Synthesis and Characterization of Hydrogen-Bonded Assemblies of W6S8L6 Clusters
Catherine M. Oertel; Ryan D. Sweeder; Sonal Patel; Craig M. Downie; Francis J. DiSalvo; Inorganic Chemistry 44 (2005) 2287–2296; doi:10.1021/ic0487225

data_4309002
_publ_contact_author
;
F. J. DiSalvo
102B Baker Laboratory
Dept. of Chemistry and Chemical Biology
Cornell University
Ithaca NY 14853
USA
;
_publ_contact_author_email       fjd3@cornell.edu
_publ_section_title
;
Synthesis and Characterization of Hydrogen-Bonded Assemblies of
W6S8L6 Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2287
_journal_page_last               2296
_journal_paper_doi               10.1021/ic0487225
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C52 H0 N15 O8 S8 W6'
_chemical_formula_weight         2322.25
_chemical_name_common
'tungsten sulfide cluster with 4-pyridineacetamide ligands'
_chemical_name_systematic
;octakis(mu!3$-sulfido)-hexakis(4-pyridineacetamide)
-hexa-tungsten dimethylformamide 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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.270(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.461(11)
_cell_length_b                   33.08(2)
_cell_length_c                   13.165(10)
_cell_measurement_temperature    173(2)
_cell_volume                     6977(8)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'phi and omega 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  0.1197
_diffrn_reflns_av_sigmaI/netI    0.1755
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20874
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    10.148
_exptl_absorpt_correction_T_max  0.8228
_exptl_absorpt_correction_T_min  0.1064
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details
;
G.M. Sheldrick, SADABS, Program for Correction of Area Detector Data, 
University of Goettingen, Goettingen, Germany, 1997.
;
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    2.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4212
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.349
_refine_diff_density_min         -4.430
_refine_diff_density_rms         0.482
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         9724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.1776
_refine_ls_R_factor_gt           0.0846
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1442P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2128
_refine_ls_wR_factor_ref         0.2704
_reflns_number_gt                4739
_reflns_number_total             9724
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0487225si20050126_015030_2.cif
_cod_data_source_block           w6s8(4-pyridineacetamide)6
_cod_original_cell_volume        6977(9)
_cod_database_code               4309002