#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/39/2103915.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_2103915
loop_
_publ_author_name
'Norberg, Stefan T.'
'Sobolev, Alexander N.'
'Streltsov, Victor A.'
_publ_section_title
;
 Cation movement and phase transitions in KTP isostructures; X-ray
 study of sodium-doped KTP at 10.5K
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              353
_journal_page_last               360
_journal_paper_doi               10.1107/S0108768103008450
_journal_volume                  59
_journal_year                    2003
_chemical_formula_moiety         'K1.886 Na0.114 O10 P2 Ti2'
_chemical_formula_structural     '(Na0.114 K0.886) K (Ti O)2 (P O4)2'
_chemical_formula_sum            'K1.886 Na0.114 O10 P2 Ti2'
_chemical_formula_weight         394.06
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7919(5)
_cell_length_b                   6.3798(4)
_cell_length_c                   10.5880(7)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    10.5(3)
_cell_measurement_theta_max      38.3
_cell_measurement_theta_min      19.5
_cell_volume                     864.08(9)
_computing_cell_refinement
;
Local diffractometer control software
;
_computing_data_collection
;
Local diffractometer control software
;
_computing_data_reduction
;
PROFIT (Streltsov & Zavodnik, 1989) and Xtal3.71 (Hall et al., 2000)
programs: DIFDAT; SORTRF; ADDREF; ABSORB
;
_computing_molecular_graphics
;
ORTEPIII for Windows (Farrugia, 1997), and Xtal3.71 (Hall et al., 2000)
programs: FOURR; SLANT; CONTRS
;
_computing_publication_material
;
Xtal3.71 (Hall et al., 2000) programs: BONDLA; ATABLE; CIFIO
;
_computing_structure_refinement
;
Xtal3.71 (Hall et al., 2000) program: CRYLSQ
;
_computing_structure_solution
;
Atomic parameters from Norberg et al. (2000)
;
_diffrn_ambient_temperature      10.5(3)
_diffrn_measurement_device_type  'Huber 512 goniometer'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  none
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.017
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16753
_diffrn_reflns_reduction_process 'No monochr Lp applied'
_diffrn_reflns_theta_max         50.14
_diffrn_reflns_theta_min         3.19
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.175
_exptl_absorpt_correction_T_max  0.521
_exptl_absorpt_correction_T_min  0.389
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(Alcock, 1974)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.029
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             764.5
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.67
_refine_diff_density_min         -1.54
_refine_ls_abs_structure_details 'Flack (1983) parameter refined'
_refine_ls_abs_structure_Flack   0.508(13)
