#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/89/2218991.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2218991
loop_
_publ_author_name
'Bejaoui, Anis'
'Horchani-Naifer, Karima'
'Férid, Mokhtar'
_publ_section_title
;
 A new polymorph of Lu(PO₃)₃
;
_journal_coeditor_code           FI2065
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i48
_journal_paper_doi               10.1107/S1600536808021995
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'Lu (P O3)3'
_chemical_formula_sum            'Lu O9 P3'
_chemical_formula_weight         411.88
_chemical_name_common            'lutetium polyphosphate'
_chemical_name_systematic
;
lutetium polyphosphate
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            24
_cell_length_a                   20.9106(6)
_cell_length_b                   20.9106(6)
_cell_length_c                   12.0859(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.10
_cell_measurement_theta_min      2.81
_cell_volume                     4576.6(3)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25139
_diffrn_reflns_theta_full        34.17
_diffrn_reflns_theta_max         34.17
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    13.594
_exptl_absorpt_correction_T_max  0.104
_exptl_absorpt_correction_T_min  0.102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             4512
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.339
_refine_diff_density_min         -2.071
_refine_ls_extinction_coef       0.000061(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         4170
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0212P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0605
_reflns_number_gt                3609
_reflns_number_total             4170
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fi2065.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'Lu1 O9 P3'
_cod_database_code               2218991
_cod_database_fobs_code          2218991
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Lu Lu1 0.6667 0.3333 0.3333 0.00741(8) Uani d S 1
Lu Lu2 0.6667 0.3333 -0.1667 0.01207(9) Uani d S 1
Lu Lu3 0.440661(9) 0.365196(10) 0.096806(14) 0.00780(5) Uani d . 1
P P1 0.63820(6) 0.45920(6) 0.16119(9) 0.00821(19) Uani d . 1
P P2 0.50313(6) 0.54494(6) 0.16810(9) 0.0096(2) Uani d . 1
P P3 0.39267(6) 0.30556(6) 0.37383(10) 0.0111(2) Uani d . 1
P P4 0.50120(6) 0.25039(6) -0.01904(10) 0.0107(2) Uani d . 1
O O1 0.44368(17) 0.46669(17) 0.1552(3) 0.0132(6) Uani d . 1
O O2 0.34108(18) 0.22020(17) 0.3991(3) 0.0132(6) Uani d . 1
O O3 0.54706(18) 0.58558(18) 0.0709(3) 0.0141(6) Uani d . 1
O O4 0.45503(18) 0.27392(18) 0.0416(3) 0.0168(7) Uani d . 1
O O5 0.55847(17) 0.42399(18) 0.1374(3) 0.0175(7) Uani d . 1
O O6 0.45659(17) 0.19780(19) -0.1185(3) 0.0155(7) Uani d . 1
O O7 0.66627(18) 0.41823(18) 0.2253(3) 0.0190(7) Uani d . 1
O O8 0.57293(19) 0.3097(2) -0.0609(3) 0.0247(8) Uani d . 1
