# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_K-TPHAP_water
_database_code_depnum_ccdc_archive 'CCDC 952977'
_audit_update_record             
;
2013-07-29 deposited with the CCDC.
2015-03-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H12 K N9 O1.94'
_chemical_formula_weight         472.51

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   P4(2)/n

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y, x+1/2, z+1/2'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y, -x-1/2, -z-1/2'
'-y-1/2, x, -z-1/2'

_cell_length_a                   20.9259(10)
_cell_length_b                   20.9259(10)
_cell_length_c                   9.6322(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4217.9(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      4.655
_cell_measurement_theta_max      51.311

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1932
_exptl_absorpt_coefficient_mu    0.294
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9600
_exptl_absorpt_correction_T_max  0.9656
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         
'microfocus source 30W maximum continuous power'
_diffrn_radiation_monochromator  'Wuazar(TM) Montel multilayer optic'
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            70522
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.38
_diffrn_reflns_theta_max         29.42
_reflns_number_total             5803
_reflns_number_gt                3523
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2 sofware Suite'
_computing_cell_refinement       'Bruker APEX2 sofware Suite'
_computing_data_reduction        'Bruker APEX2 sofware Suite'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker APEX2 sofware Suite'
_computing_publication_material  'Bruker APEX2 sofware Suite'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1099P)²+11.9337P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5803
_refine_ls_number_parameters     327
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1356
_refine_ls_R_factor_gt           0.0879
_refine_ls_wR_factor_ref         0.2823
_refine_ls_wR_factor_gt          0.2505
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
K1 K 0.33809(4) 0.98095(5) 0.14419(9) 0.0426(3) Uani 1 1 d . . .
C1 C 0.2749(2) 0.88904(19) -0.2552(4) 0.0370(9) Uani 1 1 d . A .
C2 C 0.2267(2) 0.9077(2) -0.1657(4) 0.0434(10) Uani 1 1 d . . .
H2 H 0.2343 0.9388 -0.0988 0.052 Uiso 1 1 calc R . .
C3 C 0.1665(2) 0.8793(2) -0.1769(5) 0.0474(11) Uani 1 1 d . . .
H3 H 0.1347 0.8920 -0.1153 0.057 Uiso 1 1 calc R . .
C4 C 0.2605(2) 0.8423(2) -0.3522(6) 0.0517(12) Uani 1 1 d . . .
H4 H 0.2917 0.8281 -0.4137 0.062 Uiso 1 1 calc R . .
C5 C 0.1999(3) 0.8172(3) -0.3566(7) 0.0659(16) Uani 1 1 d . . .
H5 H 0.1913 0.7860 -0.4227 0.079 Uiso 1 1 calc R . .
C6 C 0.3397(2) 0.91947(19) -0.2501(4) 0.0365(9) Uani 1 1 d . . .
C7 C 0.4842(2) 1.1258(2) 0.0210(4) 0.0425(10) Uani 1 1 d . A .
C8 C 0.5422(2) 1.1574(2) 0.0254(5) 0.0473(11) Uani 1 1 d . . .
H8 H 0.5756 1.1449 -0.0323 0.057 Uiso 1 1 calc R . .
C9 C 0.5501(3) 1.2076(2) 0.1164(5) 0.0549(12) Uani 1 1 d . . .
H9 H 0.5895 1.2282 0.1186 0.066 Uiso 1 1 calc R . .
C10 C 0.4361(3) 1.1475(2) 0.1088(5) 0.0525(12) Uani 1 1 d . . .
H10 H 0.3962 1.1281 0.1088 0.063 Uiso 1 1 calc R . .
C11 C 0.4485(3) 1.1983(2) 0.1960(6) 0.0626(15) Uani 1 1 d . . .
H11 H 0.4159 1.2123 0.2543 0.075 Uiso 1 1 calc R . .
C12 C 0.4734(2) 1.07031(19) -0.0745(4) 0.0405(9) Uani 1 1 d . . .
C13 C 0.59421(19) 0.91660(19) -0.5118(4) 0.0360(9) Uani 1 1 d . . .
C14 C 0.5855(2) 0.8655(2) -0.6015(7) 0.0613(15) Uani 1 1 d . . .
H14 H 0.5474 0.8426 -0.6008 0.074 Uiso 1 1 calc R . .
C15 C 0.6340(3) 0.8491(3) -0.6918(9) 0.094(3) Uani 1 1 d . . .
H15 H 0.6269 0.8152 -0.7524 0.112 Uiso 1 1 calc R . .
C16 C 0.6527(2) 0.9479(2) -0.5195(5) 0.0397(9) Uani 1 1 d . . .
H16 H 0.6610 0.9825 -0.4615 0.048 Uiso 1 1 calc R . .
C17 C 0.6979(2) 0.9279(2) -0.6121(6) 0.0538(13) Uani 1 1 d . . .
H17 H 0.7364 0.9501 -0.6158 0.065 Uiso 1 1 calc R . .
C18 C 0.54226(18) 0.93736(18) -0.4166(4) 0.0331(8) Uani 1 1 d . . .
C19 C 0.43963(19) 0.92609(18) -0.3416(4) 0.0327(8) Uani 1 1 d . . .
C20 C 0.4042(2) 0.9957(2) -0.1556(4) 0.0378(9) Uani 1 1 d . A .
C21 C 0.4518(2) 0.97625(19) -0.2491(4) 0.0355(8) Uani 1 1 d . A .
C22 C 0.5113(2) 1.00592(18) -0.2452(4) 0.0358(9) Uani 1 1 d . . .
N1 N 0.15233(18) 0.8350(2) -0.2712(5) 0.0533(10) Uani 1 1 d . . .
N2 N 0.5044(2) 1.22824(19) 0.2012(4) 0.0564(11) Uani 1 1 d . . .
N3 N 0.6900(2) 0.8782(3) -0.6980(8) 0.093(2) Uani 1 1 d . . .
N4 N 0.38175(16) 0.89792(17) -0.3451(3) 0.0356(7) Uani 1 1 d . A .
N5 N 0.34697(18) 0.96484(17) -0.1533(4) 0.0397(8) Uani 1 1 d . A .
N6 N 0.41510(18) 1.04367(18) -0.0674(4) 0.0425(8) Uani 1 1 d . A .
N7 N 0.52260(17) 1.05444(16) -0.1553(3) 0.0368(8) Uani 1 1 d . . .
N8 N 0.55849(16) 0.98545(15) -0.3296(3) 0.0337(7) Uani 1 1 d . . .
N9 N 0.48643(16) 0.90682(16) -0.4285(3) 0.0348(7) Uani 1 1 d . A .
O1A O 0.2861(3) 1.0954(3) 0.0269(7) 0.084(3) Uani 0.747(14) 1 d P A 1
O1B O 0.2949(15) 1.1241(17) 0.168(3) 0.151(14) Uani 0.253(14) 1 d P A -1
O2 O 0.2736(7) 1.2029(11) -0.0765(19) 0.175(12) Uani 0.436(19) 1 d P . .
O3 O 0.2827(11) 1.2283(12) 0.127(2) 0.220(10) Uani 0.50 1 d P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
K1 0.0347(5) 0.0633(6) 0.0297(4) -0.0088(4) 0.0047(3) -0.0024(4)
C1 0.039(2) 0.037(2) 0.035(2) 0.0049(16) -0.0004(17) 0.0035(16)
C2 0.049(2) 0.051(3) 0.030(2) 0.0029(18) 0.0016(18) 0.001(2)
C3 0.049(3) 0.054(3) 0.039(2) 0.011(2) 0.004(2) 0.009(2)
C4 0.035(2) 0.051(3) 0.069(3) -0.018(2) 0.008(2) 0.0063(19)
C5 0.046(3) 0.057(3) 0.095(5) -0.030(3) 0.010(3) 0.006(2)
C6 0.042(2) 0.039(2) 0.0280(19) 0.0016(16) 0.0000(16) 0.0023(17)
C7 0.060(3) 0.034(2) 0.033(2) 0.0002(17) -0.0070(19) 0.0030(19)
C8 0.057(3) 0.044(2) 0.041(2) -0.0061(19) -0.006(2) 0.004(2)
C9 0.073(3) 0.042(2) 0.050(3) -0.010(2) -0.012(2) 0.005(2)
C10 0.069(3) 0.041(2) 0.048(3) -0.003(2) 0.006(2) -0.001(2)
C11 0.090(4) 0.045(3) 0.053(3) -0.012(2) 0.017(3) -0.001(3)
C12 0.057(3) 0.032(2) 0.033(2) 0.0019(16) -0.0049(19) 0.0009(18)
C13 0.037(2) 0.0310(19) 0.040(2) 0.0013(16) -0.0049(17) 0.0004(15)
C14 0.040(2) 0.046(3) 0.099(4) -0.028(3) 0.005(3) -0.004(2)
C15 0.042(3) 0.075(4) 0.164(7) -0.076(5) 0.020(4) -0.008(3)
C16 0.038(2) 0.041(2) 0.040(2) -0.0012(17) -0.0057(17) -0.0007(17)
C17 0.030(2) 0.057(3) 0.075(3) -0.018(3) 0.003(2) -0.0035(19)
C18 0.0343(19) 0.0320(19) 0.033(2) 0.0028(15) -0.0054(15) -0.0004(15)
C19 0.039(2) 0.0328(18) 0.0265(18) 0.0034(14) -0.0047(15) -0.0006(15)
C20 0.049(2) 0.037(2) 0.0270(19) 0.0033(16) 0.0022(17) -0.0002(17)
C21 0.044(2) 0.037(2) 0.0253(18) 0.0008(15) -0.0032(16) 0.0000(16)
C22 0.046(2) 0.0303(18) 0.0308(19) 0.0041(15) -0.0056(17) 0.0002(16)
N1 0.0366(19) 0.049(2) 0.074(3) 0.000(2) 0.0022(19) 0.0061(17)
N2 0.085(3) 0.037(2) 0.047(2) -0.0062(17) -0.001(2) -0.001(2)
N3 0.041(2) 0.089(4) 0.150(6) -0.073(4) 0.024(3) -0.007(2)
N4 0.0379(17) 0.0419(18) 0.0270(16) 0.0003(13) -0.0032(13) -0.0011(14)
N5 0.047(2) 0.0422(19) 0.0294(17) -0.0015(14) 0.0017(14) -0.0024(16)
N6 0.053(2) 0.044(2) 0.0304(18) -0.0036(15) 0.0007(15) -0.0010(16)
N7 0.0444(19) 0.0318(16) 0.0343(18) -0.0014(13) -0.0051(14) -0.0007(14)
N8 0.0411(18) 0.0263(15) 0.0339(17) 0.0016(13) -0.0051(14) 0.0008(13)
N9 0.0370(17) 0.0360(17) 0.0314(17) -0.0011(13) -0.0053(13) -0.0012(13)
O1A 0.076(4) 0.102(5) 0.074(5) 0.000(3) 0.010(3) 0.033(3)
O1B 0.14(2) 0.18(3) 0.13(3) 0.01(2) -0.042(19) 0.04(2)
O2 0.091(11) 0.29(3) 0.140(16) -0.094(16) -0.005(10) 0.044(12)
O3 0.24(2) 0.28(3) 0.145(14) -0.053(16) -0.038(14) 0.099(19)

