Synthesis, Crystal Structure from Single-Crystal and Powder X-ray Diffraction Data, and Thermal Behavior of Mixed Potassium Lanthanide Squarates: Thermal Transformations of Layered [Ln(H2O)6]K(H2C4O4)(C4O4)2 into Pillared LnK(C4O4)2 (Ln = Y, La, Gd, Er)
Nathalie Mahé; Thierry Bataille; Inorganic Chemistry 43 (2004) 8379–8386; doi:10.1021/ic0488839

data_4312227
_publ_section_title
;
 Synthesis, Crystal Structure from Single-Crystal and Powder X-ray
 Diffraction Data, and Thermal Behavior of Mixed Potassium Lanthanide
 Squarates: Thermal Transformations of Layered [Ln(H2O)6]K(H2C4O4)(C4O4)2
 into Pillared LnK(C4O4)2 (Ln = Y, La, Gd, Er)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8379
_journal_page_last               8386
_journal_paper_doi               10.1021/ic0488839
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety
;
 ?
;
_chemical_formula_sum            'C24 H28 K2 O36 Y2'
_chemical_formula_weight        1148.48
_chemical_name_common
;
yttrium potassium squarate hexahydrate
;
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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
_cell_angle_beta                 90.3959(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3341(2)
_cell_length_b                   37.7094(9)
_cell_length_c                   11.7195(3)
_cell_measurement_reflns_used    5326
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.72
_cell_volume                     3683.05(16)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics    'Diamond 2.1e (Crystal Impact, Bonn)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1230
_diffrn_reflns_av_sigmaI/netI    0.0760
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22691
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    3.493
_exptl_absorpt_correction_T_max  0.8934
_exptl_absorpt_correction_T_min  0.4235
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.779
_refine_diff_density_min         -1.464
_refine_diff_density_rms         0.169
_refine_ls_extinction_coef       0.00111(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5365
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0758
_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^)+(0.0314P)^2^+62.8610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1796
_refine_ls_wR_factor_ref         0.1907
_reflns_number_gt                4026
_reflns_number_total             5365
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0488839si20040814_035930.cif
_cod_data_source_block           yksq
_cod_original_cell_volume        3683(3)
_cod_original_sg_symbol_Hall     -C2yc
_cod_database_code               4312227