#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:08:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180027 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/21/7032146.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_7032146
loop_
_publ_author_name
'Hasenaka, Yuki'
'Okamura, Taka-Aki'
'Tatsumi, Miki'
'Inazumi, Naoya'
'Onitsuka, Kiyotaka'
_publ_section_title
;
 Behavior of anionic molybdenum(iv, vi) and tungsten(iv, vi) complexes
 containing bulky hydrophobic dithiolate ligands and intramolecular NHS
 hydrogen bonds in nonpolar solvents.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15491
_journal_page_last               15502
_journal_paper_doi               10.1039/c4dt01646g
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C190 H247 N9 O6 S4 W'
_chemical_formula_sum            'C190 H247 N9 O6 S4 W'
_chemical_formula_weight         3065.04
_chemical_name_systematic
;
(NEt4)2[WO{S2C6H2[NHCOC(C6H4-t-Bu)3]2}2]-4(toluene)-3(CH3CN)-H2O
;
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Efflorescent'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-08-06
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 108.061(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   39.235(5)
_cell_length_b                   23.938(3)
_cell_length_c                   20.131(3)
_cell_measurement_reflns_used    54853
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      3.02
_cell_volume                     17976(4)
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2006)'
_computing_data_collection       'RAPID AUTO (Rigaku, 2006)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2006)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0797
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            67944
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.018
_diffrn_source
;
 MicroMax-007HF microfocus rotating anode X-ray generator
;
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_T_max  0.9293
_exptl_absorpt_correction_T_min  0.8654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             6544
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene, acetonitrile'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.948
_refine_diff_density_min         -2.106
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     929
_refine_ls_number_reflns         15799
_refine_ls_number_restraints     607
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.1484
_refine_ls_R_factor_gt           0.1265
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1143P)²+337.8758P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3199
_refine_ls_wR_factor_ref         0.3323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12222
_reflns_number_total             15799
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4dt01646g2.cif
_cod_data_source_block           1-W-4(toluene)-3(CH3CN)-H2O
_cod_depositor_comments
'Adding full bibliography for 7032142--7032147.cif.'
_cod_database_code               7032146
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.865
_shelx_estimated_absorpt_t_max   0.929
_shelxl_version_number           2014/6
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.5000 0.72928(4) 0.2500 0.0624(3) Uani 0.9801(17) 2 d DS TU P A 1
W1B W 0.5000 0.7944(11) 0.2500 0.0624(3) Uani 0.0199(17) 2 d DS TU P A 2
S1 S 0.53890(7) 0.75875(17) 0.35904(13) 0.0759(10) Uani 1 1 d D U . . .
S2 S 0.45440(6) 0.76014(16) 0.29650(13) 0.0702(9) Uani 1 1 d . U . . .
O1 O 0.5771(2) 0.7905(4) 0.6264(4) 0.083(3) Uani 1 1 d . U . . .
O2 O 0.40095(19) 0.8391(4) 0.4727(5) 0.085(3) Uani 1 1 d . U . . .
O3 O 0.5000 0.6608(4) 0.2500 0.070(2) Uani 0.9801(17) 2 d DS TU P . .
O3B O 0.5000 0.8654(11) 0.2500 0.070(2) Uani 0.0199(17) 2 d DS TU P A 2
O4 O 0.5000 0.8387(6) 0.2500 0.079(4) Uani 0.9801(17) 2 d S TU P A 1
N1 N 0.5664(2) 0.7714(5) 0.5128(4) 0.074(3) Uani 1 1 d . U . . .
H1 H 0.5771 0.7631 0.4816 0.089 Uiso 1 1 calc R U . . .
N2 N 0.4165(2) 0.7755(5) 0.4036(4) 0.063(2) Uani 1 1 d . U . . .
H2 H 0.4078 0.7541 0.3667 0.075 Uiso 1 1 calc R U . . .
N3 N 0.5037(8) 0.6128(10) 0.4930(17) 0.60(3) Uani 1 1 d D U . . .
N4 N 0.4383(16) 0.713(3) 0.656(4) 0.53(4) Uani 1 1 d D U . . .
N5 N 0.4765(7) 0.810(3) 0.7838(18) 0.65(6) Uani 0.5 1 d D U P . .
C11 C 0.5123(3) 0.7715(6) 0.4154(5) 0.071(3) Uani 1 1 d . U . . .
C12 C 0.4749(3) 0.7740(6) 0.3873(5) 0.068(3) Uani 1 1 d . U . . .
C13 C 0.4539(3) 0.7806(6) 0.4308(5) 0.064(3) Uani 1 1 d . U . . .
C14 C 0.4703(3) 0.7900(7) 0.5019(6) 0.086(5) Uani 1 1 d . U . . .
H3 H 0.4561 0.7979 0.5313 0.103 Uiso 1 1 calc R U . . .
C15 C 0.5076(3) 0.7877(7) 0.5299(6) 0.096(5) Uani 1 1 d . U . . .
H4 H 0.5186 0.7934 0.5786 0.115 Uiso 1 1 calc R U . . .
C16 C 0.5289(3) 0.7771(6) 0.4872(5) 0.074(4) Uani 1 1 d . U . . .