O O9 0.6655(2) 0.5377(2) 0.2137(4) 0.0351(11) Uani d . 1
O O10 0.5156(2) 0.1948(2) 0.0471(3) 0.0315(10) Uani d . 1
O O11 0.3569(2) 0.3473(2) 0.4088(4) 0.0298(9) Uani d . 1
O O12 0.4182(3) 0.3127(2) 0.2586(3) 0.0364(11) Uani d . 1
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O7 Lu1 O7 18_545 17 88.57(14)
O7 Lu1 O7 18_545 3_665 180.0
O7 Lu1 O7 17 3_665 91.43(14)
O7 Lu1 O7 18_545 2_655 91.43(14)
O7 Lu1 O7 17 2_655 180.0
O7 Lu1 O7 3_665 2_655 88.57(14)
O7 Lu1 O7 18_545 . 91.43(14)
O7 Lu1 O7 17 . 91.43(14)
O7 Lu1 O7 3_665 . 88.57(14)
O7 Lu1 O7 2_655 . 88.57(14)
O7 Lu1 O7 18_545 16_655 88.57(14)
O7 Lu1 O7 17 16_655 88.57(14)
O7 Lu1 O7 3_665 16_655 91.43(14)
O7 Lu1 O7 2_655 16_655 91.43(14)
O7 Lu1 O7 . 16_655 180.0
O8 Lu2 O8 17_554 2_655 180.0
O8 Lu2 O8 17_554 3_665 90.92(15)
O8 Lu2 O8 2_655 3_665 89.08(15)
O8 Lu2 O8 17_554 . 90.92(15)
O8 Lu2 O8 2_655 . 89.08(15)
O8 Lu2 O8 3_665 . 89.08(15)
O8 Lu2 O8 17_554 18_544 89.08(15)
O8 Lu2 O8 2_655 18_544 90.92(15)
O8 Lu2 O8 3_665 18_544 180.0
O8 Lu2 O8 . 18_544 90.92(15)
O8 Lu2 O8 17_554 16_654 89.08(15)
O8 Lu2 O8 2_655 16_654 90.92(15)
O8 Lu2 O8 3_665 16_654 90.92(15)
O8 Lu2 O8 . 16_654 180.0
O8 Lu2 O8 18_544 16_654 89.08(15)
O11 Lu3 O12 9_554 . 86.28(18)
O11 Lu3 O4 9_554 . 96.31(13)
O12 Lu3 O4 . . 85.59(14)
O11 Lu3 O5 9_554 . 173.76(15)
O12 Lu3 O5 . . 88.86(16)
O4 Lu3 O5 . . 87.21(12)
O11 Lu3 O1 9_554 . 91.99(13)
O12 Lu3 O1 . . 95.32(14)
O4 Lu3 O1 . . 171.70(12)
O5 Lu3 O1 . . 84.56(12)
O11 Lu3 O3 9_554 10_665 88.69(15)
O12 Lu3 O3 . 10_665 174.96(15)
O4 Lu3 O3 . 10_665 95.25(12)
O5 Lu3 O3 . 10_665 96.14(13)
O1 Lu3 O3 . 10_665 84.56(12)
O5 P1 O7 . . 119.4(2)
O5 P1 O10 . 3_665 106.7(2)
O7 P1 O10 . 3_665 110.3(2)
O5 P1 O9 . . 109.15(19)
O7 P1 O9 . . 110.6(2)
O10 P1 O9 3_665 . 98.7(3)
O3 P2 O1 . . 119.23(19)
O3 P2 O6 . 5 105.71(18)
O1 P2 O6 . 5 109.44(19)
O3 P2 O2 . 17 112.19(18)
O1 P2 O2 . 17 106.01(18)
O6 P2 O2 5 17 103.12(18)
O11 P3 O12 . . 118.6(3)
O11 P3 O9 . 18_545 105.0(2)
O12 P3 O9 . 18_545 108.6(3)
O11 P3 O2 . . 110.6(2)
O12 P3 O2 . . 107.7(2)
O9 P3 O2 18_545 . 105.49(19)
O8 P4 O4 . . 116.6(2)
O8 P4 O10 . . 107.9(2)
O4 P4 O10 . . 113.3(2)
O8 P4 O6 . . 108.8(2)
O4 P4 O6 . . 110.62(18)
O10 P4 O6 . . 97.91(19)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Lu1 O7 18_545 2.207(3)
Lu1 O7 17 2.207(3)
Lu1 O7 3_665 2.207(3)
Lu1 O7 2_655 2.207(3)
Lu1 O7 . 2.207(3)
Lu1 O7 16_655 2.207(3)
Lu2 O8 17_554 2.180(3)
Lu2 O8 2_655 2.180(3)
Lu2 O8 3_665 2.180(3)
Lu2 O8 . 2.180(3)
Lu2 O8 18_544 2.180(3)
Lu2 O8 16_654 2.180(3)
Lu3 O11 9_554 2.134(3)
Lu3 O12 . 2.176(4)
Lu3 O4 . 2.180(3)
Lu3 O5 . 2.189(3)
Lu3 O1 . 2.207(3)
Lu3 O3 10_665 2.229(3)
P1 O5 . 1.475(3)
P1 O7 . 1.477(3)
P1 O10 3_665 1.569(4)
P1 O9 . 1.578(4)
P2 O3 . 1.472(3)
P2 O1 . 1.488(3)
P2 O6 5 1.585(3)
P2 O2 17 1.593(3)
P3 O11 . 1.467(4)
P3 O12 . 1.472(4)
P3 O9 18_545 1.573(4)
P3 O2 . 1.587(3)
P4 O8 . 1.478(4)
P4 O4 . 1.478(3)
P4 O10 . 1.560(4)
P4 O6 . 1.581(3)