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
K1 N2 2.756(4) 7_476 ?
K1 O1A 2.863(6) . ?
K1 N5 2.891(4) . ?
K1 N8 2.893(3) 5_675 ?
K1 N1 2.906(4) 4_465 ?
K1 N6 2.911(4) . ?
K1 N7 3.010(4) 5_675 ?
K1 O1B 3.14(3) . ?
K1 C20 3.216(4) . ?
K1 C22 3.311(4) 5_675 ?
C1 C2 1.384(6) . ?
C1 C4 1.385(6) . ?
C1 C6 1.499(6) . ?
C2 C3 1.397(7) . ?
C3 N1 1.332(6) . ?
C4 C5 1.374(7) . ?
C5 N1 1.343(6) . ?
C6 N5 1.340(5) . ?
C6 N4 1.346(5) . ?
C7 C8 1.384(7) . ?
C7 C10 1.391(7) . ?
C7 C12 1.498(6) . ?
C8 C9 1.379(6) . ?
C9 N2 1.330(7) . ?
C10 C11 1.378(7) . ?
C11 N2 1.328(7) . ?
C12 N7 1.333(6) . ?
C12 N6 1.343(6) . ?
C13 C14 1.386(6) . ?
C13 C16 1.390(6) . ?
C13 C18 1.487(6) . ?
C14 C15 1.381(8) . ?
C15 N3 1.322(7) . ?
C16 C17 1.367(6) . ?
C17 N3 1.339(7) . ?
C18 N9 1.337(5) . ?
C18 N8 1.353(5) . ?
C19 N4 1.347(5) . ?
C19 N9 1.350(5) . ?
C19 C21 1.400(5) . ?
C20 N6 1.335(5) . ?
C20 N5 1.360(6) . ?
C20 C21 1.404(6) . ?
C21 C22 1.390(6) . ?
C22 N8 1.349(5) . ?
C22 N7 1.356(5) . ?
C22 K1 3.311(4) 5_675 ?
N1 K1 2.906(4) 3_654 ?
N2 K1 2.756(4) 8_766 ?
N7 K1 3.010(4) 5_675 ?
N8 K1 2.893(3) 5_675 ?
O1A O1B 1.50(3) . ?
O3 O3 1.64(4) 2_575 ?

