Synthesis and structure of a paramagnetic Mo(3)S(4) incomplete cuboidal cluster with seven cluster skeletal electrons.
Petrov, Pavel A.; Naumov, Dmitry Yu; Llusar, Rosa; Gómez-García, Carlos J; Polo, Víctor; Konchenko, Sergey N.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 14031–14034; doi:10.1039/c2dt31577g

data_7020444
_publ_section_title
;
 Synthesis and structure of a paramagnetic Mo(3)S(4) incomplete cuboidal
 cluster with seven cluster skeletal electrons.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14031
_journal_page_last               14034
_journal_paper_doi               10.1039/c2dt31577g
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C92.5 H94 Br2.6 Cl0.4 Mo3 O P6 S4'
_chemical_formula_weight         2044.67
_chemical_properties_physical    air-sensitive
_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                 99.5800(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8775(6)
_cell_length_b                   22.7907(8)
_cell_length_c                   25.1597(8)
_cell_measurement_reflns_used    8908
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.65
_cell_measurement_theta_min      2.21
_cell_volume                     8977.3(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            47394
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.21
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.824
_exptl_absorpt_correction_T_max  0.5677
_exptl_absorpt_correction_T_min  0.4624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4138
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.522
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     998
_refine_ls_number_reflns         16960
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0791P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1380
_reflns_number_gt                12791
_reflns_number_total             16960
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2dt31577g.txt
_cod_data_source_block           2b
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7020444