Synthesis and Characterization of Mixed Chalcogen Triangular Complexes with New Mo3(μ3-S)(μ2-Se2)34+ and M3(μ3-S)(μ2-Se)34+ (M = Mo, W) Cluster Cores
Artem L. Gushchin; Bee-Lean Ooi; Pernille Harris; Cristian Vicent; Maxim N. Sokolov; Inorganic Chemistry 48 (2009) 3832–3839; doi:10.1021/ic8023327

data_4301973
_publ_contact_author_address
;Department of Chemistry 
Kemitorvet Building 207
DK-2800 Kgs. Lyngby
Denmari
;
_publ_contact_author_email       ph@kemi.dtu.dk
_publ_contact_author_fax         +4545883136
_publ_contact_author_name        'Pernille Harris'
_publ_contact_author_phone       +4545252024
_publ_section_title
;
Synthesis and Characterization of Mixed Chalcogen Triangular Complexes with
New Mo3(\m3-S)(\m2-Se2)34+ and M3(\m3-S)(\m2-Se)34+ (M = Mo, W) Cluster Cores
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3832
_journal_page_last               3839
_journal_paper_doi               10.1021/ic8023327
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C84 H36 Mo6 N24 O35 S2 Se6'
_chemical_formula_weight         2762
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 104.4830(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.5848(11)
_cell_length_b                   18.5208(12)
_cell_length_c                   14.9836(10)
_cell_measurement_reflns_used    8236
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.404
_cell_measurement_theta_min      2.199
_cell_volume                     4456.2(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART platform ccd'
_diffrn_measurement_method       'profile data from \w/2\q 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  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30263
_diffrn_reflns_theta_full        27.94
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    3.644
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.780
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sheldrick,G.M. SADABS, 2001'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.058
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.292
_refine_diff_density_min         -1.529
_refine_diff_density_rms         0.258
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         5504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1214P)^2^+74.8004P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1934
_refine_ls_wR_factor_ref         0.2034
_reflns_number_gt                4559
_reflns_number_total             5504
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8023327_si_001_2.cif
_cod_data_source_block           sad_ag333
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_original_formula_sum        'C36 H36 C48 Mo6 N24 O35 S2 Se6'
_cod_database_code               4301973