Crystal Structures of Incommensurately Modulated Ln(PO3)3 (Ln = Tb-Yb) and Commensurate Gd(PO3)3 and Lu(PO3)3
Henning A. Höppe; Stefan J. Sedlmaier; Inorganic Chemistry 46 (2007) 3467–3474; doi:10.1021/ic0616030

data_4307096
_publ_contact_author_address
;
 Albert-Ludwigs-Universit\"at Freiburg
 Institut f\"ur Anorganische und Analytische Chemie
 Albertstr. 21
 D-79104 Freiburg
 Germany
;
_publ_contact_author_email       henning.hoeppe@ac.uni-freiburg.de
_publ_contact_author_fax         +49-(0)761-203-6012
_publ_contact_author_name        'Dr. Henning A. H\"oppe'
_publ_contact_author_phone       +49-(0)761-203-6106
_publ_section_title
;
Crystal Structures of Incommensurately Modulated Ln(PO3)3 (Ln = Tb-Yb) and
Commensurate Gd(PO3)3 and Lu(PO3)3
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3467
_journal_page_last               3474
_journal_paper_doi               10.1021/ic0616030
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'Lu O9 P3'
_chemical_formula_weight         411.88
_chemical_name_common            'lutetium metaphosphate'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 127.351(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   13.9720(13)
_cell_length_b                   20.0180(16)
_cell_length_c                   9.9556(9)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.03
_cell_volume                     2213.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
; 
360 frames, detector distance = 80 mm
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_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  0.0833
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18288
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.03
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    14.053
_exptl_absorpt_correction_T_max  0.6827
_exptl_absorpt_correction_T_min  0.4512
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
  X-Red and X-SHAPE  (Stoe & Cie, 1999),
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.708
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.265
_refine_diff_density_min         -1.128
_refine_diff_density_rms         0.242
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.49(3)
_refine_ls_extinction_coef       0.00049(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         5079
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      0.890
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0966
_reflns_number_gt                3630
_reflns_number_total             5079
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0616030-file003.cif
_cod_data_source_block           lup3o9
_cod_original_cell_volume        2213.5(3)
_cod_database_code               4307096