C17 C 0.5879(3) 0.7772(6) 0.5791(5) 0.065(3) Uani 1 1 d . U . . .
C18 C 0.6285(3) 0.7634(5) 0.5934(5) 0.055(2) Uani 1 1 d . U . . .
C27 C 0.3928(2) 0.8014(5) 0.4303(5) 0.052(2) Uani 1 1 d . U . . .
C28 C 0.3535(2) 0.7791(4) 0.4029(4) 0.0426(17) Uani 1 1 d . U . . .
C31 C 0.4731(9) 0.5907(15) 0.4337(19) 0.64(4) Uani 1 1 d D U . . .
H5 H 0.4828 0.5610 0.4105 0.769 Uiso 1 1 calc R U . . .
H6 H 0.4560 0.5727 0.4542 0.769 Uiso 1 1 calc R U . . .
C32 C 0.4525(9) 0.630(2) 0.3787(16) 0.40(2) Uani 1 1 d D U . . .
H7 H 0.4336 0.6092 0.3439 0.479 Uiso 1 1 calc R U . . .
H8 H 0.4416 0.6589 0.3998 0.479 Uiso 1 1 calc R U . . .
H9 H 0.4686 0.6471 0.3559 0.479 Uiso 1 1 calc R U . . .
C33 C 0.5307(8) 0.6412(7) 0.465(2) 0.64(4) Uani 1 1 d D U . . .
H10 H 0.5174 0.6691 0.4301 0.767 Uiso 1 1 calc R U . . .
H11 H 0.5471 0.6623 0.5040 0.767 Uiso 1 1 calc R U . . .
C34 C 0.5529(8) 0.6095(12) 0.432(2) 0.40(2) Uani 1 1 d D U . . .
H12 H 0.5686 0.6351 0.4173 0.485 Uiso 1 1 calc R U . . .
H13 H 0.5675 0.5826 0.4658 0.485 Uiso 1 1 calc R U . . .
H14 H 0.5375 0.5894 0.3914 0.485 Uiso 1 1 calc R U . . .
C35 C 0.5224(11) 0.5647(11) 0.540(2) 0.69(4) Uani 1 1 d D U . . .
H15 H 0.5059 0.5490 0.5632 0.828 Uiso 1 1 calc R U . . .
H16 H 0.5274 0.5350 0.5097 0.828 Uiso 1 1 calc R U . . .
C36 C 0.5571(11) 0.581(2) 0.5942(19) 0.84(7) Uani 1 1 d D U . . .
H17 H 0.5674 0.5475 0.6218 1.011 Uiso 1 1 calc R U . . .
H18 H 0.5739 0.5951 0.5713 1.011 Uiso 1 1 calc R U . . .
H19 H 0.5524 0.6092 0.6250 1.011 Uiso 1 1 calc R U . . .
C37 C 0.4902(10) 0.6538(9) 0.5360(18) 0.65(4) Uani 1 1 d D U . . .
H20 H 0.5091 0.6822 0.5539 0.779 Uiso 1 1 calc R U . . .
H21 H 0.4692 0.6732 0.5040 0.779 Uiso 1 1 calc R U . . .
C38 C 0.4797(15) 0.633(2) 0.596(3) 0.59(5) Uani 1 1 d D U . . .
H22 H 0.4716 0.6649 0.6183 0.707 Uiso 1 1 calc R U . . .
H23 H 0.4601 0.6063 0.5796 0.707 Uiso 1 1 calc R U . . .
H24 H 0.5002 0.6154 0.6298 0.707 Uiso 1 1 calc R U . . .
C41 C 0.4155(14) 0.744(4) 0.659(5) 0.57(6) Uani 1 1 d D U . . .
C42 C 0.3941(7) 0.7858(16) 0.6827(17) 0.275(18) Uani 1 1 d D U . . .
H25 H 0.3962 0.7793 0.7319 0.329 Uiso 1 1 calc R U . . .
H26 H 0.3689 0.7826 0.6543 0.329 Uiso 1 1 calc R U . . .
H27 H 0.4029 0.8233 0.6774 0.329 Uiso 1 1 calc R U . . .
C51 C 0.5000 0.801(4) 0.7500 0.41(5) Uani 1 2 d DS TU P . .
C52 C 0.4765(7) 0.810(3) 0.7838(18) 0.65(6) Uani 0.5 1 d D U P . .
H28 H 0.4681 0.7738 0.7958 0.783 Uiso 0.5 1 calc R U P . .
H29 H 0.4878 0.8310 0.8266 0.783 Uiso 0.5 1 calc R U P . .
H30 H 0.4561 0.8310 0.7540 0.783 Uiso 0.5 1 calc R U P . .
C111 C 0.6359(2) 0.7317(5) 0.5330(4) 0.051(2) Uani 1 1 d . U . . .
C112 C 0.6446(3) 0.6766(5) 0.5336(5) 0.064(3) Uani 1 1 d . U . . .
H31 H 0.6466 0.6557 0.5747 0.076 Uiso 1 1 calc R U . . .
C113 C 0.6506(3) 0.6500(5) 0.4791(5) 0.064(3) Uani 1 1 d . U . . .
