 
data_tb-hpo 
_publ_requested_journal          DaltonTrans.
_publ_contact_author_name        'Henning A. Höppe'
_publ_contact_author_address     
;Institut für Physik
Universität Augsburg
Universitätsstr. 1
D-86135 Augsburg
;
_publ_contact_author_email       henning@ak-hoeppe.de
loop_
_publ_author_name
_publ_author_address
'Höppe, Henning A.'
;Institut für Physik
Universität Augsburg
Universitätsstr. 1
D-86135 Augsburg
;
'Förg, Katharina'
;Institut für Physik
Universität Augsburg
Universitätsstr. 1
D-86135 Augsburg
;
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
Holmium Hydrogen-polyphosphate
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'H O12 P4 Ho'
_chemical_formula_structural      'Ho[H(PO3)4]' 
_chemical_formula_sum             'H O12 P4 Ho' 
_chemical_formula_weight          481.82 
 
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' 
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    P2(1)/c 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    13.6334(5) 
_cell_length_b                    7.0924(3) 
_cell_length_c                    9.5907(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  101.0550(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      910.15(6) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     296(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       3.04 
_cell_measurement_theta_max       25.00 
 
_exptl_crystal_description        irregular 
_exptl_crystal_colour             yellow/pink 
_exptl_crystal_size_max           0.050 
_exptl_crystal_size_mid           0.020 
_exptl_crystal_size_min           0.018 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     3.516 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              896 
_exptl_absorpt_coefficient_mu     9.462 
_exptl_absorpt_correction_type    Multi-scan 
_exptl_absorpt_correction_T_min   0.6029 
_exptl_absorpt_correction_T_max   0.7458 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_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_measurement_device_type   'Bruker D8 Venture' 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             27195 
_diffrn_reflns_av_R_equivalents   0.0537 
_diffrn_reflns_av_sigmaI/netI     0.0206 
_diffrn_reflns_limit_h_min        -16 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        -8 
_diffrn_reflns_limit_k_max        8 
_diffrn_reflns_limit_l_min        -11 
_diffrn_reflns_limit_l_max        11 
_diffrn_reflns_theta_min          3.04 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              1607 
_reflns_number_gt                 1421 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0423P)²+1.5848P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          1607 
_refine_ls_number_parameters      158 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0291 
_refine_ls_R_factor_gt            0.0228 
_refine_ls_wR_factor_ref          0.0602 
_refine_ls_wR_factor_gt           0.0576 
_refine_ls_goodness_of_fit_ref    1.030 
_refine_ls_restrained_S_all       1.030 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
 
