# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_TiHPO3
_database_code_depnum_ccdc_archive 'CCDC 1019743'
loop_
_audit_author_name
_audit_author_address
'Junbiao Wu'
;northeastern university
China
;
_audit_update_record             
;
2019-07-31 deposited with the CCDC.	2019-09-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'H2 O6 P2 Ti'
_chemical_formula_weight         207.86

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'
H H 0.0000 0.0000 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   4.8518(3)
_cell_length_b                   8.1747(5)
_cell_length_c                   6.8142(4)
_cell_angle_alpha                90
_cell_angle_beta                 105.4680(10)
_cell_angle_gamma                90
_cell_volume                     260.48(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1155
_cell_measurement_theta_min      3.9801
_cell_measurement_theta_max      28.1927

_exptl_crystal_description       Block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.650
_exptl_crystal_F_000             204
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    2.208
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.6422
_exptl_absorpt_correction_T_max  0.6919
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  Bruker
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1833
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.980
_diffrn_reflns_theta_max         28.216
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             643
_reflns_number_gt                602
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0316P)²+0.3526P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         643
_refine_ls_number_parameters     47
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0233
_refine_ls_wR_factor_ref         0.0681
_refine_ls_wR_factor_gt          0.0672
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_restrained_S_all      1.160
_refine_ls_shift/su_max          0.001
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.0000 0.0000 0.5000 0.00893(16) Uani 1 2 d S . P . .
P1 P 0.11179(12) -0.34689(7) 0.27450(8) 0.00999(17) Uani 1 1 d . . . . .
O2 O 0.0767(4) -0.1686(2) 0.3277(3) 0.0191(4) Uani 1 1 d . . . . .
O3 O 0.2626(4) -0.3526(2) 0.1049(3) 0.0169(4) Uani 1 1 d . . . . .
O4 O -0.1725(4) -0.4359(2) 0.2191(3) 0.0189(4) Uani 1 1 d . . . . .
H1 H 0.266(6) -0.415(4) 0.443(4) 0.016(7) Uiso 1 1 d . . . . .

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
Ti1 0.0110(3) 0.0066(3) 0.0116(3) 0.00039(18) 0.0072(2) 0.00074(18)
P1 0.0105(3) 0.0097(3) 0.0104(3) -0.00177(18) 0.0039(2) 0.00080(19)
O2 0.0257(9) 0.0122(8) 0.0245(9) -0.0067(6) 0.0157(8) 0.0003(7)
O3 0.0203(9) 0.0145(8) 0.0210(8) -0.0020(6) 0.0142(7) 0.0028(6)
O4 0.0161(8) 0.0237(9) 0.0174(8) -0.0046(7) 0.0051(6) -0.0074(7)

_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
Ti1 O2 1.9101(16) 3_556 ?
Ti1 O2 1.9101(16) . ?
Ti1 O3 1.9315(16) 4_556 ?
Ti1 O3 1.9315(16) 2 ?
Ti1 O4 1.9399(16) 4_656 ?
Ti1 O4 1.9399(16) 2_455 ?
P1 O4 1.5152(17) . ?
P1 O2 1.5227(16) . ?
P1 O3 1.5242(16) . ?
P1 H1 1.32(3) . ?
O3 Ti1 1.9315(16) 2_545 ?
O4 Ti1 1.9399(16) 2_445 ?

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
O2 Ti1 O2 180.0 3_556 . ?
O2 Ti1 O3 89.40(7) 3_556 4_556 ?
O2 Ti1 O3 90.60(7) . 4_556 ?
O2 Ti1 O3 90.60(7) 3_556 2 ?
O2 Ti1 O3 89.40(7) . 2 ?
O3 Ti1 O3 180.0 4_556 2 ?
O2 Ti1 O4 88.63(8) 3_556 4_656 ?
O2 Ti1 O4 91.37(8) . 4_656 ?
O3 Ti1 O4 89.63(8) 4_556 4_656 ?
O3 Ti1 O4 90.37(8) 2 4_656 ?
O2 Ti1 O4 91.37(8) 3_556 2_455 ?
O2 Ti1 O4 88.63(8) . 2_455 ?
O3 Ti1 O4 90.37(8) 4_556 2_455 ?
O3 Ti1 O4 89.63(8) 2 2_455 ?
O4 Ti1 O4 180.0 4_656 2_455 ?
O4 P1 O2 111.52(10) . . ?
O4 P1 O3 112.67(10) . . ?
O2 P1 O3 108.44(9) . . ?
O4 P1 H1 106.5(13) . . ?
O2 P1 H1 105.5(13) . . ?
O3 P1 H1 111.9(12) . . ?
P1 O2 Ti1 152.82(12) . . ?
P1 O3 Ti1 138.92(11) . 2_545 ?
P1 O4 Ti1 145.68(11) . 2_445 ?

