Synthesis and Characterization of Mo6 Chalcobromides and Cyano-Substituted Compounds Built from a Novel [(Mo6Bri6Yi2)La6]n- Discrete Cluster Unit (Yi= S or Se and La= Br or CN)
Stéphane Cordier; Nikolaï G. Naumov; Diala Salloum; Frédéric Paul; Christiane Perrin; Inorganic Chemistry 43 (2004) 219–226; doi:10.1021/ic034443q

data_4310282
_publ_contact_author_address
;
LCSIM UMR 6511 CNRS - Universit\'e de Rennes 1, Institut de Chimie
de Rennes, B\^at. 10A, Campus de Beaulieu, Avenue du G\'en\'eral Leclerc,
35042 Rennes, France
;
_publ_contact_author_email       christiane.perrin@univ-rennes1.fr
_publ_contact_author_fax         33299635704
_publ_contact_author_name        'Perrin, Christiane'
_publ_contact_author_phone       33223236253
_publ_section_title
;
 Synthesis and Characterization of Mo6 Chalcobromides and
 Cyano-Substituted Compounds Built from a Novel [(Mo6Bri6Yi2)La6]n-
 Discrete Cluster Unit (Yi= S or Se and La= Br or CN)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              219
_journal_page_last               226
_journal_paper_doi               10.1021/ic034443q
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C106 H252 Br18 Cs0.4 K0.6 Mo18 N29 O16 S6'
_chemical_formula_sum            'C106 H252 Br18 Cs0.4 K0.6 Mo18 N29 O16 S6'
_chemical_formula_weight         5623.47
_space_group_IT_number           221
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 4 2 3'
_symmetry_space_group_name_H-M   'P m -3 m'
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2002-05-16
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   17.1969(4)
_cell_length_b                   17.1969(4)
_cell_length_c                   17.1969(4)
_cell_measurement_reflns_used    20088
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.373
_cell_measurement_theta_min      2.546
_cell_volume                     5085.7(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1297
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            54672
_diffrn_reflns_theta_full        26.34
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    4.9
_exptl_absorpt_correction_T_max  0.7197
_exptl_absorpt_correction_T_min  0.6702
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2443
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.866
_refine_diff_density_min         -0.509
_refine_ls_extinction_coef       0.0006(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+6.8862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1454
_reflns_number_gt                803
_reflns_number_total             1102
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034443qsi20030428_044710_3.cif
_cod_data_source_block           analytic
_cod_database_code               4310282