#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:46:10 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179305 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/02/4320236.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_4320236
loop_
_publ_author_name
'Vladimir Kolesnichenko'
'Mark H. Mason'
'Jeff B. Botts'
'Alix M. Botts'
'Timothy E. Baroni'
'Joseph A. Heppert'
'Arnold L. Rheingold'
'Louise Liable-Sands'
'Glenn P. A. Yap'
_publ_section_title
;
 Tungsten Oxo Salicylate Complexes from Tungsten Hexachloride Reactions
 Systems
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5010
_journal_page_last               5016
_journal_paper_doi               10.1021/ic001456k
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C29 H20 Cl2 O15 W2'
_chemical_formula_weight         1047.05
_chemical_name_systematic
; 
 ? 
;
_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                 114.230(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.983(2)
_cell_length_b                   21.683(3)
_cell_length_c                   18.756(3)
_cell_measurement_temperature    251(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      7.5
_cell_volume                     6298.3(16)
_computing_cell_refinement       'Siemens P4'
_computing_data_collection       'Siemens P4'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-5.03 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS-5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      251(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       omega
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0710
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4118
_diffrn_reflns_theta_max         22.52
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        <1.0
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.544
_exptl_absorpt_correction_type   XABS2
_exptl_crystal_colour            Red-Orange
_exptl_crystal_density_diffrn    2.208
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             3968
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.285
_refine_diff_density_min         -2.858
_refine_diff_density_rms         0.251
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.314
_refine_ls_goodness_of_fit_obs   1.469
_refine_ls_hydrogen_treatment    'idealized contributions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         4112
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.345
_refine_ls_restrained_S_obs      1.469
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_obs          0.0494
_refine_ls_shift/esd_max         0.266
_refine_ls_shift/esd_mean        0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0400P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1160
_refine_ls_wR_factor_obs         0.1108
_reflns_number_observed          3226
_reflns_number_total             4118
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic001456k_2.cif
_cod_data_source_block           jhep06
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

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^)+(0.0400P)^2^+0.0000P] 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^)+(0.0400P)^2^+0.0000P] 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        6298.3(15)
_cod_database_code               4320236
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 0.87563(3) 1.04575(2) 0.88892(3) 0.0285(2) Uani 1 d . .
W2 W 0.64684(3) 1.06040(2) 0.74326(3) 0.0312(2) Uani 1 d . .
O1 O 0.7597(4) 1.0405(3) 0.8173(4) 0.023(2) Uani 1 d . .
O2 O 0.9114(5) 0.9798(3) 0.8635(4) 0.035(2) Uani 1 d . .
O3 O 0.9846(5) 1.0811(3) 0.9600(4) 0.035(2) Uani 1 d . .
O4 O 0.8917(5) 1.1040(3) 0.8144(4) 0.032(2) Uani 1 d . .
O5 O 0.9073(6) 1.1924(4) 0.7663(5) 0.053(3) Uani 1 d . .
O6 O 0.8613(5) 1.0131(3) 0.9764(4) 0.026(2) Uani 1 d . .
O7 O 0.8234(5) 1.1284(3) 0.9256(5) 0.033(2) Uani 1 d . .
O8 O 0.7523(6) 1.1816(3) 0.9804(5) 0.043(2) Uani 1 d . .
O9 O 0.5920(5) 1.0103(4) 0.7728(4) 0.041(2) Uani 1 d . .
O10 O 0.6507(6) 1.1319(3) 0.8082(4) 0.036(2) Uani 1 d . .
O11 O 0.5515(6) 1.1056(3) 0.6656(4) 0.040(2) Uani 1 d . .
O12 O 0.6749(6) 1.2291(4) 0.8449(5) 0.052(3) Uani 1 d . .
O13 O 0.7229(6) 1.1229(3) 0.7017(4) 0.037(2) Uani 1 d . .
O14 O 0.6480(5) 1.0123(3) 0.6589(4) 0.036(2) Uani 1 d . .
O15 O 0.7967(6) 1.1537(4) 0.6353(5) 0.051(3) Uani 1 d . .
C1 C 0.9306(8) 1.1578(5) 0.8221(7) 0.031(3) Uani 1 d . .
C2 C 1.0018(5) 1.1725(4) 0.8958(4) 0.040(3) Uani 1 d G .
