An effective method for the synthesis of 3D inorganic Ln(iii)‒K(i) sulfate open frameworks with unusually high thermal stability: in situ generation of sulfate anions
Zhang, Huabin; Zhang, Mingjian; Tian, Chongbin; Li, Ning; Lin, Ping; Li, Zhihua; Du, Shaowu; Journal of Materials Chemistry 22 (2012) 6831–; doi:10.1039/c2jm16779d

data_7207713
_publ_section_title
;
 An effective method for the synthesis of 3D inorganic Ln(iii)--K(i)
 sulfate open frameworks with unusually high thermal stability: in situ
 generation of sulfate anions
;
_journal_issue                   14
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              6831
_journal_paper_doi               10.1039/c2jm16779d
_journal_volume                  22
_journal_year                    2012
_chemical_formula_sum            'Er4 H8 K4 O36 S8'
_chemical_formula_weight         1666.06
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                90.00
_cell_angle_beta                 119.382(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   10.0682(12)
_cell_length_b                   8.2344(8)
_cell_length_c                   10.2663(12)
_cell_measurement_reflns_used    2389
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4700
_cell_measurement_theta_min      2.2767
_cell_volume                     741.65(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5002
_diffrn_reflns_theta_full        27.38
_diffrn_reflns_theta_max         27.38
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    12.463
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.4845
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            PINK
_exptl_crystal_density_diffrn    3.730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.960
_refine_diff_density_min         -1.597
_refine_diff_density_rms         0.287
_refine_ls_extinction_coef       0.0261(11)
_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   1.245
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.245
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+22.5578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.0896
_reflns_number_gt                1580
_reflns_number_total             1584
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2jm16779d.txt
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_refine_ls_hydrogen_treatment' value 'CONSTR' changed
to 'constr' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        741.65(14)
_cod_original_sg_symbol_H-M      P2(1)/C
_cod_original_formula_sum        'H8 Er4 K4 O36 S8'
_cod_database_code               7207713