Tungsten Oxo Salicylate Complexes from Tungsten Hexachloride Reactions Systems
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; Inorganic Chemistry 40 (2001) 5010–5016; doi:10.1021/ic001456k

data_4320236
_publ_section_title
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 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/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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