[Tris(2-aminoethyl)amine]manganese(II) heptasulfidotetraantimony(III) hemihydrate
Schaefer, Michael; Kurowski, Daniel; Pfitzner, Arno; Näther, Christian; Bensch, Wolfgang; Acta Crystallographica Section E 60 (2004) m183–m185; doi:10.1107/S1600536803027983

data_2203193
_publ_section_title
;
 [Tris(2-aminoethyl)amine]manganese(II) heptasulfidotetraantimony(III)
 hemihydrate
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m183
_journal_page_last               m185
_journal_paper_doi               10.1107/S1600536803027983
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Mn (C4 H13 N3)2] [Sb4 S7], 0.5H2 0'
_chemical_formula_moiety         'Mn C8 H26 N6 2+, Sb4 S7 2-, 0.5H2 O'
_chemical_formula_sum            'C8 H27 Mn N6 O0.5 S7 Sb4'
_chemical_formula_weight         980.71
_chemical_name_systematic
;[tris(2-aminoethyl)amine]manganese(II) tetraantimony heptasulfide
 hemihydrate,
[Mn(dien)~2~][Sb~4~S~7~].0.5H~2~0
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 91.88(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7216(19)
_cell_length_b                   16.113(3)
_cell_length_c                   17.339(4)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2.5
_cell_volume                     2714.6(10)
_computing_cell_refinement       IPDS
_computing_data_collection       'IPDS (Stoe & Cie, 1998)'
_computing_data_reduction        IPDS
_computing_molecular_graphics    'DIAMOND (Crystal Impact, 1999)'
_computing_publication_material  'CIFTAB in SHELXL97'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Stoe IPDS'
_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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31130
_diffrn_reflns_theta_full        28.01
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.931
_exptl_absorpt_correction_T_max  0.609
_exptl_absorpt_correction_T_min  0.390
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'[X-SHAPE (Stoe & Cie, 1998)and X-RED (Stoe & Cie, 1998)]'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Polyhedra
_exptl_crystal_F_000             1844
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.254
_refine_diff_density_min         -1.115
_refine_ls_extinction_coef       0.00169(13)
_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   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         6508
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0547P)^2^+3.6221P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0832
_reflns_number_gt                5824
_reflns_number_total             6508
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg6011.cif
_cod_data_source_block           I
_cod_original_cell_volume        2714.6(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2203193
_cod_database_fobs_code          2203193