_refine_ls_extinction_coef       53E2(2)
_refine_ls_extinction_expression
'Larson, 1970, Eq22 p292 "Cryst. Comp." Munksgaard 1970'
_refine_ls_extinction_method     'Isotropic Gaussian (Zachariasen, 1967)'
_refine_ls_goodness_of_fit_all   1.182
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_constraints    1
_refine_ls_number_parameters     156
_refine_ls_number_reflns         8961
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.017
_refine_ls_R_factor_gt           0.017
_refine_ls_shift/su_max          0.00086
_refine_ls_shift/su_mean         0.000054
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(F) + 0.0015(F)²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.037
_refine_ls_wR_factor_gt          0.037
_refine_ls_wR_factor_ref         0.037
_reflns_number_gt                8961
_reflns_number_total             8961
_reflns_threshold_expression     'F > 0σ(F)'
_cod_data_source_file            os0106.cif
_cod_data_source_block           10K
_cod_original_sg_symbol_Hall     'p 2c -2n'
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               2103915
_cod_database_fobs_code          2103915
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,-y,1/2+z
1/2-x,1/2+y,1/2+z
1/2+x,1/2-y,+z
loop_
_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_occupancy
K1 0.37665(3) 0.22060(4) 0.30013(4) 0.00501(10) Uani 0.886(3)
Na1 0.3435(6) 0.2317(7) 0.2723(6) 0.0067(18) Uani 0.114(3)
K2 0.104799(18) 0.30202(4) 0.05454(4) 0.00607(7) Uani 1
Ti1 0.373144(12) 0.50094(2) -0.00824(4) 0.00264(5) Uani 1
Ti2 0.246260(12) 0.73089(3) 0.24322(4) 0.00265(5) Uani 1
P1 0.49765(2) 0.66341(4) 0.25211(5) 0.00294(8) Uani 1
P2 0.18144(2) 0.49851(4) 0.50443(5) 0.00284(9) Uani 1
O1 0.48538(7) 0.51197(12) 0.14237(9) 0.0047(2) Uani 1
O2 0.50893(6) 0.53385(13) 0.37516(9) 0.0046(2) Uani 1
O3 0.39995(6) 0.80223(13) 0.27100(9) 0.0046(2) Uani 1
O4 0.59339(6) 0.80653(12) 0.23296(9) 0.0047(2) Uani 1
O11 0.27502(6) 0.53280(13) 0.13510(8) 0.0045(2) Uani 1
O12 0.22370(6) 0.96044(13) 0.38101(8) 0.0046(2) Uani 1
O5 0.11282(6) 0.69039(12) 0.53248(9) 0.0042(2) Uani 1
O6 0.11135(6) 0.30862(12) 0.47983(9) 0.0047(2) Uani 1
O7 0.25356(6) 0.46234(14) 0.61972(9) 0.0046(2) Uani 1
O8 0.25368(6) 0.53840(15) 0.3910(6) 0.0048(2) Uani 1
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
K 0.179 0.25 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Na 0.03 0.025 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Ti 0.248 0.446 'Int Tables Vol IV Tables 2.2B and 2.3.1'
P 0.09 0.095 'Int Tables Vol IV Tables 2.2B and 2.3.1'
O 0.008 0.006 'Int Tables Vol IV Tables 2.2B and 2.3.1'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
8 0 0
0 4 0
0 0 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
_geom_angle_publ_flag
O1 K1 O2 . . 52.71(3) no
O1 K1 O11 . . 55.24(2) no