H32 H 0.6567 0.6115 0.4835 0.077 Uiso 1 1 calc R U . . .
C114 C 0.6482(3) 0.6772(4) 0.4164(5) 0.054(2) Uani 1 1 d . U . . .
C115 C 0.6401(3) 0.7354(4) 0.4154(5) 0.052(2) Uani 1 1 d . U . . .
H33 H 0.6388 0.7567 0.3749 0.063 Uiso 1 1 calc R U . . .
C116 C 0.6342(2) 0.7603(4) 0.4693(5) 0.049(2) Uani 1 1 d . U . . .
H34 H 0.6286 0.7990 0.4659 0.059 Uiso 1 1 calc R U . . .
C117 C 0.6551(3) 0.6487(5) 0.3550(6) 0.066(3) Uani 1 1 d . U . . .
C118 C 0.6232(4) 0.6596(7) 0.2882(6) 0.092(4) Uani 1 1 d . U . . .
H35 H 0.6191 0.6999 0.2819 0.111 Uiso 1 1 calc R U . . .
H36 H 0.6286 0.6441 0.2476 0.111 Uiso 1 1 calc R U . . .
H37 H 0.6016 0.6417 0.2929 0.111 Uiso 1 1 calc R U . . .
C119 C 0.6889(3) 0.6740(6) 0.3428(6) 0.077(3) Uani 1 1 d . U . . .
H38 H 0.6856 0.7144 0.3354 0.093 Uiso 1 1 calc R U . . .
H39 H 0.7097 0.6669 0.3838 0.093 Uiso 1 1 calc R U . . .
H40 H 0.6927 0.6567 0.3016 0.093 Uiso 1 1 calc R U . . .
C120 C 0.6618(6) 0.5882(6) 0.3657(8) 0.116(6) Uani 1 1 d . U . . .
H41 H 0.6661 0.5720 0.3243 0.139 Uiso 1 1 calc R U . . .
H42 H 0.6828 0.5822 0.4066 0.139 Uiso 1 1 calc R U . . .
H43 H 0.6408 0.5703 0.3734 0.139 Uiso 1 1 calc R U . . .
C121 C 0.6489(3) 0.8193(5) 0.6080(5) 0.053(2) Uani 1 1 d . U . . .
C122 C 0.6836(3) 0.8253(5) 0.6009(5) 0.061(2) Uani 1 1 d . U . . .
H44 H 0.6936 0.7945 0.5837 0.073 Uiso 1 1 calc R U . . .
C123 C 0.7032(3) 0.8732(5) 0.6174(6) 0.070(3) Uani 1 1 d . U . . .
H45 H 0.7264 0.8744 0.6120 0.084 Uiso 1 1 calc R U . . .
C124 C 0.6905(3) 0.9194(5) 0.6414(6) 0.069(3) Uani 1 1 d . U . . .
C125 C 0.6569(4) 0.9138(5) 0.6485(7) 0.077(3) Uani 1 1 d . U . . .
H46 H 0.6467 0.9452 0.6642 0.092 Uiso 1 1 calc R U . . .
C126 C 0.6377(3) 0.8664(5) 0.6345(6) 0.066(3) Uani 1 1 d . U . . .
H47 H 0.6152 0.8654 0.6433 0.079 Uiso 1 1 calc R U . . .
C127 C 0.7135(5) 0.9713(6) 0.6580(7) 0.094(4) Uani 1 1 d . U . . .
C128 C 0.7476(4) 0.9603(6) 0.7144(7) 0.096(4) Uani 1 1 d . U . . .
H48 H 0.7620 0.9945 0.7243 0.115 Uiso 1 1 calc R U . . .
H49 H 0.7423 0.9483 0.7568 0.115 Uiso 1 1 calc R U . . .
H50 H 0.7609 0.9308 0.6995 0.115 Uiso 1 1 calc R U . . .
C129 C 0.7228(6) 0.9899(7) 0.5906(8) 0.125(6) Uani 1 1 d . U . . .
H51 H 0.7005 0.9974 0.5527 0.150 Uiso 1 1 calc R U . . .
H52 H 0.7374 1.0239 0.6007 0.150 Uiso 1 1 calc R U . . .
H53 H 0.7361 0.9600 0.5764 0.150 Uiso 1 1 calc R U . . .
C130 C 0.6942(6) 1.0202(7) 0.6813(11) 0.139(6) Uani 1 1 d . U . . .
H54 H 0.6716 1.0282 0.6447 0.166 Uiso 1 1 calc R U . . .
H55 H 0.6892 1.0101 0.7246 0.166 Uiso 1 1 calc R U . . .
H56 H 0.7095 1.0535 0.6894 0.166 Uiso 1 1 calc R U . . .
C131 C 0.6394(3) 0.7264(5) 0.6598(5) 0.061(2) Uani 1 1 d . U . . .
C132 C 0.6726(3) 0.7304(5) 0.7099(5) 0.067(3) Uani 1 1 d . U . . .
H57 H 0.6889 0.7584 0.7054 0.080 Uiso 1 1 calc R U . . .
C133 C 0.6825(4) 0.6950(6) 0.7657(5) 0.080(3) Uani 1 1 d . U . . .
