#------------------------------------------------------------------------------
#$Date: 2018-08-23 02:30:57 +0300 (Thu, 23 Aug 2018) $
#$Revision: 210074 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/33/86/4338654.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_4338654
loop_
_publ_author_name
'Yang, Sihai'
'Li, Guobao'
'Liu, Wei'
'Wang, Wei'
'Yan, Zhimin'
'Huang, Yining'
'Liao, Fuhui'
'Lin, Jianhua'
_publ_section_title
;
 Synthesis and Characterization of a Fluorotitanophosphate
 (NH₄)~0.16~K~1.84~[Ti₂F₂(PO₄)₂(PO₃OH)] with a
 Unique Lamella Framework
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5449
_journal_page_last               5453
_journal_paper_doi               10.1021/ic900504m
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'F2 H1.64 K1.84 N0.16 O12 P3 Ti2'
_chemical_formula_weight         494.55
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.16(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.406(3)
_cell_length_b                   8.3230(17)
_cell_length_c                   8.8260(18)
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      32.5
_cell_measurement_theta_min      2
_cell_volume                     1173.5(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4710
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         33.50
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    2.515
_exptl_absorpt_correction_T_max  0.605
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995, 1997)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.799
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             962.9
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         2182
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0308
_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)+(0.0394P)²+1.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0775
_reflns_number_gt                1881
_reflns_number_total             2182
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900504m_si_002.cif
_cod_data_source_block
;
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4338654
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'
'-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
Ti1 Ti 0.418618(19) 0.25203(4) 0.93380(3) 0.00924(8) Uani 1 1 d .
K1 K 0.28595(5) 0.08298(10) 1.19981(8) 0.02162(14) Uani 0.92 1 d P
N1 N 0.302(2) 0.113(4) 1.223(4) 0.012(7) Uiso 0.08 1 d P
H1A H 0.3386 0.1736 1.2804 0.014 Uiso 0.08 1 d P
H1B H 0.3251 0.0544 1.1648 0.014 Uiso 0.08 1 d P
H1C H 0.2646 0.1736 1.1648 0.014 Uiso 0.08 1 d P
H1D H 0.2781 0.0544 1.2804 0.014 Uiso 0.08 1 d P
P1 P 0.5000 0.03814(8) 1.2500 0.00846(12) Uani 1 2 d S
P2 P 0.38699(3) 0.38526(6) 0.56680(5) 0.01065(10) Uani 1 1 d .
O1 O 0.38075(10) 0.43511(17) 1.02972(17) 0.0180(3) Uani 1 1 d .
O2 O 0.46928(9) 0.32097(19) 0.53823(18) 0.0204(3) Uani 1 1 d .
O3 O 0.31378(10) 0.2981(2) 0.45909(18) 0.0243(3) Uani 1 1 d .
H3 H 0.2829 0.2599 0.5109 0.037 Uiso 0.50 1 calc PR
O4 O 0.38169(10) 0.36300(19) 0.73587(16) 0.0206(3) Uani 1 1 d .
O5 O 0.55742(10) -0.06321(18) 1.17543(18) 0.0200(3) Uani 1 1 d .
O6 O 0.44327(10) 0.1432(2) 1.12958(17) 0.0219(3) Uani 1 1 d .
F1 F 0.31004(7) 0.16608(14) 0.90553(13) 0.0153(2) Uani 1 1 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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
F1 Ti1 O2 175.35(6) . 2_656
F1 Ti1 O6 86.49(7) . .
O2 Ti1 O6 91.52(7) 2_656 .
F1 Ti1 O1 88.19(6) . .
O2 Ti1 O1 96.02(7) 2_656 .
O6 Ti1 O1 90.03(7) . .
F1 Ti1 O5 85.33(6) . 5_657
O2 Ti1 O5 90.55(7) 2_656 5_657
O6 Ti1 O5 92.33(7) . 5_657
O1 Ti1 O5 172.96(7) . 5_657
F1 Ti1 O4 88.26(7) . .
O2 Ti1 O4 93.90(8) 2_656 .
O6 Ti1 O4 174.19(7) . .
O1 Ti1 O4 87.32(7) . .
O5 Ti1 O4 89.73(7) 5_657 .
