# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_C1
_database_code_depnum_ccdc_archive 'CCDC 1841900'
_audit_update_record             
;
2018-05-22 deposited with the CCDC.
2018-06-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H56 O16 P2 Ti4'
_chemical_formula_sum            'C36 H56 O16 P2 Ti4'
_chemical_formula_weight         998.34

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'
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -y, -z'

_cell_length_a                   12.7384(11)
_cell_length_b                   13.8895(8)
_cell_length_c                   15.5231(14)
_cell_angle_alpha                115.032(7)
_cell_angle_beta                 103.585(8)
_cell_angle_gamma                95.731(6)
_cell_volume                     2356.2(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3342
_cell_measurement_theta_min      3.2530
_cell_measurement_theta_max      25.4570

_exptl_crystal_description       block
_exptl_crystal_colour            'orange red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_F_000             1036
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    0.783
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.27337
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1213
_diffrn_reflns_number            18054
_diffrn_reflns_av_unetI/netI     0.0905
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.044
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             9248
_reflns_number_gt                5799
_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       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.1016P)²+3.6596P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9248
_refine_ls_number_parameters     590
_refine_ls_number_restraints     172
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_gt           0.0735
_refine_ls_wR_factor_ref         0.2272
_refine_ls_wR_factor_gt          0.1877
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.028
_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_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 0.03858(8) 0.29965(7) 0.40843(7) 0.0323(2) Uani 1 1 d . . . . .
Ti2 Ti -0.15765(8) 0.46171(8) 0.36159(7) 0.0359(3) Uani 1 1 d . U . . .
Ti3 Ti -0.19368(8) 0.30279(8) 0.44747(7) 0.0368(3) Uani 1 1 d . . . . .
Ti4 Ti -0.19865(12) 0.36316(10) 0.12760(9) 0.0590(4) Uani 1 1 d . . . . .
P1 P 0.08311(12) 0.47404(11) 0.32758(10) 0.0340(3) Uani 1 1 d . . . . .
P2 P -0.18635(14) 0.19255(12) 0.23096(12) 0.0448(4) Uani 1 1 d . . . . .
O1 O -0.0817(3) 0.3815(3) 0.4129(2) 0.0289(7) Uani 1 1 d . . . . .
O2 O 0.1221(3) 0.4050(3) 0.5438(3) 0.0361(8) Uani 1 1 d . . . . .
O3 O 0.1081(3) 0.3840(3) 0.3547(3) 0.0379(9) Uani 1 1 d . . . . .
O4 O 0.1377(3) 0.5852(3) 0.4158(3) 0.0432(9) Uani 1 1 d . . . . .
O5 O -0.0418(3) 0.4650(3) 0.2884(3) 0.0437(9) Uani 1 1 d . . . . .
O6 O -0.0639(3) 0.1992(3) 0.2671(3) 0.0425(9) Uani 1 1 d . . . . .
O7 O -0.2449(3) 0.1887(3) 0.3042(3) 0.0460(10) Uani 1 1 d . . . . .
O8 O -0.2070(3) 0.2925(3) 0.2150(3) 0.0474(10) Uani 1 1 d . U . . .
O9 O -0.2486(3) 0.4788(3) 0.2494(3) 0.0436(9) Uani 1 1 d . . . . .
O10 O -0.1707(4) 0.4911(4) 0.1144(3) 0.0640(13) Uani 1 1 d . . . . .
O11 O -0.3299(5) 0.3009(4) 0.0396(4) 0.0857(17) Uani 1 1 d . . . . .
O12 O -0.1077(5) 0.2950(4) 0.0670(4) 0.0857(17) Uani 1 1 d . . . . .
O13 O 0.1260(3) 0.2060(3) 0.3927(3) 0.0430(9) Uani 1 1 d . . . . .
O14 O -0.0631(3) 0.2381(3) 0.4631(3) 0.0377(9) Uani 1 1 d . . . . .
O15 O -0.2972(4) 0.2330(4) 0.4713(4) 0.0593(12) Uani 1 1 d . U . . .
O16 O -0.2735(3) 0.3981(3) 0.4014(3) 0.0410(9) Uani 1 1 d . . . . .
C1 C 0.1463(5) 0.4672(4) 0.2350(4) 0.0400(13) Uani 1 1 d . . . . .
C2 C 0.2388(6) 0.4253(6) 0.2304(6) 0.069(2) Uani 1 1 d . . . . .
H2 H 0.264151 0.394471 0.271852 0.083 Uiso 1 1 calc R U . . .
C3 C 0.2952(7) 0.4279(7) 0.1654(7) 0.085(3) Uani 1 1 d . . . . .
H3 H 0.357993 0.399259 0.163185 0.102 Uiso 1 1 calc R U . . .
C4 C 0.2582(8) 0.4728(7) 0.1044(6) 0.080(2) Uani 1 1 d . . . . .
H4 H 0.297304 0.477223 0.062152 0.096 Uiso 1 1 calc R U . . .
C5 C 0.1648(8) 0.5108(7) 0.1053(6) 0.083(2) Uani 1 1 d . . . . .
H5 H 0.138492 0.538415 0.061342 0.100 Uiso 1 1 calc R U . . .
C6 C 0.1078(6) 0.5093(6) 0.1702(5) 0.0652(19) Uani 1 1 d . . . . .
H6 H 0.043898 0.536463 0.170459 0.078 Uiso 1 1 calc R U . . .
C7 C -0.2455(6) 0.0700(5) 0.1168(5) 0.0544(17) Uani 1 1 d . . . . .
