Molecular building blocks for solid-state chalcogenides: solvothermal synthesis of [Mn(en)~3~]Te~4~ and [Fe(en)~3~]~2~(Sb~2~Se~5~)
Chen, Zhen; Wang, Ru-Ji; Xiao-Ying Huang; Li, Jing; Acta Crystallographica Section C 56 (2000) 1100–1103; doi:10.1107/S0108270100006879

data_2011300
_publ_section_title
;
 Molecular building blocks for solid-state chalcogenides: solvothermal
 synthesis of [Mn(en)~3~]Te~4~ and [Fe(en)~3~]~2~(Sb~2~Se~5~)
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1100
_journal_page_last               1103
_journal_paper_doi               10.1107/S0108270100006879
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[Mn(C2 H8 N2 )3 ]Te 4'
_chemical_formula_moiety         'C6 H24 Mn N6 2- , Te4 2- '
_chemical_formula_sum            'C6 H24 Mn N6 Te4'
_chemical_formula_weight         745.65
_chemical_name_systematic
;
tri(ethylenediamino)manganous telluride
;
_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'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.37(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.461(2)
_cell_length_b                   15.653(3)
_cell_length_c                   14.269(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.8
_cell_measurement_theta_min      8.0
_cell_volume                     1889.2(7)
_computing_cell_refinement       'CAD4/PC Software'
_computing_data_collection       'CAD4/PC Software (Enraf-Nonius, 1992)'
_computing_data_reduction        'XCAD4/PC (Harms, 1997)'
_computing_molecular_graphics
'SCHAKAL92 (Keller, 1992) and ORTEX (McArdle, 1993)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0421
_diffrn_reflns_av_sigmaI/netI    .0429
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3444
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        5.2
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.746
_exptl_absorpt_correction_T_max  .1322
_exptl_absorpt_correction_T_min  .1196
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          .33
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .3
_refine_diff_density_max         1.365
_refine_diff_density_min         -.770
_refine_ls_extinction_coef       .00129(4)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.343
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         3306
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.346
_refine_ls_R_factor_all          .0731
_refine_ls_R_factor_gt           .0411
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0010P)^2^+5.00P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .0717
_reflns_number_gt                2382
_reflns_number_total             3306
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            da1117.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0010P)^2^+5.00P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0010P)^2^+5.00P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2011300