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_2000025
_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            'C122 H230 P6 S8 W6'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                62.161(1)
_cell_angle_beta                 78.813(1)
_cell_angle_gamma                73.48
_cell_formula_units_Z            1
_cell_length_a                   15.0729(1)
_cell_length_b                   15.2558(1)
_cell_length_c                   16.0623(2)
_cell_volume                     3123.041
_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      165(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  0.0614
_diffrn_reflns_av_sigmaI/netI    0.1186
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            18568
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    5.759
_exptl_absorpt_correction_T_max  0.6943
_exptl_absorpt_correction_T_min  0.3364
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.612
_refine_diff_density_min         -3.665
_refine_diff_density_rms         0.336
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.946
_refine_ls_goodness_of_fit_obs   0.976
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         12854
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.010
_refine_ls_restrained_S_obs      0.978
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.046
_refine_ls_R_factor_obs          0.0460
_refine_ls_shift/esd_max         0.742
_refine_ls_shift/esd_mean        0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1443
_refine_ls_wR_factor_gt          0.046
_refine_ls_wR_factor_obs         0.1201
_reflns_number_observed          9605
_reflns_number_total             12857
_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^)+(0.0450P)^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^)+(0.0450P)^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               2000025