#------------------------------------------------------------------------------
#$Date: 2018-09-26 06:29:44 +0300 (Wed, 26 Sep 2018) $
#$Revision: 211175 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/00/01/8000162.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_8000162
loop_
_publ_author_name
'Zhao, Yongnan'
'Yang, Yang'
'Yang, Xiaoqin'
'Guo, Wenjun'
_publ_section_title
;
 A New Open-structured Titanophosphate with Intersecting 12-Ring Channels
;
_journal_issue                   3
_journal_name_full               'Chemistry Letters'
_journal_page_first              456
_journal_paper_doi               10.1246/cl.2007.456
_journal_volume                  36
_journal_year                    2007
_chemical_formula_sum            'C0 H10 N O14 P3 Ti2'
_chemical_formula_weight         436.80
_space_group_IT_number           52
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.809(3)
_cell_length_b                   9.3747(19)
_cell_length_c                   11.205(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1345.5(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0753
_diffrn_reflns_av_sigmaI/netI    0.0532
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10458
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.25
_exptl_absorpt_coefficient_mu    1.614
_exptl_absorpt_correction_T_max  0.9093
_exptl_absorpt_correction_T_min  0.7384
_exptl_crystal_density_diffrn    2.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0558P)²+4.5394P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1368
_reflns_number_gt                1247
_reflns_number_total             1523
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            36-456sup1.cif
_cod_data_source_block           TJPU-2
_cod_database_code               8000162
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x, 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 0.25971(7) 0.7500 0.7500 0.0134(3) Uani 1 2 d S
Ti2 Ti 0.5000 0.5000 0.5000 0.0195(3) Uani 1 2 d S
P1 P 0.2500 0.5000 0.53328(12) 0.0127(3) Uani 1 2 d S
P2 P 0.42461(8) 0.48571(10) 0.79702(8) 0.0126(3) Uani 1 1 d .
O1 O 0.3462(2) 0.4850(3) 0.4543(3) 0.0226(7) Uani 1 1 d .
O2 O 0.2630(2) 0.6333(3) 0.6102(3) 0.0205(6) Uani 1 1 d .
O3 O 0.3748(2) 0.6321(3) 0.8201(3) 0.0203(6) Uani 1 1 d .
O4 O 0.1582(2) 0.6298(3) 0.8224(3) 0.0218(7) Uani 1 1 d .
O5 O 0.4669(3) 0.4729(4) 0.6719(3) 0.0288(8) Uani 1 1 d .
O6 O 0.5141(2) 0.4637(4) 0.8858(3) 0.0274(7) Uani 1 1 d .
H6 H 0.5570 0.5079 0.9305 0.041 Uiso 1 1 d R
O7 O 0.4872(3) 0.7173(4) 0.5191(3) 0.0329(8) Uani 1 1 d .
H7A H 0.4431 0.7570 0.5650 0.049 Uiso 1 1 d R
H7B H 0.5110 0.7739 0.4664 0.049 Uiso 1 1 d R
N1 N 0.691(5) 0.632(5) 0.923(3) 0.049(6) Uani 0.13 1 d P
N1A N 0.704(5) 0.625(5) 0.882(3) 0.049(6) Uani 0.13 1 d P
N1B N 0.802(3) 0.732(5) 0.768(3) 0.049(6) Uani 0.13 1 d P
N1C N 0.700(4) 0.692(4) 0.800(3) 0.049(6) Uani 0.13 1 d P
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'
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'
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
O4 Ti1 O4 93.77(19) 4_566 .
O4 Ti1 O2 90.28(13) 4_566 .
O4 Ti1 O2 91.47(13) . .
O4 Ti1 O2 91.47(13) 4_566 4_566
O4 Ti1 O2 90.28(13) . 4_566
O2 Ti1 O2 177.45(18) . 4_566
O4 Ti1 O3 90.51(13) 4_566 4_566
O4 Ti1 O3 175.71(13) . 4_566
O2 Ti1 O3 88.76(12) . 4_566
O2 Ti1 O3 89.37(12) 4_566 4_566
O4 Ti1 O3 175.71(13) 4_566 .
