Solvothermal synthesis, crystal structures and properties of three new thiogermanates: the only example of the thiogermanate anion [Ge2S6]4− as a bridging ligand to a lanthanide complex ion
Liu, Xing; Hu, Feilong; Zhou, Jian; An, Litao; Liang, Dawen; Lin, Jianwu; CrystEngComm 14 (2012) 3464–; doi:10.1039/c2ce25082a

data_7207867
_publ_section_title
;
 Solvothermal synthesis, crystal structures and properties of three new
 thiogermanates: the only example of the thiogermanate anion
 [Ge2S6]4&#x2212; as a bridging ligand to a lanthanide complex ion
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              3464
_journal_paper_doi               10.1039/c2ce25082a
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C12 H39 Eu N9, 0.5(Ge2 S6), Cl '
_chemical_formula_sum            'C12 H39 Cl Eu Ge N9 S3'
_chemical_formula_weight         665.76
_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                 96.434(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.567(5)
_cell_length_b                   14.633(6)
_cell_length_c                   14.465(6)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      1.99
_cell_volume                     2432.9(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_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  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12834
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    4.175
_exptl_absorpt_correction_T_max  0.7587
_exptl_absorpt_correction_T_min  0.6129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.818
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.142
_refine_diff_density_min         -1.159
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+2.8141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0694
_reflns_number_gt                3984
_reflns_number_total             4308
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25082a.txt
_cod_data_source_block           2
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C12 H39 Cl Eu Ge N9 S3 '
_cod_database_code               7207867