C8 C -0.2028(7) -0.0203(6) 0.1059(6) 0.085(3) Uani 1 1 d . . . . .
H8 H -0.143296 -0.016017 0.156383 0.102 Uiso 1 1 calc R U . . .
C9 C -0.2508(9) -0.1198(7) 0.0169(8) 0.111(4) Uani 1 1 d . . . . .
H9 H -0.222723 -0.181094 0.009644 0.133 Uiso 1 1 calc R U . . .
C10 C -0.3354(9) -0.1270(8) -0.0568(7) 0.104(3) Uani 1 1 d . . . . .
H10 H -0.365660 -0.192582 -0.115023 0.125 Uiso 1 1 calc R U . . .
C11 C -0.3765(8) -0.0380(8) -0.0457(7) 0.110(4) Uani 1 1 d . . . . .
H11 H -0.435283 -0.042706 -0.096897 0.132 Uiso 1 1 calc R U . . .
C12 C -0.3319(7) 0.0613(6) 0.0419(6) 0.089(3) Uani 1 1 d . . . . .
H12 H -0.361921 0.121519 0.048479 0.107 Uiso 1 1 calc R U . . .
C13 C -0.2445(5) 0.5756(5) 0.2437(4) 0.0454(14) Uani 1 1 d . . . . .
C14 C -0.2764(6) 0.6640(6) 0.3072(5) 0.0644(19) Uani 1 1 d . . . . .
H14 H -0.303284 0.661128 0.356994 0.077 Uiso 1 1 calc R U . . .
C15 C -0.2670(7) 0.7594(6) 0.2942(6) 0.073(2) Uani 1 1 d . . . . .
H15 H -0.288147 0.819929 0.335981 0.088 Uiso 1 1 calc R U . . .
C16 C -0.2277(7) 0.7632(6) 0.2221(6) 0.077(2) Uani 1 1 d . . . . .
H16 H -0.223407 0.825884 0.213927 0.093 Uiso 1 1 calc R U . . .
C17 C -0.1939(7) 0.6757(6) 0.1604(6) 0.071(2) Uani 1 1 d . . . . .
H17 H -0.165256 0.679959 0.111958 0.085 Uiso 1 1 calc R U . . .
C18 C -0.2029(6) 0.5806(5) 0.1707(5) 0.0550(17) Uani 1 1 d . . . . .
C19A C -0.412(4) 0.301(5) -0.026(2) 0.140(8) Uani 0.49(3) 1 d D U P A 1
H19A H -0.461787 0.240496 -0.029703 0.168 Uiso 0.49(3) 1 calc R U P A 1
C20A C -0.494(3) 0.371(3) -0.0175(19) 0.135(9) Uani 0.49(3) 1 d D U P A 1
H20A H -0.566084 0.328336 -0.033616 0.202 Uiso 0.49(3) 1 calc R U P A 1
H20B H -0.495506 0.401777 -0.062927 0.202 Uiso 0.49(3) 1 calc R U P A 1
H20C H -0.473114 0.429438 0.049628 0.202 Uiso 0.49(3) 1 calc R U P A 1
C21A C -0.420(3) 0.246(3) -0.1337(15) 0.150(9) Uani 0.49(3) 1 d D U P A 1
H21A H -0.357571 0.279493 -0.143989 0.224 Uiso 0.49(3) 1 calc R U P A 1
H21B H -0.487240 0.252223 -0.172459 0.224 Uiso 0.49(3) 1 calc R U P A 1
H21C H -0.420215 0.170252 -0.154284 0.224 Uiso 0.49(3) 1 calc R U P A 1
C19B C -0.413(3) 0.304(4) -0.043(3) 0.137(8) Uani 0.51(3) 1 d D U P A 2
H19B H -0.385663 0.349280 -0.070602 0.164 Uiso 0.51(3) 1 calc R U P A 2
C20B C -0.492(3) 0.347(2) 0.015(2) 0.143(9) Uani 0.51(3) 1 d D U P A 2
H20D H -0.553011 0.358018 -0.026998 0.215 Uiso 0.51(3) 1 calc R U P A 2
H20E H -0.453857 0.415388 0.072527 0.215 Uiso 0.51(3) 1 calc R U P A 2
H20F H -0.518086 0.295722 0.035114 0.215 Uiso 0.51(3) 1 calc R U P A 2
C21B C -0.469(3) 0.189(3) -0.1159(17) 0.145(8) Uani 0.51(3) 1 d D U P A 2
H21D H -0.509571 0.157010 -0.086232 0.218 Uiso 0.51(3) 1 calc R U P A 2
H21E H -0.413641 0.148937 -0.134628 0.218 Uiso 0.51(3) 1 calc R U P A 2
H21F H -0.518328 0.186736 -0.174099 0.218 Uiso 0.51(3) 1 calc R U P A 2
C22 C -0.0758(16) 0.2199(13) -0.0084(10) 0.185(5) Uani 1 1 d . U . . .
H22 H -0.003356 0.270344 0.017948 0.222 Uiso 1 1 d DR U . . .
C23 C -0.0186(14) 0.1455(11) 0.0233(11) 0.187(6) Uani 1 1 d . U . . .
H23A H -0.019029 0.161911 0.089814 0.280 Uiso 1 1 calc R U . . .
H23B H -0.056773 0.071141 -0.021680 0.280 Uiso 1 1 calc R U . . .
H23C H 0.056576 0.156021 0.022102 0.280 Uiso 1 1 calc DR U . . .
