Synthesis and Crystal Structures of New Lanthanide Hydroxyhalide Anion Exchange Materials, Ln2(OH)5X·1.5H2O (X = Cl, Br; Ln = Y, Dy, Er, Yb)
Poudret, Leslie; Prior, Timothy J.; McIntyre, Laura J.; Fogg, Andrew M.; Chemistry of Materials 20 (2008) 7447–; doi:10.1021/cm802301a

data_4001272
_publ_section_title
;
 Synthesis and Crystal Structures of New Lanthanide Hydroxyhalide Anion
 Exchange Materials, Ln2(OH)5X&#x00B7;1.5H2O (X = Cl, Br; Ln = Y, Dy, Er,
 Yb)
;
_journal_issue                   24
_journal_name_full               'Chemistry of Materials'
_journal_page_first              7447
_journal_paper_doi               10.1021/cm802301a
_journal_volume                  20
_journal_year                    2008
_chemical_formula_moiety         'O13 Yb4, 2(Cl)'
_chemical_formula_sum            'Cl2 O13 Yb4'
_chemical_formula_weight         971.06
_chemical_name_common            '8.4 Angstrom phase'
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.5108(10)
_cell_length_b                   8.3930(13)
_cell_length_c                   7.0438(10)
_cell_measurement_reflns_used    8425
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.85
_cell_measurement_theta_min      1.59
_cell_volume                     739.62(17)
_computing_cell_refinement       'APEXII (Bruker, 2004)'
_computing_data_collection       'APEXII (Bruker, 2004)'
_computing_data_reduction        'APEXII (Bruker, 2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'D8 with APEXII detectore.'
_diffrn_measurement_method       '\w-scans with 0.36 degree frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Station 9.8, Daresbury SRS, UK'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.69430
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7946
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.85
_diffrn_reflns_theta_min         2.85
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    25.467
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.7242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

A correct to account for beam decay and absorption was implemented

within SADABS. Max and min transmission: 0.7242 1

;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.872
_refine_diff_density_min         -4.889
_refine_diff_density_rms         0.434
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1277
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+25.7463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0733
_reflns_number_gt                1119
_reflns_number_total             1277
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm802301a_si_002.cif
_cod_data_source_block           LP18B
_cod_database_code               4001272