Dysprosium hydrogendiphosphate trihydrate: synthesis and non-merohedral twinning
Essehli, Rachid; El Bali, Brahim; Dusek, Michal; Fejfarova, Karla; Lachkar, Mohammed; Acta Crystallographica Section E 63 (2007) i85–i86; doi:10.1107/S1600536807008343

data_2212580
_publ_section_title
;
 Dysprosium hydrogendiphosphate trihydrate: synthesis and
 non-merohedral twinning
;
_journal_coeditor_code           HB2298
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i85
_journal_page_last               i86
_journal_paper_doi               10.1107/S1600536807008343
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'Dy (H O7 P2), 3H2 O'
_chemical_formula_moiety         'Dy 3+, H O7 P2 3-, 3(H2 O)'
_chemical_formula_structural     '( Dy (HP2O7) 3(H2O)'
_chemical_formula_sum            'Dy H7 O10 P2'
_chemical_formula_weight         391.5
_chemical_name_systematic
;
dysprosium 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                81.593(6)
_cell_angle_beta                 80.377(5)
_cell_angle_gamma                88.368(5)
_cell_formula_units_Z            2
_cell_length_a                   6.4371(3)
_cell_length_b                   6.9284(5)
_cell_length_c                   9.8164(7)
_cell_measurement_reflns_used    10749
_cell_measurement_temperature    294
_cell_measurement_theta_max      26.55
_cell_measurement_theta_min      2.97
_cell_volume                     427.00(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 et al., 2003)'
_diffrn_ambient_temperature      294
_diffrn_detector_area_resol_mean 8.3438
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measurement_device_type  'Oxford Diffraction CCD'
_diffrn_measurement_method       'Rotation method data acquisition using \w'
_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  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0335
_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            10749
_diffrn_reflns_reduction_process
;
 Integration of the CCD images was done by program Crysalis RED
(Oxford diffraction, 2005). The same program was used for indexing of the
crystal shape, its refinement and absorption correction.
;
_diffrn_reflns_theta_full        26.55
_diffrn_reflns_theta_max         26.55
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    9.157
_exptl_absorpt_correction_T_max  0.691
_exptl_absorpt_correction_T_min  0.438
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.0440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             362
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.63
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.09
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_constraints    5
_refine_ls_number_parameters     138
_refine_ls_number_reflns         3357
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.0094
_refine_ls_shift/su_mean         0.0004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/[\s^2^(I)+0.0016I^2^]
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0679
_reflns_number_gt                2842
_reflns_number_total             3357
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            hb2298.cif
_cod_data_source_block           I
_cod_original_formula_sum        'Dy1 H7 O10 P2'
_cod_database_code               2212580