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
N2 K1 O1A 78.64(16) 7_476 . ?
N2 K1 N5 127.02(12) 7_476 . ?
O1A K1 N5 74.40(15) . . ?
N2 K1 N8 105.26(12) 7_476 5_675 ?
O1A K1 N8 108.93(16) . 5_675 ?
N5 K1 N8 126.31(10) . 5_675 ?
N2 K1 N1 86.38(14) 7_476 4_465 ?
O1A K1 N1 154.82(17) . 4_465 ?
N5 K1 N1 99.63(12) . 4_465 ?
N8 K1 N1 94.41(11) 5_675 4_465 ?
N2 K1 N6 142.16(13) 7_476 . ?
O1A K1 N6 63.69(14) . . ?
N5 K1 N6 47.39(10) . . ?
N8 K1 N6 84.76(10) 5_675 . ?
N1 K1 N6 129.90(12) 4_465 . ?
N2 K1 N7 144.70(12) 7_476 5_675 ?
O1A K1 N7 126.01(15) . 5_675 ?
N5 K1 N7 86.80(10) . 5_675 ?
N8 K1 N7 46.63(9) 5_675 5_675 ?
N1 K1 N7 77.03(11) 4_465 5_675 ?
N6 K1 N7 66.40(10) . 5_675 ?
N2 K1 O1B 67.3(6) 7_476 . ?
O1A K1 O1B 28.4(5) . . ?
N5 K1 O1B 101.7(6) . . ?
N8 K1 O1B 86.5(5) 5_675 . ?
N1 K1 O1B 152.8(6) 4_465 . ?
N6 K1 O1B 77.3(6) . . ?
N7 K1 O1B 120.7(6) 5_675 . ?
N2 K1 C20 146.40(13) 7_476 . ?
O1A K1 C20 74.27(14) . . ?
N5 K1 C20 25.01(10) . . ?
N8 K1 C20 102.09(11) 5_675 . ?
N1 K1 C20 110.70(12) 4_465 . ?
N6 K1 C20 24.51(10) . . ?
N7 K1 C20 68.85(10) 5_675 . ?
O1B K1 C20 95.6(6) . . ?
N2 K1 C22 128.76(12) 7_476 5_675 ?
O1A K1 C22 114.10(16) . 5_675 ?
N5 K1 C22 103.88(11) . 5_675 ?
N8 K1 C22 23.93(10) 5_675 5_675 ?
N1 K1 C22 91.07(11) 4_465 5_675 ?
N6 K1 C22 68.98(10) . 5_675 ?
N7 K1 C22 24.17(9) 5_675 5_675 ?
O1B K1 C22 100.0(6) . 5_675 ?
C20 K1 C22 81.18(11) . 5_675 ?
C2 C1 C4 117.5(4) . . ?
C2 C1 C6 121.3(4) . . ?
C4 C1 C6 121.2(4) . . ?
C1 C2 C3 119.3(4) . . ?
N1 C3 C2 123.3(4) . . ?
C5 C4 C1 119.4(4) . . ?
N1 C5 C4 124.0(5) . . ?
N5 C6 N4 129.5(4) . . ?
N5 C6 C1 115.2(4) . . ?
N4 C6 C1 115.2(3) . . ?
C8 C7 C10 117.3(4) . . ?
C8 C7 C12 121.5(4) . . ?
C10 C7 C12 121.2(4) . . ?
C9 C8 C7 119.3(5) . . ?
N2 C9 C8 123.4(5) . . ?
C11 C10 C7 119.2(5) . . ?
N2 C11 C10 123.5(5) . . ?
N7 C12 N6 128.9(4) . . ?
N7 C12 C7 115.8(4) . . ?
N6 C12 C7 115.3(4) . . ?
C14 C13 C16 116.5(4) . . ?
C14 C13 C18 120.9(4) . . ?
C16 C13 C18 122.6(4) . . ?
C15 C14 C13 119.2(5) . . ?
N3 C15 C14 124.4(5) . . ?
C17 C16 C13 120.0(4) . . ?
N3 C17 C16 123.7(4) . . ?
N9 C18 N8 128.9(4) . . ?
N9 C18 C13 116.5(3) . . ?
N8 C18 C13 114.6(3) . . ?
N4 C19 N9 120.4(3) . . ?
N4 C19 C21 120.5(4) . . ?
N9 C19 C21 119.1(4) . . ?
N6 C20 N5 119.9(4) . . ?
N6 C20 C21 120.3(4) . . ?
N5 C20 C21 119.9(4) . . ?
N6 C20 K1 64.8(2) . . ?
N5 C20 K1 64.0(2) . . ?
C21 C20 K1 148.6(3) . . ?
C22 C21 C19 121.0(4) . . ?
C22 C21 C20 119.3(4) . . ?
C19 C21 C20 119.7(4) . . ?
N8 C22 N7 119.6(4) . . ?
N8 C22 C21 119.8(4) . . ?
N7 C22 C21 120.5(4) . . ?
N8 C22 K1 60.4(2) . 5_675 ?
N7 C22 K1 65.4(2) . 5_675 ?
C21 C22 K1 153.7(3) . 5_675 ?
C3 N1 C5 116.4(4) . . ?
C3 N1 K1 112.9(3) . 3_654 ?
C5 N1 K1 123.1(4) . 3_654 ?
C11 N2 C9 117.3(4) . . ?
C11 N2 K1 120.8(3) . 8_766 ?
C9 N2 K1 121.4(3) . 8_766 ?
C15 N3 C17 116.1(5) . . ?
C6 N4 C19 115.1(3) . . ?
C6 N5 C20 115.1(4) . . ?
C6 N5 K1 140.0(3) . . ?
C20 N5 K1 91.0(2) . . ?
C20 N6 C12 115.8(4) . . ?
C20 N6 K1 90.7(2) . . ?
C12 N6 K1 136.5(3) . . ?
C12 N7 C22 115.1(4) . . ?
C12 N7 K1 142.1(3) . 5_675 ?
C22 N7 K1 90.5(2) . 5_675 ?
C22 N8 C18 115.2(3) . . ?
C22 N8 K1 95.7(2) . 5_675 ?
C18 N8 K1 138.7(2) . 5_675 ?
C18 N9 C19 116.0(3) . . ?
O1B O1A K1 86.0(12) . . ?
O1A O1B K1 65.6(12) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        29.42
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.087
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1_day-dried_KTPHAP_powder_3
_database_code_depnum_ccdc_archive 'CCDC 1031002'
_audit_update_record             
;
2014-10-25 deposited with the CCDC.
2015-03-19 downloaded from the CCDC.
;

#==============================================================================

# If more than one structure is reported, sections 5-10 should be completed 
# per structure. For each data set, replace the '?' in the data_? line below
# by a unique identifier.