O4 Ti1 O3 90.51(13) . .
O2 Ti1 O3 89.37(12) . .
O2 Ti1 O3 88.76(12) 4_566 .
O3 Ti1 O3 85.21(17) 4_566 .
O5 Ti2 O5 180.000(1) 5_666 .
O5 Ti2 O1 88.36(13) 5_666 .
O5 Ti2 O1 91.64(13) . .
O5 Ti2 O1 91.64(13) 5_666 5_666
O5 Ti2 O1 88.36(13) . 5_666
O1 Ti2 O1 180.00(16) . 5_666
O5 Ti2 O7 89.49(13) 5_666 .
O5 Ti2 O7 90.51(13) . .
O1 Ti2 O7 90.99(13) . .
O1 Ti2 O7 89.01(13) 5_666 .
O5 Ti2 O7 90.51(13) 5_666 5_666
O5 Ti2 O7 89.49(13) . 5_666
O1 Ti2 O7 89.01(13) . 5_666
O1 Ti2 O7 90.99(13) 5_666 5_666
O7 Ti2 O7 180.0 . 5_666
O1 P1 O1 108.9(2) 2_565 .
O1 P1 O2 109.92(16) 2_565 .
O1 P1 O2 108.38(16) . .
O1 P1 O2 108.38(16) 2_565 2_565
O1 P1 O2 109.92(16) . 2_565
O2 P1 O2 111.3(2) . 2_565
O5 P2 O6 108.89(19) . .
O5 P2 O3 112.15(18) . .
O6 P2 O3 108.81(18) . .
O5 P2 O4 111.26(18) . 2_565
O6 P2 O4 107.51(18) . 2_565
O3 P2 O4 108.09(17) . 2_565
P1 O1 Ti2 128.93(18) . .
P1 O2 Ti1 158.2(2) . .
P2 O3 Ti1 137.17(18) . .
P2 O4 Ti1 143.85(19) 2_565 .
P2 O5 Ti2 165.2(2) . .
P2 O6 H6 143.1 . .
Ti2 O7 H7A 123.4 . .
Ti2 O7 H7B 121.2 . .
H7A O7 H7B 112.7 . .
N1B N1B N1C 111(2) 4_566 .
N1B N1B N1C 51(2) 4_566 4_566
N1C N1B N1C 60(4) . 4_566
N1A N1C N1B 108(5) . .
N1A N1C N1 14(4) . .
N1B N1C N1 114(4) . .
N1A N1C N1C 170(4) . 4_566
N1B N1C N1C 68(2) . 4_566
N1 N1C N1C 158(4) . 4_566
N1A N1C N1B 125(5) . 4_566
N1B N1C N1B 17(2) . 4_566
N1 N1C N1B 130(4) . 4_566
N1C N1C N1B 51.3(19) 4_566 4_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O4 1.902(3) 4_566
Ti1 O4 1.902(3) .
Ti1 O2 1.910(3) .
Ti1 O2 1.910(3) 4_566
Ti1 O3 2.003(3) 4_566
Ti1 O3 2.003(3) .
Ti2 O5 1.988(3) 5_666
Ti2 O5 1.988(3) .
Ti2 O1 2.041(3) .
Ti2 O1 2.041(3) 5_666
Ti2 O7 2.055(3) .
Ti2 O7 2.055(3) 5_666
P1 O1 1.523(3) 2_565
P1 O1 1.523(3) .
P1 O2 1.528(3) .
P1 O2 1.528(3) 2_565
P2 O5 1.508(3) .
P2 O6 1.532(3) .
P2 O3 1.535(3) .
P2 O4 1.542(3) 2_565
O4 P2 1.542(3) 2_565
O6 H6 0.8505 .
O7 H7A 0.8500 .
O7 H7B 0.8500 .
N1 N1C 1.49(5) .
N1A N1C 1.11(5) .
N1B N1B 0.53(7) 4_566
N1B N1C 1.41(6) .
N1B N1C 1.68(6) 4_566
N1C N1C 1.57(7) 4_566
N1C N1B 1.68(6) 4_566
