#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:23:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179108 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/70/4307096.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4307096
loop_
_publ_author_name
'Henning A. Höppe'
'Stefan J. Sedlmaier'
_publ_contact_author_address
;
 Albert-Ludwigs-Universität Freiburg
 Institut für 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. Höppe'
_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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0445P)²+0.0000P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
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
Lu1 Lu 0.18168(14) 0.91176(8) 0.01846(17) 0.0247(3) Uani 1 1 d . . .
Lu2 Lu -0.30137(5) 0.75566(5) 0.05355(6) 0.0224(3) Uani 1 1 d . . .
Lu3 Lu 0.18302(13) 0.57770(7) 0.01561(17) 0.0243(3) Uani 1 1 d . . .
P11 P -0.1667(7) 1.0342(4) -0.1453(10) 0.0297(17) Uani 1 1 d D . .
O111 O -0.2052(15) 0.9995(7) -0.3014(15) 0.031(3) Uani 1 1 d D . .
O112 O -0.2670(12) 1.0614(9) -0.151(2) 0.035(3) Uani 1 1 d D . .
O11 O -0.0603(15) 1.0851(8) -0.081(2) 0.034(6) Uani 1 1 d D . .
P12 P -0.0461(7) 1.1376(5) -0.1906(9) 0.0245(17) Uani 1 1 d D . .
O121 O 0.0475(12) 1.1839(6) -0.0672(16) 0.031(3) Uani 1 1 d D . .
O122 O -0.1588(10) 1.1675(7) -0.3323(15) 0.031(3) Uani 1 1 d D . .
O12 O 0.006(2) 1.0971(7) -0.270(3) 0.038(4) Uani 1 1 d D . .
P13 P 0.0279(7) 1.0309(4) -0.3246(9) 0.0252(16) Uani 1 1 d D . .
O131 O 0.058(2) 0.9791(8) -0.201(2) 0.040(4) Uani 1 1 d D . .
O132 O 0.1139(13) 1.0430(9) -0.360(2) 0.034(4) Uani 1 1 d D . .
O13 O -0.0991(12) 1.0196(9) -0.5012(16) 0.040(4) Uani 1 1 d D . .
P21 P -0.0786(6) 0.5286(3) 0.2430(7) 0.0243(13) Uani 1 1 d D . .
O211 O -0.1848(9) 0.4903(6) 0.1087(14) 0.031(2) Uani 1 1 d D . .
O212 O 0.0389(8) 0.4963(6) 0.3644(13) 0.031(2) Uani 1 1 d D . .
O21 O -0.0593(15) 0.5852(6) 0.1508(18) 0.032(4) Uani 1 1 d D . .
P22 P 0.0425(7) 0.6359(3) 0.1925(9) 0.0224(16) Uani 1 1 d D . .
O221 O 0.0900(13) 0.6688(8) 0.3544(14) 0.031(3) Uani 1 1 d D . .
O222 O 0.1243(12) 0.6020(9) 0.170(2) 0.031(3) Uani 1 1 d D . .
O22 O -0.0320(11) 0.6881(6) 0.0438(15) 0.030(3) Uani 1 1 d D . .
P23 P -0.1604(7) 0.6990(4) -0.1300(9) 0.0245(17) Uani 1 1 d D . .
O231 O -0.2530(12) 0.7129(9) -0.108(2) 0.035(3) Uani 1 1 d D . .
O232 O -0.1870(15) 0.6469(7) -0.2511(19) 0.035(3) Uani 1 1 d D . .
O23 O -0.1378(13) 0.7696(6) -0.1773(19) 0.034(3) Uani 1 1 d D . .
P24 P -0.0721(6) 0.8084(4) -0.2398(8) 0.0263(15) Uani 1 1 d D . .
O241 O 0.0496(9) 0.8293(8) -0.0995(17) 0.041(3) Uani 1 1 d D . .
O242 O -0.1573(12) 0.8593(6) -0.3565(17) 0.041(3) Uani 1 1 d D . .
O24 O -0.0527(14) 0.7554(7) -0.3390(18) 0.030(4) Uani 1 1 d D . .
P25 P 0.0415(7) 0.6976(4) -0.2909(9) 0.0230(17) Uani 1 1 d D . .
O251 O 0.0689(16) 0.6635(8) -0.1401(15) 0.029(3) Uani 1 1 d D . .
O252 O 0.1407(12) 0.7265(9) -0.2858(19) 0.029(3) Uani 1 1 d D . .
O25 O -0.0312(15) 0.6491(7) -0.4480(18) 0.048(3) Uani 1 1 d D . .
P26 P -0.1523(8) 0.6367(4) 0.3730(10) 0.0238(16) Uani 1 1 d D . .
O261 O -0.1703(17) 0.6871(7) 0.254(2) 0.037(4) Uani 1 1 d D . .