C24 C -0.0900(16) 0.2199(14) -0.0946(10) 0.205(6) Uani 1 1 d . U . . .
H24A H -0.164214 0.181510 -0.137159 0.307 Uiso 1 1 calc R U . . .
H24B H -0.038134 0.184379 -0.125392 0.307 Uiso 1 1 calc R U . . .
H24C H -0.078155 0.293667 -0.084669 0.307 Uiso 1 1 calc R U . . .
C25 C 0.1640(7) 0.1181(6) 0.3326(7) 0.082(3) Uani 1 1 d . . . . .
H25 H 0.096804 0.063519 0.283870 0.099 Uiso 1 1 calc R U . . .
C26 C 0.2178(11) 0.0669(10) 0.3880(10) 0.156(6) Uani 1 1 d . . . . .
H26A H 0.288635 0.113200 0.432688 0.234 Uiso 1 1 calc R U . . .
H26B H 0.227968 -0.001781 0.342695 0.234 Uiso 1 1 calc R U . . .
H26C H 0.172767 0.055034 0.425821 0.234 Uiso 1 1 calc R U . . .
C27 C 0.2204(12) 0.1450(10) 0.2754(10) 0.155(6) Uani 1 1 d . . . . .
H27A H 0.182023 0.188288 0.250151 0.233 Uiso 1 1 calc R U . . .
H27B H 0.223191 0.079381 0.220477 0.233 Uiso 1 1 calc R U . . .
H27C H 0.294422 0.185715 0.316360 0.233 Uiso 1 1 calc R U . . .
C28 C -0.0390(5) 0.1616(5) 0.5025(5) 0.0491(15) Uani 1 1 d . . . . .
H28 H 0.038448 0.156935 0.508406 0.059 Uiso 1 1 calc R U . . .
C29 C -0.1123(7) 0.0499(5) 0.4265(6) 0.078(2) Uani 1 1 d . . . . .
H29A H -0.188742 0.052618 0.419373 0.117 Uiso 1 1 calc R U . . .
H29B H -0.095004 -0.002971 0.448840 0.117 Uiso 1 1 calc R U . . .
H29C H -0.099496 0.029716 0.363185 0.117 Uiso 1 1 calc R U . . .
C30 C -0.0515(7) 0.2039(6) 0.6046(6) 0.070(2) Uani 1 1 d . . . . .
H30A H -0.004998 0.275680 0.646606 0.105 Uiso 1 1 calc R U . . .
H30B H -0.030271 0.156205 0.632474 0.105 Uiso 1 1 calc R U . . .
H30C H -0.127458 0.206883 0.600365 0.105 Uiso 1 1 calc R U . . .
C31A C -0.3745(19) 0.1909(15) 0.5034(16) 0.110(4) Uani 0.514(18) 1 d D U P B 1
H31A H -0.320595 0.174459 0.548898 0.131 Uiso 0.514(18) 1 d R U P B 1
C32A C -0.427(2) 0.0770(16) 0.434(2) 0.143(7) Uani 0.514(18) 1 d D U P B 1
H32A H -0.397301 0.054104 0.378707 0.215 Uiso 0.514(18) 1 d R U P B 1
H32B H -0.505871 0.066184 0.409477 0.215 Uiso 0.514(18) 1 d R U P B 1
H32C H -0.409501 0.034774 0.468667 0.215 Uiso 0.514(18) 1 d R U P B 1
C33A C -0.387(2) 0.270(2) 0.5964(17) 0.156(7) Uani 0.514(18) 1 d D U P B 1
H33A H -0.330196 0.287657 0.657393 0.234 Uiso 0.514(18) 1 d R U P B 1
H33B H -0.458176 0.250347 0.602413 0.234 Uiso 0.514(18) 1 d R U P B 1
H33C H -0.383646 0.331667 0.583603 0.234 Uiso 0.514(18) 1 d R U P B 1
C31B C -0.408(2) 0.1716(18) 0.4593(15) 0.118(5) Uani 0.486(18) 1 d D U P B 2
H31B H -0.357422 0.127372 0.473582 0.141 Uiso 0.486(18) 1 d R U P B 2
C32B C -0.450(2) 0.078(2) 0.361(2) 0.162(10) Uani 0.486(18) 1 d D U P B 2
H32D H -0.497561 0.104848 0.322667 0.243 Uiso 0.486(18) 1 d R U P B 2
H32E H -0.492981 0.016268 0.360107 0.243 Uiso 0.486(18) 1 d R U P B 2
H32F H -0.392321 0.055788 0.332097 0.243 Uiso 0.486(18) 1 d R U P B 2
C33B C -0.414(2) 0.194(3) 0.5580(19) 0.146(7) Uani 0.486(18) 1 d D U P B 2
H33D H -0.343295 0.214650 0.607221 0.219 Uiso 0.486(18) 1 d R U P B 2
H33E H -0.461405 0.136630 0.559031 0.219 Uiso 0.486(18) 1 d R U P B 2
H33F H -0.447395 0.256160 0.572771 0.219 Uiso 0.486(18) 1 d R U P B 2
C34 C -0.3856(5) 0.4076(6) 0.4009(6) 0.0657(19) Uani 1 1 d . . . . .
H34 H -0.400648 0.385127 0.449603 0.079 Uiso 1 1 calc R U . . .
C35 C -0.4648(7) 0.3269(10) 0.3018(9) 0.137(5) Uani 1 1 d . . . . .
H35A H -0.464965 0.353693 0.254016 0.205 Uiso 1 1 calc R U . . .
H35B H -0.537952 0.316390 0.307627 0.205 Uiso 1 1 calc R U . . .
