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:

data_4114996
_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_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C68 H97 N5 P S8 W6'
_chemical_formula_weight         2375.06
_chemical_name_common            'tungsten sulfide cluster'
_chemical_name_systematic
; 
octakis(mu!3$-sulfido)-pentakis(tert-butylpyridine)-triethylphosphine- 
hexa-tungsten bezene solvate 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 91.4768(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1816(4)
_cell_length_b                   15.9178(4)
_cell_length_c                   29.4907(8)
_cell_measurement_temperature    173(2)
_cell_volume                     7593.6(3)
_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      173(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  0.1062
_diffrn_reflns_av_sigmaI/netI    0.1364
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            36845
_diffrn_reflns_theta_max         24.76
_diffrn_reflns_theta_min         1.26
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    9.335
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.5222
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'DARK RED'
_exptl_crystal_density_diffrn    2.077
_exptl_crystal_density_meas      ?
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             4508
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.748
_refine_diff_density_min         -2.468
_refine_diff_density_rms         0.423
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.099
_refine_ls_goodness_of_fit_obs   1.205
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         9171
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.184
_refine_ls_restrained_S_obs      1.208
_refine_ls_R_factor_all          0.1579
_refine_ls_R_factor_obs          0.0571
_refine_ls_shift/esd_max         0.009
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1660
_refine_ls_wR_factor_obs         0.1122
_reflns_number_observed          5455
_reflns_number_total             12741
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja0257873_s2_1.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^)+(0.0474P)^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^)+(0.0474P)^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               4114996