O262 O -0.2498(12) 0.6283(8) 0.387(2) 0.035(4) Uani 1 1 d D . .
O26 O -0.1188(18) 0.5657(7) 0.342(2) 0.048(3) Uani 1 1 d D . .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O132 Lu1 O211 91.4(6) 2_575 3 ?
O132 Lu1 O262 176.4(8) 2_575 4_564 ?
O211 Lu1 O262 86.3(5) 3 4_564 ?
O132 Lu1 O241 95.9(6) 2_575 . ?
O211 Lu1 O241 172.2(6) 3 . ?
O262 Lu1 O241 86.3(6) 4_564 . ?
O132 Lu1 O232 90.6(7) 2_575 4_565 ?
O211 Lu1 O232 89.5(5) 3 4_565 ?
O262 Lu1 O232 92.1(7) 4_564 4_565 ?
O241 Lu1 O232 93.1(6) . 4_565 ?
O132 Lu1 O131 87.4(7) 2_575 . ?
O211 Lu1 O131 85.9(6) 3 . ?
O262 Lu1 O131 89.7(7) 4_564 . ?
O241 Lu1 O131 91.7(7) . . ?
O232 Lu1 O131 175.0(9) 4_565 . ?
O261 Lu2 O221 171.2(6) . 4_464 ?
O261 Lu2 O122 88.4(6) . 2_575 ?
O221 Lu2 O122 84.2(5) 4_464 2_575 ?
O261 Lu2 O121 94.8(6) . 3_445 ?
O221 Lu2 O121 92.7(5) 4_464 3_445 ?
O122 Lu2 O121 176.4(5) 2_575 3_445 ?
O261 Lu2 O252 85.1(5) . 4_465 ?
O221 Lu2 O252 100.7(6) 4_464 4_465 ?
O122 Lu2 O252 97.3(6) 2_575 4_465 ?
O121 Lu2 O252 81.4(7) 3_445 4_465 ?
O261 Lu2 O231 88.0(7) . . ?
O221 Lu2 O231 87.6(7) 4_464 . ?
O122 Lu2 O231 93.7(6) 2_575 . ?
O121 Lu2 O231 88.1(6) 3_445 . ?
O252 Lu2 O231 166.9(6) 4_465 . ?
O111 Lu3 O112 97.6(6) 4_565 3_545 ?
O111 Lu3 O242 87.8(6) 4_565 4_565 ?
O112 Lu3 O242 81.0(7) 3_545 4_565 ?
O111 Lu3 O222 87.4(6) 4_565 . ?
O112 Lu3 O222 174.9(8) 3_545 . ?
O242 Lu3 O222 98.5(6) 4_565 . ?
O111 Lu3 O212 89.3(5) 4_565 2_564 ?
O112 Lu3 O212 87.8(6) 3_545 2_564 ?
O242 Lu3 O212 168.0(6) 4_565 2_564 ?
O222 Lu3 O212 93.0(5) . 2_564 ?
O111 Lu3 O251 171.2(6) 4_565 . ?
O112 Lu3 O251 90.7(6) 3_545 . ?
O242 Lu3 O251 90.4(6) 4_565 . ?
O222 Lu3 O251 84.3(6) . . ?
O212 Lu3 O251 94.1(6) 2_564 . ?
O111 P11 O112 113.9(11) . . ?
O111 P11 O13 105.8(11) . 2_575 ?
O112 P11 O13 108.5(12) . 2_575 ?
O111 P11 O11 112.4(12) . . ?
O112 P11 O11 114.6(12) . . ?
O13 P11 O11 100.1(9) 2_575 . ?
P11 O111 Lu3 147.0(11) . 4_464 ?
P11 O112 Lu3 139.9(11) . 3_455 ?
P11 O11 P12 128.2(13) . . ?
O121 P12 O122 116.3(11) . . ?
O121 P12 O12 107.3(11) . . ?
O122 P12 O12 106.3(11) . . ?
O121 P12 O11 105.1(9) . . ?
O122 P12 O11 114.7(10) . . ?
O12 P12 O11 106.4(11) . . ?
P12 O121 Lu2 160.6(12) . 3 ?
P12 O122 Lu2 152.9(11) . 2_574 ?
P13 O12 P12 150.8(12) . . ?
O132 P13 O131 117.5(12) . . ?
O132 P13 O12 108.2(10) . . ?
O131 P13 O12 109.3(11) . . ?
O132 P13 O13 106.8(11) . . ?
O131 P13 O13 112.9(13) . . ?
O12 P13 O13 100.8(11) . . ?
P13 O131 Lu1 155.1(14) . . ?
P13 O132 Lu1 156.5(11) . 2_574 ?
P11 O13 P13 139.5(12) 2_574 . ?
O212 P21 O211 121.6(9) . . ?
O212 P21 O21 107.0(9) . . ?
