Poly[hexaaquaocta-μ~3~-hydroxido-tetrakis(μ~3~-methylenedisulfonato)-μ~6~-oxido-hexaytterbium(III)]: the first lanthanide sulfonate containing a hexanuclear Ln‒hydroxide/oxide cluster synthesized <i>via</i> `ligand-controlled acidolysis' of lanthanide oxide
Zhang, Zai-Chao; Acta Crystallographica Section C 64 (2008) m381–m383; doi:10.1107/S0108270108033684

data_2016839
_publ_section_title
;Poly[hexaaquaocta-\m~3~-hydroxido-tetrakis(\m~3~-methylenedisulfonato)-\m~6~-oxido-hexaytterbium(III)]:
 the first lanthanide sulfonate containing a hexanuclear Ln--hydroxide/oxide
 cluster synthesized <i>via</i> `ligand-controlled acidolysis' of lanthanide
 oxide
;
_journal_coeditor_code           MX3004
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m381
_journal_page_last               m383
_journal_paper_doi               10.1107/S0108270108033684
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Yb6 (C H2 O6 S2)4 (O H)8 O (H2 O)6]'
_chemical_formula_moiety         'C4 H28 O39 S8 Yb6'
_chemical_formula_sum            'C4 H28 O39 S8 Yb6'
_chemical_formula_weight         1994.98
_chemical_name_systematic
;
Poly[hexaaquaocta-\m~3~-hydroxido-tetrakis(\m~3~-methylenedisulfonato)-\m~6~-
oxido-hexaytterbium(III)]
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 96.1580(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.7633(2)
_cell_length_b                   12.4480(2)
_cell_length_c                   16.2201(3)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      55.04
_cell_measurement_theta_min      6.02
_cell_volume                     1759.17(6)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14471
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    16.393
_exptl_absorpt_correction_T_max  0.09
_exptl_absorpt_correction_T_min  0.06
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.766
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism-like
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          .20
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .15
_refine_diff_density_max         0.953
_refine_diff_density_min         -1.498
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         3100
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0556P)^2^+2.8927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0749
_reflns_number_gt                2962
_reflns_number_total             3100
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            mx3004.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2016839
_cod_database_fobs_code          2016839