H35C H -0.442402 0.258676 0.279959 0.205 Uiso 1 1 calc R U . . .
C36 C -0.3911(9) 0.5251(8) 0.4402(10) 0.130(5) Uani 1 1 d . . . . .
H36A H -0.345527 0.565023 0.508634 0.196 Uiso 1 1 calc R U . . .
H36B H -0.466418 0.530990 0.435802 0.196 Uiso 1 1 calc R U . . .
H36C H -0.364925 0.554515 0.401184 0.196 Uiso 1 1 calc R U . . .


_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 O13 1.772(4) . ?
Ti1 O2 1.930(4) . ?
Ti1 O3 1.955(4) . ?
Ti1 O1 1.994(3) . ?
Ti1 O14 2.009(4) . ?
Ti1 O6 2.041(4) . ?
Ti2 O2 1.735(4) 2_566 ?
Ti2 O1 1.848(3) . ?
Ti2 O9 1.972(4) . ?
Ti2 O16 1.993(4) . ?
Ti2 O5 2.071(4) . ?
Ti2 O8 2.368(4) . ?
Ti3 O15 1.759(4) . ?
Ti3 O4 1.925(4) 2_566 ?
Ti3 O14 1.982(4) . ?
Ti3 O7 2.003(4) . ?
Ti3 O16 2.006(4) . ?
Ti3 O1 2.016(3) . ?
Ti4 O11 1.746(6) . ?
Ti4 O12 1.760(5) . ?
Ti4 O10 1.882(5) . ?
Ti4 O8 1.997(4) . ?
Ti4 O9 2.182(4) . ?
Ti4 O5 2.515(4) . ?
P1 O4 1.514(4) . ?
P1 O3 1.517(4) . ?
P1 O5 1.536(4) . ?
P1 C1 1.780(5) . ?
P2 O6 1.508(4) . ?
P2 O7 1.515(4) . ?
P2 O8 1.547(4) . ?
P2 C7 1.781(6) . ?
O9 C13 1.381(7) . ?
O10 C18 1.352(8) . ?
O11 C19A 1.28(4) . ?
O11 C19B 1.48(5) . ?
O12 C22 1.378(10) . ?
O13 C25 1.402(7) . ?
O14 C28 1.458(6) . ?
O15 C31A 1.387(17) . ?
O15 C31B 1.50(2) . ?
O16 C34 1.446(7) . ?
C1 C2 1.369(9) . ?
C1 C6 1.385(8) . ?
C2 C3 1.378(10) . ?
C3 C4 1.362(11) . ?
C4 C5 1.349(11) . ?
C5 C6 1.379(9) . ?
C7 C12 1.353(10) . ?
C7 C8 1.377(10) . ?
C8 C9 1.419(11) . ?
C9 C10 1.334(13) . ?
C10 C11 1.350(13) . ?
C11 C12 1.403(11) . ?
C13 C14 1.381(9) . ?
C13 C18 1.382(9) . ?
C14 C15 1.420(9) . ?
C15 C16 1.346(11) . ?
C16 C17 1.377(11) . ?
C17 C18 1.393(9) . ?
C19A C21A 1.49(3) . ?
C19A C20A 1.49(3) . ?
C19B C21B 1.49(3) . ?
C19B C20B 1.49(3) . ?
C22 C24 1.308(15) . ?
C22 C23 1.500(10) . ?
C25 C27 1.403(12) . ?
C25 C26 1.433(12) . ?
C28 C30 1.494(9) . ?
C28 C29 1.521(9) . ?
C31A C33A 1.452(12) . ?
C31A C32A 1.456(12) . ?
C31B C33B 1.453(12) . ?
C31B C32B 1.454(12) . ?
C34 C35 1.493(12) . ?
C34 C36 1.496(11) . ?

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
O13 Ti1 O2 97.32(17) . . ?
O13 Ti1 O3 96.97(16) . . ?
O2 Ti1 O3 91.58(15) . . ?
O13 Ti1 O1 169.84(16) . . ?
O2 Ti1 O1 90.50(14) . . ?
O3 Ti1 O1 89.26(14) . . ?
O13 Ti1 O14 98.49(16) . . ?
O2 Ti1 O14 88.59(15) . . ?
O3 Ti1 O14 164.39(15) . . ?
O1 Ti1 O14 75.13(14) . . ?
O13 Ti1 O6 89.52(17) . . ?
O2 Ti1 O6 173.12(15) . . ?
O3 Ti1 O6 88.39(16) . . ?
O1 Ti1 O6 82.62(14) . . ?
O14 Ti1 O6 89.59(16) . . ?
O2 Ti2 O1 106.93(16) 2_566 . ?
O2 Ti2 O9 100.72(16) 2_566 . ?
O1 Ti2 O9 151.84(16) . . ?
O2 Ti2 O16 99.57(17) 2_566 . ?
O1 Ti2 O16 79.15(15) . . ?
O9 Ti2 O16 101.64(16) . . ?
O2 Ti2 O5 101.53(17) 2_566 . ?
O1 Ti2 O5 89.03(15) . . ?
O9 Ti2 O5 80.24(16) . . ?
O16 Ti2 O5 158.07(16) . . ?
O2 Ti2 O8 170.77(16) 2_566 . ?
O1 Ti2 O8 80.70(14) . . ?
O9 Ti2 O8 71.29(14) . . ?
O16 Ti2 O8 86.83(15) . . ?
O5 Ti2 O8 72.97(15) . . ?
O15 Ti3 O4 92.82(19) . 2_566 ?