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 
Ho1 Ho 0.729532(17) 0.05657(3) 0.05931(3) 0.00637(13) Uani 1 1 d . . . 
P1 P 0.90118(10) -0.3250(2) 0.12488(15) 0.0080(3) Uani 1 1 d . . . 
P2 P 0.89935(9) 0.1530(2) -0.18799(15) 0.0073(3) Uani 1 1 d . . . 
P3 P 0.38820(10) 0.2885(2) 0.20467(15) 0.0070(3) Uani 1 1 d . . . 
P4 P 0.59443(10) 0.3988(2) 0.21039(15) 0.0070(3) Uani 1 1 d . . . 
OBR1 O 0.9438(3) -0.0209(6) -0.2624(4) 0.0138(9) Uani 1 1 d . . . 
OBR2 O 0.9995(3) -0.2308(5) 0.0942(4) 0.0101(8) Uani 1 1 d . . . 
OBR3 O 0.4186(3) 0.1212(5) 0.3132(4) 0.0111(8) Uani 1 1 d . . . 
OBR4 O 0.4853(3) 0.3257(6) 0.1412(4) 0.0107(8) Uani 1 1 d . . . 
OT1 O 0.8334(3) -0.1891(5) 0.1737(4) 0.0117(8) Uani 1 1 d . . . 
OT2 O 0.8395(3) 0.0788(6) -0.0889(5) 0.0166(9) Uani 1 1 d . . . 
OT3 O 0.8581(3) 0.2080(6) 0.2034(4) 0.0154(9) Uani 1 1 d . . . 
OT4 O 0.6349(3) -0.0475(5) 0.2120(4) 0.0125(9) Uani 1 1 d . . . 
OT5 O 0.6904(3) -0.2267(6) -0.0824(4) 0.0119(8) Uani 1 1 d . . . 
OT6 O 0.6161(3) 0.1414(6) -0.1351(4) 0.0132(9) Uani 1 1 d . . . 
OT7 O 0.6633(3) 0.3331(5) 0.1200(4) 0.0121(9) Uani 1 1 d . . . 
OH1 O 0.8568(3) -0.4297(6) -0.0126(5) 0.0178(10) Uani 1 1 d D . . 
H1 H 0.795(3) -0.394(12) -0.068(7) 0.050 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 
Ho1 0.00672(16) 0.00555(17) 0.00677(17) -0.00023(10) 0.00109(10) -0.00002(10) 
P1 0.0072(6) 0.0059(7) 0.0103(7) 0.0007(6) 0.0004(6) -0.0001(6) 
P2 0.0053(6) 0.0069(7) 0.0094(7) -0.0003(6) 0.0008(5) -0.0011(6) 
P3 0.0066(6) 0.0054(7) 0.0088(7) -0.0006(6) 0.0010(5) -0.0006(5) 
P4 0.0069(6) 0.0048(7) 0.0090(7) -0.0015(6) 0.0002(6) 0.0001(5) 
OBR1 0.0094(19) 0.012(2) 0.019(2) -0.0050(18) -0.0009(17) 0.0009(17) 
OBR2 0.0121(19) 0.011(2) 0.0064(18) 0.0006(17) 0.0004(15) -0.0025(16) 
OBR3 0.018(2) 0.0037(19) 0.010(2) 0.0033(17) 0.0002(17) -0.0011(17) 
OBR4 0.0084(18) 0.015(2) 0.0093(19) -0.0018(17) 0.0029(15) -0.0026(16) 
OT1 0.0139(19) 0.010(2) 0.011(2) 0.0014(17) 0.0020(16) 0.0033(16) 
OT2 0.014(2) 0.019(2) 0.018(2) 0.0005(19) 0.0064(18) -0.0033(17) 
OT3 0.0119(19) 0.014(2) 0.018(2) -0.0014(19) -0.0037(17) -0.0012(17) 
OT4 0.014(2) 0.010(2) 0.016(2) 0.0020(17) 0.0067(17) -0.0008(16) 
OT5 0.0091(18) 0.010(2) 0.015(2) 0.0004(18) -0.0015(16) 0.0002(16) 
OT6 0.016(2) 0.010(2) 0.013(2) -0.0019(17) 0.0000(17) 0.0043(17) 
OT7 0.0105(18) 0.010(2) 0.018(2) -0.0016(18) 0.0068(17) 0.0006(16) 
OH1 0.015(2) 0.018(2) 0.017(2) -0.0100(19) -0.0039(18) 0.0004(17) 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
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 
Ho1 OT4 2.254(4) . ? 
Ho1 OT2 2.261(4) . ? 
Ho1 OT6 2.263(4) . ? 
Ho1 OT7 2.281(4) . ? 
Ho1 OT3 2.282(4) . ? 
Ho1 OT1 2.377(4) . ? 
Ho1 OT5 2.427(4) . ? 
P1 OT1 1.473(4) . ? 
P1 OH1 1.533(4) . ? 
P1 OBR1 1.568(4) 4_556 ? 
P1 OBR2 1.575(4) . ? 
P2 OT2 1.463(4) . ? 
P2 OT3 1.466(4) 4_565 ? 
P2 OBR2 1.594(4) 3_755 ? 
P2 OBR1 1.601(4) . ? 
P3 OT4 1.479(4) 2_655 ? 
P3 OT5 1.495(4) 3_655 ? 
P3 OBR3 1.580(4) . ? 
P3 OBR4 1.581(4) . ? 
P4 OT7 1.471(4) . ? 
P4 OT6 1.482(4) 4_566 ? 
P4 OBR4 1.595(4) . ? 
P4 OBR3 1.599(4) 2_655 ? 
OBR1 P1 1.568(4) 4 ? 
OBR2 P2 1.594(4) 3_755 ? 
OBR3 P4 1.599(4) 2_645 ? 
OT3 P2 1.466(4) 4_566 ? 
OT4 P3 1.479(4) 2_645 ? 
OT5 P3 1.495(4) 3_655 ? 
OT6 P4 1.482(4) 4_565 ? 
OH1 H1 0.939(10) . ? 
 
