#------------------------------------------------------------------------------
#$Date: 2017-04-04 05:59:54 +0300 (Tue, 04 Apr 2017) $
#$Revision: 194695 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/55/4345565.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_4345565
loop_
_publ_author_name
'Stauber, Julia M.'
'Cummins, Christopher C.'
_publ_section_title
;
 Terminal Titanyl Complexes of Tri- and Tetrametaphosphate: Synthesis,
 Structures, and Reactivity with Hydrogen Peroxide.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3022
_journal_page_last               3029
_journal_paper_doi               10.1021/acs.inorgchem.6b03149
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C38.5 H34 N1.5 O7 P4 Ti0.5'
_chemical_formula_weight         777.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                92.9790(10)
_cell_angle_beta                 112.5450(10)
_cell_angle_gamma                109.6980(10)
_cell_formula_units_Z            4
_cell_length_a                   16.3690(11)
_cell_length_b                   16.3925(11)
_cell_length_c                   17.2399(12)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.92
_cell_measurement_theta_min      2.20
_cell_volume                     3934.1(5)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            133174
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.017
_diffrn_reflns_theta_min         1.308
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1610
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.7069
_refine_diff_density_max         1.273
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     931
_refine_ls_number_reflns         18880
_refine_ls_number_restraints     1488
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0468P)²+3.9354P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1047
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16280
_reflns_number_total             18880
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b03149_si_005.cif
_cod_data_source_block           OTi_4
_cod_original_formula_sum        'C38.50 H34 N1.50 O7 P4 Ti0.50'
_cod_database_code               4345565
_shelx_shelxl_version_number     2014/7
_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. 
;
_shelx_estimated_absorpt_t_min   0.967
_shelx_estimated_absorpt_t_max   0.974
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Ti1 Ti 1.12092(2) 1.00594(2) 0.60960(2) 0.01331(6) Uani 1 1 d . U
O1 O 1.21222(9) 1.01475(9) 0.69735(8) 0.0225(3) Uani 1 1 d . U
O2 O 1.00439(9) 0.95220(8) 0.63029(8) 0.0184(2) Uani 1 1 d . U
O3 O 1.07602(9) 0.88637(8) 0.53840(8) 0.0196(3) Uani 1 1 d . U
O4 O 0.82540(9) 0.94164(8) 0.47011(8) 0.0196(3) Uani 1 1 d . U
O5 O 0.90017(9) 0.88182(8) 0.37671(9) 0.0205(3) Uani 1 1 d . U
O6 O 0.83352(8) 0.84567(8) 0.57912(8) 0.0157(2) Uani 1 1 d . U
O7 O 0.78766(9) 0.77900(8) 0.42755(8) 0.0175(2) Uani 1 1 d . U
O8 O 0.93284(9) 0.75374(8) 0.43654(8) 0.0180(2) Uani 1 1 d . U
O9 O 0.95923(8) 0.78842(8) 0.58928(8) 0.0162(2) Uani 1 1 d . U
P1 P 0.94317(3) 0.86391(3) 0.63788(3) 0.01330(8) Uani 1 1 d . U
P2 P 0.77445(3) 0.85160(3) 0.48250(3) 0.01531(9) Uani 1 1 d . U
P3 P 0.85220(3) 0.78551(3) 0.37572(3) 0.01606(9) Uani 1 1 d . U