#==============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C22 N9 O2 K1'
_chemical_formula_weight         460.98
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and 
# natural products

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_length_neutron # include if applicable
? ? ? ? ? ?

#==============================================================================

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 2/a'
_space_group_name_Hall           ?
_symmetry_space_group_name_H-M   'P 2/a'
_symmetry_Int_Tables_number      13

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z
3 -x+1/2,y,-z
4 x+1/2,-y,z

_cell_length_a                   20.904(11)
_cell_length_b                   15.931(10)
_cell_length_c                   9.711(5)
_cell_angle_alpha                90
_cell_angle_beta                 104.65(3)
_cell_angle_gamma                90
_cell_volume                     3128(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    298

_cell_special_details            
; ?
;

# The next three fields give the specimen dimensions in mm.  The equatorial 
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              20 # perpendicular to 
# equatorial plane

_pd_spec_size_equat              20 # parallel to 
# scattering vector 
# in transmission

_pd_spec_size_thick              0.5 # parallel to 
# scattering vector 
# in reflection

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
# This field should be
# used to give details of the 
# container.
; ?
;
_pd_spec_mount_mode              reflection # options are 'reflection' 
# or 'transmission'

_pd_spec_shape                   flat_sheet # options are 'cylinder' 
# 'flat_sheet' or 'irregular'

_pd_char_particle_morphology     ?
_pd_char_colour                  'pale yellow'


# The following three fields describe the preparation of the specimen.   
# The cooling rate is in K/min.  The pressure at which the sample was  
# prepared is in kPa.  The temperature of preparation is in K.

_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             ?

# The next four fields are normally only needed for transmission experiments.
_exptl_absorpt_coefficient_mu    ?
_exptl_absorpt_correction_type   ? # include if applicable
_exptl_absorpt_process_details   ? # include if applicable
_exptl_absorpt_correction_T_min  ? # include if applicable
_exptl_absorpt_correction_T_max  ? # include if applicable

#==============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# The following item is used to identify the equipment used to record 
# the powder pattern when the diffractogram was measured at a laboratory 
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ?
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; ?
;

_diffrn_ambient_temperature      298
_diffrn_source                   Conventional
_diffrn_source_target            Cu
_diffrn_source_type              'Sealed tube'
_diffrn_radiation_type           'Cu K_alpha radiation'
_diffrn_measurement_device_type  'D8 ADVANCE'
_diffrn_detector                 Scintillation
_diffrn_detector_type            LynxEye # make or model of detector

_pd_meas_scan_method             step # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
;  A air-tight dorm type cell was used to set up sample.
;

# The following six items are used for angular dispersive measurements only.

_diffrn_radiation_wavelength     1.5406
_diffrn_radiation_monochromator  'Ge 111'

#  The following four items give details of the measured (not processed)
#  powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        2555
_pd_meas_2theta_range_min        3.0000
_pd_meas_2theta_range_max        49.9971
_pd_meas_2theta_range_inc        0.0184

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          ?
_pd_instr_dist_spec/detc         ?
_pd_meas_2theta_fixed            ?


#==============================================================================

# 8. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
; ?
;

# The next three items are given as text.

_pd_proc_ls_profile_function     'Modified split pseudo-Voigt function'
_pd_proc_ls_background_function  'Refine background parameters'
_pd_proc_ls_pref_orient_corr     
; ?
;

_pd_proc_ls_prof_R_factor        0.03043
_pd_proc_ls_prof_wR_factor       0.04847
_pd_proc_ls_prof_wR_expected     0.07351
_refine_ls_R_I_factor            0.01002
_refine_ls_R_Fsqd_factor         0.00953
_refine_ls_R_factor_all          0.01443

_refine_special_details          
; ?
;

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     185
_refine_ls_number_restraints     160
_refine_ls_number_constraints    0

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   0.6594
_refine_ls_restrained_S_all      ?
_refine_ls_shift/su_max          1.0E-6
_refine_ls_shift/su_mean         ?

# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the 
# intensities used in the refinement.

_pd_proc_2theta_range_min        ?
_pd_proc_2theta_range_max        ?
_pd_proc_2theta_range_inc        ?
_pd_proc_wavelength              ?

# Each refinement must be accompanied by a listing of the powder data
# in CIF format. Each listing should be sent as a separate file consisting 
# of one data block containing a single powder profile. The value of 
# _pd_block_diffractogram_id is used to associate each refinement with 
# its corresponding powder profile, since it must match the value
# of _pd_block_id in the file containing the powder data. A template 
# for supplying powder data in CIF format is available by ftp at
# ftp://ftp.iucr.org/pub/rietdataform.cif and an example is given 
# at ftp://ftp.iucr.org/pub/rietdataxmpl.cif.

_pd_block_diffractogram_id       '1 d-dried_3'


# Give appropriate details in the next two text fields.

_pd_proc_info_excluded_regions   49.4446-49.9971
_pd_proc_info_data_reduction     ?

# The following items are used to identify the programs used.

_computing_data_collection       'DIFFRAC plus'
_computing_cell_refinement       'RIETAN-FP (Izumi and Momma, 2007)'
_computing_data_reduction        ?
_computing_structure_solution    DASH
_computing_structure_refinement  'RIETAN-FP (Izumi and Momma, 2007)'
_computing_molecular_graphics    'VESTA (Momma and Izumi, 2008)'
_computing_publication_material  ?


