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_7217789
_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 Pr, 0.5(Ge2 S6), Cl '
_chemical_formula_sum            'C12 H39 Cl Ge N9 Pr S3'
_chemical_formula_weight         654.70
_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                 98.149(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.637(3)
_cell_length_b                   14.143(3)
_cell_length_c                   15.120(3)
_cell_measurement_temperature    296(2)
_cell_volume                     2463.4(10)
_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 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17095
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    3.555
_exptl_absorpt_correction_T_max  0.5454
_exptl_absorpt_correction_T_min  0.3121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4249
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0202P)^2^+3.4646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0570
_reflns_number_gt                3818
_reflns_number_total             4249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra07812h2.cif
_cod_data_source_block           Ia
_cod_original_cell_volume        2463.5(10)
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7217789