#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:46:10 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179305 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/02/4320235.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_4320235
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            'C18 H17 Cl1.86 O7.14 W'
_chemical_formula_weight         597.34
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 93.5660(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.97010(10)
_cell_length_b                   15.67030(10)
_cell_length_c                   12.5001(2)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     1949.17(4)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Siemens P4_CCD'
_diffrn_measurement_method       'omega/phi 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  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10644
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    6.220
_exptl_absorpt_correction_T_max  0.3693
_exptl_absorpt_correction_T_min  0.1899
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    2.036
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1151
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.852
_refine_diff_density_min         -1.243
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0232
_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)+(0.0300P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0594
_reflns_number_gt                3370
_reflns_number_total             3791
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001456k_1.cif
_cod_data_source_block           jhep04r
_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 
;
_cod_database_code               4320235
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
W W -0.299948(13) 0.024840(8) 0.226111(11) 0.02781(7) Uani 1 1 d . . .
Cl1 Cl -0.35524(11) -0.05295(7) 0.07123(9) 0.0504(3) Uani 1 1 d . . .
ClO Cl -0.41432(11) 0.13504(7) 0.18474(10) 0.0463(3) Uani 0.93 1 d P . .
O2 O -0.4271(3) -0.03238(16) 0.3071(2) 0.0362(6) Uani 1 1 d . . .
O3 O -0.1846(2) -0.09570(17) 0.2664(2) 0.0387(6) Uani 1 1 d . . .
O4 O -0.1365(3) -0.22393(17) 0.3309(2) 0.0438(7) Uani 1 1 d . . .
H4B H -0.0725 -0.2175 0.2936 0.066 Uiso 1 1 calc R . .
O5 O -0.1336(2) 0.05509(16) 0.17285(19) 0.0299(5) Uani 1 1 d . . .
O6 O -0.2139(3) 0.05872(19) 0.3649(2) 0.0391(6) Uani 1 1 d . . .
O7 O -0.0687(3) 0.0990(2) 0.4952(2) 0.0529(8) Uani 1 1 d . . .
C1 C -0.4317(3) -0.0972(2) 0.3776(3) 0.0291(7) Uani 1 1 d . . .
C2 C -0.3310(3) -0.1606(2) 0.3873(3) 0.0283(7) Uani 1 1 d . . .
C3 C -0.2118(3) -0.1577(2) 0.3236(3) 0.0314(8) Uani 1 1 d . . .
C4 C -0.5418(3) -0.1014(2) 0.4389(3) 0.0340(8) Uani 1 1 d . . .
H4A H -0.6086 -0.0600 0.4314 0.041 Uiso 1 1 calc R . .
C5 C -0.5528(4) -0.1671(2) 0.5113(3) 0.0389(9) Uani 1 1 d . . .
H5A H -0.6265 -0.1694 0.5533 0.047 Uiso 1 1 calc R . .
C6 C -0.4550(4) -0.2298(2) 0.5221(3) 0.0422(9) Uani 1 1 d . . .
H6A H -0.4637 -0.2739 0.5709 0.051 Uiso 1 1 calc R . .
C7 C -0.3456(4) -0.2271(2) 0.4612(3) 0.0360(8) Uani 1 1 d . . .
H7A H -0.2805 -0.2696 0.4687 0.043 Uiso 1 1 calc R . .
C8 C -0.0054(3) 0.0608(2) 0.2178(3) 0.0255(7) Uani 1 1 d . . .
C9 C 0.0185(3) 0.0705(2) 0.3274(3) 0.0302(7) Uani 1 1 d . . .
C10 C -0.0882(4) 0.0776(2) 0.4032(3) 0.0354(8) Uani 1 1 d . . .
C11 C 0.1523(4) 0.0791(3) 0.3680(3) 0.0418(9) Uani 1 1 d . . .
H11A H 0.1710 0.0862 0.4413 0.050 Uiso 1 1 calc R . .
C12 C 0.2558(4) 0.0773(3) 0.3006(4) 0.0445(10) Uani 1 1 d . . .
H12A H 0.3440 0.0828 0.3285 0.053 Uiso 1 1 calc R . .
C13 C 0.2296(4) 0.0672(3) 0.1917(3) 0.0399(9) Uani 1 1 d . . .
H13A H 0.3003 0.0660 0.1465 0.048 Uiso 1 1 calc R . .
C14 C 0.0990(3) 0.0588(2) 0.1496(3) 0.0321(8) Uani 1 1 d . . .
H14A H 0.0812 0.0520 0.0762 0.038 Uiso 1 1 calc R . .
O21 O 0.0637(3) -0.21950(17) 0.2155(2) 0.0406(6) Uani 1 1 d . . .
C21 C 0.1764(4) -0.1713(3) 0.2629(4) 0.0475(10) Uani 1 1 d . . .
