#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:26:56 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179328 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/25/4322543.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_4322543
loop_
_publ_author_name
'Peter A. Tanner'
'Thomas C. W. Mak'
_publ_section_title
;
 Synthesis, Structure, and Spectroscopy of Rare Earth Hypophosphites. 2.
 Uranyl Hypophosphite Monohydrate and Uranyl Hypophosphite-Hypophosphorous
 Acid (1/1)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6024
_journal_page_last               6031
_journal_paper_doi               10.1021/ic990188r
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'H6 O6 P3 Yb'
_chemical_formula_weight         368.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 122.26(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.281(3)
_cell_length_b                   5.6580(10)
_cell_length_c                   12.006(2)
_cell_measurement_temperature    293(2)
_cell_volume                     820.4(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            3237
_diffrn_reflns_theta_full        42.50
_diffrn_reflns_theta_max         42.50
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    11.960
_exptl_crystal_density_diffrn    2.980
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             676
_refine_diff_density_max         1.609
_refine_diff_density_min         -2.544
_refine_diff_density_rms         0.253
_refine_ls_extinction_coef       0.0072(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         3149
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0480P)²+0.7199P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1076
_reflns_number_gt                2091
_reflns_number_total             3149
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990188r_3.cif
_cod_data_source_block           ybhyp3
_cod_original_cell_volume        820.4(3)
_cod_database_code               4322543
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 0.5000 0.0000 0.0000 0.02623(8) Uani 1 4 d S . .
Yb2 Yb 0.5000 0.0000 0.5000 0.02483(7) Uani 1 4 d S . .
P1 P 0.32204(11) 0.5000 -0.08788(14) 0.0316(3) Uani 1 2 d SD . .
O1 O 0.3819(2) 0.2762(5) -0.0227(3) 0.0471(7) Uani 1 1 d . . .
H1 H 0.213(3) 0.5000 -0.102(7) 0.050 Uiso 1 2 d SD . .
H2 H 0.300(6) 0.5000 -0.222(4) 0.050 Uiso 1 2 d SD . .
P2 P 0.41066(12) -0.5000 0.28524(13) 0.0313(3) Uani 1 2 d SD . .
O2 O 0.4109(2) -0.2755(5) 0.3508(3) 0.0439(7) Uani 1 1 d . . .
H3 H 0.502(3) -0.5000 0.263(5) 0.050 Uiso 1 2 d SD . .
H4 H 0.303(3) -0.5000 0.161(4) 0.050 Uiso 1 2 d SD . .
P3 P 0.65955(13) 0.0000 0.35365(15) 0.0531(5) Uani 1 2 d SD . .
O3 O 0.5755(5) 0.0000 0.2135(4) 0.0659(16) Uani 1 2 d S . .
O4 O 0.6283(3) 0.0000 0.4516(4) 0.0479(11) Uani 1 2 d S . .
H5 H 0.716(4) 0.229(7) 0.383(5) 0.080 Uiso 1 1 d 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
Yb1 0.03087(13) 0.02011(11) 0.02532(12) 0.000 0.01340(10) 0.000
Yb2 0.03041(13) 0.02065(11) 0.02640(12) 0.000 0.01714(10) 0.000
P1 0.0314(6) 0.0251(5) 0.0385(6) 0.000 0.0189(5) 0.000
O1 0.0477(16) 0.0278(13) 0.0677(19) 0.0063(13) 0.0321(15) 0.0088(12)
P2 0.0402(6) 0.0243(5) 0.0308(5) 0.000 0.0199(5) 0.000
O2 0.0528(16) 0.0316(13) 0.0410(13) -0.0107(12) 0.0207(13) -0.0059(13)
P3 0.0328(6) 0.1012(16) 0.0291(6) 0.000 0.0192(6) 0.000
O3 0.072(3) 0.092(5) 0.0266(18) 0.000 0.021(2) 0.000
O4 0.039(2) 0.081(3) 0.0325(18) 0.000 0.0246(17) 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Yb1 O3 180.0(3) 5_655 . ?
O3 Yb1 O1 89.37(14) 5_655 6 ?
O3 Yb1 O1 90.63(14) . 6 ?
O3 Yb1 O1 90.63(14) 5_655 2_655 ?
O3 Yb1 O1 89.37(14) . 2_655 ?
O1 Yb1 O1 180.00(13) 6 2_655 ?
O3 Yb1 O1 89.37(14) 5_655 . ?
O3 Yb1 O1 90.63(13) . . ?
O1 Yb1 O1 90.20(16) 6 . ?
O1 Yb1 O1 89.80(16) 2_655 . ?
O3 Yb1 O1 90.63(14) 5_655 5_655 ?
O3 Yb1 O1 89.37(14) . 5_655 ?
O1 Yb1 O1 89.80(16) 6 5_655 ?
O1 Yb1 O1 90.20(16) 2_655 5_655 ?
O1 Yb1 O1 180.00(16) . 5_655 ?
O2 Yb2 O2 180.0 . 5_656 ?
O2 Yb2 O2 90.39(16) . 6 ?
O2 Yb2 O2 89.61(16) 5_656 6 ?
O2 Yb2 O2 89.61(16) . 2_656 ?
O2 Yb2 O2 90.39(16) 5_656 2_656 ?
O2 Yb2 O2 180.00(14) 6 2_656 ?
O2 Yb2 O4 89.21(11) . . ?
O2 Yb2 O4 90.79(11) 5_656 . ?
O2 Yb2 O4 89.21(11) 6 . ?
O2 Yb2 O4 90.79(11) 2_656 . ?
O2 Yb2 O4 90.79(11) . 5_656 ?
O2 Yb2 O4 89.21(11) 5_656 5_656 ?
O2 Yb2 O4 90.79(11) 6 5_656 ?
O2 Yb2 O4 89.21(11) 2_656 5_656 ?
O4 Yb2 O4 180.0 . 5_656 ?
O1 P1 O1 115.9(3) 6_565 . ?
P1 O1 Yb1 148.3(2) . . ?
O2 P2 O2 116.6(2) . 6_545 ?
P2 O2 Yb2 150.5(2) . . ?
O3 P3 O4 120.8(3) . . ?
P3 O3 Yb1 160.4(4) . . ?
P3 O4 Yb2 150.1(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb1 O3 2.187(4) 5_655 ?
Yb1 O3 2.187(4) . ?
Yb1 O1 2.206(3) 6 ?
Yb1 O1 2.206(3) 2_655 ?
Yb1 O1 2.206(3) . ?
Yb1 O1 2.206(3) 5_655 ?
Yb2 O2 2.197(3) . ?
Yb2 O2 2.197(3) 5_656 ?
Yb2 O2 2.197(3) 6 ?
Yb2 O2 2.197(3) 2_656 ?
Yb2 O4 2.198(4) . ?
Yb2 O4 2.198(4) 5_656 ?
P1 O1 1.494(3) 6_565 ?
P1 O1 1.494(3) . ?
P2 O2 1.493(3) . ?
P2 O2 1.493(3) 6_545 ?
P3 O3 1.454(5) . ?
P3 O4 1.464(4) . ?