P4 P 1.01763(3) 0.79077(3) 0.53188(3) 0.01584(9) Uani 1 1 d . U
O01 O 0.95141(9) 0.84921(9) 0.72282(8) 0.0200(3) Uani 1 1 d . U
O03 O 0.67424(9) 0.82408(10) 0.46773(8) 0.0258(3) Uani 1 1 d . U
O05 O 0.79677(10) 0.72176(9) 0.29381(8) 0.0251(3) Uani 1 1 d . U
O06 O 1.06513(10) 0.72843(9) 0.55202(9) 0.0233(3) Uani 1 1 d . U
N1 N 1.41360(10) 0.74571(10) 0.78218(9) 0.0176(3) Uani 1 1 d . U
P01 P 1.43728(3) 0.82416(3) 0.85519(3) 0.01517(9) Uani 1 1 d . U
P02 P 1.41995(3) 0.73609(3) 0.69299(3) 0.01481(9) Uani 1 1 d . U
C1A C 1.32820(12) 0.82800(11) 0.85324(11) 0.0155(3) Uani 1 1 d . U
C2A C 1.33034(12) 0.88040(12) 0.92127(11) 0.0192(3) Uani 1 1 d . U
H2A H 1.3881 0.9078 0.9722 0.023 Uiso 1 1 calc R U
C3A C 1.24783(13) 0.89222(13) 0.91426(12) 0.0221(4) Uani 1 1 d . U
H3A H 1.2494 0.9283 0.9601 0.027 Uiso 1 1 calc R U
C4A C 1.16292(13) 0.85125(13) 0.84009(12) 0.0217(4) Uani 1 1 d . U
H4A H 1.1069 0.8602 0.8351 0.026 Uiso 1 1 calc R U
C5A C 1.15989(12) 0.79750(12) 0.77363(12) 0.0202(3) Uani 1 1 d . U
H5A H 1.1013 0.7684 0.7238 0.024 Uiso 1 1 calc R U
C6A C 1.24249(12) 0.78595(12) 0.77959(11) 0.0172(3) Uani 1 1 d . U
H6A H 1.2404 0.7495 0.7336 0.021 Uiso 1 1 calc R U
C1B C 1.50572(12) 0.80488(12) 0.95715(11) 0.0186(3) Uani 1 1 d . U
C2B C 1.50109(13) 0.71904(13) 0.96289(13) 0.0243(4) Uani 1 1 d . U
H2B H 1.4635 0.6726 0.9132 0.029 Uiso 1 1 calc R U
C3B C 1.56199(13) 0.87274(13) 1.03042(12) 0.0227(4) Uani 1 1 d . U
H3B H 1.5651 0.9313 1.0271 0.027 Uiso 1 1 calc R U
C4B C 1.60793(15) 0.76926(16) 1.11328(13) 0.0307(4) Uani 1 1 d . U
H4B H 1.6431 0.7571 1.1664 0.037 Uiso 1 1 calc R U
C5B C 1.61328(14) 0.85496(15) 1.10807(12) 0.0280(4) Uani 1 1 d . U
H5B H 1.6520 0.9014 1.1576 0.034 Uiso 1 1 calc R U
C6B C 1.55127(15) 0.70121(15) 1.04103(14) 0.0314(4) Uani 1 1 d . U
H6B H 1.5468 0.6424 1.0451 0.038 Uiso 1 1 calc R U
C1C C 1.50331(12) 0.93298(12) 0.84602(11) 0.0186(3) Uani 1 1 d . U
C2C C 1.60258(13) 0.96165(14) 0.87152(12) 0.0243(4) Uani 1 1 d . U
H2C H 1.6357 0.9256 0.8977 0.029 Uiso 1 1 calc R U
C3C C 1.65197(15) 1.04280(14) 0.85833(13) 0.0306(4) Uani 1 1 d . U
H3C H 1.7191 1.0624 0.8755 0.037 Uiso 1 1 calc R U
C4C C 1.60372(17) 1.09532(14) 0.82027(15) 0.0340(5) Uani 1 1 d . U
H4C H 1.6381 1.1512 0.8121 0.041 Uiso 1 1 calc R U
C5C C 1.50552(17) 1.06698(14) 0.79407(15) 0.0325(5) Uani 1 1 d . U
H5C H 1.4728 1.1030 0.7671 0.039 Uiso 1 1 calc R U
C6C C 1.45498(14) 0.98623(13) 0.80706(13) 0.0243(4) Uani 1 1 d . U
H6C H 1.3878 0.9671 0.7896 0.029 Uiso 1 1 calc R U
C1D C 1.53733(12) 0.74461(12) 0.70630(11) 0.0177(3) Uani 1 1 d . U
C2D C 1.60945(13) 0.76092(14) 0.78809(12) 0.0255(4) Uani 1 1 d . U
H2D H 1.5949 0.7602 0.8364 0.031 Uiso 1 1 calc R U
C3D C 1.70306(14) 0.77835(16) 0.79939(14) 0.0328(5) Uani 1 1 d . U
H3D H 1.7522 0.7898 0.8556 0.039 Uiso 1 1 calc R U
C4D C 1.72501(14) 0.77914(14) 0.72952(15) 0.0297(4) Uani 1 1 d . U
H4D H 1.7892 0.7922 0.7377 0.036 Uiso 1 1 calc R U
C5D C 1.65319(16) 0.76090(17) 0.64788(15) 0.0354(5) Uani 1 1 d . U
H5D H 1.6678 0.7603 0.5996 0.042 Uiso 1 1 calc R U
C6D C 1.55958(15) 0.74337(16) 0.63593(13) 0.0305(5) Uani 1 1 d . U
H6D H 1.5104 0.7305 0.5795 0.037 Uiso 1 1 calc R U
C1E C 1.33168(12) 0.62854(12) 0.63053(12) 0.0193(3) Uani 1 1 d . U