O15 Ti3 O14 107.03(19) . . ?
O4 Ti3 O14 91.73(16) 2_566 . ?
O15 Ti3 O7 89.88(19) . . ?
O4 Ti3 O7 177.17(17) 2_566 . ?
O14 Ti3 O7 86.68(16) . . ?
O15 Ti3 O16 102.49(19) . . ?
O4 Ti3 O16 93.12(16) 2_566 . ?
O14 Ti3 O16 149.79(16) . . ?
O7 Ti3 O16 87.10(17) . . ?
O15 Ti3 O1 176.64(18) . . ?
O4 Ti3 O1 89.58(15) 2_566 . ?
O14 Ti3 O1 75.23(14) . . ?
O7 Ti3 O1 87.75(15) . . ?
O16 Ti3 O1 75.01(14) . . ?
O11 Ti4 O12 104.7(3) . . ?
O11 Ti4 O10 99.4(2) . . ?
O12 Ti4 O10 98.5(2) . . ?
O11 Ti4 O8 99.4(2) . . ?
O12 Ti4 O8 100.0(2) . . ?
O10 Ti4 O8 149.22(19) . . ?
O11 Ti4 O9 98.1(2) . . ?
O12 Ti4 O9 157.2(2) . . ?
O10 Ti4 O9 78.38(17) . . ?
O8 Ti4 O9 75.05(15) . . ?
O11 Ti4 O5 163.6(2) . . ?
O12 Ti4 O5 90.3(2) . . ?
O10 Ti4 O5 84.65(18) . . ?
O8 Ti4 O5 70.87(15) . . ?
O9 Ti4 O5 66.97(14) . . ?
O4 P1 O3 110.8(2) . . ?
O4 P1 O5 110.1(2) . . ?
O3 P1 O5 112.6(2) . . ?
O4 P1 C1 105.1(2) . . ?
O3 P1 C1 108.2(2) . . ?
O5 P1 C1 109.7(3) . . ?
O6 P2 O7 112.3(2) . . ?
O6 P2 O8 110.9(2) . . ?
O7 P2 O8 107.5(2) . . ?
O6 P2 C7 108.1(3) . . ?
O7 P2 C7 107.8(3) . . ?
O8 P2 C7 110.3(3) . . ?
Ti2 O1 Ti1 145.99(19) . . ?
Ti2 O1 Ti3 105.21(16) . . ?
Ti1 O1 Ti3 103.86(14) . . ?
Ti2 O2 Ti1 148.9(2) 2_566 . ?
P1 O3 Ti1 136.1(2) . . ?
P1 O4 Ti3 159.1(2) . 2_566 ?
P1 O5 Ti2 126.7(2) . . ?
P1 O5 Ti4 138.9(2) . . ?
Ti2 O5 Ti4 87.17(14) . . ?
P2 O6 Ti1 125.2(2) . . ?
P2 O7 Ti3 121.4(2) . . ?
P2 O8 Ti4 144.2(2) . . ?
P2 O8 Ti2 115.8(2) . . ?
Ti4 O8 Ti2 93.07(14) . . ?
C13 O9 Ti2 125.1(3) . . ?
C13 O9 Ti4 109.1(3) . . ?
Ti2 O9 Ti4 99.69(16) . . ?
C18 O10 Ti4 120.0(4) . . ?
C19A O11 Ti4 150(4) . . ?
C19B O11 Ti4 145(3) . . ?
C22 O12 Ti4 157.6(10) . . ?
C25 O13 Ti1 151.7(5) . . ?
C28 O14 Ti3 131.2(4) . . ?
C28 O14 Ti1 124.2(3) . . ?
Ti3 O14 Ti1 104.56(16) . . ?
C31A O15 Ti3 171.8(8) . . ?
C31B O15 Ti3 160.8(10) . . ?
C34 O16 Ti2 135.3(4) . . ?
C34 O16 Ti3 124.3(4) . . ?
Ti2 O16 Ti3 100.36(16) . . ?
C2 C1 C6 118.5(6) . . ?
C2 C1 P1 120.0(5) . . ?
C6 C1 P1 121.3(5) . . ?
C1 C2 C3 121.2(7) . . ?
C4 C3 C2 119.5(8) . . ?
C5 C4 C3 120.1(7) . . ?
C4 C5 C6 121.1(7) . . ?
C5 C6 C1 119.5(7) . . ?
C12 C7 C8 119.0(6) . . ?
C12 C7 P2 122.8(6) . . ?
C8 C7 P2 118.1(6) . . ?
C7 C8 C9 119.2(8) . . ?
C10 C9 C8 121.2(9) . . ?
C9 C10 C11 119.2(8) . . ?
C10 C11 C12 121.1(9) . . ?
C7 C12 C11 120.3(8) . . ?
O9 C13 C14 123.6(6) . . ?
O9 C13 C18 115.5(5) . . ?
C14 C13 C18 120.9(6) . . ?
C13 C14 C15 118.1(7) . . ?
C16 C15 C14 120.6(7) . . ?
C15 C16 C17 121.0(7) . . ?
C16 C17 C18 119.7(7) . . ?
O10 C18 C13 116.4(6) . . ?
O10 C18 C17 123.9(7) . . ?
C13 C18 C17 119.6(7) . . ?
O11 C19A C21A 121(2) . . ?
O11 C19A C20A 131.6(19) . . ?
C21A C19A C20A 106(3) . . ?
O11 C19B C21B 106(4) . . ?
O11 C19B C20B 96(3) . . ?