F1 Ti1 K1 46.55(4) . 7_557
O2 Ti1 K1 137.81(6) 2_656 7_557
O6 Ti1 K1 118.07(5) . 7_557
O1 Ti1 K1 57.61(5) . 7_557
O5 Ti1 K1 115.55(5) 5_657 7_557
O4 Ti1 K1 56.21(5) . 7_557
F1 Ti1 K1 44.46(4) . .
O2 Ti1 K1 134.97(5) 2_656 .
O6 Ti1 K1 45.71(5) . .
O1 Ti1 K1 74.53(5) . .
O5 Ti1 K1 102.52(5) 5_657 .
O4 Ti1 K1 128.50(5) . .
K1 Ti1 K1 73.73(2) 7_557 .
F1 Ti1 K1 41.33(4) . 6
O2 Ti1 K1 135.01(5) 2_656 6
O6 Ti1 K1 96.87(6) . 6
O1 Ti1 K1 127.94(5) . 6
O5 Ti1 K1 45.16(5) 5_657 6
O4 Ti1 K1 80.76(6) . 6
K1 Ti1 K1 74.12(2) 7_557 6
K1 Ti1 K1 74.342(18) . 6
F1 K1 F1 144.78(3) 7_557 6_556
F1 K1 F1 71.25(5) 7_557 .
F1 K1 F1 140.90(4) 6_556 .
F1 K1 O5 152.71(5) 7_557 2_657
F1 K1 O5 55.42(4) 6_556 2_657
F1 K1 O5 99.18(5) . 2_657
F1 K1 O6 106.35(5) 7_557 .
F1 K1 O6 106.22(5) 6_556 .
F1 K1 O6 54.94(5) . .
O5 K1 O6 50.91(4) 2_657 .
F1 K1 O3 76.19(5) 7_557 1_556
F1 K1 O3 88.32(5) 6_556 1_556
F1 K1 O3 123.84(5) . 1_556
O5 K1 O3 89.57(6) 2_657 1_556
O6 K1 O3 94.41(6) . 1_556
F1 K1 O4 56.33(4) 7_557 7_557
F1 K1 O4 89.31(5) 6_556 7_557
F1 K1 O4 118.21(5) . 7_557
O5 K1 O4 142.19(5) 2_657 7_557
O6 K1 O4 161.02(6) . 7_557
O3 K1 O4 74.81(5) 1_556 7_557
F1 K1 O1 55.14(4) 7_557 7_557
F1 K1 O1 112.44(5) 6_556 7_557
F1 K1 O1 71.77(5) . 7_557
O5 K1 O1 147.64(5) 2_657 7_557
O6 K1 O1 126.46(5) . 7_557
O3 K1 O1 121.62(5) 1_556 7_557
O4 K1 O1 52.93(4) 7_557 7_557
F1 K1 O3 103.79(5) 7_557 4_546
F1 K1 O3 72.23(5) 6_556 4_546
F1 K1 O3 86.53(5) . 4_546
O5 K1 O3 100.96(5) 2_657 4_546
O6 K1 O3 117.33(5) . 4_546
O3 K1 O3 146.07(4) 1_556 4_546
O4 K1 O3 77.36(5) 7_557 4_546
O1 K1 O3 48.66(4) 7_557 4_546
F1 K1 P1 129.36(4) 7_557 .
F1 K1 P1 81.00(4) 6_556 .
F1 K1 P1 77.98(4) . .
O5 K1 P1 25.59(3) 2_657 .
O6 K1 P1 25.57(3) . .
O3 K1 P1 89.58(5) 1_556 .
O4 K1 P1 161.91(4) 7_557 .
O1 K1 P1 145.11(4) 7_557 .
O3 K1 P1 113.55(4) 4_546 .