C3 C 1.0487(6) 1.2259(3) 0.9000(4) 0.052(4) Uani 1 d G .
H3A H 1.0315(9) 1.2529(4) 0.8570(6) 0.062 Uiso 1 calc R .
C4 C 1.1211(6) 1.2395(3) 0.9678(5) 0.060(4) Uani 1 d G .
H4A H 1.1529(8) 1.2756(4) 0.9706(7) 0.072 Uiso 1 calc R .
C5 C 1.1466(5) 1.1996(4) 1.0314(4) 0.060(4) Uani 1 d G .
H5A H 1.1956(6) 1.2088(6) 1.0772(5) 0.072 Uiso 1 calc R .
C6 C 1.0997(6) 1.1462(3) 1.0271(4) 0.045(4) Uani 1 d G .
H6A H 1.1169(8) 1.1192(5) 1.0701(5) 0.055 Uiso 1 calc R .
C7 C 1.0272(5) 1.1326(3) 0.9594(4) 0.036(3) Uani 1 d G .
C8 C 0.8016(8) 1.1354(5) 0.9804(7) 0.030(3) Uani 1 d . .
C9 C 0.8271(6) 1.0933(3) 1.0467(3) 0.028(3) Uani 1 d G .
C10 C 0.8237(6) 1.1128(2) 1.1160(4) 0.040(3) Uani 1 d G .
H10A H 0.8031(8) 1.1524(3) 1.1194(6) 0.049 Uiso 1 calc R .
C11 C 0.8508(6) 1.0736(3) 1.1803(3) 0.047(4) Uani 1 d G .
H11A H 0.8485(9) 1.0868(4) 1.2272(4) 0.056 Uiso 1 calc R .
C12 C 0.8813(6) 1.0150(3) 1.1754(3) 0.044(4) Uani 1 d G .
H12A H 0.8996(9) 0.9885(4) 1.2189(4) 0.053 Uiso 1 calc R .
C13 C 0.8847(5) 0.9955(2) 1.1061(4) 0.035(3) Uani 1 d G .
H13A H 0.9053(8) 0.9559(3) 1.1028(5) 0.042 Uiso 1 calc R .
C14 C 0.8576(6) 1.0346(3) 1.0418(3) 0.035(3) Uani 1 d G .
C15 C 0.7376(8) 1.1189(5) 0.6414(7) 0.033(3) Uani 1 d . .
C16 C 0.6938(6) 1.0764(3) 0.5784(3) 0.037(3) Uani 1 d G .
C17 C 0.6961(6) 1.0865(3) 0.5061(4) 0.050(4) Uani 1 d G .
H17A H 0.7250(8) 1.1212(4) 0.4984(6) 0.060 Uiso 1 calc R .
C18 C 0.6556(7) 1.0453(4) 0.4451(3) 0.060(4) Uani 1 d G .
H18A H 0.6571(10) 1.0522(5) 0.3962(4) 0.072 Uiso 1 calc R .
C19 C 0.6129(6) 0.9941(4) 0.4564(4) 0.058(4) Uani 1 d G .
H19A H 0.5855(9) 0.9663(5) 0.4152(5) 0.069 Uiso 1 calc R .
C20 C 0.6107(5) 0.9841(3) 0.5288(4) 0.045(4) Uani 1 d G .
H20A H 0.5818(8) 0.9494(4) 0.5364(6) 0.053 Uiso 1 calc R .
C21 C 0.6511(6) 1.0252(3) 0.5898(3) 0.031(3) Uani 1 d G .
C22 C 0.6379(9) 1.1921(5) 0.7933(7) 0.037(3) Uani 1 d . .
C23 C 0.5787(5) 1.2098(3) 0.7135(3) 0.040(3) Uani 1 d G .
C24 C 0.5616(6) 1.2722(3) 0.6985(4) 0.047(4) Uani 1 d G .
H24A H 0.5896(8) 1.3014(4) 0.7379(5) 0.057 Uiso 1 calc R .
C25 C 0.5029(6) 1.2916(3) 0.6253(5) 0.059(4) Uani 1 d G .
H25A H 0.4913(9) 1.3339(3) 0.6151(7) 0.071 Uiso 1 calc R .
C26 C 0.4615(5) 1.2485(4) 0.5670(4) 0.058(4) Uani 1 d G .
H26A H 0.4218(7) 1.2616(5) 0.5175(4) 0.069 Uiso 1 calc R .
