 0.045 Uiso 0.430(5) 1 calc PR A 2
H52B H 0.0934 0.4829 0.0597 0.045 Uiso 0.430(5) 1 calc PR A 2
C53 C 0.0862(7) 0.5479(4) 0.1218(9) 0.036(2) Uani 0.430(5) 1 d PDU A 2
H53A H 0.0588 0.5695 0.0808 0.043 Uiso 0.430(5) 1 calc PR A 2
H53B H 0.1360 0.5510 0.1041 0.043 Uiso 0.430(5) 1 calc PR A 2
C54 C 0.0743(7) 0.5560(4) 0.2367(8) 0.033(2) Uani 0.430(5) 1 d PDU A 2
H54A H 0.1145 0.5719 0.2670 0.039 Uiso 0.430(5) 1 calc PR A 2
H54B H 0.0318 0.5741 0.2482 0.039 Uiso 0.430(5) 1 calc PR A 2
C55 C 0.0646(14) 0.5023(7) 0.3879(9) 0.031(4) Uani 0.430(5) 1 d PDU A 2
H55A H 0.0706 0.5305 0.4255 0.047 Uiso 0.430(5) 1 calc PR A 2
H55B H 0.1021 0.4814 0.4057 0.047 Uiso 0.430(5) 1 calc PR A 2
H55C H 0.0197 0.4888 0.4053 0.047 Uiso 0.430(5) 1 calc PR A 2
O5 O 0.0538(4) 0.4388(3) 0.2337(6) 0.034(2) Uani 0.430(5) 1 d PDU A 2
H5 H 0.0150 0.4350 0.2619 0.051 Uiso 0.430(5) 1 calc PR A 2
N5 N 0.0669(5) 0.5115(3) 0.2796(6) 0.0290(16) Uani 0.430(5) 1 d PDU A 2
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
Cl1 W1 Cl4 177.59(5) . .
Cl1 W1 Cl6 91.04(6) . .
Cl4 W1 Cl6 89.09(5) . .
Cl1 W1 Cl2 91.16(5) . .
Cl4 W1 Cl2 91.25(4) . .
Cl6 W1 Cl2 89.97(5) . .
Cl1 W1 Cl3 90.49(6) . .
Cl4 W1 Cl3 89.39(5) . .
Cl6 W1 Cl3 178.47(5) . .
Cl2 W1 Cl3 89.98(5) . .
Cl1 W1 Cl5 88.01(5) . .
Cl4 W1 Cl5 89.58(5) . .
Cl6 W1 Cl5 91.05(5) . .
Cl2 W1 Cl5 178.70(5) . .
Cl3 W1 Cl5 89.03(5) . .
Cl9 W2 Cl9 178.74(7) . 7_565
Cl9 W2 Cl11 90.60(4) . .
Cl9 W2 Cl11 90.60(4) 7_565 .
Cl9 W2 Cl7 90.21(4) . .
Cl9 W2 Cl7 90.21(4) 7_565 .
Cl11 W2 Cl7 89.99(7) . .
Cl9 W2 Cl10 89.80(4) . .
Cl9 W2 Cl10 89.80(4) 7_565 .
Cl11 W2 Cl10 89.75(7) . .
Cl7 W2 Cl10 179.74(7) . .
Cl9 W2 Cl8 89.40(4) . .
Cl9 W2 Cl8 89.40(4) 7_565 .
Cl11 W2 Cl8 179.71(7) . .
Cl7 W2 Cl8 90.30(7) . .
Cl10 W2 Cl8 89.96(7) . .
Cl16 W3 Cl14 90.70(5) . 7_565
Cl16 W3 Cl14 90.70(5) . .
Cl14 W3 Cl14 178.40(11) 7_565 .
Cl16 W3 Cl15 90.92(9) . .
Cl14 W3 Cl15 90.39(5) 7_565 .
Cl14 W3 Cl15 90.39(5) . .
Cl16 W3 Cl13 89.74(7) . .
Cl14 W3 Cl13 89.61(5) 7_565 .
Cl14 W3 Cl13 89.61(5) . .
Cl15 W3 Cl13 179.35(8) . .
Cl16 W3 Cl12 179.35(8) . .