C2E C 1.3099(2) 0.60402(17) 0.54569(16) 0.0578(9) Uani 1 1 d . U
H2E H 1.3409 0.6442 0.5184 0.069 Uiso 1 1 calc R U
C3E C 1.2422(3) 0.52004(19) 0.49942(18) 0.0719(11) Uani 1 1 d . U
H3E H 1.2263 0.5039 0.4402 0.086 Uiso 1 1 calc R U
C4E C 1.19831(17) 0.46062(14) 0.53777(15) 0.0356(5) Uani 1 1 d . U
H4E H 1.1542 0.4027 0.5062 0.043 Uiso 1 1 calc R U
C5E C 1.2184(2) 0.48522(16) 0.62138(18) 0.0466(6) Uani 1 1 d . U
H5E H 1.1868 0.4448 0.6481 0.056 Uiso 1 1 calc R U
C6E C 1.2855(2) 0.56967(16) 0.66879(17) 0.0447(6) Uani 1 1 d . U
C1F C 1.39671(12) 0.81877(11) 0.63303(11) 0.0164(3) Uani 1 1 d . U
C2F C 1.30249(13) 0.81383(13) 0.59076(12) 0.0211(4) Uani 1 1 d . U
H2F H 1.2505 0.7638 0.5888 0.025 Uiso 1 1 calc R U
C3F C 1.28522(14) 0.88213(14) 0.55173(13) 0.0265(4) Uani 1 1 d . U
H3F H 1.2213 0.8787 0.5229 0.032 Uiso 1 1 calc R U
C4F C 1.36093(15) 0.95527(14) 0.55471(13) 0.0275(4) Uani 1 1 d . U
H4F H 1.3487 1.0020 0.5284 0.033 Uiso 1 1 calc R U
C5F C 1.45438(14) 0.96063(13) 0.59577(13) 0.0261(4) Uani 1 1 d . U
H5F H 1.5059 1.0105 0.5968 0.031 Uiso 1 1 calc R U
C6F C 1.47268(13) 0.89298(12) 0.63548(12) 0.0211(4) Uani 1 1 d . U
H6F H 1.5368 0.8971 0.6643 0.025 Uiso 1 1 calc R U
N2 N 0.10440(10) 0.65715(10) 0.15627(9) 0.0172(3) Uani 1 1 d . U
P03 P 0.18500(3) 0.61846(3) 0.17582(3) 0.01487(9) Uani 1 1 d . U
P04 P 0.04612(3) 0.68231(3) 0.20223(3) 0.01591(9) Uani 1 1 d . U
C1G C 0.29647(12) 0.68457(12) 0.26619(11) 0.0177(3) Uani 1 1 d . U
C2G C 0.29382(13) 0.71644(14) 0.34130(12) 0.0252(4) Uani 1 1 d . U
H2G H 0.2341 0.7010 0.3447 0.030 Uiso 1 1 calc R U
C3G C 0.37774(14) 0.77046(14) 0.41117(12) 0.0253(4) Uani 1 1 d . U
H3G H 0.3751 0.7934 0.4615 0.030 Uiso 1 1 calc R U
C4G C 0.46523(13) 0.79094(13) 0.40759(12) 0.0229(4) Uani 1 1 d . U
H4G H 0.5228 0.8275 0.4556 0.028 Uiso 1 1 calc R U
C5G C 0.46882(13) 0.75800(14) 0.33379(12) 0.0261(4) Uani 1 1 d . U
H5G H 0.5290 0.7713 0.3317 0.031 Uiso 1 1 calc R U
C6G C 0.38497(13) 0.70572(13) 0.26297(12) 0.0229(4) Uani 1 1 d . U
H6G H 0.3878 0.6843 0.2122 0.027 Uiso 1 1 calc R U
C1H C 0.21064(12) 0.61469(11) 0.08381(11) 0.0164(3) Uani 1 1 d . U
C2H C 0.25294(14) 0.55780(13) 0.06992(12) 0.0227(4) Uani 1 1 d . U
H2H H 0.2639 0.5178 0.1069 0.027 Uiso 1 1 calc R U
C3H C 0.27903(15) 0.55968(14) 0.00187(13) 0.0270(4) Uani 1 1 d . U
H3H H 0.3084 0.5214 -0.0074 0.032 Uiso 1 1 calc R U
C4H C 0.26206(14) 0.61733(13) -0.05213(12) 0.0252(4) Uani 1 1 d . U
H4H H 0.2799 0.6186 -0.0985 0.030 Uiso 1 1 calc R U
C5H C 0.21926(14) 0.67332(13) -0.03927(13) 0.0245(4) Uani 1 1 d . U
H5H H 0.2068 0.7120 -0.0774 0.029 Uiso 1 1 calc R U
C6H C 0.19433(13) 0.67307(12) 0.02950(12) 0.0199(3) Uani 1 1 d . U
H6H H 0.1664 0.7125 0.0392 0.024 Uiso 1 1 calc R U
C1I C 0.15004(12) 0.50823(12) 0.19516(11) 0.0179(3) Uani 1 1 d . U
C2I C 0.20842(15) 0.48552(13) 0.26621(13) 0.0288(4) Uani 1 1 d . U
H2I H 0.2690 0.5285 0.3055 0.035 Uiso 1 1 calc R U
C3I C 0.17744(18) 0.39972(15) 0.27911(14) 0.0368(5) Uani 1 1 d . U
H3I H 0.2171 0.3839 0.3274 0.044 Uiso 1 1 calc R U
C4I C 0.08924(16) 0.33692(14) 0.22229(14) 0.0304(4) Uani 1 1 d . U
H4I H 0.0679 0.2787 0.2324 0.037 Uiso 1 1 calc R U
C5I C 0.03191(14) 0.35893(13) 0.15065(13) 0.0253(4) Uani 1 1 d . U
