Ligand Substitution Reactions of W6S8L6 with Tricyclohexylphosphine (L = 4-tert-Butylpyridine or n-Butylamine): 31P NMR and Structural Studies of W6S8(PCy3)n(4-tert-butylpyridine)6-n (0 < n <= 6) Complexes
Song Jin; D. Venkataraman; Francis J. DiSalvo; Inorganic Chemistry 39 (2000) 2747–2757; doi:10.1021/ic991426l

data_2000023
_publ_contact_author
; 
Prof. Francis J. DiSalvo 
Department of Chemistry and Chemical Biology 
Cornell University 
Ithaca, NY 14853 
;
_publ_contact_author_email       fjd3@cornell.edu
_publ_contact_author_fax         607-255-4137
_publ_contact_author_phone       607-255-7238
_publ_section_title
;
Ligand Substitution Reactions of W6S8L6 with Tricyclohexylphosphine (L =
4-tert-Butylpyridine or n-Butylamine): 31P NMR and Structural Studies of
W6S8(PCy3)n(4-tert-butylpyridine)6-n (0 < n <= 6) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2747
_journal_page_last               2757
_journal_paper_doi               10.1021/ic991426l
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C104 H190 N2 P4 S8 W6'
_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
_cell_angle_alpha                90
_cell_angle_beta                 111.321(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.2094(2)
_cell_length_b                   13.1764(2)
_cell_length_c                   29.4518(5)
_cell_volume                     11282.464
_computing_cell_refinement       'BRUKER SAINT'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        SHELXTL
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART CCD Diffractometer'
_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  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            32739
_diffrn_reflns_theta_max         28.48
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    6.341
_exptl_absorpt_correction_T_max  0.9211
_exptl_absorpt_correction_T_min  0.5766
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_F_000             5840
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.933
_refine_diff_density_min         -2.434
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.146
_refine_ls_goodness_of_fit_obs   1.204
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         12611
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.162
_refine_ls_restrained_S_obs      1.204
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0365
_refine_ls_R_factor_obs          0.0365
_refine_ls_shift/esd_max         0.607
_refine_ls_shift/esd_mean        0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0704
_refine_ls_wR_factor_gt          0.0365
_refine_ls_wR_factor_obs         0.0632
_reflns_number_observed          9584
_reflns_number_total             12621
_reflns_observed_criterion       >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^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^)+(0.0000P)^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_sg_symbol_H-M      'C 2/c'
_cod_database_code               2000023