#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/56/2015649.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_2015649
loop_
_publ_author_name
'Artem A. Babaryk'
'Igor V. Zatovsky'
'Vyacheslav N. Baumer'
'Nikolay S. Slobodyanik'
'Oleg V. Shishkin'
_publ_section_title
;
 Centrosymmetric aliovalent KTP isomorphs
 KMIII~0.5~Nb~0.5~OPO₄ (M = Cr and Fe)
;
_journal_coeditor_code           IZ3009
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i91
_journal_page_last               i93
_journal_paper_doi               10.1107/S0108270106028678
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'K Fe0.5 Nb0.5 O P O4'
_chemical_formula_moiety         'K +, Fe0.5 Nb0.5 O5 P1 -'
_chemical_formula_sum            'Fe0.5 K Nb0.5 O5 P'
_chemical_formula_weight         224.45
_chemical_name_systematic
;
potassium iron niobium oxide phosphate
;
_space_group_IT_number           52
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.9675(13)
_cell_length_b                   10.705(3)
_cell_length_c                   6.4638(7)
_cell_measurement_reflns_used    450
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      15
_cell_volume                     897.3(3)
_computing_cell_refinement       'CrysAlis CCD'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2005)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2005)'
_computing_molecular_graphics
'Ortep-3 for Windows (Farrugia, 1997) and DIAMOND Bradenburg, 2006)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Oxford Diffraction XCalibur-3'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            18570
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         3.14
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.219
_exptl_absorpt_correction_T_max  0.4956
_exptl_absorpt_correction_T_min  0.3871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(Blessing, 1995)
;
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    3.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.468
_refine_diff_density_min         -1.323
_refine_ls_extinction_coef       0.0048(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.326
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         1087
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.325
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+22.5550P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1125
_reflns_number_gt                1021
_reflns_number_total             1087
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            iz3009.cif
_cod_data_source_block           II
_cod_original_formula_sum        'Fe0.50 K Nb0.50 O5 P'
_cod_database_code               2015649
_cod_database_fobs_code          2015649
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'x, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'-x, y-1/2, z-1/2'
'x-1/2, -y-1/2, z-1/2'
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_thermal_displace_type
_atom_site_occupancy
Nb Nb2 0.38100(10) 0.2500000 0.2500000 0.0094 Uani 0.869
Nb Nb1 0.5000000 0.0000000 0.0000000 0.0112 Uani 0.131
Fe Fe1 0.5000000 0.0000000 0.0000000 0.0112 Uani 0.869
P P1 0.4329(2) 0.2500000 0.7500000 0.0097 Uani 1.000
P P2 0.2500000 0.0000000 0.08400(10) 0.0098 Uani 1.000
Fe Fe2 0.38100(10) 0.2500000 0.2500000 0.0094 Uani 0.131
O O1 0.3451(7) -0.0178(6) -0.05140(10) 0.0139 Uani 1.000
O O2 0.4758000 0.1248(5) 0.2143(8) 0.0127 Uani 1.000
O O3 0.2625(6) 0.1151(2) 0.2267(4) 0.0153 Uani 1.000
O O4 0.5016(8) 0.3639(3) 0.71450(10) 0.0146 Uani 1.000
O O5 0.3624(6) 0.2270(3) 0.5627(6) 0.0152 Uani 1.000
K K1 0.1292000 0.0536(4) 0.5307(6) 0.0333 Uani 0.500
K K2 0.14540(10) 0.1897(8) 0.5557(9) 0.0374 Uani 0.500
