#------------------------------------------------------------------------------
#$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $
#$Revision: 966 $
#$URL: svn://www.crystallography.net/cod/cif/4/4000464.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4000464
loop_
_publ_author_name
'Berta Gomez-Lor'
'Enrique GutierrezPuebla'
'M. Angeles Monge'
'Caridad Ruiz Valero'
'Natalia Snejko'
'Concepci\'on Cascales'
_publ_section_abstract
;
Two isostructural ammonium rare-earth R double sulfate monohydrates 
NH4R(SO4)2·H
R = Y, Ho, have been hydrothermally synthesized at 170 oC for one week. The 
crys
structures have been established by single-crystal X-ray diffraction to be 
monoc
space group P21/n, Z = 4, with unit cell parameters a = 10.2171(7) and 
10.219(2)
b = 8.3349(5) and 8.338(1), c = 10.3267(7) and 10.323(2) \%A, and \&s = 
119.5290(10)
and 119.482(3)\%, for R = Y and Ho respectively. The most interesting feature 
of
the 3D structure is the existence of helical channels along the a direction,
where isolated RO8 polyhedra alternate with the two kinds of sulfate groups, 
wit
the ammonium cations located inside the channels. Their infrared and thermal
stability analyses have been also performed. These materials behave as active
catalysts in hydrogenation reactions of olefins and nitroaromatics, and in 
highl
selective oxidation of organic sulfides. High yielding, mild conditions of
reactions, suitability for solid-phase reactions and reusability with no 
detrime
of selectivity, activity or yield, are among the advantages of these new 
develop
solid catalysts.
;
_publ_section_title
;
Catalytic behavior of rare-earth sulfates: applications
in organic hydrogenation and oxidation reactions
;
_journal_name_full               'Chemistry of Materials'
_journal_year                    2004
_chemical_formula_sum            'H6 Ho N O9 S2'
_chemical_formula_weight         393.05
_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                 119.5290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2171(7)
_cell_length_b                   8.3349(5)
_cell_length_c                   10.3267(7)
_cell_measurement_temperature    296(2)
_cell_volume                     765.18(9)
_diffrn_ambient_temperature      296(2)
_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  0.0785
_diffrn_reflns_av_sigmaI/netI    0.0701
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3584
_diffrn_reflns_theta_max         32.07
_diffrn_reflns_theta_min         3.33
_exptl_absorpt_coefficient_mu    10.915
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.418
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    3.412
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_crystal_thermal_history   'synthesized at 170 oC for one week'
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.984
_refine_ls_goodness_of_fit_obs   1.053
_refine_ls_hydrogen_treatment    ?
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_restrained_S_obs      1.053
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_obs          0.0373
_refine_ls_shift/esd_max         -4.257
_refine_ls_shift/esd_mean        0.325
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all         0.0916
_refine_ls_wR_factor_obs         0.0876
_reflns_number_observed          1592
_reflns_number_total             1966
_reflns_observed_criterion       >2sigma(I)
_[local]_cod_cif_authors_sg_H-M  P2(1)/n
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ho1 Ho 0.28036(4) 0.36065(4) 0.03605(3) 0.00794(11) Uani 1 d . .
S1 S 0.6250(2) 0.3633(2) 0.1823(2) 0.0099(3) Uani 1 d . .
S2 S 0.1036(2) 0.7044(2) 0.0998(2) 0.0095(3) Uani 1 d . .
O1 O 0.2964(7) 0.5657(7) -0.1089(7) 0.0195(12) Uani 1 d . .
O2 O 0.2380(7) 0.2159(8) -0.1815(6) 0.0188(12) Uani 1 d . .
O3 O 0.5109(7) 0.2449(7) 0.0811(6) 0.0179(12) Uani 1 d . .
O4 O 0.5378(7) 0.4842(7) 0.2122(7) 0.0196(13) Uani 1 d . .
O5 O 0.0521(8) 0.7887(8) -0.0398(6) 0.0230(13) Uani 1 d . .
O6 O 0.3288(7) 0.3187(7) 0.2751(6) 0.0152(11) Uani 1 d . .
O7 O 0.2238(7) 0.5868(7) 0.1266(6) 0.0165(11) Uani 1 d . .
O8 O 0.0234(8) 0.3779(7) -0.1016(7) 0.0186(12) Uani 1 d . .
O9 O 0.2196(7) 0.0842(7) 0.0509(7) 0.0185(12) Uani 1 d . .
N1 N 0.4728(12) -0.1590(11) 0.1817(11) 0.021(2) Uani 1 d . .
H91 H 0.0998 0.0542 0.9518 0.050 Uiso 1 d . .
H92 H 0.2224 0.0873 0.1337 0.050 Uiso 1 d . .
H11 H 0.5520 0.8060 0.1460 0.050 Uiso 1 d . .
H12 H 0.5210 0.8282 0.2923 0.050 Uiso 1 d . .
H13 H 0.4920 0.9420 0.1880 0.050 Uiso 1 d . .
H14 H 0.4360 0.7460 0.1850 0.050 Uiso 1 d . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ho1 0.0103(2) 0.0050(2) 0.01029(15) 0.00028(12) 0.00639(13) 0.00055(13)
S1 0.0099(9) 0.0108(8) 0.0105(7) 0.0015(6) 0.0062(7) 0.0006(7)
S2 0.0117(10) 0.0075(8) 0.0104(7) -0.0014(6) 0.0063(7) 0.0000(6)
O1 0.020(4) 0.022(3) 0.020(3) 0.010(2) 0.013(3) 0.004(2)
O2 0.014(3) 0.029(3) 0.014(2) -0.013(2) 0.008(2) -0.005(2)
O3 0.012(3) 0.024(3) 0.018(3) -0.005(2) 0.008(3) -0.002(2)
O4 0.025(4) 0.011(3) 0.029(3) -0.005(2) 0.018(3) -0.001(2)
O5 0.035(4) 0.018(3) 0.015(3) 0.002(2) 0.012(3) 0.002(3)
O6 0.022(3) 0.010(3) 0.016(2) 0.007(2) 0.011(3) 0.005(2)
O7 0.018(3) 0.016(3) 0.019(3) -0.001(2) 0.011(3) 0.002(2)
O8 0.018(3) 0.016(3) 0.026(3) -0.004(2) 0.014(3) -0.005(2)
O9 0.020(4) 0.013(3) 0.026(3) 0.002(2) 0.014(3) 0.000(2)
N1 0.022(6) 0.017(5) 0.025(5) -0.002(4) 0.014(4) 0.000(4)
_cod_database_code 4000464