O211 P21 O21 106.1(9) . . ?
O212 P21 O26 109.5(9) . . ?
O211 P21 O26 105.5(10) . . ?
O21 P21 O26 106.0(10) . . ?
P21 O211 Lu1 152.9(9) . 3_445 ?
P21 O212 Lu3 163.7(9) . 2_565 ?
P21 O21 P22 138.5(11) . . ?
O222 P22 O221 120.2(9) . . ?
O222 P22 O22 107.1(10) . . ?
O221 P22 O22 109.4(9) . . ?
O222 P22 O21 109.0(10) . . ?
O221 P22 O21 108.0(10) . . ?
O22 P22 O21 101.6(8) . . ?
P22 O221 Lu2 153.7(11) . 4_565 ?
P22 O222 Lu3 150.9(12) . . ?
P23 O22 P22 141.5(10) . . ?
O231 P23 O232 117.0(10) . . ?
O231 P23 O22 112.6(10) . . ?
O232 P23 O22 110.9(9) . . ?
O231 P23 O23 103.1(10) . . ?
O232 P23 O23 112.9(11) . . ?
O22 P23 O23 98.6(8) . . ?
P23 O231 Lu2 148.4(10) . . ?
P23 O232 Lu1 150.4(11) . 4_464 ?
P23 O23 P24 145.1(12) . . ?
O242 P24 O241 118.5(10) . . ?
O242 P24 O24 109.7(9) . . ?
O241 P24 O24 104.3(10) . . ?
O242 P24 O23 105.5(9) . . ?
O241 P24 O23 112.3(10) . . ?
O24 P24 O23 106.0(10) . . ?
P24 O241 Lu1 146.5(11) . . ?
P24 O242 Lu3 157.2(11) . 4_464 ?
P24 O24 P25 136.3(11) . . ?
O251 P25 O252 119.3(11) . . ?
O251 P25 O25 109.7(11) . . ?
O252 P25 O25 107.6(11) . . ?
O251 P25 O24 107.4(10) . . ?
O252 P25 O24 108.3(11) . . ?
O25 P25 O24 103.4(8) . . ?
P25 O251 Lu3 134.8(10) . . ?
P25 O252 Lu2 141.8(9) . 4_564 ?
P26 O25 P25 145.9(11) 1_554 . ?
O262 P26 O261 116.5(10) . . ?
O262 P26 O25 109.7(11) . 1_556 ?
O261 P26 O25 110.6(12) . 1_556 ?
O262 P26 O26 108.5(11) . . ?
O261 P26 O26 112.9(11) . . ?
O25 P26 O26 96.9(10) 1_556 . ?
P26 O261 Lu2 144.2(11) . . ?
P26 O262 Lu1 150.4(10) . 4_465 ?
P26 O26 P21 142.9(15) . . ?
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
Lu1 O132 2.141(10) 2_575 ?
Lu1 O211 2.174(10) 3 ?
Lu1 O262 2.191(11) 4_564 ?
Lu1 O241 2.209(12) . ?
Lu1 O232 2.214(11) 4_565 ?
Lu1 O131 2.236(12) . ?
Lu2 O261 2.186(12) . ?
Lu2 O221 2.207(11) 4_464 ?
Lu2 O122 2.208(11) 2_575 ?
Lu2 O121 2.211(11) 3_445 ?
Lu2 O252 2.216(11) 4_465 ?
Lu2 O231 2.261(11) . ?
Lu3 O111 2.166(11) 4_565 ?
Lu3 O112 2.176(14) 3_545 ?
Lu3 O242 2.177(10) 4_565 ?
Lu3 O222 2.187(11) . ?
Lu3 O212 2.199(9) 2_564 ?
Lu3 O251 2.214(14) . ?
O111 Lu3 2.166(11) 4_464 ?
O112 Lu3 2.176(14) 3_455 ?
O11 P12 1.610(17) . ?
O121 Lu2 2.211(11) 3 ?
O122 Lu2 2.208(10) 2_574 ?
O12 P13 1.534(13) . ?
P13 O132 1.46(2) . ?
P13 O131 1.462(19) . ?
P13 O13 1.583(8) . ?
O132 Lu1 2.141(10) 2_574 ?
O13 P11 1.570(15) 2_574 ?
O211 Lu1 2.174(10) 3_445 ?
O212 Lu3 2.199(9) 2_565 ?
O21 P22 1.584(13) . ?
O221 Lu2 2.207(11) 4_565 ?
O22 P23 1.579(12) . ?
O232 Lu1 2.214(11) 4_464 ?
O23 P24 1.589(12) . ?
O242 Lu3 2.177(10) 4_464 ?
O24 P25 1.592(13) . ?
O252 Lu2 2.216(11) 4_564 ?
O25 P26 1.562(13) 1_554 ?
O262 Lu1 2.191(11) 4_465 ?