_refine_diff_density_max         0.290
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.107

_shelx_res_file                  
;

    c.res created by SHELXL-2014/7


TITL TiHPO3 in P2(1)/n
CELL 0.71073   4.8518   8.1747   6.8142  90.000 105.468  90.000
ZERR    2.00   0.0003   0.0005   0.0004   0.000   0.001   0.000
LATT  1
SYMM 0.5-X, 0.5+Y, 0.5-Z
SFAC O H P TI
UNIT 12  4 4 2
TEMP 23.000

L.S. 4
BOND $H
FMAP 2
PLAN 20
acta

WGHT    0.031600    0.352600
FVAR       0.41771
TI1   4    0.000000    0.000000    0.500000    10.50000    0.01101    0.00656 =
         0.01161    0.00039    0.00719    0.00074
P1    3    0.111788   -0.346892    0.274500    11.00000    0.01049    0.00969 =
         0.01044   -0.00177    0.00393    0.00080
O2    1    0.076746   -0.168566    0.327739    11.00000    0.02571    0.01217 =
         0.02449   -0.00669    0.01572    0.00027
O3    1    0.262553   -0.352550    0.104927    11.00000    0.02026    0.01454 =
         0.02095   -0.00201    0.01420    0.00284
O4    1   -0.172473   -0.435859    0.219067    11.00000    0.01612    0.02367 =
         0.01736   -0.00460    0.00511   -0.00744
H1    2    0.266155   -0.414594    0.443332    11.00000    0.01625
HKLF 4

REM  c in P2(1)/n
REM R1 =  0.0233 for     602 Fo > 4sig(Fo)  and  0.0249 for all     643 data
REM     47 parameters refined using      0 restraints

END

WGHT      0.0309      0.3680

REM Highest difference peak  0.290,  deepest hole -0.440,  1-sigma level  0.107
Q1    1  -0.2399 -0.3856  0.1628  11.00000  0.05    0.29
Q2    1  -0.1377 -0.4858  0.1403  11.00000  0.05    0.28
Q3    1   0.2039 -0.3689  0.1894  11.00000  0.05    0.26
Q4    1   0.2152 -0.4004  0.3634  11.00000  0.05    0.26
Q5    1   0.3840 -0.4572  0.5935  11.00000  0.05    0.25
Q6    1  -0.0710 -0.1542  0.2942  11.00000  0.05    0.25
Q7    1   0.1292 -0.1397  0.2914  11.00000  0.05    0.23
Q8    1   0.5905 -0.1922  0.1545  11.00000  0.05    0.22
Q9    1  -0.1249 -0.0938  0.2672  11.00000  0.05    0.22
Q10   1   0.0485 -0.1253  0.3953  11.00000  0.05    0.22
Q11   1  -0.3001 -0.1616  0.2489  11.00000  0.05    0.22
Q12   1   0.1643 -0.3858  0.0598  11.00000  0.05    0.21
Q13   1   0.0819 -0.2373  0.3610  11.00000  0.05    0.21
Q14   1   0.0497 -0.0682  0.2004  11.00000  0.05    0.21
Q15   1   0.0344 -0.4391 -0.0611  11.00000  0.05    0.21
Q16   1   0.2648 -0.3890  0.5533  11.00000  0.05    0.21
Q17   1  -0.2116 -0.4044  0.2855  11.00000  0.05    0.21
Q18   1   0.3777 -0.4187  0.4442  11.00000  0.05    0.20
Q19   1  -0.2152 -0.4810  0.2557  11.00000  0.05    0.20
Q20   1   0.4483 -0.3594  0.6001  11.00000  0.05    0.19
;
_shelx_res_checksum              56939
