Unique Formation of a Pentanuclear Lanthanum(III) Thiolate Oxide Cluster via Control of Hydrolysis
Li, Hong-Xi; Cheng, Mei-Ling; Ren, Zhi-Gang; Zhang, Wen-Hua; Lang, Jian-Ping; Shen, Qi; Inorganic Chemistry 45 (2006) 1885–1887; doi:10.1021/ic052073v

data_4332037
_publ_section_title
;
 Unique Formation of a Pentanuclear Lanthanum(III) Thiolate Oxide Cluster
 via Control of Hydrolysis
;
_journal_issue                   5
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1885
_journal_page_last               1887
_journal_paper_doi               10.1021/ic052073v
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C32 H62 La Li N2 O2 S2 Si4'
_chemical_formula_sum            'C32 H62 La Li N2 O2 S2 Si4'
_chemical_formula_weight         829.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.077(11)
_cell_angle_beta                 96.329(12)
_cell_angle_gamma                90.864(7)
_cell_formula_units_Z            2
_cell_length_a                   8.718(3)
_cell_length_b                   11.384(4)
_cell_length_c                   22.573(8)
_cell_measurement_reflns_used    7435
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.0
_cell_volume                     2167.0(13)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.974
_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     0.71070
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_sigmaI/netI    0.1001
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17997
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.220
_exptl_absorpt_correction_T_max  0.8195
_exptl_absorpt_correction_T_min  0.7752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Jacobson, R. (1998) Private communication to Rigaku Company.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.225
_refine_diff_density_min         -1.016
_refine_diff_density_rms         0.154
_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     385
_refine_ls_number_reflns         7744
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0695
_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^)+(0.1023P)^2^+1.4923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.1912
_reflns_number_gt                5800
_reflns_number_total             7744
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic052073vsup3.cif
_cod_data_source_block           4
_cod_original_cell_volume        2167.1(12)
_cod_database_code               4332037