C21B C19B C20B 106(3) . . ?
C24 C22 O12 122.2(11) . . ?
C24 C22 C23 125.7(11) . . ?
O12 C22 C23 112.0(10) . . ?
O13 C25 C27 112.0(7) . . ?
O13 C25 C26 111.3(8) . . ?
C27 C25 C26 117.2(9) . . ?
O14 C28 C30 109.6(5) . . ?
O14 C28 C29 107.8(5) . . ?
C30 C28 C29 115.2(6) . . ?
O15 C31A C33A 113.7(14) . . ?
O15 C31A C32A 111.6(13) . . ?
C33A C31A C32A 134.7(16) . . ?
C33B C31B C32B 134.8(17) . . ?
C33B C31B O15 108.3(14) . . ?
C32B C31B O15 110.1(15) . . ?
O16 C34 C35 109.5(6) . . ?
O16 C34 C36 109.4(6) . . ?
C35 C34 C36 118.6(9) . . ?

_refine_diff_density_max         1.520
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.095

####################################################################### 
# 
# 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_C2
_database_code_depnum_ccdc_archive 'CCDC 1841901'
_audit_update_record             
;
2018-05-22 deposited with the CCDC.
2018-06-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H58 O16 P2 Ti4'
_chemical_formula_sum            'C40 H58 O16 P2 Ti4'
_chemical_formula_weight         1048.40

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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.4222(3)
_cell_length_b                   26.1161(6)
_cell_length_c                   12.7525(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.683(2)
_cell_angle_gamma                90
_cell_volume                     5011.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    9324
_cell_measurement_theta_min      3.1170
_cell_measurement_theta_max      26.0830

_exptl_crystal_description       block
_exptl_crystal_colour            'orange yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_F_000             2176
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    0.740
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85955
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1213
_diffrn_reflns_number            43749
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.814
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             9806
_reflns_number_gt                6529
_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       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0814P)²+4.7098P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9806
_refine_ls_number_parameters     626
_refine_ls_number_restraints     182
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0590
_refine_ls_wR_factor_ref         0.1718
_refine_ls_wR_factor_gt          0.1461
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.050
_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 0.62117(4) 0.51851(3) 0.64695(5) 0.03617(19) Uani 1 1 d . . . . .
Ti2 Ti 0.46839(5) 0.59478(3) 0.64789(6) 0.0407(2) Uani 1 1 d . . . . .
Ti3 Ti 0.50604(4) 0.59328(3) 0.41330(6) 0.03720(19) Uani 1 1 d . . . . .
Ti4 Ti 0.81782(5) 0.56551(4) 0.67844(8) 0.0594(3) Uani 1 1 d . . . . .
P1 P 0.64065(8) 0.64364(4) 0.61067(9) 0.0460(3) Uani 1 1 d . . . . .
P2 P 0.66103(6) 0.51034(4) 0.41025(8) 0.0393(3) Uani 1 1 d . . . . .
O1 O 0.53477(16) 0.55529(10) 0.55385(19) 0.0347(6) Uani 1 1 d . . . . .
O2 O 0.58345(16) 0.45644(10) 0.6445(2) 0.0384(6) Uani 1 1 d . . . . .
O3 O 0.62184(18) 0.45797(11) 0.3787(2) 0.0500(7) Uani 1 1 d . . . . .
O4 O 0.69469(17) 0.51403(11) 0.5323(2) 0.0456(7) Uani 1 1 d . . . . .
O5 O 0.59621(17) 0.55253(11) 0.3652(2) 0.0439(7) Uani 1 1 d . . . . .
O6 O 0.60772(18) 0.63979(11) 0.4900(2) 0.0463(7) Uani 1 1 d . . . . .
O7 O 0.56470(19) 0.64763(11) 0.6688(2) 0.0491(7) Uani 1 1 d . . . . .
O8 O 0.69854(18) 0.59742(11) 0.6596(2) 0.0454(7) Uani 1 1 d . . . . .
O9 O 0.4848(2) 0.63633(11) 0.3043(2) 0.0505(7) Uani 1 1 d . . . . .
O10 O 0.42615(17) 0.62430(10) 0.5010(2) 0.0418(6) Uani 1 1 d . . . . .
O11 O 0.4114(2) 0.62648(12) 0.7351(2) 0.0572(8) Uani 1 1 d . U . . .
O12 O 0.55614(18) 0.55096(11) 0.7501(2) 0.0434(7) Uani 1 1 d . . . . .
O13 O 0.8728(3) 0.59297(16) 0.8001(4) 0.0976(14) Uani 1 1 d D . . . .
O14 O 0.8582(3) 0.59880(16) 0.5800(4) 0.0988(14) Uani 1 1 d D . . . .
O15 O 0.88464(19) 0.50496(13) 0.6744(3) 0.0625(9) Uani 1 1 d . . . . .
O16 O 0.74239(16) 0.50974(11) 0.7441(2) 0.0410(6) Uani 1 1 d . . . . .
C1 C 0.7069(3) 0.70022(19) 0.6381(4) 0.0594(12) Uani 1 1 d . . . . .
C2 C 0.7601(5) 0.7081(3) 0.7374(6) 0.116(3) Uani 1 1 d . . . . .
H2 H 0.764713 0.683440 0.790975 0.139 Uiso 1 1 calc R U . . .
C3 C 0.8077(7) 0.7541(3) 0.7568(8) 0.155(4) Uani 1 1 d . . . . .
H3 H 0.842598 0.760284 0.824901 0.186 Uiso 1 1 calc R U . . .