H21A H 0.2184 -0.2012 0.3241 0.057 Uiso 1 1 calc R . .
H21B H 0.1477 -0.1154 0.2858 0.057 Uiso 1 1 calc R . .
C22 C 0.2709(4) -0.1638(3) 0.1751(4) 0.0499(11) Uani 1 1 d . . .
H22A H 0.3344 -0.2108 0.1777 0.060 Uiso 1 1 calc R . .
H22B H 0.3204 -0.1106 0.1807 0.060 Uiso 1 1 calc R . .
C23 C 0.1807(5) -0.1666(4) 0.0717(4) 0.0593(13) Uani 1 1 d . . .
H23A H 0.1797 -0.1118 0.0357 0.071 Uiso 1 1 calc R . .
H23B H 0.2114 -0.2098 0.0233 0.071 Uiso 1 1 calc R . .
C24 C 0.0430(5) -0.1884(3) 0.1074(4) 0.0491(10) Uani 1 1 d . . .
H24A H -0.0140 -0.1382 0.1052 0.059 Uiso 1 1 calc R . .
H24B H 0.0009 -0.2318 0.0613 0.059 Uiso 1 1 calc R . .
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'
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
O5 W O2 159.94(11) . . ?
O5 W O6 84.16(11) . . ?
O2 W O6 85.77(12) . . ?
O5 W ClO 100.43(8) . . ?
O2 W ClO 98.53(8) . . ?
O6 W ClO 101.23(9) . . ?
O5 W O3 80.90(10) . . ?
O2 W O3 80.39(10) . . ?
O6 W O3 80.80(11) . . ?
ClO W O3 177.65(7) . . ?
O5 W Cl1 90.34(8) . . ?
O2 W Cl1 93.71(9) . . ?
O6 W Cl1 161.27(9) . . ?
ClO W Cl1 97.36(4) . . ?
O3 W Cl1 80.66(8) . . ?
C1 O2 W 139.2(2) . . ?
C3 O3 W 131.0(2) . . ?
C8 O5 W 133.8(2) . . ?
C10 O6 W 136.1(2) . . ?
O2 C1 C4 117.4(3) . . ?
O2 C1 C2 122.2(3) . . ?
C4 C1 C2 120.4(3) . . ?
C7 C2 C1 118.4(3) . . ?
C7 C2 C3 119.9(3) . . ?
C1 C2 C3 121.7(3) . . ?
O3 C3 O4 121.7(3) . . ?
O3 C3 C2 123.2(3) . . ?
O4 C3 C2 115.2(3) . . ?
C5 C4 C1 119.8(3) . . ?
C4 C5 C6 120.6(4) . . ?
C7 C6 C5 120.3(4) . . ?
C6 C7 C2 120.4(4) . . ?
O5 C8 C9 120.9(3) . . ?
O5 C8 C14 117.7(3) . . ?
C9 C8 C14 121.4(3) . . ?
C8 C9 C11 118.0(3) . . ?
C8 C9 C10 123.9(3) . . ?
C11 C9 C10 118.0(3) . . ?
O7 C10 O6 119.5(4) . . ?
O7 C10 C9 123.8(3) . . ?
O6 C10 C9 116.7(3) . . ?
C12 C11 C9 120.7(4) . . ?
C11 C12 C13 120.4(3) . . ?
C12 C13 C14 120.2(4) . . ?
C13 C14 C8 119.3(3) . . ?
C24 O21 C21 105.6(3) . . ?
O21 C21 C22 104.4(4) . . ?
C21 C22 C23 104.7(4) . . ?
C24 C23 C22 104.7(4) . . ?
O21 C24 C23 105.9(3) . . ?
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
W O5 1.885(2) . ?
W O2 1.896(3) . ?
W O6 1.960(3) . ?
W ClO 2.1158(10) . ?
W O3 2.252(3) . ?
W Cl1 2.3248(10) . ?
O2 C1 1.348(4) . ?
O3 C3 1.246(4) . ?
O4 C3 1.282(4) . ?
O5 C8 1.367(4) . ?
O6 C10 1.346(4) . ?
O7 C10 1.203(4) . ?
C1 C4 1.378(5) . ?
C1 C2 1.413(5) . ?
C2 C7 1.405(5) . ?
C2 C3 1.471(5) . ?
C4 C5 1.380(5) . ?
C5 C6 1.384(6) . ?
C6 C7 1.370(5) . ?
C8 C9 1.384(5) . ?
C8 C14 1.387(5) . ?
C9 C11 1.404(5) . ?
C9 C10 1.472(5) . ?
C11 C12 1.372(6) . ?
C12 C13 1.379(6) . ?
C13 C14 1.380(5) . ?
O21 C24 1.440(5) . ?
O21 C21 1.449(5) . ?
C21 C22 1.495(6) . ?
C22 C23 1.529(7) . ?
C23 C24 1.508(7) . ?
