Crystal structure of [Y~6~(μ~6~-O)(μ~3~-OH)~8~(H~2~O)~24~]I~8~·8H~2~O
Le Natur, François; Calvez, Guillaume; Guillou, Olivier; Daiguebonne, Carole; Bernot, Kevin; Acta Crystallographica Section E 70 (2014) 577–579; doi:10.1107/S1600536814025434

data_2240252
_publ_section_title
;
 Crystal structure of
 [Y~6~(\m~6~-O)(\m~3~-OH)~8~(H~2~O)~24~]I~8~&#x00B7;8H~2~O
;
_journal_coeditor_code           WM5083
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              577
_journal_page_last               579
_journal_paper_doi               10.1107/S1600536814025434
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Y6 O (OH)8 (H2 O)24] I8, 8H2 O'
_chemical_formula_moiety         'H56 Y6 O33 8+, 8(I -), 8(H2 O)'
_chemical_formula_sum            'H72 I8 O41 Y6'
_chemical_formula_weight         2277.24
_chemical_name_systematic
;
Octa-\m~3~-hydroxido-\m~6~-oxido-hexakis[tetraaquayttrium(III)] octaiodide
octahydrate
;
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.8210(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.9099(2)
_cell_length_b                   14.8050(2)
_cell_length_c                   14.7933(3)
_cell_measurement_reflns_used    62388
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2827.17(8)
_computing_cell_refinement
;
COLLECT (Nonius, 1998)
;
_computing_data_collection
;
COLLECT (Nonius, 1998)
;
_computing_data_reduction
;
EVALCCD (Duisenberg <i>et al.</i>,  2003)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.1242
_diffrn_reflns_av_sigmaI/netI    0.0583
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35352
_diffrn_reflns_theta_full        27.39
_diffrn_reflns_theta_max         27.39
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    10.542
_exptl_absorpt_correction_T_max  0.0913
_exptl_absorpt_correction_T_min  0.0178
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(Coppens <i>et al.</i>, 1965)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2116
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.623
_refine_diff_density_min         -1.830
_refine_ls_extinction_coef       0.00258(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL97 (Sheldrick, 2008)
;
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         6374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0671
_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^)+(0.0487P)^2^+43.8859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1717
_refine_ls_wR_factor_ref         0.1778
_reflns_number_gt                5449
_reflns_number_total             6374
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            wm5083sup1.cf
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2240252
_cod_database_fobs_code          2240252