# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               CrystEngComm
_journal_coden_cambridge         1350
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_author_name                'Hengzhen Shi'
_publ_contact_author_name        'Shi, Hengzhen'
_publ_contact_author_email       hzshi@nynu.edu.cn

data_a
_database_code_depnum_ccdc_archive 'CCDC 834984'
#TrackingRef 'CSD422338-R3.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B H3 O10 P2 Ti'
_chemical_formula_weight         283.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
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'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4(1)/amd

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z+1/2'
'x, -y, -z'
'y+1/4, x+3/4, -z+1/4'
'-y+1/4, -x+1/4, -z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1'
'x+1/2, -y+1/2, -z+1/2'
'y+3/4, x+5/4, -z+3/4'
'-y+3/4, -x+3/4, -z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z-1/2'
'-x, y, z'
'-y-1/4, -x-3/4, z-1/4'
'y-1/4, x-1/4, z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
'-y+1/4, -x-1/4, z+1/4'
'y+1/4, x+1/4, z-1/4'

_cell_length_a                   6.316(2)
_cell_length_b                   6.316(2)
_cell_length_c                   16.446(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     656.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.872
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             560
_exptl_absorpt_coefficient_mu    1.837
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8376
_exptl_absorpt_correction_T_max  0.8822
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1872
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         4.96
_diffrn_reflns_theta_max         28.35
_reflns_number_total             236
_reflns_number_gt                211
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0871P)^2^+23.7491P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    CONSTR
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       ?
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         236
_refine_ls_number_parameters     28
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0694
_refine_ls_wR_factor_ref         0.1955
_refine_ls_wR_factor_gt          0.1906
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_restrained_S_all      1.223
_refine_ls_shift/su_max          0.000
_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
Ti1 Ti 0.5000 0.2500 0.1250 0.0044(10) Uani 1 8 d SU . .
P1 P 0.5773(7) 0.2500 -0.0776(2) 0.0055(10) Uani 0.50 2 d SPU . .
O1 O 0.5000 0.2500 0.0083(5) 0.0108(18) Uani 1 4 d SU . .
O2 O 0.5000 0.0559(9) -0.1245(3) 0.0095(14) Uani 1 2 d SU . .
O3 O 0.8185(14) 0.2500 -0.0693(5) 0.036(2) Uani 1 2 d SU . .
H1 H 0.8610 0.2500 -0.0152 0.036 Uiso 0.75 2 calc SPR . .
B1 B 1.0000 0.2500 -0.1250 0.026(3) Uani 1 8 d SU . .

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 0.0038(11) 0.0038(11) 0.0056(14) 0.000 0.000 0.000
P1 0.0099(17) 0.0027(17) 0.0040(17) 0.000 -0.0006(12) 0.000
O1 0.010(4) 0.014(4) 0.009(4) 0.000 0.000 0.000
O2 0.014(3) 0.004(3) 0.010(2) -0.002(2) 0.000 0.000
O3 0.025(2) 0.043(3) 0.041(3) 0.000 0.001(2) 0.000
B1 0.014(3) 0.014(3) 0.051(9) 0.000 0.000 0.000

_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 O1 1.919(9) 27_565 ?
Ti1 O1 1.919(9) . ?
Ti1 O2 1.932(6) 12_554 ?
Ti1 O2 1.932(6) 17_655 ?
Ti1 O2 1.932(6) 26 ?
Ti1 O2 1.932(6) 3_545 ?
P1 P1 0.977(8) 10_554 ?
P1 O1 1.495(9) . ?
P1 O2 1.529(6) . ?
P1 O2 1.529(6) 10_554 ?
P1 O3 1.530(10) . ?
O1 P1 1.495(9) 10_554 ?
O2 P1 1.529(6) 10_554 ?
O2 Ti1 1.932(6) 17_655 ?
O3 B1 1.467(9) . ?
O3 H1 0.9300 . ?
B1 O3 1.467(9) 28_645 ?
B1 O3 1.467(9) 10_654 ?
B1 O3 1.467(9) 19_675 ?

