Solvothermal Syntheses, Crystal Structures, and Thermal Properties of New Manganese Thioantimonates(III): The First Example of the Thermal Transformation of an Amine-Rich Thioantimonate into an Amine-Poorer Thioantimonate
Michael Schaefer; Christian Näther; Nicolai Lehnert; Wolfgang Bensch; Inorganic Chemistry 43 (2004) 2914–2921; doi:10.1021/ic034970+

data_4327365
_publ_section_title
;
 Solvothermal Syntheses, Crystal Structures, and Thermal Properties of New
 Manganese Thioantimonates(III): The First Example of the Thermal
 Transformation of an Amine-Rich Thioantimonate into an Amine-Poorer
 Thioantimonate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2914
_journal_page_last               2921
_journal_paper_doi               10.1021/ic034970+
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C6 H18 Mn N4 S2.5 Sb'
_chemical_formula_weight         403.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.6313(4)
_cell_length_b                   18.9876(10)
_cell_length_c                   16.4104(10)
_cell_measurement_temperature    293(2)
_cell_volume                     2689.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0152
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23823
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    3.310
_exptl_absorpt_correction_T_max  0.6595
_exptl_absorpt_correction_T_min  0.5604
_exptl_absorpt_correction_type   numerical
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_F_000             1584
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         3167
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+3.0753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0726
_reflns_number_gt                2471
_reflns_number_total             3167
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0349702Bsi20031219_082121_1.cif
_cod_data_source_block           '[Mn(tren)]2Sb2S5'
_cod_original_formula_sum        'C6 H18 Mn N4 S2.50 Sb'
_cod_database_code               4327365