C4 C 0.8040(6) 0.7893(3) 0.6796(8) 0.135(3) Uani 1 1 d . . . . .
H4 H 0.836677 0.819358 0.694564 0.162 Uiso 1 1 calc R U . . .
C5 C 0.7539(6) 0.7815(3) 0.5815(7) 0.121(3) Uani 1 1 d . . . . .
H5 H 0.752119 0.805824 0.527799 0.146 Uiso 1 1 calc R U . . .
C6 C 0.7044(4) 0.7367(2) 0.5602(5) 0.0886(19) Uani 1 1 d . . . . .
H6 H 0.669088 0.731397 0.491973 0.106 Uiso 1 1 calc R U . . .
C7 C 0.7530(3) 0.51582(18) 0.3467(3) 0.0488(11) Uani 1 1 d . . . . .
C8 C 0.7405(3) 0.5380(3) 0.2466(4) 0.0810(18) Uani 1 1 d . . . . .
H8 H 0.686601 0.553681 0.216771 0.097 Uiso 1 1 calc R U . . .
C9 C 0.8071(4) 0.5372(3) 0.1902(5) 0.105(2) Uani 1 1 d . . . . .
H9 H 0.797835 0.551821 0.122166 0.126 Uiso 1 1 calc R U . . .
C10 C 0.8859(4) 0.5152(3) 0.2341(6) 0.094(2) Uani 1 1 d . . . . .
H10 H 0.930434 0.514157 0.195335 0.112 Uiso 1 1 calc R U . . .
C11 C 0.9011(3) 0.4943(3) 0.3349(5) 0.0859(19) Uani 1 1 d . . . . .
H11 H 0.956160 0.480163 0.365599 0.103 Uiso 1 1 calc R U . . .
C12 C 0.8338(3) 0.4945(2) 0.3905(4) 0.0645(14) Uani 1 1 d . . . . .
H12 H 0.843484 0.479986 0.458702 0.077 Uiso 1 1 calc R U . . .
C13 C 0.7851(3) 0.46348(17) 0.7599(3) 0.0444(10) Uani 1 1 d . . . . .
C14 C 0.8644(3) 0.46184(19) 0.7201(4) 0.0512(11) Uani 1 1 d . . . . .
C15 C 0.9119(3) 0.4173(2) 0.7278(4) 0.0678(14) Uani 1 1 d . . . . .
H15 H 0.962761 0.415776 0.700025 0.081 Uiso 1 1 calc R U . . .
C16 C 0.8850(3) 0.3738(2) 0.7767(5) 0.0688(14) Uani 1 1 d . . . . .
C17 C 0.9318(5) 0.3278(3) 0.7816(6) 0.102(2) Uani 1 1 d . . . . .
H17 H 0.982169 0.325720 0.752946 0.122 Uiso 1 1 calc R U . . .
C18 C 0.9038(6) 0.2862(3) 0.8281(8) 0.125(3) Uani 1 1 d . . . . .
H18 H 0.935313 0.255641 0.830761 0.151 Uiso 1 1 calc R U . . .
C19 C 0.8285(5) 0.2881(3) 0.8722(7) 0.119(3) Uani 1 1 d . . . . .
H19 H 0.811285 0.259591 0.906239 0.143 Uiso 1 1 calc R U . . .
C20 C 0.7812(4) 0.3317(2) 0.8648(6) 0.093(2) Uani 1 1 d . . . . .
H20 H 0.729808 0.332604 0.891739 0.111 Uiso 1 1 calc R U . . .
C21 C 0.8071(3) 0.3757(2) 0.8178(4) 0.0615(13) Uani 1 1 d . . . . .
C22 C 0.7576(3) 0.42210(19) 0.8069(4) 0.0558(12) Uani 1 1 d . . . . .
H22 H 0.705722 0.423897 0.832554 0.067 Uiso 1 1 calc R U . . .
C23 C 0.5092(8) 0.6750(3) 0.2386(6) 0.151(3) Uani 1 1 d . U . . .
H23 H 0.571387 0.668906 0.274101 0.181 Uiso 1 1 d DR U . . .
C24 C 0.5164(8) 0.7233(3) 0.2774(8) 0.177(4) Uani 1 1 d . U . . .
H24A H 0.564068 0.740543 0.254468 0.266 Uiso 1 1 calc R U . . .
H24B H 0.528615 0.722401 0.354517 0.266 Uiso 1 1 calc R U . . .
H24C H 0.461808 0.741379 0.250821 0.266 Uiso 1 1 calc R U . . .
C25 C 0.5235(10) 0.6553(4) 0.1414(7) 0.207(5) Uani 1 1 d . U . . .
H25A H 0.540363 0.683533 0.101777 0.311 Uiso 1 1 d R U . . .
H25B H 0.470103 0.640023 0.100577 0.311 Uiso 1 1 d R U . . .
H25C H 0.570283 0.630343 0.154527 0.311 Uiso 1 1 d DR U . . .
C26 C 0.3547(3) 0.6602(2) 0.4594(4) 0.0608(13) Uani 1 1 d . . . . .
H26 H 0.350218 0.664198 0.382011 0.073 Uiso 1 1 calc R U . . .
C27 C 0.2682(3) 0.6394(2) 0.4763(5) 0.0832(18) Uani 1 1 d . . . . .
H27A H 0.259559 0.605389 0.447165 0.125 Uiso 1 1 calc R U . . .
H27B H 0.220429 0.660991 0.440587 0.125 Uiso 1 1 calc R U . . .
H27C H 0.269304 0.638399 0.551780 0.125 Uiso 1 1 calc R U . . .