F1 K1 Ti1 31.01(3) 7_557 7_557
F1 K1 Ti1 119.72(4) 6_556 7_557
F1 K1 Ti1 85.37(4) . 7_557
O5 K1 Ti1 175.07(4) 2_657 7_557
O6 K1 Ti1 134.00(4) . 7_557
O3 K1 Ti1 89.44(5) 1_556 7_557
O4 K1 Ti1 33.05(3) 7_557 7_557
O1 K1 Ti1 32.44(3) 7_557 7_557
O3 K1 Ti1 77.32(4) 4_546 7_557
P1 K1 Ti1 159.22(3) . 7_557
F1 K1 P2 79.42(4) 7_557 4_546
F1 K1 P2 93.45(4) 6_556 4_546
F1 K1 P2 76.47(4) . 4_546
O5 K1 P2 124.20(5) 2_657 4_546
O6 K1 P2 123.59(4) . 4_546
O3 K1 P2 139.40(4) 1_556 4_546
O4 K1 P2 64.67(4) 7_557 4_546
O1 K1 P2 24.30(3) 7_557 4_546
O3 K1 P2 24.48(3) 4_546 4_546
P1 K1 P2 130.78(3) . 4_546
Ti1 K1 P2 54.87(2) 7_557 4_546
F1 K1 H1A 90.1 7_557 .
F1 K1 H1A 96.0 6_556 .
F1 K1 H1A 98.9 . .
O5 K1 H1A 65.6 2_657 .
O6 K1 H1A 57.8 . .
O3 K1 H1A 36.7 1_556 .
O4 K1 H1A 110.7 7_557 .
O1 K1 H1A 145.3 7_557 .
O3 K1 H1A 166.0 4_546 .
P1 K1 H1A 55.8 . .
Ti1 K1 H1A 115.8 7_557 .
P2 K1 H1A 169.5 4_546 .
F1 K1 H1B 123.9 7_557 .
F1 K1 H1B 91.3 6_556 .
F1 K1 H1B 55.0 . .
O5 K1 H1B 45.0 2_657 .
O6 K1 H1B 29.2 . .
O3 K1 H1B 119.6 1_556 .
O4 K1 H1B 165.6 7_557 .
O1 K1 H1B 114.0 7_557 .
O3 K1 H1B 89.1 4_546 .
P1 K1 H1B 31.4 . .
Ti1 K1 H1B 139.1 7_557 .
P2 K1 H1B 100.9 4_546 .
H1A K1 H1B 83.6 . .
F1 K1 H1C 12.0 7_557 .
F1 K1 H1C 153.2 6_556 .
F1 K1 H1C 65.3 . .
O5 K1 H1C 141.0 2_657 .
O6 K1 H1C 94.8 . .
O3 K1 H1C 73.5 1_556 .
O4 K1 H1C 67.4 7_557 .
O1 K1 H1C 64.4 7_557 .
O3 K1 H1C 112.7 4_546 .
P1 K1 H1C 117.4 . .
Ti1 K1 H1C 42.9 7_557 .
P2 K1 H1C 88.3 4_546 .
H1A K1 H1C 81.1 . .
H1B K1 H1C 114.6 . .
F1 K1 H1D 110.4 7_557 .
F1 K1 H1D 36.6 6_556 .
F1 K1 H1D 176.4 . .
O5 K1 H1D 80.7 2_657 .
O6 K1 H1D 126.5 . .
O3 K1 H1D 59.8 1_556 .
O4 K1 H1D 61.6 7_557 .
O1 K1 H1D 106.4 7_557 .
O3 K1 H1D 90.0 4_546 .
P1 K1 H1D 102.8 . .
Ti1 K1 H1D 94.6 7_557 .
P2 K1 H1D 100.6 4_546 .
H1A K1 H1D 84.4 . .
H1B K1 H1D 124.2 . .
H1C K1 H1D 116.9 . .
H1A N1 H1B 109.5 . .
H1A N1 H1C 108.6 . .
H1B N1 H1C 109.4 . .
H1A N1 H1D 109.5 . .
H1B N1 H1D 110.3 . .
H1C N1 H1D 109.4 . .
O6 P1 O6 109.74(14) 2_657 .
O6 P1 O5 106.30(8) 2_657 .
O6 P1 O5 110.94(9) . .
O6 P1 O5 110.94(9) 2_657 2_657
O6 P1 O5 106.30(8) . 2_657
O5 P1 O5 112.65(13) . 2_657
O6 P1 K1 53.57(6) 2_657 2_657
O6 P1 K1 118.01(7) . 2_657
O5 P1 K1 53.45(6) . 2_657
O5 P1 K1 135.66(6) 2_657 2_657
O6 P1 K1 118.01(7) 2_657 .