Cl14 W3 Cl12 89.30(5) 7_565 .
Cl14 W3 Cl12 89.30(5) . .
Cl15 W3 Cl12 89.74(9) . .
Cl13 W3 Cl12 89.61(7) . .
O1 C11 N1 122.1(5) . .
O1 C11 C12 125.8(5) . .
N1 C11 C12 112.1(5) . .
C11 C12 C13 102.6(5) . .
C11 C12 H12A 111.2 . .
C13 C12 H12A 111.2 . .
C11 C12 H12B 111.2 . .
C13 C12 H12B 111.2 . .
H12A C12 H12B 109.2 . .
C14 C13 C12 105.9(5) . .
C14 C13 H13A 110.5 . .
C12 C13 H13A 110.5 . .
C14 C13 H13B 110.5 . .
C12 C13 H13B 110.5 . .
H13A C13 H13B 108.7 . .
N1 C14 C13 104.7(5) . .
N1 C14 H14A 110.8 . .
C13 C14 H14A 110.8 . .
N1 C14 H14B 110.8 . .
C13 C14 H14B 110.8 . .
H14A C14 H14B 108.9 . .
N1 C15 H15A 109.5 . .
N1 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
N1 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C11 O1 H1 109.5 . .
C11 N1 C15 125.4(5) . .
C11 N1 C14 112.2(5) . .
C15 N1 C14 122.3(5) . .
O2 C21 N2 122.9(5) . .
O2 C21 C22 126.1(5) . .
N2 C21 C22 111.0(5) . .
C21 C22 C23 104.0(5) . .
C21 C22 H22A 111.0 . .
C23 C22 H22A 111.0 . .
C21 C22 H22B 111.0 . .
C23 C22 H22B 111.0 . .
H22A C22 H22B 109.0 . .
C24 C23 C22 105.7(5) . .
C24 C23 H23A 110.6 . .
C22 C23 H23A 110.6 . .
C24 C23 H23B 110.6 . .
C22 C23 H23B 110.6 . .
H23A C23 H23B 108.7 . .
N2 C24 C23 103.8(5) . .
N2 C24 H24A 111.0 . .
C23 C24 H24A 111.0 . .
N2 C24 H24B 111.0 . .
C23 C24 H24B 111.0 . .
H24A C24 H24B 109.0 . .
N2 C25 H25A 109.5 . .
N2 C25 H25B 109.5 . .
H25A C25 H25B 109.5 . .
N2 C25 H25C 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
C21 N2 C25 124.1(5) . .
C21 N2 C24 113.6(4) . .
C25 N2 C24 122.1(5) . .
O3 C31 N3 123.0(6) . .
O3 C31 C32 128.0(6) . .
N3 C31 C32 108.9(6) . .
C31 C32 C33 104.2(5) . .
C31 C32 H32A 110.9 . .
C33 C32 H32A 110.9 . .
C31 C32 H32B 110.9 . .
C33 C32 H32B 110.9 . .
H32A C32 H32B 108.9 . .
C32 C33 C34 103.7(6) . .
C32 C33 H33A 111.0 . .
C34 C33 H33A 111.0 . .
C32 C33 H33B 111.0 . .
C34 C33 H33B 111.0 . .
H33A C33 H33B 109.0 . .
N3 C34 C33 105.0(6) . .
N3 C34 H34A 110.7 . .
C33 C34 H34A 110.7 . .
N3 C34 H34B 110.7 . .
C33 C34 H34B 110.7 . .
H34A C34 H34B 108.8 . .
N3 C35 H35A 109.5 . .
N3 C35 H35B 109.5 . .
H35A C35 H35B 109.5 . .
N3 C35 H35C 109.5 . .
H35A C35 H35C 109.5 . .
H35B C35 H35C 109.5 . .
C31 N3 C34 115.2(6) . .
C31 N3 C35 122.4(6) . .
C34 N3 C35 122.1(6) . .
O4 C41 N4 121.4(8) . .
O4 C41 C42 128.2(9) . .
N4 C41 C42 110.4(7) . .
C41 C42 C43 103.6(7) . .
C41 C42 H42A 111.0 . .