O1 K1 O8 . . 90.19(8) no
O1 K1 O3 . '1 545' 121.43(3) no
O1 K1 O12 . '1 545' 159.31(3) no
O1 K1 O5 . '3 544' 55.87(3) no
O1 K1 O7 . '3 544' 104.66(3) no
O2 K1 O11 . . 87.21(2) no
O2 K1 O8 . . 73.30(4) no
O2 K1 O3 . '1 545' 133.31(3) no
O2 K1 O12 . '1 545' 143.47(3) no
O2 K1 O5 . '3 544' 108.03(3) no
O2 K1 O7 . '3 544' 157.25(3) no
O11 K1 O8 . . 57.03(13) no
O11 K1 O3 . '1 545' 130.34(3) no
O11 K1 O12 . '1 545' 106.44(3) no
O11 K1 O5 . '3 544' 58.44(2) no
O11 K1 O7 . '3 544' 75.58(3) no
O8 K1 O3 . '1 545' 146.49(5) no
O8 K1 O12 . '1 545' 85.85(5) no
O8 K1 O5 . '3 544' 115.30(13) no
O8 K1 O7 . '3 544' 107.99(8) no
O3 K1 O12 '1 545' '1 545' 60.66(3) no
O3 K1 O5 '1 545' '3 544' 79.29(3) no
O3 K1 O7 '1 545' '3 544' 56.67(3) no
O12 K1 O5 '1 545' '3 544' 107.95(3) no
O12 K1 O7 '1 545' '3 544' 57.79(3) no
O5 K1 O7 '3 544' '3 544' 50.16(2) no
O1 Na1 O2 . . 49.24(11) no
O1 Na1 O11 . . 58.80(12) no
O1 Na1 O8 . . 92.40(16) no
O1 Na1 O3 . '1 545' 115.8(2) no
O1 Na1 O12 . '1 545' 176.1(2) no
O1 Na1 O5 . '3 544' 57.76(13) no
O1 Na1 O7 . '3 544' 113.7(2) no
O2 Na1 O11 . . 88.04(15) no
O2 Na1 O8 . . 70.05(13) no
O2 Na1 O3 . '1 545' 115.7(2) no
O2 Na1 O12 . '1 545' 132.3(2) no
O2 Na1 O5 . '3 544' 105.1(2) no
O2 Na1 O7 . '3 544' 160.6(3) no
O11 Na1 O8 . . 63.76(18) no
O11 Na1 O3 . '1 545' 144.0(2) no
O11 Na1 O12 . '1 545' 123.5(3) no
O11 Na1 O5 . '3 544' 66.29(14) no
O11 Na1 O7 . '3 544' 88.9(2) no
O8 Na1 O3 . '1 545' 147.6(3) no
O8 Na1 O12 . '1 545' 91.5(2) no
O8 Na1 O5 . '3 544' 129.9(3) no
O8 Na1 O7 . '3 544' 125.0(3) no
O3 Na1 O12 '1 545' '1 545' 60.36(11) no
O3 Na1 O5 '1 545' '3 544' 80.99(15) no
O3 Na1 O7 '1 545' '3 544' 59.50(11) no
O12 Na1 O5 '1 545' '3 544' 119.5(2) no
O12 Na1 O7 '1 545' '3 544' 64.01(14) no
O5 Na1 O7 '3 544' '3 544' 56.34(12) no
O11 K2 O5 . '2 564' 143.29(3) no
O11 K2 O2 . '3 544' 154.02(3) no
O11 K2 O3 . '3 544' 108.92(3) no
O11 K2 O12 . '3 544' 55.93(2) no
O11 K2 O7 . '3 544' 80.38(3) no
O11 K2 O8 . '3 544' 90.08(5) no
O11 K2 O1 . '4 455' 137.63(3) no
O11 K2 O4 . '4 465' 54.99(2) no
O5 K2 O2 '2 564' '3 544' 57.54(2) no
O5 K2 O3 '2 564' '3 544' 84.04(3) no
O5 K2 O12 '2 564' '3 544' 131.59(3) no
O5 K2 O7 '2 564' '3 544' 130.81(2) no
O5 K2 O8 '2 564' '3 544' 124.02(7) no
O5 K2 O1 '2 564' '4 455' 58.34(3) no
O5 K2 O4 '2 564' '4 465' 89.44(2) no
O2 K2 O3 '3 544' '3 544' 49.05(2) no
O2 K2 O12 '3 544' '3 544' 99.23(3) no
O2 K2 O7 '3 544' '3 544' 91.60(3) no
O2 K2 O8 '3 544' '3 544' 66.55(6) no
O2 K2 O1 '3 544' '4 455' 60.55(3) no
O2 K2 O4 '3 544' '4 465' 146.05(2) no
O3 K2 O12 '3 544' '3 544' 53.79(2) no
O3 K2 O7 '3 544' '3 544' 104.49(3) no
O3 K2 O8 '3 544' '3 544' 55.85(10) no
O3 K2 O1 '3 544' '4 455' 109.57(3) no
O3 K2 O4 '3 544' '4 465' 126.96(2) no
O12 K2 O7 '3 544' '3 544' 86.64(2) no
O12 K2 O8 '3 544' '3 544' 53.45(5) no
