Synthesis and Properties of the Heterospin (S1 = S2 = (1)/2) Radical-Ion Salt Bis(mesitylene)molybdenum(I) [1,2,5]Thiadiazolo[3,4-c][1,2,5]thiadiazolidyl.
Pushkarevsky, Nikolay A.; Semenov, Nikolay A.; Dmitriev, Alexey A.; Kuratieva, Natalia V.; Bogomyakov, Artem S.; Irtegova, Irina G.; Vasilieva, Nadezhda V.; Bode, Bela E.; Gritsan, Nina P.; Konstantinova, Lidia S.; Woollins, J. Derek; Rakitin, Oleg A.; Konchenko, Sergey N.; Ovcharenko, Victor I.; Zibarev, Andrey V.; Inorganic chemistry 54 (2015) 7007–7013; doi:10.1021/acs.inorgchem.5b01033

data_4343461
_publ_section_title
;
 Synthesis and Properties of the Heterospin (S1 = S2 = (1)/2) Radical-Ion
 Salt Bis(mesitylene)molybdenum(I)
 [1,2,5]Thiadiazolo[3,4-c][1,2,5]thiadiazolidyl.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7007
_journal_page_last               7013
_journal_paper_doi               10.1021/acs.inorgchem.5b01033
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C18 H24 Mo, C2 N4 S2'
_chemical_formula_sum            'C20 H24 Mo N4 S2'
_chemical_formula_weight         480.49
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.139(2)
_cell_angle_beta                 104.494(2)
_cell_angle_gamma                92.145(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4459(3)
_cell_length_b                   8.4852(3)
_cell_length_c                   14.5051(6)
_cell_measurement_reflns_used    5715
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.44
_cell_measurement_theta_min      3.97
_cell_volume                     1000.45(7)
_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 0.909
_diffrn_measured_fraction_theta_max 0.910
_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  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0704
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7735
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         4.38
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  0.9575
_exptl_absorpt_correction_T_min  0.8441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3458
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0740
_reflns_number_gt                2832
_reflns_number_total             3458
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic5b01033_si_002.cif
_cod_data_source_block           np579
_cod_depositor_comments          'Adding full bibliography for 4343461.cif.'
_cod_database_code               4343461