O6 P1 K1 53.57(6) . .
O5 P1 K1 135.66(6) . .
O5 P1 K1 53.45(6) 2_657 .
K1 P1 K1 167.61(3) 2_657 .
O4 P2 O2 111.64(9) . .
O4 P2 O1 108.19(9) . 6_565
O2 P2 O1 109.04(9) . 6_565
O4 P2 O3 109.74(9) . .
O2 P2 O3 109.22(10) . .
O1 P2 O3 108.96(10) 6_565 .
O4 P2 K1 118.52(7) . 4_556
O2 P2 K1 129.82(6) . 4_556
O1 P2 K1 54.22(6) 6_565 4_556
O3 P2 K1 55.11(7) . 4_556
P2 O1 Ti1 149.37(10) 6_566 .
P2 O1 K1 101.48(7) 6_566 7_557
Ti1 O1 K1 89.95(5) . 7_557
P2 O2 Ti1 163.16(11) . 2_656
P2 O3 K1 138.77(10) . 1_554
P2 O3 K1 100.41(9) . 4_556
K1 O3 K1 98.53(5) 1_554 4_556
P2 O3 H3 109.5 . .
K1 O3 H3 101.4 1_554 .
K1 O3 H3 103.0 4_556 .
P2 O4 Ti1 149.30(10) . .
P2 O4 K1 115.51(8) . 7_557
Ti1 O4 K1 90.73(6) . 7_557
P1 O5 Ti1 152.14(10) . 5_657
P1 O5 K1 100.96(7) . 2_657
Ti1 O5 K1 105.91(6) 5_657 2_657
P1 O6 Ti1 151.03(10) . .
P1 O6 K1 100.86(7) . .
Ti1 O6 K1 105.43(7) . .
Ti1 F1 K1 102.44(5) . 7_557
Ti1 F1 K1 111.51(6) . 6
K1 F1 K1 112.39(5) 7_557 6
Ti1 F1 K1 107.45(6) . .
K1 F1 K1 108.75(5) 7_557 .
K1 F1 K1 113.60(4) 6 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 F1 1.8828(12) .
Ti1 O2 1.8883(15) 2_656
Ti1 O6 1.9108(14) .
Ti1 O1 1.9142(14) .
Ti1 O5 1.9304(15) 5_657
Ti1 O4 1.9467(14) .
Ti1 K1 3.5689(11) 7_557
Ti1 K1 3.8154(11) .
Ti1 K1 3.8379(11) 6
K1 F1 2.6532(14) 7_557
K1 F1 2.7245(14) 6_556
K1 F1 2.8015(15) .
K1 O5 2.8298(18) 2_657
K1 O6 2.8331(18) .
K1 O3 2.8594(19) 1_556
K1 O4 2.9663(18) 7_557
K1 O1 3.014(2) 7_557
K1 O3 3.036(2) 4_546
K1 P1 3.4582(10) .
K1 Ti1 3.5689(11) 7_557
K1 P2 3.6406(14) 4_546
K1 H1A 1.2419 .
K1 H1B 0.8091 .
K1 H1C 0.8594 .
K1 H1D 0.7877 .
N1 H1A 0.8600 .
N1 H1B 0.8597 .
N1 H1C 0.8604 .
N1 H1D 0.8598 .
P1 O6 1.5199(15) 2_657
P1 O6 1.5199(15) .
P1 O5 1.5213(15) .
P1 O5 1.5213(15) 2_657
P1 K1 3.4582(10) 2_657
P2 O4 1.5257(15) .
P2 O2 1.5257(16) .
P2 O1 1.5289(15) 6_565
P2 O3 1.5336(16) .
P2 K1 3.6406(14) 4_556
O1 P2 1.5289(15) 6_566
O1 K1 3.014(2) 7_557
O2 Ti1 1.8883(15) 2_656
O3 K1 2.8594(19) 1_554
O3 K1 3.036(2) 4_556
O3 H3 0.8200 .
O4 K1 2.9663(18) 7_557
O5 Ti1 1.9304(14) 5_657
O5 K1 2.8298(18) 2_657
F1 K1 2.6532(14) 7_557
F1 K1 2.7245(14) 6
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3 O3 0.82 1.74 2.496(3) 153.5 7_556