#==============================================================================


# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_occupancy
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_B_iso_or_equiv
_atom_site_type_symbol
C1 1.0 -0.392793 0.605947 0.107742 Biso 3.000000 C
C2 1.0 -0.408291 0.688373 0.044820 Biso 3.000000 C
N3 1.0 -0.414218 0.534167 0.024613 Biso 3.000000 N
N4 1.0 -0.365460 0.595952 0.260856 Biso 3.000000 N
C5 1.0 -0.447178 0.696596 -0.110802 Biso 3.000000 C
C6 1.0 -0.396128 0.762223 0.138913 Biso 3.000000 C
C7 1.0 -0.453063 0.547538 -0.113035 Biso 3.000000 C
C8 1.0 -0.351241 0.668122 0.338552 Biso 3.000000 C
N9 1.0 -0.469814 0.623771 -0.186858 Biso 3.000000 N
N10 1.0 -0.465307 0.778011 -0.169654 Biso 3.000000 N
N11 1.0 -0.415442 0.847314 0.076853 Biso 3.000000 N
N12 1.0 -0.363733 0.752459 0.289979 Biso 3.000000 N
C13 1.0 -0.472501 0.461971 -0.204533 Biso 3.000000 C
C14 1.0 -0.321380 0.655684 0.513388 Biso 3.000000 C
C15 1.0 -0.446002 0.848522 -0.074848 Biso 3.000000 C
C16 1.0 -0.452486 0.448832 -0.335156 Biso 3.000000 C
C17 1.0 -0.498994 0.387945 -0.144509 Biso 3.000000 C
C18 1.0 -0.308775 0.575219 0.574703 Biso 3.000000 C
C19 1.0 -0.302472 0.724809 0.606456 Biso 3.000000 C
C20 1.0 -0.473662 0.936845 -0.140453 Biso 3.000000 C
C21 1.0 -0.464463 0.370456 -0.405848 Biso 3.000000 C
C22 1.0 -0.508619 0.313605 -0.224813 Biso 3.000000 C
C23 1.0 -0.277158 0.566481 0.723287 Biso 3.000000 C
C24 1.0 -0.278485 0.707575 0.755486 Biso 3.000000 C
C25 1.0 -0.436914 0.991676 -0.196141 Biso 3.000000 C
C26 1.0 -0.539465 0.962499 -0.143499 Biso 3.000000 C
N27 1.0 -0.488828 0.302740 -0.352156 Biso 3.000000 N
N28 1.0 -0.263048 0.629734 0.813256 Biso 3.000000 N
C29 1.0 -0.466683 1.065960 -0.265427 Biso 3.000000 C
C30 1.0 -0.564154 1.038150 -0.215416 Biso 3.000000 C
N31 1.0 -0.529019 1.087280 -0.281259 Biso 3.000000 N
O32 1.0 0.249961 -0.148256 0.275770 Biso 3.000000 O
O33 1.0 -0.409318 0.247311 -0.903542 Biso 3.000000 O
K34 1.0 0.821139 0.377422 -0.222506 Biso 3.000000 K



# Note: if the displacement parameters were refined anisotropically 
# the U matrices should be given as for single-crystal studies.

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
_atom_site_aniso_type_symbol
? ? ? ? ? ? ? ?

#==============================================================================


# 10. MOLECULAR GEOMETRY

_geom_special_details            ?

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
? ? ? ? ? ?

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
? ? ? ? ? ? ? ?

#==============================================================================
# Additional structures (sections 5-10 and associated data_? identifiers)
# may be added at this point.
#==============================================================================

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set.
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./                 

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1_min_dried_KTPHAP_powder
_database_code_depnum_ccdc_archive 'CCDC 1031003'
_audit_update_record             
;
2014-10-25 deposited with the CCDC.
2015-03-19 downloaded from the CCDC.
;

#==============================================================================

# If more than one structure is reported, sections 5-10 should be completed 
# per structure. For each data set, replace the '?' in the data_? line below
# by a unique identifier.

#==============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C22 N9 O6 K1'
_chemical_formula_weight         524.96
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and 
# natural products

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_length_neutron # include if applicable
? ? ? ? ? ?

#==============================================================================

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 2/a'
_space_group_name_Hall           ?
_symmetry_space_group_name_H-M   'P 2/a'
_symmetry_Int_Tables_number      13

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z
3 -x+1/2,y,-z
4 x+1/2,-y,z

_cell_length_a                   20.656(6)
_cell_length_b                   15.978(4)
_cell_length_c                   16.801(10)
_cell_angle_alpha                90
_cell_angle_beta                 100.68(3)
_cell_angle_gamma                90
_cell_volume                     5449(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    298

_cell_special_details            
; ?
;

# The next three fields give the specimen dimensions in mm.  The equatorial 
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              20 # perpendicular to 
# equatorial plane

_pd_spec_size_equat              20 # parallel to 
# scattering vector 
# in transmission

_pd_spec_size_thick              0.5 # parallel to 
# scattering vector 
# in reflection

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
# This field should be
# used to give details of the 
# container.
; ?
;
_pd_spec_mount_mode              reflection # options are 'reflection' 
# or 'transmission'

_pd_spec_shape                   flat_sheet # options are 'cylinder' 
# 'flat_sheet' or 'irregular'

_pd_char_particle_morphology     ?
_pd_char_colour                  'pale yellow'


# The following three fields describe the preparation of the specimen.   
# The cooling rate is in K/min.  The pressure at which the sample was  
# prepared is in kPa.  The temperature of preparation is in K.

_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             ?

# The next four fields are normally only needed for transmission experiments.
_exptl_absorpt_coefficient_mu    ?
_exptl_absorpt_correction_type   ? # include if applicable
_exptl_absorpt_process_details   ? # include if applicable
_exptl_absorpt_correction_T_min  ? # include if applicable
_exptl_absorpt_correction_T_max  ? # include if applicable

#==============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# The following item is used to identify the equipment used to record 
# the powder pattern when the diffractogram was measured at a laboratory 
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ?
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; ?
;

_diffrn_ambient_temperature      298
_diffrn_source                   synchrotron
_diffrn_source_target            ?
_diffrn_source_type              'bending magnet'
_diffrn_radiation_type           synchrotron
_diffrn_measurement_device_type  'Pohang Light Source 9B HRPD beamline'
_diffrn_detector                 'Na(I) Scintillation'
_diffrn_detector_type            KOUZU # make or model of detector

_pd_meas_scan_method             step # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
;  A air-tight dorm type cell was used to set up sample.
;

# The following six items are used for angular dispersive measurements only.

_diffrn_radiation_wavelength     1.4639
_diffrn_radiation_monochromator  'Si 111'

#  The following four items give details of the measured (not processed)
#  powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        14051
_pd_meas_2theta_range_min        3.50
_pd_meas_2theta_range_max        124.00
_pd_meas_2theta_range_inc        0.01

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          ?
_pd_instr_dist_spec/detc         ?
_pd_meas_2theta_fixed            ?