H5I H -0.0281 0.3154 0.1110 0.030 Uiso 1 1 calc R U
C6I C 0.06199(13) 0.44415(12) 0.13678(12) 0.0208(4) Uani 1 1 d . U
H6I H 0.0228 0.4591 0.0875 0.025 Uiso 1 1 calc R U
C1J C 0.10712(13) 0.79549(12) 0.26057(11) 0.0189(3) Uani 1 1 d . U
C2J C 0.19093(15) 0.84889(13) 0.25587(14) 0.0310(5) Uani 1 1 d . U
H2J H 0.2166 0.8250 0.2237 0.037 Uiso 1 1 calc R U
C3J C 0.23696(17) 0.93713(14) 0.29829(16) 0.0378(5) Uani 1 1 d . U
H3J H 0.2950 0.9732 0.2962 0.045 Uiso 1 1 calc R U
C4J C 0.19857(16) 0.97281(13) 0.34377(14) 0.0293(4) Uani 1 1 d . U
H4J H 0.2296 1.0336 0.3715 0.035 Uiso 1 1 calc R U
C5J C 0.11504(14) 0.91994(12) 0.34885(12) 0.0219(4) Uani 1 1 d . U
H5J H 0.0893 0.9443 0.3805 0.026 Uiso 1 1 calc R U
C6J C 0.06937(13) 0.83141(12) 0.30751(11) 0.0192(3) Uani 1 1 d . U
H6J H 0.0124 0.7951 0.3111 0.023 Uiso 1 1 calc R U
C1K C -0.06691(12) 0.67341(12) 0.12079(12) 0.0191(3) Uani 1 1 d . U
C2K C -0.07956(14) 0.67229(13) 0.03629(12) 0.0241(4) Uani 1 1 d . U
H2K H -0.0299 0.6720 0.0207 0.029 Uiso 1 1 calc R U
C3K C -0.16493(15) 0.67155(15) -0.02546(14) 0.0312(4) Uani 1 1 d . U
H3K H -0.1739 0.6701 -0.0834 0.037 Uiso 1 1 calc R U
C4K C -0.23704(15) 0.67296(15) -0.00245(15) 0.0345(5) Uani 1 1 d . U
H4K H -0.2949 0.6734 -0.0445 0.041 Uiso 1 1 calc R U
C5K C -0.22457(15) 0.67367(15) 0.08170(15) 0.0330(5) Uani 1 1 d . U
H5K H -0.2742 0.6743 0.0971 0.040 Uiso 1 1 calc R U
C6K C -0.14011(14) 0.67343(14) 0.14370(13) 0.0263(4) Uani 1 1 d . U
H6K H -0.1321 0.6733 0.2013 0.032 Uiso 1 1 calc R U
C1L C 0.01919(13) 0.61088(12) 0.27246(12) 0.0195(3) Uani 1 1 d . U
C2L C 0.06132(14) 0.63652(13) 0.36157(13) 0.0247(4) Uani 1 1 d . U
H2L H 0.1020 0.6966 0.3887 0.030 Uiso 1 1 calc R U
C3L C 0.04372(19) 0.57391(15) 0.41076(14) 0.0356(5) Uani 1 1 d . U
H3L H 0.0720 0.5914 0.4716 0.043 Uiso 1 1 calc R U
C4L C -0.01499(19) 0.48608(15) 0.37130(16) 0.0385(5) Uani 1 1 d . U
H4L H -0.0254 0.4433 0.4053 0.046 Uiso 1 1 calc R U
C5L C -0.05844(17) 0.46054(14) 0.28289(15) 0.0341(5) Uani 1 1 d . U
H5L H -0.0994 0.4005 0.2561 0.041 Uiso 1 1 calc R U
C6L C -0.04221(14) 0.52254(13) 0.23314(13) 0.0259(4) Uani 1 1 d . U
H6L H -0.0728 0.5051 0.1723 0.031 Uiso 1 1 calc R U
O3A O 0.10975(15) 0.83472(14) 0.02793(16) 0.0605(6) Uani 1 1 d D U
C31 C 0.0617(2) 0.87397(19) 0.0183(2) 0.0544(7) Uani 1 1 d D U
C32 C 0.0733(3) 0.9407(3) 0.0920(2) 0.0891(14) Uani 1 1 d D U
H32A H 0.1327 0.9507 0.1425 0.134 Uiso 1 1 calc R U
H32B H 0.0186 0.9170 0.1063 0.134 Uiso 1 1 calc R U
H32C H 0.0760 0.9969 0.0739 0.134 Uiso 1 1 calc R U
C33 C -0.0167(3) 0.8665(3) -0.0652(2) 0.0699(9) Uani 1 1 d D U
H33A H -0.0235 0.8203 -0.1083 0.105 Uiso 1 1 calc R U
H33B H -0.0016 0.9233 -0.0834 0.105 Uiso 1 1 calc R U
H33C H -0.0769 0.8511 -0.0591 0.105 Uiso 1 1 calc R U
N0A1 N 1.20248(17) 1.08860(17) 0.99399(13) 0.0477(5) Uani 1 1 d . U
C0A1 C 1.17062(16) 1.08612(16) 0.92240(14) 0.0338(5) Uani 1 1 d . U
C0A2 C 1.12950(18) 1.08167(19) 0.83014(14) 0.0422(6) Uani 1 1 d . U
H0A1 H 1.1362 1.1411 0.8192 0.063 Uiso 1 1 calc R U
H0A2 H 1.0614 1.0426 0.8046 0.063 Uiso 1 1 calc R U
H0A3 H 1.1633 1.0583 0.8045 0.063 Uiso 1 1 calc R U
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
O1 Ti1 O4 106.15(6) . 2_776
O1 Ti1 O2 106.76(6) . .
