Terbium hydrogendiphosphate trihydrate: synthesis and non-merohedral twinning
Essehli, Rachid; El Bali, Brahim; Dusek, Michal; Fejfarova, Karla; Lachkar, Mohammed; Acta Crystallographica Section E 63 (2007) i87–i88; doi:10.1107/S160053680700832X

data_2212570
_publ_section_title
;
 Terbium hydrogendiphosphate trihydrate: synthesis and non-merohedral
 twinning
;
_journal_coeditor_code           HB2288
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i87
_journal_page_last               i88
_journal_paper_doi               10.1107/S160053680700832X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'Tb (H P2 O7), 3H2 O'
_chemical_formula_moiety         'Tb 3+, H O7 P2 3-, 3(H2 O)'
_chemical_formula_structural     '( Tb (HP2O7) 3(H2O)'
_chemical_formula_sum            'H7 O10 P2 Tb'
_chemical_formula_weight         387.9
_chemical_name_systematic
;
terbium hydrogendiphosphate trihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                81.621(6)
_cell_angle_beta                 80.464(6)
_cell_angle_gamma                88.341(6)
_cell_formula_units_Z            2
_cell_length_a                   6.4551(5)
_cell_length_b                   6.9597(4)
_cell_length_c                   9.8253(7)
_cell_measurement_reflns_used    10460
_cell_measurement_temperature    294
_cell_measurement_theta_max      26.57
_cell_measurement_theta_min      3.2
_cell_volume                     430.66(5)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2005)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2005)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  JANA2000
_computing_structure_refinement  'JANA2000 (Petricek <i>et al.</i>,  2000)'
_computing_structure_solution    'SIR2002 (Burla <i>et al.</i>,  2003)'
_diffrn_ambient_temperature      294
_diffrn_detector_area_resol_mean 8.3438
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measurement_device_type  'Oxford Diffraction CCD'
_diffrn_measurement_method
'Rotation method data acquisition using \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10460
_diffrn_reflns_reduction_process
; Integration of the CCD images was done by program Crysalis RED
(Oxford diffraction, 2004). The same program was used for indexing of the
crystal shape, its refinement and absorption correction.
;
_diffrn_reflns_theta_full        26.57
_diffrn_reflns_theta_max         26.57
_diffrn_reflns_theta_min         3.20
_exptl_absorpt_coefficient_mu    8.614
_exptl_absorpt_correction_T_max  0.659
_exptl_absorpt_correction_T_min  0.419
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.9905
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.97
_refine_diff_density_min         -0.66
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.13
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_constraints    5
_refine_ls_number_parameters     144
_refine_ls_number_reflns         3399
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.0191
_refine_ls_shift/su_mean         0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/[\s^2^(I)+0.0004I^2^]
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0562
_reflns_number_gt                2737
_reflns_number_total             3399
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            hb2288.cif
_cod_data_source_block           II
_cod_original_formula_sum        'H7 O10 P2 Tb1'
_cod_database_code               2212570