K~2~Mo~15~S~19~: a novel ternary reduced molybdenum sulfide containing Mo~6~ and Mo~9~ clusters
Picard, S.; Gougeon, P.; Potel, M.; Acta Crystallographica Section E 58 (2002) i12–i14; doi:10.1107/S1600536801021651

data_2200816
_publ_section_title
;
 K~2~Mo~15~S~19~: a novel ternary reduced molybdenum sulfide containing
 Mo~6~ and Mo~9~ clusters
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i12
_journal_page_last               i14
_journal_paper_doi               10.1107/S1600536801021651
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'K2 Mo15 S19'
_chemical_formula_moiety         'K2 Mo15 S19'
_chemical_formula_sum            'K2 Mo15 S19'
_chemical_formula_weight         2126.44
_chemical_name_systematic
;
?
;
_space_group_IT_number           167
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   9.3857(9)
_cell_length_b                   9.3857(9)
_cell_length_c                   56.261(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.18
_cell_measurement_theta_min      6.3
_cell_volume                     4292.1(9)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'WinGX (Farrugia, 1999)'
_computing_molecular_graphics    'DIAMOND (Bergerhoff, 1996)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \q-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0158
_diffrn_reflns_av_sigmaI/netI    .0201
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       90
_diffrn_reflns_limit_l_min       -90
_diffrn_reflns_number            4181
_diffrn_reflns_theta_full        34.94
_diffrn_reflns_theta_max         34.94
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        <1%
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.997
_exptl_absorpt_correction_T_max  .527
_exptl_absorpt_correction_T_min  .501
_exptl_absorpt_correction_type   \y-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.936
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pseudo-cube
_exptl_crystal_F_000             5832
_exptl_crystal_size_max          .1
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .08
_refine_diff_density_max         .808
_refine_diff_density_min         -.867
_refine_ls_extinction_coef       .000086(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         2102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          .0285
_refine_ls_R_factor_gt           .0189
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0122p)^2^+8.4803p] where p = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .0361
_refine_ls_wR_factor_ref         .0377
_reflns_number_gt                1753
_reflns_number_total             2102
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            br6039.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_adp_type' value 'uani' changed to 'Uani' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (9
times).

'_atom_site_refinement_flags' value 's' changed to 'S' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (5
times).

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (5 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_atom_site_adp_type' value 'uani' changed to 'Uani' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (9
times).

'_atom_site_refinement_flags' value 's' changed to 'S'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (5
times).

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (5 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               2200816
_cod_database_fobs_code          2200816