O4 Ti1 O2 147.01(6) 2_776 .
O1 Ti1 O3 106.54(6) . .
O4 Ti1 O3 88.68(5) 2_776 .
O2 Ti1 O3 84.28(5) . .
O1 Ti1 O5 105.78(6) . 2_776
O4 Ti1 O5 84.69(5) 2_776 2_776
O2 Ti1 O5 84.26(5) . 2_776
O3 Ti1 O5 147.59(6) . 2_776
P1 O2 Ti1 139.37(8) . .
P4 O3 Ti1 139.93(8) . .
P2 O4 Ti1 138.74(8) . 2_776
P3 O5 Ti1 138.24(8) . 2_776
P1 O6 P2 135.14(8) . .
P2 O7 P3 133.40(8) . .
P3 O8 P4 135.46(8) . .
P1 O9 P4 133.18(8) . .
O01 P1 O2 118.84(8) . .
O01 P1 O6 107.89(7) . .
O2 P1 O6 108.18(7) . .
O01 P1 O9 110.91(7) . .
O2 P1 O9 107.80(7) . .
O6 P1 O9 101.87(7) . .
O03 P2 O4 119.36(8) . .
O03 P2 O6 107.26(7) . .
O4 P2 O6 107.63(7) . .
O03 P2 O7 110.36(8) . .
O4 P2 O7 108.54(7) . .
O6 P2 O7 102.29(7) . .
O05 P3 O5 119.42(8) . .
O05 P3 O8 108.16(7) . .
O5 P3 O8 107.93(7) . .
O05 P3 O7 110.36(7) . .
O5 P3 O7 107.52(7) . .
O8 P3 O7 102.04(7) . .
O06 P4 O3 119.48(8) . .
O06 P4 O8 108.66(7) . .
O3 P4 O8 107.68(7) . .
O06 P4 O9 109.69(7) . .
O3 P4 O9 107.91(7) . .
O8 P4 O9 102.00(7) . .
P02 N1 P01 136.86(10) . .
N1 P01 C1A 110.09(8) . .
N1 P01 C1B 108.36(8) . .
C1A P01 C1B 109.59(8) . .
N1 P01 C1C 115.09(8) . .
C1A P01 C1C 105.30(8) . .
C1B P01 C1C 108.30(9) . .
N1 P02 C1D 111.79(8) . .
N1 P02 C1F 114.56(8) . .
C1D P02 C1F 105.25(8) . .
N1 P02 C1E 106.48(8) . .
C1D P02 C1E 110.02(8) . .
C1F P02 C1E 108.72(8) . .
C6A C1A C2A 119.78(15) . .
C6A C1A P01 119.54(13) . .
C2A C1A P01 120.34(13) . .
C3A C2A C1A 119.88(16) . .
C3A C2A H2A 120.1 . .
C1A C2A H2A 120.1 . .
C2A C3A C4A 120.07(17) . .
C2A C3A H3A 120.0 . .
C4A C3A H3A 120.0 . .
C5A C4A C3A 120.20(16) . .
C5A C4A H4A 119.9 . .
C3A C4A H4A 119.9 . .
C4A C5A C6A 120.19(16) . .
C4A C5A H5A 119.9 . .
C6A C5A H5A 119.9 . .
C5A C6A C1A 119.84(16) . .
C5A C6A H6A 120.1 . .
C1A C6A H6A 120.1 . .
C2B C1B C3B 119.40(17) . .
C2B C1B P01 118.50(14) . .
C3B C1B P01 122.09(15) . .
C6B C2B C1B 120.15(19) . .
C6B C2B H2B 119.9 . .
C1B C2B H2B 119.9 . .
C5B C3B C1B 120.29(19) . .
C5B C3B H3B 119.9 . .
C1B C3B H3B 119.9 . .
C5B C4B C6B 120.19(19) . .
C5B C4B H4B 119.9 . .
C6B C4B H4B 119.9 . .
C4B C5B C3B 119.91(19) . .
C4B C5B H5B 120.0 . .
C3B C5B H5B 120.0 . .
C4B C6B C2B 120.0(2) . .
C4B C6B H6B 120.0 . .
C2B C6B H6B 120.0 . .
C6C C1C C2C 119.76(17) . .
C6C C1C P01 120.19(14) . .
C2C C1C P01 119.84(15) . .
C3C C2C C1C 119.7(2) . .
C3C C2C H2C 120.2 . .
C1C C2C H2C 120.2 . .
C4C C3C C2C 120.21(19) . .
C4C C3C H3C 119.9 . .
C2C C3C H3C 119.9 . .
C3C C4C C5C 120.4(2) . .
C3C C4C H4C 119.8 . .
C5C C4C H4C 119.8 . .
C6C C5C C4C 120.2(2) . .
C6C C5C H5C 119.9 . .
C4C C5C H5C 119.9 . .
C5C C6C C1C 119.75(19) . .
C5C C6C H6C 120.1 . .