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Fe Fe 0.346 0.844 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.201 0.249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.073 0.622 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.102 0.094 '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
_geom_angle_publ_flag
O1 Nb1 O2 . . 91.2(3) no
O1 Nb1 O4 . 3_555 88.0(7) no
O1 Nb1 O1 . 5_655 180.0000 no
O1 Nb1 O2 . 5_655 88.7(7) no
O1 Nb1 O4 . 7_644 91.9(3) no
O2 Nb1 O4 . 3_555 89.7(3) no
O1 Nb1 O2 5_655 . 88.7(7) no
O2 Nb1 O2 . 5_655 180.0000 no
O2 Nb1 O4 . 7_644 90.2(7) no
O1 Nb1 O4 5_655 3_555 91.9(3) no
O2 Nb1 O4 5_655 3_555 90.2(7) no
O4 Nb1 O4 3_555 7_644 180.0000 no
O1 Nb1 O2 5_655 5_655 91.2(3) no
O1 Nb1 O4 5_655 7_644 88.0(7) no
O2 Nb1 O4 5_655 7_644 89.7(3) no
O2 Nb2 O3 . . 88.8000 no
O2 Nb2 O5 . . 96.6000 no
O2 Nb2 O2 . 3_555 95.7(6) no
O2 Nb2 O3 . 3_555 174.7(4) no
O2 Nb2 O5 . 3_555 92.4(3) no
O3 Nb2 O5 . . 84.4(3) no
O2 Nb2 O3 3_555 . 174.7(4) no
O3 Nb2 O3 . 3_555 86.7(7) no
O3 Nb2 O5 . 3_555 85.7(9) no
O2 Nb2 O5 3_555 . 92.4(3) no
O3 Nb2 O5 3_555 . 85.7(9) no
O5 Nb2 O5 . 3_555 166.5(3) no
O2 Nb2 O3 3_555 3_555 88.8000 no
O2 Nb2 O5 3_555 3_555 96.6000 no
O3 Nb2 O5 3_555 3_555 84.4(3) no
O1 Fe1 O2 . . 91.2(3) no
O1 Fe1 O4 . 3_555 88.0(7) no
O1 Fe1 O1 . 5_655 180.0000 no
O1 Fe1 O2 . 5_655 88.7(7) no
O1 Fe1 O4 . 7_644 91.9(3) no
O2 Fe1 O4 . 3_555 89.7(3) no
O1 Fe1 O2 5_655 . 88.7(7) no
O2 Fe1 O2 . 5_655 180.0000 no
O2 Fe1 O4 . 7_644 90.2(7) no
O1 Fe1 O4 5_655 3_555 91.9(3) no
O2 Fe1 O4 5_655 3_555 90.2(7) no
O4 Fe1 O4 3_555 7_644 180.0000 no
O1 Fe1 O2 5_655 5_655 91.2(3) no
O1 Fe1 O4 5_655 7_644 88.0(7) no
O2 Fe1 O4 5_655 7_644 89.7(3) no
O2 Fe2 O3 . 3_555 174.7(4) no
O2 Fe2 O5 . 3_555 92.4(3) no
O3 Fe2 O5 . . 84.4(3) no
O2 Fe2 O3 3_555 . 174.7(4) no
O3 Fe2 O3 . 3_555 86.7(7) no
O3 Fe2 O5 . 3_555 85.7(9) no
O2 Fe2 O5 3_555 . 92.4(3) no
O3 Fe2 O5 3_555 . 85.7(9) no
O5 Fe2 O5 . 3_555 166.5(3) no
O2 Fe2 O3 3_555 3_555 88.8000 no
O2 Fe2 O5 3_555 3_555 96.6000 no
O3 Fe2 O5 3_555 3_555 84.4(3) no
O2 Fe2 O3 . . 88.8000 no
O2 Fe2 O5 . . 96.6000 no
O2 Fe2 O2 . 3_555 95.7(6) no
O4 P1 O5 . . 110.9(2) no
O4 P1 O4 . 3_556 108.60(10) no
O4 P1 O5 . 3_556 109.7(3) no
O4 P1 O5 3_556 . 109.7(3) no
O5 P1 O5 . 3_556 107.00(10) no
O4 P1 O5 3_556 3_556 110.9(2) no
O1 P2 O3 . . 110.9(4) no
O1 P2 O1 . 2_555 109.9(4) no
O1 P2 O3 . 2_555 109.10(10) no
O1 P2 O3 2_555 . 109.10(10) no
O3 P2 O3 . 2_555 106.8(4) no
O1 P2 O3 2_555 2_555 110.9000 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 K2 . 1.481(3) yes
K1 O2 6_456 2.693(7) yes
K1 O3 . 2.700(7) yes
K1 O1 2_556 2.748(7) yes
K1 O4 8_454 2.774(7) yes
K1 O5 2_555 3.013(7) yes
K1 O3 2_555 3.016(7) yes
K1 O2 2_555 3.113(7) yes
K1 O4 4_546 3.117(7) yes
K2 O3 . 2.734(7) yes
K2 O2 6_456 2.743(7) yes
K2 O5 . 2.844(7) yes
K2 O4 8_454 2.944(7) yes
K2 O1 4_555 3.132(8) yes
K2 O2 8_455 3.134(7) yes
K2 O4 6_456 3.162(7) yes
K2 O3 3_555 3.163(7) yes
Nb1 O2 . 1.950(6) no
Nb1 O4 3_555 2.011(2) no
Nb1 O1 5_655 2.044000 no
Nb1 O2 5_655 1.950(6) no
Nb1 O4 7_644 2.011(2) no
Nb1 O1 . 2.044000 no
Nb2 O5 3_555 2.050(7) no
Nb2 O2 . 1.832(6) no
Nb2 O3 . 2.113(5) no
Nb2 O5 . 2.050(7) no
Nb2 O2 3_555 1.832(6) no
Nb2 O3 3_555 2.113(5) no
Fe1 O1 . 2.044000 yes
Fe1 O2 . 1.950(6) yes
Fe1 O4 3_555 2.011(2) yes
Fe1 O1 5_655 2.044000 no
Fe1 O2 5_655 1.950(6) no
Fe1 O4 7_644 2.011(2) no
Fe2 O5 . 2.050(7) yes
Fe2 O2 . 1.832(6) yes
Fe2 O3 . 2.113(5) yes
Fe2 O5 3_555 2.050(7) no
Fe2 O2 3_555 1.832(6) no
Fe2 O3 3_555 2.113(5) no
P1 O4 . 1.527(7) yes
P1 O5 . 1.537(6) yes
P1 O4 3_556 1.527(7) no
P1 O5 3_556 1.537(6) no
P2 O1 . 1.524(7) yes
P2 O3 . 1.548(3) yes
P2 O1 2_555 1.524(7) no
P2 O3 2_555 1.548(3) no
