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_2011301
_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          '[Fe (C2 H8 N2 )3 ]2 , Sb2 Se5 '
_chemical_formula_moiety         '2C6 H24 Fe N6 2+ , Sb2 Se5 4- '
_chemical_formula_sum            'C12 H48 Fe2 N12 Sb2 Se5'
_chemical_formula_weight         1110.62
_chemical_name_systematic
;
di[tri(ethylenediamino)ferro] antimony selenide
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.774(3)
_cell_length_b                   11.739(2)
_cell_length_c                   18.239(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.0
_cell_measurement_theta_min      7.5
_cell_volume                     3377.3(11)
_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  .1150
_diffrn_reflns_av_sigmaI/netI    .1578
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6283
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.43
_diffrn_standards_decay_%        5.0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.837
_exptl_absorpt_correction_T_max  .2105
_exptl_absorpt_correction_T_min  .0178
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al,, 1968)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .2
_refine_diff_density_max         .791
_refine_diff_density_min         -.949
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         3321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          .1820
_refine_ls_R_factor_gt           .0823
_refine_ls_shift/su_max          .000
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0556P)^2^+2.0077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1711
_reflns_number_gt                1719
_reflns_number_total             3321
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            da1117.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0556P)^2^+2.0077P] 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^)+(0.0556P)^2^+2.0077P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2011301
_cod_database_fobs_code          2011301