C1C C6C H6C 120.1 . .
C2D C1D C6D 119.07(16) . .
C2D C1D P02 119.88(13) . .
C6D C1D P02 120.78(14) . .
C1D C2D C3D 120.08(18) . .
C1D C2D H2D 120.0 . .
C3D C2D H2D 120.0 . .
C4D C3D C2D 120.52(19) . .
C4D C3D H3D 119.7 . .
C2D C3D H3D 119.7 . .
C5D C4D C3D 119.66(18) . .
C5D C4D H4D 120.2 . .
C3D C4D H4D 120.2 . .
C4D C5D C6D 120.25(19) . .
C4D C5D H5D 119.9 . .
C6D C5D H5D 119.9 . .
C5D C6D C1D 120.39(19) . .
C5D C6D H6D 119.8 . .
C1D C6D H6D 119.8 . .
C2E C1E C6E 119.22(19) . .
C2E C1E P02 121.21(16) . .
C6E C1E P02 119.57(15) . .
C1E C2E C3E 119.8(2) . .
C1E C2E H2E 120.1 . .
C3E C2E H2E 120.1 . .
C4E C3E C2E 121.1(2) . .
C4E C3E H3E 119.5 . .
C2E C3E H3E 119.5 . .
C5E C4E C3E 119.2(2) . .
C5E C4E H4E 120.4 . .
C3E C4E H4E 120.4 . .
C4E C5E C6E 120.6(2) . .
C4E C5E H5E 119.7 . .
C6E C5E H5E 119.7 . .
C1E C6E C5E 120.0(2) . .
C6F C1F C2F 119.35(17) . .
C6F C1F P02 120.53(13) . .
C2F C1F P02 119.80(14) . .
C3F C2F C1F 119.96(18) . .
C3F C2F H2F 120.0 . .
C1F C2F H2F 120.0 . .
C4F C3F C2F 120.19(18) . .
C4F C3F H3F 119.9 . .
C2F C3F H3F 119.9 . .
C3F C4F C5F 120.40(18) . .
C3F C4F H4F 119.8 . .
C5F C4F H4F 119.8 . .
C4F C5F C6F 119.98(18) . .
C4F C5F H5F 120.0 . .
C6F C5F H5F 120.0 . .
C5F C6F C1F 120.12(17) . .
C5F C6F H6F 119.9 . .
C1F C6F H6F 119.9 . .
P03 N2 P04 139.16(10) . .
N2 P03 C1H 107.92(8) . .
N2 P03 C1I 113.53(8) . .
C1H P03 C1I 107.44(8) . .
N2 P03 C1G 114.07(8) . .
C1H P03 C1G 106.82(8) . .
C1I P03 C1G 106.67(8) . .
N2 P04 C1K 108.15(8) . .
N2 P04 C1J 111.22(8) . .
C1K P04 C1J 106.74(8) . .
N2 P04 C1L 114.42(8) . .
C1K P04 C1L 106.55(8) . .
C1J P04 C1L 109.37(8) . .
C2G C1G C6G 119.12(16) . .
C2G C1G P03 118.68(13) . .
C6G C1G P03 122.20(14) . .
C3G C2G C1G 120.49(17) . .
C3G C2G H2G 119.8 . .
C1G C2G H2G 119.8 . .
C4G C3G C2G 120.04(18) . .
C4G C3G H3G 120.0 . .
C2G C3G H3G 120.0 . .
C3G C4G C5G 119.91(17) . .
C3G C4G H4G 120.0 . .
C5G C4G H4G 120.0 . .
C4G C5G C6G 120.31(17) . .
C4G C5G H5G 119.8 . .
C6G C5G H5G 119.8 . .
C5G C6G C1G 120.11(17) . .
C5G C6G H6G 119.9 . .
C1G C6G H6G 119.9 . .
C6H C1H C2H 119.97(16) . .
C6H C1H P03 119.73(13) . .
C2H C1H P03 120.16(14) . .
C3H C2H C1H 119.93(18) . .
C3H C2H H2H 120.0 . .
C1H C2H H2H 120.0 . .
C4H C3H C2H 119.81(18) . .
C4H C3H H3H 120.1 . .
C2H C3H H3H 120.1 . .
C3H C4H C5H 120.58(17) . .
C3H C4H H4H 119.7 . .
C5H C4H H4H 119.7 . .
C4H C5H C6H 120.09(18) . .
C4H C5H H5H 120.0 . .
C6H C5H H5H 120.0 . .
C1H C6H C5H 119.60(17) . .
C1H C6H H6H 120.2 . .
C5H C6H H6H 120.2 . .
C2I C1I C6I 119.84(17) . .
C2I C1I P03 121.69(14) . .
C6I C1I P03 118.47(14) . .
C3I C2I C1I 119.50(19) . .
C3I C2I H2I 120.3 . .
C1I C2I H2I 120.3 . .
C4I C3I C2I 120.5(2) . .
C4I C3I H3I 119.7 . .
C2I C3I H3I 119.7 . .
C3I C4I C5I 120.03(19) . .
C3I C4I H4I 120.0 . .
C5I C4I H4I 120.0 . .
