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_4327366
_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            'C12 H36 Mn4 N8 S10 Sb4'
_chemical_formula_weight         1319.85
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                101.11(3)
_cell_angle_beta                 105.27(3)
_cell_angle_gamma                91.76(3)
_cell_formula_units_Z            1
_cell_length_a                   8.4200(17)
_cell_length_b                   9.900(2)
_cell_length_c                   11.430(2)
_cell_measurement_temperature    293(2)
_cell_volume                     898.6(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.836
_diffrn_measured_fraction_theta_max 0.836
_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  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7625
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    4.919
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    2.439
_exptl_crystal_F_000             628
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.0023(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         3611
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0202
_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^)+(0.0206P)^2^+0.4322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0515
_refine_ls_wR_factor_ref         0.0526
_reflns_number_gt                3434
_reflns_number_total             3611
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0349702Bsi20031219_082121_2.cif
_cod_data_source_block           '[Mn(tren)]2Mn2Sb4S10'
_cod_database_code               4327366