Solvothermal syntheses of lanthanide thiogermanates displaying three new structural moieties
Zhao, Rongqing; Zhou, Jian; Liu, Xing; Zhang, Li; Tang, Qiuling; Tan, XiaoFeng; RSC Advances  (2014) –; doi:10.1039/C4RA07812H

data_7217790
_publ_section_title
;
 Solvothermal syntheses of lanthanide thiogermanates displaying three new
 structural moieties
;
_journal_name_full               'RSC Advances'
_journal_paper_doi               10.1039/C4RA07812H
_journal_year                    2014
_chemical_formula_moiety         'C12 H39 N9 Sm, 0.5(Ge2 S6), Cl'
_chemical_formula_sum            'C12 H39 Cl Ge N9 S3 Sm'
_chemical_formula_weight         664.15
_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                 97.105(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.532(3)
_cell_length_b                   14.423(4)
_cell_length_c                   14.573(4)
_cell_measurement_temperature    296(2)
_cell_volume                     2405.3(11)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16607
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    4.056
_exptl_absorpt_correction_T_max  0.6159
_exptl_absorpt_correction_T_min  0.3199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.077
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4206
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0245
_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^)+(0.0274P)^2^+5.5956P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0647
_refine_ls_wR_factor_ref         0.0667
_reflns_number_gt                3864
_reflns_number_total             4206
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra07812h2.cif
_cod_data_source_block           Ib
_cod_original_cell_volume        2405.3(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7217790