C43 C42 H42A 111.0 . .
C41 C42 H42B 111.0 . .
C43 C42 H42B 111.0 . .
H42A C42 H42B 109.0 . .
C42 C43 C44 104.4(9) . .
C42 C43 H43A 110.9 . .
C44 C43 H43A 110.9 . .
C42 C43 H43B 110.9 . .
C44 C43 H43B 110.9 . .
H43A C43 H43B 108.9 . .
N4 C44 C43 103.6(8) . .
N4 C44 H44A 111.0 . .
C43 C44 H44A 111.0 . .
N4 C44 H44B 111.0 . .
C43 C44 H44B 111.0 . .
H44A C44 H44B 109.0 . .
N4 C45 H45A 109.5 . .
N4 C45 H45B 109.5 . .
H45A C45 H45B 109.5 . .
N4 C45 H45C 109.5 . .
H45A C45 H45C 109.5 . .
H45B C45 H45C 109.5 . .
C41 N4 C44 112.9(7) . .
C41 N4 C45 124.0(8) . .
C44 N4 C45 122.6(8) . .
O5 C51 N5 121.9(10) . .
O5 C51 C52 127.7(10) . .
N5 C51 C52 110.4(9) . .
C51 C52 C53 103.7(10) . .
C51 C52 H52A 111.0 . .
C53 C52 H52A 111.0 . .
C51 C52 H52B 111.0 . .
C53 C52 H52B 111.0 . .
H52A C52 H52B 109.0 . .
C52 C53 C54 104.1(10) . .
C52 C53 H53A 110.9 . .
C54 C53 H53A 110.9 . .
C52 C53 H53B 110.9 . .
C54 C53 H53B 110.9 . .
H53A C53 H53B 109.0 . .
N5 C54 C53 105.0(9) . .
N5 C54 H54A 110.8 . .
C53 C54 H54A 110.8 . .
N5 C54 H54B 110.8 . .
C53 C54 H54B 110.8 . .
H54A C54 H54B 108.8 . .
N5 C55 H55A 109.5 . .
N5 C55 H55B 109.5 . .
H55A C55 H55B 109.5 . .
N5 C55 H55C 109.5 . .
H55A C55 H55C 109.5 . .
H55B C55 H55C 109.5 . .
C51 O5 H5 109.5 . .
C51 N5 C54 113.2(8) . .
C51 N5 C55 122.6(11) . .
C54 N5 C55 124.1(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 Cl1 2.3013(13) .
W1 Cl4 2.3046(12) .
W1 Cl6 2.3171(14) .
W1 Cl2 2.3219(13) .
W1 Cl3 2.3311(15) .
W1 Cl5 2.3383(13) .
W2 Cl9 2.2993(16) .
W2 Cl9 2.2993(16) 7_565
W2 Cl11 2.3207(18) .
W2 Cl7 2.327(2) .
W2 Cl10 2.3305(19) .
W2 Cl8 2.3362(18) .
W3 Cl16 2.307(2) .
W3 Cl14 2.3102(16) 7_565
W3 Cl14 2.3102(16) .
W3 Cl15 2.311(2) .
W3 Cl13 2.3190(19) .
W3 Cl12 2.330(2) .
C11 O1 1.272(6) .
C11 N1 1.295(7) .
C11 C12 1.497(7) .
C12 C13 1.517(9) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 C14 1.502(9) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 N1 1.449(7) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 N1 1.435(7) .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
O1 H1 0.8400 .
C21 O2 1.271(6) .
C21 N2 1.295(6) .
C21 C22 1.491(7) .
C22 C23 1.521(8) .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
C23 C24 1.513(8) .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C24 N2 1.466(7) .
C24 H24A 0.9900 .
C24 H24B 0.9900 .
C25 N2 1.455(7) .
C25 H25A 0.9800 .
C25 H25B 0.9800 .
C25 H25C 0.9800 .
C31 O3 1.221(7) .
C31 N3 1.310(7) .
C31 C32 1.506(9) .
C32 C33 1.521(9) .
C32 H32A 0.9900 .
C32 H32B 0.9900 .
C33 C34 1.531(10) .
C33 H33A 0.9900 .
