#------------------------------------------------------------------------------
#$Date: 2009-11-16 03:43:51 +0200 (Mon, 16 Nov 2009) $
#$Revision: 853 $
#$URL: svn://cod.ibt.lt/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
_journal_name_full 'Chemistry of Materials'
_journal_year    2004
_publ_section_title
;
Catalytic behavior of rare-earth sulfates: applications
in organic hydrogenation and oxidation reactions
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_[local]_cod_cif_authors_sg_H-M  P2(1)/n
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&#x00B7;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.
;
_chemical_formula_sum             'H6 Ho N O9 S2'
_chemical_formula_weight          393.05
_symmetry_cell_setting            Monoclinic
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'
_cell_length_a                    10.2171(7)
_cell_length_b                    8.3349(5)
_cell_length_c                    10.3267(7)
_cell_angle_alpha                 90.00
_cell_angle_beta                  119.5290(10)
_cell_angle_gamma                 90.00
_cell_volume                      765.18(9)
_cell_formula_units_Z             4
_cell_measurement_temperature     296(2)
_exptl_crystal_description        prismatic
_exptl_crystal_colour             pink
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.12
_exptl_crystal_size_min           0.12
_exptl_crystal_density_diffrn     3.412
_exptl_crystal_F_000              736
_exptl_absorpt_coefficient_mu     10.915
_exptl_absorpt_correction_type    SADABS
_exptl_absorpt_correction_T_min   0.418
_exptl_absorpt_correction_T_max   1.000
_diffrn_ambient_temperature       296(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_reflns_number             3584
_diffrn_reflns_av_R_equivalents   0.0785
_diffrn_reflns_av_sigmaI/netI     0.0701
_diffrn_reflns_limit_h_min        -6
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        8
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        5
_diffrn_reflns_theta_min          3.33
_diffrn_reflns_theta_max          32.07
_reflns_number_total              1966
_reflns_number_observed           1592
_reflns_observed_criterion        >2sigma(I)
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme
 'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     ?
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          1966
_refine_ls_number_parameters      118
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0509
_refine_ls_R_factor_obs           0.0373
_refine_ls_wR_factor_all          0.0916
_refine_ls_wR_factor_obs          0.0876
_refine_ls_goodness_of_fit_all    0.984
_refine_ls_goodness_of_fit_obs    1.053
_refine_ls_restrained_S_all       0.984
_refine_ls_restrained_S_obs       1.053
_refine_ls_shift/esd_max          -4.257
_refine_ls_shift/esd_mean         0.325
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)
