Synthesis, characterization and properties of Mo6S8(4-tert-butylpyridine)6 and related M6S8L6 cluster complexes (M = Mo, W)
Jin, Song; Popp, Friedrich; Boettcher, Shannon W.; Yuan, Min; Oertel, Catherine M.; DiSalvo, Francis J.; Journal of the Chemical Society, Dalton Transactions  (2002) 3096–; doi:10.1039/b202246j

data_2000017
_publ_section_title
;
 Synthesis, characterization and properties of
 Mo6S8(4-tert-butylpyridine)6 and related M6S8L6 cluster complexes (M =
 Mo, W)
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3096
_journal_paper_doi               10.1039/b202246j
_journal_year                    2002
_chemical_formula_moiety         Mo6S8(C9H13N)6(C4H10O)2
_chemical_formula_sum            'C62 H98 Mo6 N6 O2 S8'
_chemical_formula_weight         1791.58
_chemical_name_common            'Molybdenum sulfide cluster with'
_chemical_name_systematic
; 
octakis(mu!3$-sulfido)-hexakis(4-tert-butylpyridine) 
-hexa-molybdenum-bis(diethylether)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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.450(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.192(3)
_cell_length_b                   9.3346(8)
_cell_length_c                   27.803(2)
_cell_measurement_temperature    173(2)
_cell_volume                     7620.8(11)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0516
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27811
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.218
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.800861
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             3632
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.999
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.345
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         6478
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.377
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          1.416
_refine_ls_shift/su_mean         0.050
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0975
_reflns_number_gt                5009
_reflns_number_total             6478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b202246j.txt
_cod_data_source_block           final_1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        7620.7(11)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2000017