O12 K2 O1 '3 544' '4 455' 150.38(3) no
O12 K2 O4 '3 544' '4 465' 97.65(2) no
O7 K2 O8 '3 544' '3 544' 49.22(10) no
O7 K2 O1 '3 544' '4 455' 73.52(3) no
O7 K2 O4 '3 544' '4 465' 118.67(3) no
O8 K2 O1 '3 544' '4 455' 97.13(4) no
O8 K2 O4 '3 544' '4 465' 144.87(4) no
O1 K2 O4 '4 455' '4 465' 111.05(3) no
O1 Ti1 O11 . . 81.44(4) no
O1 Ti1 O2 . '2 664' 87.53(4) no
O1 Ti1 O12 . '3 544' 171.87(4) no
O1 Ti1 O5 . '3 544' 79.37(3) no
O1 Ti1 O6 . '3 554' 87.01(3) no
O11 Ti1 O2 . '2 664' 168.94(4) no
O11 Ti1 O12 . '3 544' 94.66(4) no
O11 Ti1 O5 . '3 544' 89.63(4) no
O11 Ti1 O6 . '3 554' 90.61(4) no
O2 Ti1 O12 '2 664' '3 544' 96.17(4) no
O2 Ti1 O5 '2 664' '3 544' 87.44(4) no
O2 Ti1 O6 '2 664' '3 554' 89.71(4) no
O12 Ti1 O5 '3 544' '3 544' 93.53(4) no
O12 Ti1 O6 '3 544' '3 554' 100.22(4) no
O5 Ti1 O6 '3 544' '3 554' 166.19(4) no
O3 Ti2 O11 . . 93.04(4) no
O3 Ti2 O12 . . 82.87(3) no
O3 Ti2 O8 . . 88.76(4) no
O3 Ti2 O7 . '3 554' 85.84(3) no
O3 Ti2 O4 . '4 465' 172.07(4) no
O11 Ti2 O12 . . 174.99(4) no
O11 Ti2 O8 . . 93.38(12) no
O11 Ti2 O7 . '3 554' 96.15(4) no
O11 Ti2 O4 . '4 465' 94.89(4) no
O12 Ti2 O8 . . 83.68(12) no
O12 Ti2 O7 . '3 554' 86.46(4) no
O12 Ti2 O4 . '4 465' 89.22(3) no
O8 Ti2 O7 . '3 554' 169.28(12) no
O8 Ti2 O4 . '4 465' 90.91(4) no
O7 Ti2 O4 '3 554' '4 465' 93.17(3) no
O1 P1 O2 . . 108.27(5) no
O1 P1 O3 . . 112.34(5) no
O1 P1 O4 . . 111.00(5) no
O2 P1 O3 . . 105.80(5) no
O2 P1 O4 . . 110.65(5) no
O3 P1 O4 . . 108.68(4) no
O5 P2 O6 . . 109.22(5) no
O5 P2 O7 . . 107.89(5) no
O5 P2 O8 . . 111.29(6) no
O6 P2 O7 . . 111.45(5) no
O6 P2 O8 . . 110.53(13) no
O7 P2 O8 . . 106.42(15) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
K1 O1 . 2.8601(10) no
K1 O2 . 2.7365(9) no
K1 O3 '1 545' 2.7034(9) no
K1 O11 . 2.9513(9) no
K1 O12 '1 545' 2.7048(9) no
K1 O5 '3 544' 2.8437(10) no
K1 O7 '3 544' 3.0229(9) no
K1 O8 . 2.741(2) no
K1 Na1 . 0.521(7) no
Na1 O1 . 2.896(6) no
Na1 O2 . 3.063(7) no
Na1 O3 '1 545' 2.833(5) no
Na1 O11 . 2.563(6) no
Na1 O12 '1 545' 2.582(6) no
Na1 O5 '3 544' 2.613(6) no
Na1 O7 '3 544' 2.665(6) no
Na1 O8 . 2.594(7) no
K2 O1 '4 455' 2.6854(9) no
K2 O2 '3 544' 2.9412(9) no
K2 O3 '3 544' 3.0027(11) no
K2 O4 '4 465' 3.1348(9) no
K2 O11 . 2.7635(9) no
K2 O12 '3 544' 3.0348(9) no
K2 O5 '2 564' 2.7940(8) no
K2 O7 '3 544' 2.9078(9) no
K2 O8 '3 544' 3.017(4) no
Ti1 O1 . 2.1469(10) no
Ti1 O2 '2 664' 1.9619(9) no
Ti1 O11 . 1.9800(9) no
Ti1 O12 '3 544' 1.7253(9) no
Ti1 O5 '3 544' 2.0356(8) no
Ti1 O6 '3 554' 1.9769(8) no
Ti2 O3 . 2.0393(8) no
Ti2 O4 '4 465' 1.9730(8) no
Ti2 O11 . 1.7444(9) no
Ti2 O12 . 2.0872(9) no
Ti2 O7 '3 554' 1.9723(10) no
Ti2 O8 . 1.992(5) no
P1 O1 . 1.5193(10) no
P1 O2 . 1.5497(10) no
P1 O3 . 1.5447(8) no
P1 O4 . 1.5410(8) no
P2 O5 . 1.5354(8) no
P2 O6 . 1.5296(8) no
P2 O7 . 1.5474(10) no
P2 O8 . 1.536(5) no