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
O1 Ti1 O1 180.000(1) 27_565 . ?
O1 Ti1 O2 89.76(16) 27_565 12_554 ?
O1 Ti1 O2 90.24(16) . 12_554 ?
O1 Ti1 O2 90.24(16) 27_565 17_655 ?
O1 Ti1 O2 89.76(16) . 17_655 ?
O2 Ti1 O2 90.001(1) 12_554 17_655 ?
O1 Ti1 O2 90.24(16) 27_565 26 ?
O1 Ti1 O2 89.76(16) . 26 ?
O2 Ti1 O2 90.001(2) 12_554 26 ?
O2 Ti1 O2 179.5(3) 17_655 26 ?
O1 Ti1 O2 89.76(16) 27_565 3_545 ?
O1 Ti1 O2 90.24(16) . 3_545 ?
O2 Ti1 O2 179.5(3) 12_554 3_545 ?
O2 Ti1 O2 90.001(2) 17_655 3_545 ?
O2 Ti1 O2 90.001(2) 26 3_545 ?
P1 P1 O1 70.93(19) 10_554 . ?
P1 P1 O2 71.36(17) 10_554 . ?
O1 P1 O2 111.9(3) . . ?
P1 P1 O2 71.36(17) 10_554 10_554 ?
O1 P1 O2 111.9(3) . 10_554 ?
O2 P1 O2 106.7(4) . 10_554 ?
P1 P1 O3 174.9(4) 10_554 . ?
O1 P1 O3 104.0(4) . . ?
O2 P1 O3 111.3(3) . . ?
O2 P1 O3 111.3(3) 10_554 . ?
P1 O1 P1 38.1(4) 10_554 . ?
P1 O1 Ti1 160.93(19) 10_554 . ?
P1 O1 Ti1 160.93(19) . . ?
P1 O2 P1 37.3(3) . 10_554 ?
P1 O2 Ti1 143.5(3) . 17_655 ?
P1 O2 Ti1 143.5(3) 10_554 17_655 ?
B1 O3 P1 136.3(7) . . ?
B1 O3 H1 111.9 . . ?
P1 O3 H1 111.9 . . ?
O3 B1 O3 112.9(4) 28_645 10_654 ?
O3 B1 O3 112.9(4) 28_645 . ?
O3 B1 O3 102.8(7) 10_654 . ?
O3 B1 O3 102.8(7) 28_645 19_675 ?
O3 B1 O3 112.9(4) 10_654 19_675 ?
O3 B1 O3 112.9(4) . 19_675 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 P1 O1 P1 -59.8(2) . . . 10_554 ?
O2 P1 O1 P1 59.8(2) 10_554 . . 10_554 ?
O3 P1 O1 P1 180.0 . . . 10_554 ?
P1 P1 O1 Ti1 180.0 10_554 . . . ?
O2 P1 O1 Ti1 120.2(2) . . . . ?
O2 P1 O1 Ti1 -120.2(2) 10_554 . . . ?
O3 P1 O1 Ti1 0.0 . . . . ?
O1 Ti1 O1 P1 0(100) 27_565 . . 10_554 ?
O2 Ti1 O1 P1 180.0 12_554 . . 10_554 ?
O2 Ti1 O1 P1 90.0 17_655 . . 10_554 ?
O2 Ti1 O1 P1 -90.0 26 . . 10_554 ?
O2 Ti1 O1 P1 0.0 3_545 . . 10_554 ?
O1 Ti1 O1 P1 180(100) 27_565 . . . ?
O2 Ti1 O1 P1 0.0 12_554 . . . ?
O2 Ti1 O1 P1 -90.0 17_655 . . . ?
O2 Ti1 O1 P1 90.0 26 . . . ?
O2 Ti1 O1 P1 180.0 3_545 . . . ?
O1 P1 O2 P1 59.5(3) . . . 10_554 ?
O2 P1 O2 P1 -63.1(3) 10_554 . . 10_554 ?
O3 P1 O2 P1 175.4(3) . . . 10_554 ?
P1 P1 O2 Ti1 -117.1(4) 10_554 . . 17_655 ?
O1 P1 O2 Ti1 -57.6(5) . . . 17_655 ?
O2 P1 O2 Ti1 179.79(15) 10_554 . . 17_655 ?
O3 P1 O2 Ti1 58.2(6) . . . 17_655 ?
P1 P1 O3 B1 180.000(3) 10_554 . . . ?
O1 P1 O3 B1 180.0 . . . . ?
O2 P1 O3 B1 59.4(3) . . . . ?
O2 P1 O3 B1 -59.4(3) 10_554 . . . ?
P1 O3 B1 O3 -58.0(2) . . . 28_645 ?
P1 O3 B1 O3 180.0 . . . 10_654 ?
P1 O3 B1 O3 58.0(2) . . . 19_675 ?

_diffrn_measured_fraction_theta_max 0.960
_diffrn_reflns_theta_full        28.35
_diffrn_measured_fraction_theta_full 0.959
_refine_diff_density_max         1.073
_refine_diff_density_min         -1.591
_refine_diff_density_rms         0.243