C6I C5I C4I 120.06(18) . .
C6I C5I H5I 120.0 . .
C4I C5I H5I 120.0 . .
C5I C6I C1I 119.99(17) . .
C5I C6I H6I 120.0 . .
C1I C6I H6I 120.0 . .
C2J C1J C6J 119.72(17) . .
C2J C1J P04 119.26(14) . .
C6J C1J P04 120.97(14) . .
C3J C2J C1J 119.83(18) . .
C3J C2J H2J 120.1 . .
C1J C2J H2J 120.1 . .
C2J C3J C4J 120.27(19) . .
C2J C3J H3J 119.9 . .
C4J C3J H3J 119.9 . .
C5J C4J C3J 120.24(18) . .
C5J C4J H4J 119.9 . .
C3J C4J H4J 119.9 . .
C6J C5J C4J 119.74(17) . .
C6J C5J H5J 120.1 . .
C4J C5J H5J 120.1 . .
C5J C6J C1J 120.18(17) . .
C5J C6J H6J 119.9 . .
C1J C6J H6J 119.9 . .
C2K C1K C6K 120.04(17) . .
C2K C1K P04 120.17(14) . .
C6K C1K P04 119.66(15) . .
C1K C2K C3K 119.95(18) . .
C1K C2K H2K 120.0 . .
C3K C2K H2K 120.0 . .
C4K C3K C2K 120.0(2) . .
C4K C3K H3K 120.0 . .
C2K C3K H3K 120.0 . .
C5K C4K C3K 120.0(2) . .
C5K C4K H4K 120.0 . .
C3K C4K H4K 120.0 . .
C4K C5K C6K 120.49(19) . .
C4K C5K H5K 119.8 . .
C6K C5K H5K 119.8 . .
C5K C6K C1K 119.48(19) . .
C5K C6K H6K 120.3 . .
C1K C6K H6K 120.3 . .
C2L C1L C6L 119.59(17) . .
C2L C1L P04 124.11(14) . .
C6L C1L P04 116.07(14) . .
C3L C2L C1L 119.77(19) . .
C3L C2L H2L 120.1 . .
C1L C2L H2L 120.1 . .
C4L C3L C2L 120.2(2) . .
C4L C3L H3L 119.9 . .
C2L C3L H3L 119.9 . .
C5L C4L C3L 120.3(2) . .
C5L C4L H4L 119.8 . .
C3L C4L H4L 119.8 . .
C4L C5L C6L 120.0(2) . .
C4L C5L H5L 120.0 . .
C6L C5L H5L 120.0 . .
C5L C6L C1L 120.09(19) . .
C5L C6L H6L 120.0 . .
C1L C6L H6L 120.0 . .
O3A C31 C33 123.9(3) . .
O3A C31 C32 122.8(3) . .
C33 C31 C32 113.3(3) . .
C31 C32 H32A 109.5 . .
C31 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
C31 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
C31 C33 H33A 109.5 . .
C31 C33 H33B 109.5 . .
H33A C33 H33B 109.5 . .
C31 C33 H33C 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
N0A1 C0A1 C0A2 179.2(3) . .
C0A1 C0A2 H0A1 109.5 . .
C0A1 C0A2 H0A2 109.5 . .
H0A1 C0A2 H0A2 109.5 . .
C0A1 C0A2 H0A3 109.5 . .
H0A1 C0A2 H0A3 109.5 . .
H0A2 C0A2 H0A3 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O1 1.6252(13) .
Ti1 O4 1.9844(13) 2_776
Ti1 O2 1.9909(12) .
Ti1 O3 1.9939(13) .
Ti1 O5 2.0014(13) 2_776
O2 P1 1.5028(12) .
O3 P4 1.5073(13) .
O4 P2 1.5031(13) .
O4 Ti1 1.9844(13) 2_776
O5 P3 1.5035(13) .
O5 Ti1 2.0014(13) 2_776
O6 P1 1.5968(12) .
O6 P2 1.6013(12) .
O7 P2 1.6043(13) .
O7 P3 1.6074(12) .
O8 P3 1.6037(13) .
O8 P4 1.6048(13) .
O9 P1 1.6072(12) .
O9 P4 1.6121(12) .
P1 O01 1.4587(13) .
P2 O03 1.4588(13) .
P3 O05 1.4609(14) .
P4 O06 1.4612(13) .
N1 P02 1.5839(15) .
N1 P01 1.5842(15) .
P01 C1A 1.7954(17) .
P01 C1B 1.7975(18) .
P01 C1C 1.7988(18) .
P02 C1D 1.8004(17) .
P02 C1F 1.8005(18) .
P02 C1E 1.8022(18) .
C1A C6A 1.395(2) .
C1A C2A 1.399(2) .
C2A C3A 1.389(2) .
C2A H2A 0.9500 .
C3A C4A 1.392(3) .
C3A H3A 0.9500 .
C4A C5A 1.383(3) .
C4A H4A 0.9500 .
C5A C6A 1.394(2) .
C5A H5A 0.9500 .
C6A H6A 0.9500 .
C1B C2B 1.394(3) .
C1B C3B 1.397(3) .