#==============================================================================

# 8. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
; ?
;

# The next three items are given as text.

_pd_proc_ls_profile_function     'Modified split pseudo-Voigt function'
_pd_proc_ls_background_function  'Legendre polynomials'
_pd_proc_ls_pref_orient_corr     
; ?
;

_pd_proc_ls_prof_R_factor        0.03844
_pd_proc_ls_prof_wR_factor       0.05575
_pd_proc_ls_prof_wR_expected     0.08674
_refine_ls_R_I_factor            0.00455
_refine_ls_R_Fsqd_factor         0.00497
_refine_ls_R_factor_all          0.00499

_refine_special_details          
; We attempted several numbers of water (3 to 10 molecules) and potassium ions
 (one atom with occ. = 1 or two atoms with occ. = 0.5)
  with one TPHAP as initial models.
  The best model for the structure determination was two potassium atoms
  with 0.5 occupancy factors,
  ten disordered water molecules, and two TPHAP with 0.5 occupancy factors.
  In the case of one TPHAP, we could not obtain acceptable molecular geometry,
  residual intensity and reasonable water positions
  with moderate peak intensities.
  Using two TPHAP models, firstly atomic coordinates
  of two TPHAP were refined alternatively
  and then all coordinates were refined together.
  At the final refinement, the coordinates of one of TPHAP were fixed
  to avoid strong correlation between two TPHAP parameters.
  All displacement parameters were fixed with 3.0 during refinement.
;

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     227
_refine_ls_number_restraints     360
_refine_ls_number_constraints    0

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   0.6428
_refine_ls_restrained_S_all      ?
_refine_ls_shift/su_max          1.0E-6
_refine_ls_shift/su_mean         ?

# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the 
# intensities used in the refinement.

_pd_proc_2theta_range_min        ?
_pd_proc_2theta_range_max        ?
_pd_proc_2theta_range_inc        ?
_pd_proc_wavelength              ?

# Each refinement must be accompanied by a listing of the powder data
# in CIF format. Each listing should be sent as a separate file consisting 
# of one data block containing a single powder profile. The value of 
# _pd_block_diffractogram_id is used to associate each refinement with 
# its corresponding powder profile, since it must match the value
# of _pd_block_id in the file containing the powder data. A template 
# for supplying powder data in CIF format is available by ftp at
# ftp://ftp.iucr.org/pub/rietdataform.cif and an example is given 
# at ftp://ftp.iucr.org/pub/rietdataxmpl.cif.

_pd_block_diffractogram_id       '1 min-dried'


# Give appropriate details in the next two text fields.

_pd_proc_info_excluded_regions   45.01-124.00
_pd_proc_info_data_reduction     ?

# The following items are used to identify the programs used.

_computing_data_collection       'PLS-II 9B HRPD Beamline software'
_computing_cell_refinement       'RIETAN-FP (Izumi and Momma, 2007)'
_computing_data_reduction        ?
_computing_structure_solution    DASH
_computing_structure_refinement  'RIETAN-FP (Izumi and Momma, 2007)'
_computing_molecular_graphics    'VESTA (Momma and Izumi, 2008)'
_computing_publication_material  ?


#==============================================================================


# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_occupancy
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_B_iso_or_equiv
_atom_site_type_symbol
C1 0.5000 0.108428 0.300313 0.137851 Biso 3.000000 C
C2 0.5000 0.165031 0.346489 0.163199 Biso 3.000000 C
N3 0.5000 0.086741 0.286665 0.052572 Biso 3.000000 N
N4 0.5000 0.079886 0.256147 0.197768 Biso 3.000000 N
C5 0.5000 0.198014 0.388315 0.106726 Biso 3.000000 C
C6 0.5000 0.184505 0.364446 0.250437 Biso 3.000000 C
C7 0.5000 0.123997 0.321628 0.000706 Biso 3.000000 C
C8 0.5000 0.104848 0.273288 0.277652 Biso 3.000000 C
N9 0.5000 0.178287 0.373058 0.019982 Biso 3.000000 N
N10 0.5000 0.256286 0.433089 0.137878 Biso 3.000000 N
N11 0.5000 0.243895 0.403789 0.277785 Biso 3.000000 N
N12 0.5000 0.156245 0.322084 0.306388 Biso 3.000000 N
C13 0.5000 0.101171 0.295829 -0.091195 Biso 3.000000 C
C14 0.5000 0.079176 0.218546 0.345680 Biso 3.000000 C
C15 0.5000 0.273239 0.440509 0.219068 Biso 3.000000 C
C16 0.5000 0.142199 0.305925 -0.149830 Biso 3.000000 C
C17 0.5000 0.045797 0.248416 -0.114999 Biso 3.000000 C
C18 0.5000 0.054502 0.136469 0.331522 Biso 3.000000 C
C19 0.5000 0.091056 0.245239 0.428370 Biso 3.000000 C
C20 0.5000 0.340583 0.481634 0.253837 Biso 3.000000 C
C21 0.5000 0.117890 0.274945 -0.229406 Biso 3.000000 C
C22 0.5000 0.028084 0.218821 -0.196550 Biso 3.000000 C
C23 0.5000 0.038290 0.087726 0.394580 Biso 3.000000 C
C24 0.5000 0.074277 0.194054 0.487906 Biso 3.000000 C
C25 0.5000 0.357442 0.497482 0.335555 Biso 3.000000 C
C26 0.5000 0.391172 0.489197 0.207599 Biso 3.000000 C
N27 0.5000 0.060212 0.233876 -0.253548 Biso 3.000000 N
N28 0.5000 0.050106 0.111808 0.471088 Biso 3.000000 N
C29 0.5000 0.418209 0.526090 0.367005 Biso 3.000000 C
C30 0.5000 0.451284 0.518903 0.244352 Biso 3.000000 C
N31 0.5000 0.466028 0.533871 0.324828 Biso 3.000000 N
K32 0.5000 0.770579 0.313267 -0.417967 Biso 3.000000 K
O33 0.5000 -0.239039 0.294187 0.101179 Biso 3.000000 O
O34 0.5000 -0.477625 0.791652 0.094560 Biso 3.000000 O
K35 0.5000 0.246913 -0.315382 0.225127 Biso 3.000000 K
O37 0.5000 -0.920606 -0.916457 0.709605 Biso 3.000000 O
O38 1.0 -0.639547 0.806882 -0.500118 Biso 3.000000 O
O39 0.5000 -0.659736 0.544611 1.082670 Biso 3.000000 O
O40 1.0 -0.781834 -0.009286 0.773080 Biso 3.000000 O
O41 0.5000 0.760069 -0.706837 -0.903268 Biso 3.000000 O
O42 0.0000 -0.549090 -0.753588 -0.553431 Biso 1.000000 O
C1A 0.5000 0.201032 0.271331 0.278668 Biso 3.000000 C
C2A 0.5000 0.254793 0.320438 0.305947 Biso 3.000000 C
N3A 0.5000 0.181826 0.254512 0.189271 Biso 3.000000 N
N4A 0.5000 0.159820 0.250160 0.333193 Biso 3.000000 N
C5A 0.5000 0.285838 0.362828 0.255055 Biso 3.000000 C
C6A 0.5000 0.272254 0.339662 0.395117 Biso 3.000000 C
C7A 0.5000 0.212043 0.300325 0.143840 Biso 3.000000 C
C8A 0.5000 0.181171 0.276839 0.412933 Biso 3.000000 C
N9A 0.5000 0.262336 0.355885 0.167841 Biso 3.000000 N
N10A 0.5000 0.343008 0.412961 0.289984 Biso 3.000000 N
N11A 0.5000 0.319677 0.383707 0.422498 Biso 3.000000 N
N12A 0.5000 0.235066 0.315896 0.444166 Biso 3.000000 N
C13A 0.5000 0.192317 0.286919 0.048485 Biso 3.000000 C
C14A 0.5000 0.137494 0.259598 0.473752 Biso 3.000000 C
C15A 0.5000 0.354445 0.414508 0.370211 Biso 3.000000 C
C16A 0.5000 0.239360 0.289027 0.000468 Biso 3.000000 C
C17A 0.5000 0.125365 0.283718 0.006467 Biso 3.000000 C
C18A 0.5000 0.072718 0.236973 0.452497 Biso 3.000000 C
C19A 0.5000 0.164240 0.266369 0.556347 Biso 3.000000 C
C20A 0.5000 0.413972 0.458936 0.409395 Biso 3.000000 C
C21A 0.5000 0.221309 0.280380 -0.086027 Biso 3.000000 C
C22A 0.5000 0.110663 0.277024 -0.079850 Biso 3.000000 C
C23A 0.5000 0.038891 0.219898 0.513864 Biso 3.000000 C
C24A 0.5000 0.125152 0.242824 0.608574 Biso 3.000000 C
C25A 0.5000 0.425921 0.470526 0.491502 Biso 3.000000 C
C26A 0.5000 0.461605 0.479623 0.365777 Biso 3.000000 C
N27A 0.5000 0.159292 0.277014 -0.127788 Biso 3.000000 N
N28A 0.5000 0.063805 0.216688 0.589028 Biso 3.000000 N
C29A 0.5000 0.485536 0.505751 0.529209 Biso 3.000000 C
C30A 0.5000 0.519587 0.514312 0.407133 Biso 3.000000 C
N31A 0.5000 0.535559 0.525072 0.486051 Biso 3.000000 N
O341 0.5000 -0.512256 0.762852 0.207866 Biso 3.000000 O
O371 0.5000 -0.747473 -0.834679 0.749810 Biso 3.000000 O
O391 0.5000 -0.707461 0.459617 1.044190 Biso 3.000000 O