H58 H 0.7056 0.6997 0.7988 0.095 Uiso 1 1 calc R U . . .
C134 C 0.6623(5) 0.6551(6) 0.7764(6) 0.091(4) Uani 1 1 d . U . . .
C135 C 0.6288(5) 0.6495(7) 0.7274(7) 0.099(4) Uani 1 1 d . U . . .
H59 H 0.6133 0.6209 0.7333 0.118 Uiso 1 1 calc R U . . .
C136 C 0.6175(4) 0.6840(6) 0.6708(6) 0.088(4) Uani 1 1 d . U . . .
H60 H 0.5943 0.6790 0.6384 0.106 Uiso 1 1 calc R U . . .
C137 C 0.6771(5) 0.6177(6) 0.8420(7) 0.109(5) Uani 1 1 d D U . . .
C138 C 0.7174(5) 0.6273(8) 0.8816(9) 0.162(7) Uani 1 1 d D U . . .
H61 H 0.7210 0.6659 0.8984 0.195 Uiso 1 1 calc R U . . .
H62 H 0.7250 0.6017 0.9215 0.195 Uiso 1 1 calc R U . . .
H63 H 0.7315 0.6203 0.8500 0.195 Uiso 1 1 calc R U . . .
C139 C 0.6616(6) 0.6381(7) 0.8963(7) 0.125(6) Uani 1 1 d . U . . .
H64 H 0.6639 0.6788 0.8999 0.150 Uiso 1 1 calc R U . . .
H65 H 0.6362 0.6277 0.8833 0.150 Uiso 1 1 calc R U . . .
H66 H 0.6745 0.6212 0.9414 0.150 Uiso 1 1 calc R U . . .
C140 C 0.6782(7) 0.5595(6) 0.8228(10) 0.163(8) Uani 1 1 d D U . . .
H67 H 0.6896 0.5565 0.7860 0.196 Uiso 1 1 calc R U . . .
H68 H 0.6921 0.5381 0.8638 0.196 Uiso 1 1 calc R U . . .
H69 H 0.6538 0.5447 0.8057 0.196 Uiso 1 1 calc R U . . .
C211 C 0.3337(2) 0.8010(4) 0.3290(5) 0.0443(19) Uani 1 1 d . U . . .
C212 C 0.3507(3) 0.8222(4) 0.2835(5) 0.052(2) Uani 1 1 d . U . . .
H70 H 0.3761 0.8248 0.2985 0.063 Uiso 1 1 calc R U . . .
C213 C 0.3318(3) 0.8397(5) 0.2170(5) 0.057(2) Uani 1 1 d . U . . .
H71 H 0.3445 0.8534 0.1871 0.068 Uiso 1 1 calc R U . . .
C214 C 0.2941(3) 0.8377(4) 0.1924(5) 0.054(2) Uani 1 1 d . U . . .
C215 C 0.2775(3) 0.8182(5) 0.2383(5) 0.057(2) Uani 1 1 d . U . . .
H72 H 0.2521 0.8164 0.2238 0.068 Uiso 1 1 calc R U . . .
C216 C 0.2962(2) 0.8012(4) 0.3039(5) 0.056(2) Uani 1 1 d . U . . .
H73 H 0.2833 0.7890 0.3341 0.067 Uiso 1 1 calc R U . . .
C217 C 0.2727(3) 0.8582(5) 0.1193(6) 0.070(3) Uani 1 1 d . U . . .
C218 C 0.2960(5) 0.8822(11) 0.0790(9) 0.152(8) Uani 1 1 d . U . . .
H74 H 0.3138 0.8544 0.0761 0.183 Uiso 1 1 calc R U . . .
H75 H 0.2810 0.8923 0.0318 0.183 Uiso 1 1 calc R U . . .
H76 H 0.3083 0.9156 0.1030 0.183 Uiso 1 1 calc R U . . .
C219 C 0.2532(6) 0.8092(8) 0.0779(8) 0.143(7) Uani 1 1 d . U . . .
H77 H 0.2706 0.7808 0.0746 0.171 Uiso 1 1 calc R U . . .
H78 H 0.2370 0.7932 0.1012 0.171 Uiso 1 1 calc R U . . .
H79 H 0.2394 0.8216 0.0309 0.171 Uiso 1 1 calc R U . . .
C220 C 0.2456(5) 0.9009(8) 0.1236(8) 0.124(6) Uani 1 1 d . U . . .
H80 H 0.2579 0.9332 0.1504 0.148 Uiso 1 1 calc R U . . .
H81 H 0.2318 0.9129 0.0763 0.148 Uiso 1 1 calc R U . . .
H82 H 0.2294 0.8846 0.1467 0.148 Uiso 1 1 calc R U . . .
C221 C 0.3548(2) 0.7142(4) 0.4041(4) 0.0426(18) Uani 1 1 d . U . . .
C222 C 0.3778(2) 0.6864(4) 0.4621(5) 0.052(2) Uani 1 1 d . U . . .
H83 H 0.3929 0.7082 0.4989 0.062 Uiso 1 1 calc R U . . .
C223 C 0.3795(3) 0.6308(5) 0.4683(5) 0.059(2) Uani 1 1 d . U . . .