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 
OT4 Ho1 OT2 164.33(14) . . ? 
OT4 Ho1 OT6 103.68(14) . . ? 
OT2 Ho1 OT6 83.92(14) . . ? 
OT4 Ho1 OT7 79.16(13) . . ? 
OT2 Ho1 OT7 116.30(14) . . ? 
OT6 Ho1 OT7 74.96(14) . . ? 
OT4 Ho1 OT3 103.30(14) . . ? 
OT2 Ho1 OT3 79.78(15) . . ? 
OT6 Ho1 OT3 134.25(14) . . ? 
OT7 Ho1 OT3 74.72(14) . . ? 
OT4 Ho1 OT1 79.90(13) . . ? 
OT2 Ho1 OT1 86.17(14) . . ? 
OT6 Ho1 OT1 145.84(14) . . ? 
OT7 Ho1 OT1 137.94(13) . . ? 
OT3 Ho1 OT1 75.23(13) . . ? 
OT4 Ho1 OT5 90.05(13) . . ? 
OT2 Ho1 OT5 78.86(14) . . ? 
OT6 Ho1 OT5 73.54(13) . . ? 
OT7 Ho1 OT5 143.10(13) . . ? 
OT3 Ho1 OT5 142.13(13) . . ? 
OT1 Ho1 OT5 72.48(13) . . ? 
OT1 P1 OH1 115.0(2) . . ? 
OT1 P1 OBR1 114.1(2) . 4_556 ? 
OH1 P1 OBR1 106.7(2) . 4_556 ? 
OT1 P1 OBR2 113.0(2) . . ? 
OH1 P1 OBR2 104.7(2) . . ? 
OBR1 P1 OBR2 102.0(2) 4_556 . ? 
OT2 P2 OT3 121.2(2) . 4_565 ? 
OT2 P2 OBR2 106.7(2) . 3_755 ? 
OT3 P2 OBR2 109.9(2) 4_565 3_755 ? 
OT2 P2 OBR1 108.5(2) . . ? 
OT3 P2 OBR1 109.1(2) 4_565 . ? 
OBR2 P2 OBR1 99.1(2) 3_755 . ? 
OT4 P3 OT5 117.4(2) 2_655 3_655 ? 
OT4 P3 OBR3 106.9(2) 2_655 . ? 
OT5 P3 OBR3 110.8(2) 3_655 . ? 
OT4 P3 OBR4 110.9(2) 2_655 . ? 
OT5 P3 OBR4 105.9(2) 3_655 . ? 
OBR3 P3 OBR4 104.2(2) . . ? 
OT7 P4 OT6 120.1(2) . 4_566 ? 
OT7 P4 OBR4 107.6(2) . . ? 
OT6 P4 OBR4 110.2(2) 4_566 . ? 
OT7 P4 OBR3 107.2(2) . 2_655 ? 
OT6 P4 OBR3 109.1(2) 4_566 2_655 ? 
OBR4 P4 OBR3 101.1(2) . 2_655 ? 
P1 OBR1 P2 136.3(3) 4 . ? 
P1 OBR2 P2 135.8(2) . 3_755 ? 
P3 OBR3 P4 129.8(3) . 2_645 ? 
P3 OBR4 P4 132.6(3) . . ? 
P1 OT1 Ho1 133.4(2) . . ? 
P2 OT2 Ho1 162.3(3) . . ? 
P2 OT3 Ho1 153.1(2) 4_566 . ? 
P3 OT4 Ho1 144.7(2) 2_645 . ? 
P3 OT5 Ho1 136.8(2) 3_655 . ? 
P4 OT6 Ho1 138.3(2) 4_565 . ? 
P4 OT7 Ho1 138.7(2) . . ? 
P1 OH1 H1 121(5) . . ? 
 
_diffrn_measured_fraction_theta_max    0.999 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.999 
_refine_diff_density_max    1.981 
_refine_diff_density_min   -0.841 
_refine_diff_density_rms    0.195 
