The Dean-Evans Relation in 31P NMR Spectroscopy and Its Application to the Chemistry of Octahedral Tungsten Sulfide Clusters
Song Jin; Jennifer Adamchuk; Bosong Xiang; Francis J. DiSalvo; Journal of the American Chemical Society 124 (2002) 9229–9240; doi:10.1021/ja0257873

data_4114997
_publ_contact_author
; 
Prof. Francis J. DiSalvo 
Department of Chemistry and Chemical Biology 
Cornell University 
Ithaca, NY 14853, USA 
;
_publ_contact_author_email       fjd3@cornell.edu
_publ_contact_author_fax         607-255-4137
_publ_contact_author_phone       607-255-7238
_publ_section_title
;
 The Dean-Evans Relation in 31P NMR Spectroscopy and Its Application to
 the Chemistry of Octahedral Tungsten Sulfide Clusters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9229
_journal_page_last               9240
_journal_paper_doi               10.1021/ja0257873
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         'W6 S8 (PEt3)3(PCy3)3'
_chemical_formula_sum            'C84 H156 P6 S8 W6'
_chemical_formula_weight         2711.49
_chemical_name_common            'Tungsten sulfide cluster with mixed'
_chemical_name_systematic
; 
octakis(mu!3$-sulfido)-mer-tris(triethylphosphine) 
-tris(tricyclohexylphosphine)-hexa-tungsten 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                88.980(2)
_cell_angle_beta                 74.256(2)
_cell_angle_gamma                78.297(2)
_cell_formula_units_Z            2
_cell_length_a                   15.0562(10)
_cell_length_b                   16.2762(10)
_cell_length_c                   20.4880(13)
_cell_measurement_temperature    446(2)
_cell_volume                     4728.2(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      446(2)
_diffrn_measurement_device       'Bruker SMART CCD'
_diffrn_measurement_method       '\w 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  0.0660
_diffrn_reflns_av_sigmaI/netI    0.1126
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            41218
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.03
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    7.588
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.492930
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'brown red'
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2644
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.994
_refine_diff_density_min         -1.423
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.967
_refine_ls_goodness_of_fit_obs   1.064
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     877
_refine_ls_number_reflns         19023
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_restrained_S_obs      1.064
_refine_ls_R_factor_all          0.1227
_refine_ls_R_factor_obs          0.0498
_refine_ls_shift/esd_max         0.017
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1122
_refine_ls_wR_factor_obs         0.0780
_reflns_number_observed          10285
_reflns_number_total             19029
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja0257873_s2_4.cif
_cod_data_source_block           final
_cod_depositor_comments
;
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^)+(0.0298P)^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^)+(0.0298P)^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_database_code               4114997