H84 H 0.3958 0.6143 0.5086 0.071 Uiso 1 1 calc R U . . .
C224 C 0.3572(3) 0.5962(4) 0.4148(5) 0.057(2) Uani 1 1 d . U . . .
C225 C 0.3347(3) 0.6245(4) 0.3570(5) 0.056(2) Uani 1 1 d . U . . .
H85 H 0.3195 0.6032 0.3196 0.067 Uiso 1 1 calc R U . . .
C226 C 0.3338(2) 0.6799(4) 0.3521(5) 0.050(2) Uani 1 1 d . U . . .
H86 H 0.3180 0.6967 0.3113 0.060 Uiso 1 1 calc R U . . .
C227 C 0.3582(4) 0.5324(5) 0.4196(7) 0.078(3) Uani 1 1 d . U . . .
C228 C 0.3242(5) 0.5110(7) 0.4243(15) 0.168(9) Uani 1 1 d . U . . .
H87 H 0.3184 0.5297 0.4627 0.202 Uiso 1 1 calc R U . . .
H88 H 0.3052 0.5184 0.3803 0.202 Uiso 1 1 calc R U . . .
H89 H 0.3262 0.4707 0.4329 0.202 Uiso 1 1 calc R U . . .
C229 C 0.3717(8) 0.5090(7) 0.3640(12) 0.183(11) Uani 1 1 d . U . . .
H90 H 0.3946 0.5266 0.3664 0.220 Uiso 1 1 calc R U . . .
H91 H 0.3751 0.4686 0.3708 0.220 Uiso 1 1 calc R U . . .
H92 H 0.3542 0.5162 0.3182 0.220 Uiso 1 1 calc R U . . .
C230 C 0.3858(5) 0.5105(6) 0.4859(10) 0.120(6) Uani 1 1 d . U . . .
H93 H 0.4098 0.5230 0.4872 0.144 Uiso 1 1 calc R U . . .
H94 H 0.3802 0.5249 0.5270 0.144 Uiso 1 1 calc R U . . .
H95 H 0.3851 0.4696 0.4861 0.144 Uiso 1 1 calc R U . . .
C231 C 0.3341(2) 0.8009(4) 0.4539(4) 0.0418(18) Uani 1 1 d . U . . .
C232 C 0.3186(3) 0.7671(4) 0.4920(5) 0.053(2) Uani 1 1 d . U . . .
H96 H 0.3193 0.7277 0.4868 0.064 Uiso 1 1 calc R U . . .
C233 C 0.3020(3) 0.7891(4) 0.5374(5) 0.054(2) Uani 1 1 d . U . . .
H97 H 0.2920 0.7640 0.5629 0.065 Uiso 1 1 calc R U . . .
C234 C 0.2993(3) 0.8450(5) 0.5474(5) 0.053(2) Uani 1 1 d . U . . .
C235 C 0.3139(3) 0.8794(4) 0.5068(5) 0.060(3) Uani 1 1 d . U . . .
H98 H 0.3129 0.9188 0.5116 0.072 Uiso 1 1 calc R U . . .
C236 C 0.3296(3) 0.8572(4) 0.4598(5) 0.061(3) Uani 1 1 d . U . . .
H99 H 0.3375 0.8819 0.4307 0.073 Uiso 1 1 calc R U . . .
C237 C 0.2830(3) 0.8696(5) 0.6007(6) 0.066(3) Uani 1 1 d D U . . .
C238 C 0.2538(6) 0.8384(10) 0.6055(14) 0.194(10) Uani 1 1 d . U . . .
H100 H 0.2350 0.8383 0.5601 0.232 Uiso 1 1 calc R U . . .
H101 H 0.2615 0.7999 0.6189 0.232 Uiso 1 1 calc R U . . .
H102 H 0.2444 0.8550 0.6408 0.232 Uiso 1 1 calc R U . . .
C239 C 0.3105(5) 0.8688(10) 0.6693(7) 0.144(7) Uani 1 1 d . U . . .
H103 H 0.3314 0.8905 0.6672 0.173 Uiso 1 1 calc R U . . .
H104 H 0.3008 0.8852 0.7042 0.173 Uiso 1 1 calc R U . . .
H105 H 0.3178 0.8301 0.6823 0.173 Uiso 1 1 calc R U . . .
C240 C 0.2746(7) 0.9308(7) 0.5912(10) 0.168(8) Uani 1 1 d D U . . .
H106 H 0.2958 0.9510 0.5881 0.201 Uiso 1 1 calc R U . . .
H107 H 0.2547 0.9366 0.5482 0.201 Uiso 1 1 calc R U . . .
H108 H 0.2679 0.9448 0.6312 0.201 Uiso 1 1 calc R U . . .
C311 C 0.6080(8) 1.0059(17) 0.3266(18) 0.48(3) Uani 1 1 d G U . . .
C312 C 0.6131(9) 1.0245(14) 0.394(2) 0.42(2) Uani 1 1 d DG U . . .
H109 H 0.6175 1.0630 0.4054 0.508 Uiso 1 1 calc R U . . .
C313 C 0.6116(9) 0.987(2) 0.4461(16) 0.37(2) Uani 1 1 d G U . . .