C27 C 0.4786(5) 1.1860(3) 0.5820(4) 0.047(4) Uani 1 d G .
H27A H 0.4506(8) 1.1569(4) 0.5426(5) 0.057 Uiso 1 calc R .
C28 C 0.5373(6) 1.1667(2) 0.6552(4) 0.035(3) Uani 1 d G .
C90 C 0.6608(38) 0.8365(24) 0.7104(23) 0.303(34) Uani 1 d . .
Cl1 Cl 0.6327(11) 0.8246(6) 0.6354(7) 0.123(5) Uani 0.50 d P .
Cl1' Cl 0.5504(18) 0.8714(9) 0.6612(19) 0.293(16) Uani 0.50 d P .
Cl2 Cl 0.7125(7) 0.8711(5) 0.7872(7) 0.102(4) Uani 0.50 d P .
Cl2' Cl 0.6583(34) 0.8428(10) 0.7831(18) 0.507(39) Uani 0.50 d P .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
O2 W1 O1 98.0(3) . . ?
O2 W1 O6 96.7(3) . . ?
O1 W1 O6 97.3(3) . . ?
O2 W1 O3 100.1(4) . . ?
O1 W1 O3 160.1(3) . . ?
O6 W1 O3 88.7(3) . . ?
O2 W1 O4 99.8(3) . . ?
O1 W1 O4 86.6(3) . . ?
O6 W1 O4 162.3(3) . . ?
O3 W1 O4 82.2(3) . . ?
O2 W1 O7 176.0(3) . . ?
O1 W1 O7 80.6(3) . . ?
O6 W1 O7 79.8(3) . . ?
O3 W1 O7 81.8(3) . . ?
O4 W1 O7 83.9(3) . . ?
O9 W2 O1 98.2(3) . . ?
O9 W2 O14 96.8(4) . . ?
O1 W2 O14 97.6(3) . . ?
O9 W2 O11 99.8(4) . . ?
O1 W2 O11 160.8(3) . . ?
O14 W2 O11 86.7(3) . . ?
O9 W2 O10 100.9(4) . . ?
O1 W2 O10 87.6(3) . . ?
O14 W2 O10 160.7(3) . . ?
O11 W2 O10 82.6(3) . . ?
O9 W2 O13 176.9(3) . . ?
O1 W2 O13 80.6(3) . . ?
O14 W2 O13 80.6(3) . . ?
O11 W2 O13 81.7(3) . . ?
O10 W2 O13 81.9(3) . . ?
W1 O1 W2 163.2(4) . . ?
C7 O3 W1 133.9(6) . . ?
C1 O4 W1 133.9(7) . . ?
C14 O6 W1 137.4(6) . . ?
C8 O7 W1 130.4(7) . . ?
C22 O10 W2 133.2(7) . . ?
C28 O11 W2 130.6(6) . . ?
C15 O13 W2 129.3(8) . . ?
C21 O14 W2 134.7(6) . . ?
O5 C1 O4 118.8(10) . . ?
O5 C1 C2 122.3(10) . . ?
O4 C1 C2 118.9(9) . . ?
C3 C2 C7 120.0 . . ?
C3 C2 C1 118.2(7) . . ?
C7 C2 C1 121.7(7) . . ?
C2 C3 C4 120.0 . . ?
C5 C4 C3 120.0 . . ?
C6 C5 C4 120.0 . . ?
C5 C6 C7 120.0 . . ?
O3 C7 C6 116.7(6) . . ?
O3 C7 C2 123.3(6) . . ?
C6 C7 C2 120.0 . . ?
O7 C8 O8 120.3(10) . . ?
O7 C8 C9 123.2(9) . . ?
O8 C8 C9 116.5(10) . . ?
C10 C9 C14 120.0 . . ?
C10 C9 C8 119.7(6) . . ?
C14 C9 C8 120.3(6) . . ?
C9 C10 C11 120.0 . . ?
C12 C11 C10 120.0 . . ?
C11 C12 C13 120.0 . . ?
C12 C13 C14 120.0 . . ?
O6 C14 C13 117.4(5) . . ?
O6 C14 C9 122.6(5) . . ?
C13 C14 C9 120.0 . . ?
O13 C15 O15 119.1(11) . . ?
O13 C15 C16 123.7(11) . . ?
