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_4301974
_publ_contact_author_address
;Nikolaev Institute of Inorganic Chemistry,
SB Russian Academy of Sciences,
Akad. Lavrentiev prospekt 3,
Novosibirsk 90,
630090 Russia
;
_publ_contact_author_email       d.y.naumov@ngs.ru
_publ_contact_author_fax         7(383)3309489
_publ_contact_author_name        'Dr. Dmitry Yu. Naumov'
_publ_contact_author_phone       7(383)3309466
_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            'C48 H104 Br7 Mo3 N3 Se7'
_chemical_formula_weight         2123.25
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 97.049(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.224(2)
_cell_length_b                   13.463(2)
_cell_length_c                   42.744(6)
_cell_measurement_reflns_used    4812
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.28
_cell_measurement_theta_min      2.29
_cell_volume                     7552.4(19)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2004)'
_computing_publication_material  'SHELXTL (Bruker, 2004)'
_computing_structure_refinement  'SHELXTL (Bruker, 2004)'
_computing_structure_solution    'SHELXTL (Bruker, 2004)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_sigmaI/netI    0.0965
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            37452
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         0.96
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.597
_exptl_absorpt_correction_T_max  0.6585
_exptl_absorpt_correction_T_min  0.3953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4088
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.963
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         15372
_refine_ls_number_restraints     372
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.1330
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0757P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1576
_reflns_number_gt                7892
_reflns_number_total             15372
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic8023327_si_002.cif
_cod_data_source_block           ag237
_cod_original_cell_volume        7552(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4301974