H110 H 0.6151 0.9997 0.4924 0.450 Uiso 1 1 calc R U . . .
C314 C 0.6051(9) 0.9307(18) 0.430(2) 0.43(3) Uani 1 1 d G U . . .
H111 H 0.6042 0.9050 0.4653 0.515 Uiso 1 1 calc R U . . .
C315 C 0.6001(11) 0.9120(13) 0.362(3) 0.43(3) Uani 1 1 d G U . . .
H112 H 0.5956 0.8736 0.3512 0.520 Uiso 1 1 calc R U . . .
C316 C 0.6015(10) 0.9496(19) 0.311(2) 0.48(3) Uani 1 1 d DG U . . .
H113 H 0.5980 0.9369 0.2642 0.574 Uiso 1 1 calc R U . . .
C317 C 0.6094(15) 1.047(3) 0.269(3) 0.60(5) Uani 1 1 d D U . . .
H114 H 0.6150 1.0844 0.2896 0.718 Uiso 1 1 calc R U . . .
H115 H 0.5861 1.0477 0.2329 0.718 Uiso 1 1 calc R U . . .
H116 H 0.6280 1.0352 0.2492 0.718 Uiso 1 1 calc R U . . .
C321 C 0.5384(16) 0.976(4) 0.094(3) 1.16(5) Uani 1 1 d G U . . .
C322 C 0.529(3) 0.922(3) 0.106(5) 1.16(5) Uani 1 1 d DG U . . .
H117 H 0.5389 0.8905 0.0896 1.393 Uiso 1 1 calc R U . . .
C323 C 0.504(3) 0.913(5) 0.141(4) 1.17(5) Uani 1 1 d G U . . .
H118 H 0.4968 0.8763 0.1487 1.403 Uiso 1 1 calc R U . . .
C324 C 0.4884(13) 0.959(8) 0.1639(6) 1.17(5) Uani 1 1 d G U . . .
H119 H 0.4713 0.9530 0.1879 1.405 Uiso 1 1 calc R U . . .
C325 C 0.498(3) 1.013(6) 0.152(5) 1.17(5) Uani 1 1 d G U . . .
H120 H 0.4880 1.0438 0.1681 1.399 Uiso 1 1 calc R U . . .
C326 C 0.523(3) 1.021(3) 0.117(5) 1.16(5) Uani 1 1 d DG U . . .
H121 H 0.5300 1.0580 0.1089 1.390 Uiso 1 1 calc R U . . .
C327 C 0.566(2) 0.985(8) 0.055(4) 1.13(5) Uani 1 1 d D U . . .
H122 H 0.5700 1.0251 0.0510 1.350 Uiso 1 1 calc R U . . .
H123 H 0.5888 0.9671 0.0809 1.350 Uiso 1 1 calc R U . . .
H124 H 0.5572 0.9686 0.0080 1.350 Uiso 1 1 calc R U . . .
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'
S S 0.1246 0.1234 '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
O3 W1 S1 107.40(10) . 2_655
O3 W1 S1 107.39(10) . .
S1 W1 S1 145.21(19) 2_655 .
O3 W1 S2 108.09(9) . 2_655
S1 W1 S2 83.66(9) 2_655 2_655
S1 W1 S2 85.68(9) . 2_655
O3 W1 S2 108.09(9) . .
S1 W1 S2 85.68(9) 2_655 .
S1 W1 S2 83.66(9) . .
S2 W1 S2 143.82(18) 2_655 .
O3B W1B S2 109.9(6) . 2_655
O3B W1B S2 109.9(6) . .
S2 W1B S2 140.2(12) 2_655 .
O3B W1B S1 110.7(6) . 2_655
S2 W1B S1 82.1(4) 2_655 2_655
S2 W1B S1 84.1(4) . 2_655
O3B W1B S1 110.7(6) . .
S2 W1B S1 84.1(4) 2_655 .
S2 W1B S1 82.1(4) . .
S1 W1B S1 138.5(11) 2_655 .
C11 S1 W1 107.7(3) . .
C11 S1 W1B 100.9(4) . .
C12 S2 W1 107.7(3) . .
C12 S2 W1B 100.4(4) . .
C17 N1 C16 128.1(9) . .
C27 N2 C13 124.5(9) . .
C31 N3 C37 110.5(12) . .
C31 N3 C33 109.8(12) . .
C37 N3 C33 109.6(13) . .
C31 N3 C35 109.7(14) . .
C37 N3 C35 109.1(12) . .
C33 N3 C35 108.1(12) . .
C16 C11 C12 120.5(9) . .
C16 C11 S1 119.8(7) . .
C12 C11 S1 119.6(7) . .
C13 C12 C11 120.2(9) . .
C13 C12 S2 120.0(7) . .
C11 C12 S2 119.3(8) . .
C12 C13 C14 119.5(9) . .
C12 C13 N2 119.9(9) . .
C14 C13 N2 120.6(9) . .
C13 C14 C15 120.0(10) . .
C16 C15 C14 120.7(10) . .
C11 C16 C15 118.7(9) . .
C11 C16 N1 117.9(9) . .
C15 C16 N1 123.4(9) . .
