Inorganic Frameworks from Selenidotetrelate Anions [T2Se6]4-(T = Ge, Sn): Synthesis, Structures, and Ionic Conductivity of [K2(H2O)3][MnGe4Se10] and (NMe4)2[MSn4Se10] (M = Mn, Fe)
Sima Haddadpour; Maike Melullis; Halgard Staesche; C. R. Mariappan; Bernhard Roling; Rodolphe Clérac; Stefanie Dehnen; Inorganic Chemistry 48 (2009) 1689–1698; doi:10.1021/ic802170f

data_4301513
_publ_section_title
;
Inorganic Frameworks from Selenidotetrelate Anions [T2Se6]4-(T = Ge, Sn):
Synthesis, Structures, and Ionic Conductivity of [K2(H2O)3][MnGe4Se10] and
(NMe4)2[MSn4Se10] (M = Mn, Fe)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1689
_journal_page_last               1698
_journal_paper_doi               10.1021/ic802170f
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C18 H56 N4 O2 Se6 Sn2'
_chemical_formula_weight         1071.81
_chemical_name_systematic
; 
 ? 
;
_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'
_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                 107.81(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.207(2)
_cell_length_b                   9.785(2)
_cell_length_c                   17.651(4)
_cell_measurement_temperature    193(2)
_cell_volume                     1842.9(7)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_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  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0912
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8723
_diffrn_reflns_theta_full        25.89
_diffrn_reflns_theta_max         25.89
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    7.300
_exptl_absorpt_correction_T_max  0.4014
_exptl_absorpt_correction_T_min  0.2190
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.932
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.75
_exptl_crystal_size_min          0.60
_refine_diff_density_max         1.128
_refine_diff_density_min         -0.917
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.807
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.807
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0722
_reflns_number_gt                2203
_reflns_number_total             3520
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802170f_si_001_4.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1842.8(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4301513