C2B C6B 1.389(3) .
C2B H2B 0.9500 .
C3B C5B 1.388(3) .
C3B H3B 0.9500 .
C4B C5B 1.388(3) .
C4B C6B 1.389(3) .
C4B H4B 0.9500 .
C5B H5B 0.9500 .
C6B H6B 0.9500 .
C1C C6C 1.399(3) .
C1C C2C 1.404(2) .
C2C C3C 1.386(3) .
C2C H2C 0.9500 .
C3C C4C 1.384(3) .
C3C H3C 0.9500 .
C4C C5C 1.386(3) .
C4C H4C 0.9500 .
C5C C6C 1.386(3) .
C5C H5C 0.9500 .
C6C H6C 0.9500 .
C1D C2D 1.387(3) .
C1D C6D 1.395(3) .
C2D C3D 1.392(3) .
C2D H2D 0.9500 .
C3D C4D 1.382(3) .
C3D H3D 0.9500 .
C4D C5D 1.380(3) .
C4D H4D 0.9500 .
C5D C6D 1.388(3) .
C5D H5D 0.9500 .
C6D H6D 0.9500 .
C1E C2E 1.368(3) .
C1E C6E 1.377(3) .
C2E C3E 1.393(3) .
C2E H2E 0.9500 .
C3E C4E 1.364(4) .
C3E H3E 0.9500 .
C4E C5E 1.355(3) .
C4E H4E 0.9500 .
C5E C6E 1.400(3) .
C5E H5E 0.9500 .
C1F C6F 1.401(2) .
C1F C2F 1.401(2) .
C2F C3F 1.390(3) .
C2F H2F 0.9500 .
C3F C4F 1.385(3) .
C3F H3F 0.9500 .
C4F C5F 1.386(3) .
C4F H4F 0.9500 .
C5F C6F 1.391(3) .
C5F H5F 0.9500 .
C6F H6F 0.9500 .
N2 P03 1.5817(15) .
N2 P04 1.5870(15) .
P03 C1H 1.7927(17) .
P03 C1I 1.7933(18) .
P03 C1G 1.8008(18) .
P04 C1K 1.7946(18) .
P04 C1J 1.7993(18) .
P04 C1L 1.8000(19) .
C1G C2G 1.393(2) .
C1G C6G 1.395(2) .
C2G C3G 1.387(3) .
C2G H2G 0.9500 .
C3G C4G 1.383(3) .
C3G H3G 0.9500 .
C4G C5G 1.386(3) .
C4G H4G 0.9500 .
C5G C6G 1.386(3) .
C5G H5G 0.9500 .
C6G H6G 0.9500 .
C1H C6H 1.392(3) .
C1H C2H 1.395(2) .
C2H C3H 1.393(3) .
C2H H2H 0.9500 .
C3H C4H 1.381(3) .
C3H H3H 0.9500 .
C4H C5H 1.383(3) .
C4H H4H 0.9500 .
C5H C6H 1.394(2) .
C5H H5H 0.9500 .
C6H H6H 0.9500 .
C1I C2I 1.393(3) .
C1I C6I 1.397(2) .
C2I C3I 1.387(3) .
C2I H2I 0.9500 .
C3I C4I 1.383(3) .
C3I H3I 0.9500 .
C4I C5I 1.386(3) .
C4I H4I 0.9500 .
C5I C6I 1.383(3) .
C5I H5I 0.9500 .
C6I H6I 0.9500 .
C1J C2J 1.392(3) .
C1J C6J 1.401(2) .
C2J C3J 1.388(3) .
C2J H2J 0.9500 .
C3J C4J 1.389(3) .
C3J H3J 0.9500 .
C4J C5J 1.389(3) .
C4J H4J 0.9500 .
C5J C6J 1.388(3) .
C5J H5J 0.9500 .
C6J H6J 0.9500 .
C1K C2K 1.389(3) .
C1K C6K 1.398(2) .
C2K C3K 1.390(3) .
C2K H2K 0.9500 .
C3K C4K 1.388(3) .
C3K H3K 0.9500 .
C4K C5K 1.384(3) .
C4K H4K 0.9500 .
C5K C6K 1.387(3) .
C5K H5K 0.9500 .
C6K H6K 0.9500 .
C1L C2L 1.392(3) .
C1L C6L 1.400(3) .
C2L C3L 1.391(3) .
C2L H2L 0.9500 .
C3L C4L 1.387(3) .
C3L H3L 0.9500 .
C4L C5L 1.381(3) .
C4L H4L 0.9500 .
C5L C6L 1.386(3) .
C5L H5L 0.9500 .
C6L H6L 0.9500 .
O3A C31 1.145(3) .
C31 C33 1.482(5) .
C31 C32 1.541(5) .
C32 H32A 0.9800 .
C32 H32B 0.9800 .
C32 H32C 0.9800 .
C33 H33A 0.9800 .
C33 H33B 0.9800 .
C33 H33C 0.9800 .
N0A1 C0A1 1.133(3) .
C0A1 C0A2 1.457(3) .
C0A2 H0A1 0.9800 .
C0A2 H0A2 0.9800 .
C0A2 H0A3 0.9800 .