# Note: if the displacement parameters were refined anisotropically 
# the U matrices should be given as for single-crystal studies.

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
_atom_site_aniso_type_symbol
? ? ? ? ? ? ? ?

#==============================================================================


# 10. MOLECULAR GEOMETRY

_geom_special_details            ?

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
? ? ? ? ? ?

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
? ? ? ? ? ? ? ?

#==============================================================================
# Additional structures (sections 5-10 and associated data_? identifiers)
# may be added at this point.
#==============================================================================

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set.
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./                 

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_hydrated_KTPHAP_powder_2
_database_code_depnum_ccdc_archive 'CCDC 1031004'
_audit_update_record             
;
2014-10-25 deposited with the CCDC.
2015-03-19 downloaded from the CCDC.
;

#==============================================================================

# If more than one structure is reported, sections 5-10 should be completed
# per structure. For each data set, replace the '?' in the data_? line below
# by a unique identifier.

#==============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C22 N9 O8.5 K1'
_chemical_formula_weight         565.39
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_length_neutron # include if applicable
? ? ? ? ? ?

#==============================================================================

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 2/n'
_space_group_name_Hall           ?
_symmetry_space_group_name_H-M   'P 2/n'
_symmetry_Int_Tables_number      13

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z
3 -x+1/2,y,-z+1/2
4 x+1/2,-y,z+1/2

_cell_length_a                   24.131(5)
_cell_length_b                   19.458(2)
_cell_length_c                   16.672(4)
_cell_angle_alpha                90
_cell_angle_beta                 122.52(2)
_cell_angle_gamma                90
_cell_volume                     6601(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    298

_cell_special_details            
; ?
;

# The next three fields give the specimen dimensions in mm.  The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              20 # perpendicular to
# equatorial plane

_pd_spec_size_equat              20 # parallel to
# scattering vector
# in transmission

_pd_spec_size_thick              0.5 # parallel to
# scattering vector
# in reflection

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
# This field should be
# used to give details of the
# container.
; ?
;
_pd_spec_mount_mode              reflection # options are 'reflection'
# or 'transmission'

_pd_spec_shape                   flat_sheet # options are 'cylinder'
# 'flat_sheet' or 'irregular'

_pd_char_particle_morphology     ?
_pd_char_colour                  'pale yellow'


# The following three fields describe the preparation of the specimen.
# The cooling rate is in K/min.  The pressure at which the sample was
# prepared is in kPa.  The temperature of preparation is in K.

_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             ?

# The next four fields are normally only needed for transmission experiments.
_exptl_absorpt_coefficient_mu    ?
_exptl_absorpt_correction_type   ? # include if applicable
_exptl_absorpt_process_details   ? # include if applicable
_exptl_absorpt_correction_T_min  ? # include if applicable
_exptl_absorpt_correction_T_max  ? # include if applicable

#==============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# The following item is used to identify the equipment used to record
# the powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ?
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; ?
;

_diffrn_ambient_temperature      298
_diffrn_source                   synchrotron
_diffrn_source_target            ?
_diffrn_source_type              'bending magnet'
_diffrn_radiation_type           synchrotron
_diffrn_measurement_device_type  'Pohang Light Source 9B HRPD beamline'
_diffrn_detector                 'Na(I) Scintillation'
_diffrn_detector_type            KOUZU # make or model of detector

_pd_meas_scan_method             step # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
;  A air-tight dorm type cell was used to set up sample.
;

# The following six items are used for angular dispersive measurements only.

_diffrn_radiation_wavelength     1.4639
_diffrn_radiation_monochromator  'Si 111'

#  The following four items give details of the measured (not processed)
#  powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        14051
_pd_meas_2theta_range_min        3.00
_pd_meas_2theta_range_max        123.50
_pd_meas_2theta_range_inc        0.01

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          ?
_pd_instr_dist_spec/detc         ?
_pd_meas_2theta_fixed            ?


