Synthesis, Structural Evolution, and Theoretical and Physical Studies of the Novel Compounds M2Mo9S11 (M = K, Rb) and Related Metastable Materials CuxK1.8Mo9S11 (x = 0 or 2) Containing Bioctahedral Mo9 Clusters
Soazig Picard; Patrick Gougeon; Michel Potel; Inorganic Chemistry 38 (1999) 4422–4429; doi:10.1021/ic990362b

data_4322279
_publ_contact_author_address
;
Gougeon, P.
Laboratoire de Chimie du Solide et Inorganique Mol\'eculaire
URA CNRS No. 1495
Universit\'e de Rennes I
Avenue du G\'en\'eral Leclerc
35042 Rennes CEDEX
France
;
_publ_contact_author_email       Patrick.Gougeon@univ-rennes1.fr
_publ_contact_author_fax         '(33) 2 99 63 57 04'
_publ_contact_author_name        ' Gougeon, P.'
_publ_contact_author_phone       '(33) 2 99 28 62 54'
_publ_section_title
;
 Synthesis, Structural Evolution, and Theoretical and Physical Studies of
 the Novel Compounds M2Mo9S11 (M = K, Rb) and Related Metastable Materials
 CuxK1.8Mo9S11 (x = 0 or 2) Containing Bioctahedral Mo9 Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4422
_journal_page_last               4429
_journal_paper_doi               10.1021/ic990362b
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'Cu2 K1.8 Mo9 S11'
_chemical_formula_weight         1413.6
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   9.4215(4)
_cell_length_b                   9.4215(4)
_cell_length_c                   35.444(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      40
_cell_measurement_theta_min      2
_cell_volume                     2724.7(2)
_diffrn_measurement_device       'Nonius CAD4'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            3739
_diffrn_reflns_theta_max         39.93
_diffrn_reflns_theta_min         2.75
_diffrn_standards_decay_%        <1%
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.932
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.936
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    5.167
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3876
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.07
_refine_diff_density_min         -1.89
_refine_ls_extinction_coef       0.137(3)
_refine_ls_extinction_method     'B-C type 1 Lorentzian isotropic'
_refine_ls_goodness_of_fit_all   1.42
_refine_ls_goodness_of_fit_obs   1.56
_refine_ls_number_parameters     67
_refine_ls_number_reflns         1874
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_obs          0.0238
_refine_ls_shift/esd_max         0.0228
_refine_ls_shift/esd_mean        0.0044
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/\s^2^(F)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0222
_refine_ls_wR_factor_obs         0.0213
_reflns_limit_h_max              0
_reflns_limit_h_min              -14
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              63
_reflns_limit_l_min              0
_reflns_number_observed          1443
_reflns_number_total             1874
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ic990362b_3.cif
_cod_data_source_block           Cu2K1.8Mo9S11
_cod_original_cell_volume        2724.6(2)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_original_formula_sum        'K1.8 Mo9 S11 Cu2'
_cod_database_code               4322279