C33 H33B 0.9900 .
C34 N3 1.396(8) .
C34 H34A 0.9900 .
C34 H34B 0.9900 .
C35 N3 1.448(8) .
C35 H35A 0.9800 .
C35 H35B 0.9800 .
C35 H35C 0.9800 .
C41 O4 1.273(9) .
C41 N4 1.339(10) .
C41 C42 1.499(10) .
C42 C43 1.536(12) .
C42 H42A 0.9900 .
C42 H42B 0.9900 .
C43 C44 1.538(12) .
C43 H43A 0.9900 .
C43 H43B 0.9900 .
C44 N4 1.457(8) .
C44 H44A 0.9900 .
C44 H44B 0.9900 .
C45 N4 1.471(9) .
C45 H45A 0.9800 .
C45 H45B 0.9800 .
C45 H45C 0.9800 .
O4 H4 0.8400 .
C51 O5 1.245(10) .
C51 N5 1.334(10) .
C51 C52 1.519(12) .
C52 C53 1.531(13) .
C52 H52A 0.9900 .
C52 H52B 0.9900 .
C53 C54 1.556(12) .
C53 H53A 0.9900 .
C53 H53B 0.9900 .
C54 N5 1.442(10) .
C54 H54A 0.9900 .
C54 H54B 0.9900 .
C55 N5 1.459(11) .
C55 H55A 0.9800 .
C55 H55B 0.9800 .
C55 H55C 0.9800 .
O5 H5 0.8400 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O2 0.84 1.62 2.430(5) 159.9 6_556
O4 H4 O3 0.84 1.86 2.660(10) 157.9 .
O5 H5 Cl6 0.84 2.84 3.404(8) 126.0 5_566
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
O1 C11 C12 C13 -174.6(5)
N1 C11 C12 C13 5.5(6)
C11 C12 C13 C14 -12.9(7)
C12 C13 C14 N1 15.6(7)
O1 C11 N1 C15 0.8(8)
C12 C11 N1 C15 -179.3(5)
O1 C11 N1 C14 -175.2(5)
C12 C11 N1 C14 4.8(6)
C13 C14 N1 C11 -13.0(6)
C13 C14 N1 C15 170.9(5)
O2 C21 C22 C23 171.9(6)
N2 C21 C22 C23 -7.7(7)
C21 C22 C23 C24 12.9(7)
C22 C23 C24 N2 -13.4(7)
O2 C21 N2 C25 3.1(9)
C22 C21 N2 C25 -177.3(5)
O2 C21 N2 C24 179.3(5)
C22 C21 N2 C24 -1.1(7)
C23 C24 N2 C21 9.4(7)
C23 C24 N2 C25 -174.3(5)
O3 C31 C32 C33 -172.6(7)
N3 C31 C32 C33 8.3(7)
C31 C32 C33 C34 -15.1(7)
C32 C33 C34 N3 16.9(8)
O3 C31 N3 C34 -176.1(7)
C32 C31 N3 C34 3.0(8)
O3 C31 N3 C35 -2.0(10)
C32 C31 N3 C35 177.1(5)
C33 C34 N3 C31 -13.0(8)
C33 C34 N3 C35 172.9(6)
O4 C41 C42 C43 170.5(13)
N4 C41 C42 C43 -11.4(13)
C41 C42 C43 C44 20.4(14)
C42 C43 C44 N4 -22.2(14)
O4 C41 N4 C44 175.0(10)
C42 C41 N4 C44 -3.3(12)
O4 C41 N4 C45 3.2(16)
C42 C41 N4 C45 -175.1(8)
C43 C44 N4 C41 16.4(13)
C43 C44 N4 C45 -171.6(10)
O5 C51 C52 C53 -168.4(14)
N5 C51 C52 C53 13.0(18)
C51 C52 C53 C54 -18.2(16)
C52 C53 C54 N5 17.8(15)
O5 C51 N5 C54 179.9(12)
C52 C51 N5 C54 -1.5(17)
O5 C51 N5 C55 -2(2)
C52 C51 N5 C55 177.0(16)
C53 C54 N5 C51 -10.6(14)
C53 C54 N5 C55 171.0(15)