#==============================================================================

# 8. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
; ?
;

# The next three items are given as text.

_pd_proc_ls_profile_function     'Modified split pseudo-Voigt function'
_pd_proc_ls_background_function  'Legendre polynomials'
_pd_proc_ls_pref_orient_corr     
; ?
;

_pd_proc_ls_prof_R_factor        0.07145
_pd_proc_ls_prof_wR_factor       0.10700
_pd_proc_ls_prof_wR_expected     0.10689
_refine_ls_R_I_factor            0.06738
_refine_ls_R_Fsqd_factor         0.10349
_refine_ls_R_factor_all          0.10199

_refine_special_details          
; ?
;

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     216
_refine_ls_number_restraints     165
_refine_ls_number_constraints    40

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   1.0010
_refine_ls_restrained_S_all      ?
_refine_ls_shift/su_max          1.0E-6
_refine_ls_shift/su_mean         ?

# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the
# intensities used in the refinement.

_pd_proc_2theta_range_min        ?
_pd_proc_2theta_range_max        ?
_pd_proc_2theta_range_inc        ?
_pd_proc_wavelength              ?

# Each refinement must be accompanied by a listing of the powder data
# in CIF format. Each listing should be sent as a separate file consisting
# of one data block containing a single powder profile. The value of
# _pd_block_diffractogram_id is used to associate each refinement with
# its corresponding powder profile, since it must match the value
# of _pd_block_id in the file containing the powder data. A template
# for supplying powder data in CIF format is available by ftp at
# ftp://ftp.iucr.org/pub/rietdataform.cif and an example is given
# at ftp://ftp.iucr.org/pub/rietdataxmpl.cif.

_pd_block_diffractogram_id       hydrated_2


# Give appropriate details in the next two text fields.

_pd_proc_info_excluded_regions   49.45-123.50
_pd_proc_info_data_reduction     ?

# The following items are used to identify the programs used.

_computing_data_collection       'PLS-II 9B HRPD Beamline software'
_computing_cell_refinement       'RIETAN-FP (Izumi and Momma, 2007)'
_computing_data_reduction        ?
_computing_structure_solution    DASH
_computing_structure_refinement  'RIETAN-FP (Izumi and Momma, 2007)'
_computing_molecular_graphics    'VESTA (Momma and Izumi, 2008)'
_computing_publication_material  ?


#==============================================================================


# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_occupancy
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_B_iso_or_equiv
_atom_site_type_symbol
C1 1.0 0.349499 0.412153 0.614319 Biso 5.263390 C
C2 1.0 0.393464 0.397614 0.581546 Biso 5.263390 C
N3 1.0 0.287295 0.416201 0.552824 Biso 5.263390 N
N4 1.0 0.369915 0.410436 0.704750 Biso 5.263390 N
C5 1.0 0.369779 0.406426 0.482899 Biso 5.263390 C
C6 1.0 0.454710 0.379895 0.642652 Biso 5.263390 C
C7 1.0 0.268592 0.412587 0.465027 Biso 5.263390 C
C8 1.0 0.428118 0.400632 0.760900 Biso 5.263390 C
N9 1.0 0.307635 0.410501 0.423356 Biso 5.263390 N
N10 1.0 0.409128 0.397958 0.451039 Biso 5.263390 N
N11 1.0 0.497176 0.373321 0.611404 Biso 5.263390 N
N12 1.0 0.478205 0.380841 0.739400 Biso 5.263390 N
C13 1.0 0.187741 0.409813 0.391024 Biso 5.263390 C
C14 1.0 0.448326 0.391298 0.869177 Biso 5.263390 C
C15 1.0 0.465268 0.380460 0.509003 Biso 5.263390 C
C16 1.0 0.158258 0.398724 0.294273 Biso 5.263390 C
C17 1.0 0.145245 0.408059 0.428981 Biso 5.263390 C
C18 1.0 0.399255 0.401367 0.894222 Biso 5.263390 C
C19 1.0 0.507594 0.368147 0.937799 Biso 5.263390 C
C20 1.0 0.508491 0.374529 0.469849 Biso 5.263390 C
C21 1.0 0.087867 0.390289 0.237133 Biso 5.263390 C
C22 1.0 0.078215 0.398491 0.368206 Biso 5.263390 C
C23 1.0 0.417033 0.395312 0.988774 Biso 5.263390 C
C24 1.0 0.520115 0.361698 1.031270 Biso 5.263390 C
C25 1.0 0.573912 0.356016 0.524908 Biso 5.263390 C
C26 1.0 0.482226 0.388176 0.373483 Biso 5.263390 C
N27 1.0 0.049325 0.386491 0.273987 Biso 5.263390 N
N28 1.0 0.475838 0.378234 1.057150 Biso 5.263390 N
C29 1.0 0.612965 0.353917 0.483019 Biso 5.263390 C
C30 1.0 0.523570 0.389234 0.337734 Biso 5.263390 C
N31 1.0 0.589601 0.375577 0.391882 Biso 5.263390 N
K32 0.5000 0.761229 0.476074 0.167225 Biso 2.059050 K
K33 0.5000 0.051597 0.164900 0.845807 Biso 2.059050 K
O34 1.0 0.248836 0.982115 1.026430 Biso 2.059050 O
O35 1.0 0.536287 -0.905887 -0.651930 Biso 2.059050 O
O36 1.0 0.542359 -0.939988 -0.469615 Biso 2.059050 O
O37 0.5000 0.234681 -0.690840 -0.321975 Biso 2.059050 O
O39 1.0 0.009673 0.150285 0.142867 Biso 2.059050 O
O40 1.0 0.250116 0.976421 -0.414692 Biso 2.059050 O
O41 1.0 0.744010 0.469980 0.943696 Biso 2.059050 O
O42 1.0 -0.682345 0.791644 0.625899 Biso 2.059050 O
O43 1.0 -0.256364 -0.960117 -0.363925 Biso 2.059050 O



# Note: if the displacement parameters were refined anisotropically
# the U matrices should be given as for single-crystal studies.

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
_atom_site_aniso_type_symbol
? ? ? ? ? ? ? ?

#==============================================================================


# 10. MOLECULAR GEOMETRY

_geom_special_details            ?

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
? ? ? ? ? ?

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
? ? ? ? ? ? ? ?

#==============================================================================
# Additional structures (sections 5-10 and associated data_? identifiers)
# may be added at this point.
#==============================================================================

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set.
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./


