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_2000014
_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         'Mo6 S8 (CH5N)6'
_chemical_formula_sum            'C6 H30 Mo6 N6 S8'
_chemical_formula_weight         1018.48
_chemical_name_common            'molybdenum sulfide cluster with'
_chemical_name_systematic
; 
octakis(mu!3$-sulfido)-hexakis(methylamine) 
-hexa-molybdenum 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                116.821(2)
_cell_angle_beta                 103.418(2)
_cell_angle_gamma                106.402(2)
_cell_formula_units_Z            1
_cell_length_a                   9.0965(10)
_cell_length_b                   9.1746(10)
_cell_length_c                   9.5609(10)
_cell_measurement_temperature    173(2)
_cell_volume                     619.97(12)
_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 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6962
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.623
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.461776
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.728
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       wedge
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.050
_refine_diff_density_min         -1.372
_refine_diff_density_rms         0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         2882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1092
_reflns_number_gt                2349
_reflns_number_total             2882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b202246j.txt
_cod_data_source_block           final_3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_sg_symbol_H-M      P-1
_cod_database_code               2000014