Bis(diethylenetriamine)cobalt(II) tetrathiomolybdate(VI) oxotrithiamolybdate(VI)
Poisot, Martha; Näther, Christian; Bensch, Wolfgang; Acta Crystallographica Section E 62 (2006) m1326–m1328; doi:10.1107/S1600536806017934

data_2209107
_publ_section_title
;
 Bis(diethylenetriamine)cobalt(II) tetrathiomolybdate(VI)
 oxotrithiamolybdate(VI)
;
_journal_coeditor_code           BT2081
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1326
_journal_page_last               m1328
_journal_paper_doi               10.1107/S1600536806017934
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Co (C4 H13 N3)2]2 [Mo S4] [Mo O S3]'
_chemical_formula_moiety         '2C8 H26 Co N6 2+, Mo S4 2-, Mo O S3 2-'
_chemical_formula_sum            'C16 H52 Co2 Mo2 N12 O S7'
_chemical_formula_weight         962.86
_chemical_name_systematic
;
Bis(diethylenetriamine)cobalt(II) tetrathiomolybdate(VI)
oxotrithiamolybdate(VI)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.063(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.4164(5)
_cell_length_b                   15.9171(11)
_cell_length_c                   15.4070(12)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     1816.2(2)
_computing_cell_refinement       'IPDS Program Package'
_computing_data_collection       'IPDS Program Package (Stoe & Cie, 1998)'
_computing_data_reduction        'IPDS Program Package'
_computing_molecular_graphics
;
XP in SHELXTL (Bruker, 1998) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material  'CIFTAB in SHELXTL'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Stoe IPDS-1'
_diffrn_measurement_method       \f
_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  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11766
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.007
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red--orange
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.601
_refine_ls_extinction_coef       0.0022(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         3269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0458P)^2^+2.2351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                2455
_reflns_number_total             3269
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt2081.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2209107