O1 C17 N1 123.1(10) . .
O1 C17 C18 120.0(9) . .
N1 C17 C18 116.8(9) . .
C111 C18 C121 111.5(8) . .
C111 C18 C131 109.3(9) . .
C121 C18 C131 110.1(8) . .
C111 C18 C17 113.1(8) . .
C121 C18 C17 106.9(9) . .
C131 C18 C17 105.8(8) . .
O2 C27 N2 123.6(9) . .
O2 C27 C28 121.2(9) . .
N2 C27 C28 115.2(9) . .
C211 C28 C231 108.8(7) . .
C211 C28 C221 111.1(7) . .
C231 C28 C221 110.2(7) . .
C211 C28 C27 111.8(7) . .
C231 C28 C27 106.6(7) . .
C221 C28 C27 108.2(7) . .
C32 C31 N3 119.2(15) . .
C34 C33 N3 121.6(16) . .
C36 C35 N3 114.4(17) . .
C38 C37 N3 119.4(18) . .
N4 C41 C42 164(6) . .
C52 C51 N5 162.4 2_656 .
C52 C51 N5 0.0 2_656 2_656
N5 C51 N5 162(10) . 2_656
C112 C111 C116 114.4(9) . .
C112 C111 C18 125.5(9) . .
C116 C111 C18 120.1(9) . .
C113 C112 C111 123.8(9) . .
C112 C113 C114 122.3(11) . .
C113 C114 C115 114.8(9) . .
C113 C114 C117 123.4(10) . .
C115 C114 C117 121.8(9) . .
C116 C115 C114 121.6(9) . .
C115 C116 C111 123.1(9) . .
C120 C117 C114 113.2(10) . .
C120 C117 C119 106.6(12) . .
C114 C117 C119 109.5(9) . .
C120 C117 C118 110.6(12) . .
C114 C117 C118 109.4(10) . .
C119 C117 C118 107.4(10) . .
C126 C121 C122 112.8(10) . .
C126 C121 C18 125.3(10) . .
C122 C121 C18 121.7(9) . .
C123 C122 C121 123.2(11) . .
C124 C123 C122 121.9(11) . .
C123 C124 C125 115.2(12) . .
C123 C124 C127 119.2(12) . .
C125 C124 C127 125.7(13) . .
C126 C125 C124 123.7(12) . .
C125 C126 C121 123.2(11) . .
C128 C127 C124 110.9(12) . .
C128 C127 C130 108.2(14) . .
C124 C127 C130 112.1(14) . .
C128 C127 C129 108.3(14) . .
C124 C127 C129 108.9(11) . .
C130 C127 C129 108.3(14) . .
C132 C131 C136 115.0(11) . .
C132 C131 C18 122.4(10) . .
C136 C131 C18 122.4(10) . .
C133 C132 C131 121.4(12) . .
C134 C133 C132 124.0(14) . .
C133 C134 C135 116.5(12) . .
C133 C134 C137 118.5(15) . .
C135 C134 C137 125.0(16) . .
C136 C135 C134 121.9(14) . .
C135 C136 C131 121.2(13) . .
C140 C137 C139 124.4(16) . .
C140 C137 C134 111.3(12) . .
C139 C137 C134 107.8(12) . .
C140 C137 C138 99.6(12) . .
C139 C137 C138 99.0(14) . .
C134 C137 C138 113.9(14) . .
C212 C211 C216 115.3(8) . .
C212 C211 C28 124.2(8) . .
C216 C211 C28 120.5(8) . .
C213 C212 C211 121.9(9) . .
C212 C213 C214 121.5(9) . .
C215 C214 C213 116.3(9) . .
C215 C214 C217 121.6(10) . .
C213 C214 C217 122.1(9) . .
C216 C215 C214 122.1(9) . .
C215 C216 C211 122.8(9) . .
C220 C217 C219 108.5(14) . .
C220 C217 C218 109.2(14) . .
C219 C217 C218 106.7(15) . .
C220 C217 C214 110.6(10) . .
C219 C217 C214 108.4(11) . .
C218 C217 C214 113.2(10) . .
C226 C221 C222 115.2(9) . .
C226 C221 C28 124.9(8) . .
C222 C221 C28 119.8(8) . .
C223 C222 C221 123.5(9) . .
C222 C223 C224 120.5(10) . .
C225 C224 C223 115.4(9) . .
C225 C224 C227 122.2(10) . .
C223 C224 C227 122.4(10) . .
C226 C225 C224 122.7(10) . .
C225 C226 C221 122.7(9) . .
C228 C227 C229 117.4(18) . .
C228 C227 C230 103.8(14) . .
C229 C227 C230 102.0(15) . .
C228 C227 C224 110.4(12) . .
C229 C227 C224 109.7(11) . .
C230 C227 C224 113.3(11) . .
C236 C231 C232 116.0(8) . .
C236 C231 C28 119.5(8) . .
C232 C231 C28 124.4(8) . .
C231 C232 C233 121.6(9) . .
C234 C233 C232 123.2(9) . .
C233 C234 C235 115.2(9) . .
C233 C234 C237 123.5(9) . .
C235 C234 C237 121.2(10) . .
C236 C235 C234 121.5(10) . .