O15 C15 C16 117.2(10) . . ?
C17 C16 C21 120.0 . . ?
C17 C16 C15 119.3(7) . . ?
C21 C16 C15 120.7(7) . . ?
C18 C17 C16 120.0 . . ?
C19 C18 C17 120.0 . . ?
C18 C19 C20 120.0 . . ?
C19 C20 C21 120.0 . . ?
O14 C21 C20 117.2(6) . . ?
O14 C21 C16 122.8(6) . . ?
C20 C21 C16 120.0 . . ?
O12 C22 O10 119.5(11) . . ?
O12 C22 C23 123.5(10) . . ?
O10 C22 C23 116.9(10) . . ?
C24 C23 C28 120.0 . . ?
C24 C23 C22 117.3(7) . . ?
C28 C23 C22 122.6(7) . . ?
C25 C24 C23 120.0 . . ?
C26 C25 C24 120.0 . . ?
C25 C26 C27 120.0 . . ?
C26 C27 C28 120.0 . . ?
O11 C28 C27 117.0(6) . . ?
O11 C28 C23 123.0(6) . . ?
C27 C28 C23 120.0 . . ?
Cl1 C90 Cl2' 158.0(54) . . ?
Cl1 C90 Cl2 156.3(30) . . ?
Cl2' C90 Cl2 43.0(22) . . ?
Cl1 C90 Cl1' 72.6(25) . . ?
Cl2' C90 Cl1' 90.9(49) . . ?
Cl2 C90 Cl1' 109.5(43) . . ?
C90 Cl1 Cl1' 67.2(30) . . ?
C90 Cl1' Cl1 40.2(17) . . ?
C90 Cl1' Cl2' 36.2(21) . . ?
Cl1 Cl1' Cl2' 75.6(17) . . ?
Cl2' Cl2 C90 61.0(26) . . ?
Cl2 Cl2' C90 76.0(38) . . ?
Cl2 Cl2' Cl1' 102.8(22) . . ?
C90 Cl2' Cl1' 53.0(32) . . ?
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 O2 1.698(8) . ?
W1 O1 1.877(7) . ?
W1 O6 1.892(7) . ?
W1 O3 1.940(8) . ?
W1 O4 1.983(7) . ?
W1 O7 2.229(7) . ?
W2 O9 1.666(8) . ?
W2 O1 1.898(7) . ?
W2 O14 1.902(7) . ?
W2 O11 1.942(8) . ?
W2 O10 1.957(7) . ?
W2 O13 2.222(8) . ?
O3 C7 1.334(9) . ?
O4 C1 1.319(13) . ?
O5 C1 1.216(13) . ?
O6 C14 1.337(8) . ?
O7 C8 1.236(13) . ?
O8 C8 1.307(13) . ?
O10 C22 1.333(13) . ?
O11 C28 1.345(9) . ?
O12 C22 1.216(14) . ?
O13 C15 1.257(13) . ?
O14 C21 1.349(9) . ?
O15 C15 1.297(14) . ?
C1 C2 1.450(13) . ?
C2 C3 1.39 . ?
C2 C7 1.39 . ?
C3 C4 1.39 . ?
C4 C5 1.39 . ?
C5 C6 1.39 . ?
C6 C7 1.39 . ?
C8 C9 1.458(12) . ?
C9 C10 1.39 . ?
C9 C14 1.39 . ?
C10 C11 1.39 . ?
C11 C12 1.39 . ?
C12 C13 1.39 . ?
C13 C14 1.39 . ?
C15 C16 1.442(13) . ?
C16 C17 1.39 . ?
C16 C21 1.39 . ?
C17 C18 1.39 . ?
C18 C19 1.39 . ?
C19 C20 1.39 . ?
C20 C21 1.39 . ?
C22 C23 1.471(13) . ?
C23 C24 1.39 . ?
C23 C28 1.39 . ?
C24 C25 1.39 . ?
C25 C26 1.39 . ?
C26 C27 1.39 . ?
C27 C28 1.39 . ?
C90 Cl1 1.31(4) . ?
C90 Cl2' 1.39(6) . ?
C90 Cl2 1.54(4) . ?
C90 Cl1' 1.88(6) . ?
Cl1 Cl1' 1.94(3) . ?
Cl1' Cl2' 2.35(4) . ?
Cl2 Cl2' 1.08(4) . ?
