Synthesis, Characterization, and Ligand Exchange Studies of W6S8L6 Cluster Compounds
Song Jin; Ran Zhou; Ellen M. Scheuer; Jennifer Adamchuk; Lori L. Rayburn; Francis J. DiSalvo; Inorganic Chemistry 40 (2001) 2666–2674; doi:10.1021/ic001314q

data_1004007
_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
;
Synthesis, Characterization, and Ligand Exchange Studies of W6S8L6 Cluster
Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2666
_journal_page_last               2674
_journal_paper_doi               10.1021/ic001314q
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        ?
_chemical_formula_analytical     ?
_chemical_formula_moiety         'W6 S8 (C4H11N)6 (C4H11N)'
_chemical_formula_structural     ?
_chemical_formula_sum            'C32 H88 N8 S8 W6'
_chemical_formula_weight         1944.68
_chemical_melting_point          ?
_chemical_name_common            'Tungsten Sulfide cluster'
_chemical_name_systematic
;
octakis(\mu~3~-sulfido)-hexakis(tert-butylamine)-hexa-tungsten
tert-butylamine solvate
;
_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                 99.7030(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.1036(4)
_cell_length_b                   20.8216(3)
_cell_length_c                   11.497
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_cell_volume                     5451.46(12)
_computing_cell_refinement       'Bruker SAINT Plus'
_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       ?
_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  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15950
_diffrn_reflns_theta_max         28.19
_diffrn_reflns_theta_min         1.33
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    12.946
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_crystal_colour            BROWN-RED
_exptl_crystal_density_diffrn    2.369
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3632
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.354
_refine_diff_density_min         -3.972
_refine_diff_density_rms         0.542
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.061
_refine_ls_goodness_of_fit_obs   0.969
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         5964
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.061
_refine_ls_restrained_S_obs      0.969
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_obs          0.0325
_refine_ls_shift/esd_max         -1.915
_refine_ls_shift/esd_mean        0.039
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0905
_refine_ls_wR_factor_obs         0.0747
_reflns_number_observed          4914
_reflns_number_total             5964
_reflns_observed_criterion       >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0398P)^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^)+(0.0398P)^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 

The following automatic conversions were performed:
data name '_publ_contact_email' replaced with
'_publ_contact_author_email' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1004007