C231 C236 C235 122.2(9) . .
C238 C237 C239 107.9(17) . .
C238 C237 C240 112.3(16) . .
C239 C237 C240 101.6(15) . .
C238 C237 C234 111.9(11) . .
C239 C237 C234 108.0(10) . .
C240 C237 C234 114.3(9) . .
C312 C311 C316 120.0 . .
C312 C311 C317 120.3(11) . .
C316 C311 C317 119.7(11) . .
C311 C312 C313 120.0 . .
C312 C313 C314 120.0 . .
C315 C314 C313 120.0 . .
C316 C315 C314 120.0 . .
C315 C316 C311 120.0 . .
C322 C321 C326 120.0 . .
C322 C321 C327 120.0(11) . .
C326 C321 C327 120.0(11) . .
C323 C322 C321 120.0 . .
C324 C323 C322 120.0 . .
C323 C324 C325 120.0 . .
C326 C325 C324 120.0 . .
C325 C326 C321 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O3 1.638(8) .
W1 S1 2.360(3) 2_655
W1 S1 2.360(3) .
W1 S2 2.379(3) 2_655
W1 S2 2.379(3) .
W1B O3B 1.700(10) .
W1B S2 2.405(9) 2_655
W1B S2 2.406(9) .
W1B S1 2.408(9) 2_655
W1B S1 2.408(9) .
S1 C11 1.790(10) .
S2 C12 1.785(10) .
O1 C17 1.199(12) .
O2 C27 1.215(12) .
N1 C17 1.348(12) .
N1 C16 1.406(12) .
N2 C27 1.359(13) .
N2 C13 1.404(12) .
N3 C31 1.501(17) .
N3 C37 1.507(18) .
N3 C33 1.510(18) .
N3 C35 1.521(18) .
N4 C41 1.171(18) .
N5 C51 1.320(18) .
C11 C16 1.395(14) .
C11 C12 1.400(13) .
C12 C13 1.386(14) .
C13 C14 1.393(14) .
C14 C15 1.397(15) .
C15 C16 1.395(14) .
C17 C18 1.561(14) .
C18 C111 1.537(14) .
C18 C121 1.540(15) .
C18 C131 1.550(14) .
C27 C28 1.562(12) .
C28 C211 1.540(12) .
C28 C231 1.547(11) .
C28 C221 1.554(13) .
C31 C32 1.484(19) .
C33 C34 1.458(17) .
C35 C36 1.509(19) .
C37 C38 1.475(19) .
C41 C42 1.478(18) .
C51 C52 1.320(18) 2_656
C51 N5 1.321(18) 2_656
C111 C112 1.360(15) .
C111 C116 1.436(13) .
C112 C113 1.352(15) .
C113 C114 1.396(14) .
C114 C115 1.429(15) .
C114 C117 1.508(15) .
C115 C116 1.319(13) .
C117 C120 1.474(18) .
C117 C119 1.545(17) .
C117 C118 1.549(16) .
C121 C126 1.376(15) .
C121 C122 1.421(14) .
C122 C123 1.365(15) .
C123 C124 1.362(17) .
C124 C125 1.376(18) .
C124 C127 1.510(18) .
C125 C126 1.343(17) .
C127 C128 1.49(2) .
C127 C130 1.54(2) .
C127 C129 1.57(2) .
C131 C132 1.384(14) .
C131 C136 1.389(16) .
C132 C133 1.363(15) .
C133 C134 1.30(2) .
C134 C135 1.38(2) .
C134 C137 1.552(17) .
C135 C136 1.366(18) .
C137 C140 1.449(15) .
C137 C139 1.488(19) .
C137 C138 1.552(16) .
C211 C212 1.386(13) .
C211 C216 1.401(12) .
C212 C213 1.380(13) .
C213 C214 1.406(14) .
C214 C215 1.368(14) .
C214 C217 1.531(14) .
C215 C216 1.360(13) .
C217 C220 1.497(17) .
C217 C219 1.50(2) .
C217 C218 1.51(2) .
C221 C226 1.383(13) .
C221 C222 1.403(13) .
C222 C223 1.335(14) .
C223 C224 1.423(15) .
C224 C225 1.399(15) .
C224 C227 1.531(16) .
C225 C226 1.331(14) .
C227 C228 1.46(2) .
C227 C229 1.49(2) .
C227 C230 1.53(2) .
C231 C236 1.370(14) .
C231 C232 1.379(13) .
C232 C233 1.380(12) .
C233 C234 1.363(14) .
C234 C235 1.400(14) .
C234 C237 1.527(13) .
C235 C236 1.385(13) .
C237 C238 1.40(2) .
C237 C239 1.465(19) .
C237 C240 1.500(15) .
C311 C312 1.3900 .
C311 C316 1.3900 .
C311 C317 1.529(16) .
C312 C313 1.3900 .
C313 C314 1.3900 .
C314 C315 1.3900 .
C315 C316 1.3900 .
C321 C322 1.3900 .
C321 C326 1.3900 .
C321 C327 1.540(16) .
C322 C323 1.3900 .
C323 C324 1.3900 .
C324 C325 1.3900 .
C325 C326 1.3900 .