C28 C 0.3782(5) 0.7117(2) 0.5127(6) 0.093(2) Uani 1 1 d . . . . .
H28A H 0.388541 0.707840 0.589322 0.140 Uiso 1 1 calc R U . . .
H28B H 0.330090 0.735216 0.488874 0.140 Uiso 1 1 calc R U . . .
H28C H 0.430967 0.724677 0.493734 0.140 Uiso 1 1 calc R U . . .
C29 C 0.3569(6) 0.6379(3) 0.8053(7) 0.129(2) Uani 1 1 d D U . . .
H29 H 0.401489 0.645795 0.870746 0.155 Uiso 1 1 calc R U . . .
C30 C 0.3140(8) 0.5945(4) 0.8411(10) 0.195(5) Uani 1 1 d D U . . .
H30A H 0.304386 0.601147 0.911711 0.293 Uiso 1 1 calc R U . . .
H30B H 0.350889 0.564820 0.843022 0.293 Uiso 1 1 calc R U . . .
H30C H 0.257853 0.588689 0.792366 0.293 Uiso 1 1 calc R U . . .
C31 C 0.3066(8) 0.6840(4) 0.7923(10) 0.204(5) Uani 1 1 d D U . . .
H31A H 0.277107 0.687933 0.718236 0.306 Uiso 1 1 calc R U . . .
H31B H 0.345585 0.712555 0.814149 0.306 Uiso 1 1 calc R U . . .
H31C H 0.263151 0.682649 0.835872 0.306 Uiso 1 1 calc R U . . .
C32 C 0.5676(4) 0.5507(2) 0.8657(4) 0.0705(16) Uani 1 1 d . . . . .
H32 H 0.511195 0.561850 0.881694 0.085 Uiso 1 1 calc R U . . .
C33 C 0.5845(7) 0.4993(3) 0.9072(5) 0.134(3) Uani 1 1 d . . . . .
H33A H 0.539142 0.476700 0.869326 0.201 Uiso 1 1 calc R U . . .
H33B H 0.584089 0.498938 0.982383 0.201 Uiso 1 1 calc R U . . .
H33C H 0.641464 0.488013 0.897473 0.201 Uiso 1 1 calc R U . . .
C34 C 0.6368(6) 0.5904(4) 0.9129(5) 0.139(3) Uani 1 1 d . . . . .
H34A H 0.692413 0.581647 0.895377 0.209 Uiso 1 1 calc R U . . .
H34B H 0.643963 0.591159 0.989587 0.209 Uiso 1 1 calc R U . . .
H34C H 0.617914 0.623427 0.883673 0.209 Uiso 1 1 calc R U . . .
C35A C 0.935(2) 0.602(2) 0.892(2) 0.170(7) Uani 0.499(11) 1 d D U P A 1
H35A H 0.916929 0.629796 0.932720 0.204 Uiso 0.499(11) 1 d R U P A 1
C36A C 0.9630(13) 0.5571(9) 0.9596(15) 0.170(7) Uani 0.499(11) 1 d D U P A 1
H36A H 1.016629 0.539633 0.953995 0.256 Uiso 0.499(11) 1 d R U P A 1
H36B H 0.915229 0.532813 0.951675 0.256 Uiso 0.499(11) 1 d R U P A 1
H36C H 0.971389 0.573293 1.028665 0.256 Uiso 0.499(11) 1 d R U P A 1
C37A C 1.0242(11) 0.6118(10) 0.8771(17) 0.176(7) Uani 0.499(11) 1 d D U P A 1
H37A H 1.065199 0.588247 0.919542 0.264 Uiso 0.499(11) 1 calc R U P A 1
H37B H 1.040825 0.646225 0.899386 0.264 Uiso 0.499(11) 1 calc R U P A 1
H37C H 1.025568 0.607803 0.802616 0.264 Uiso 0.499(11) 1 calc R U P A 1
C35B C 0.948(2) 0.5982(19) 0.8787(18) 0.163(7) Uani 0.501(11) 1 d D U P A 2
H35B H 0.996975 0.574064 0.879722 0.196 Uiso 0.501(11) 1 d R U P A 2
C36B C 0.9103(15) 0.5969(10) 0.9743(16) 0.186(7) Uani 0.501(11) 1 d D U P A 2
H36D H 0.954156 0.608015 1.035662 0.278 Uiso 0.501(11) 1 calc R U P A 2
H36E H 0.892150 0.562587 0.985959 0.278 Uiso 0.501(11) 1 calc R U P A 2
H36F H 0.859712 0.619260 0.964053 0.278 Uiso 0.501(11) 1 calc R U P A 2
C37B C 0.9752(14) 0.6518(9) 0.8974(17) 0.187(8) Uani 0.501(11) 1 d D U P A 2
H37D H 0.967376 0.669253 0.829757 0.280 Uiso 0.501(11) 1 calc R U P A 2
H37E H 1.036650 0.653234 0.933915 0.280 Uiso 0.501(11) 1 calc R U P A 2
H37F H 0.939467 0.667882 0.940751 0.280 Uiso 0.501(11) 1 calc R U P A 2
C38A C 0.893(2) 0.6357(12) 0.523(2) 0.164(6) Uani 0.364(15) 1 d D U P B 1
H38A H 0.942284 0.618914 0.500070 0.197 Uiso 0.364(15) 1 calc R U P B 1
C39A C 0.928(2) 0.6759(12) 0.577(2) 0.171(7) Uani 0.364(15) 1 d D U P B 1
H39A H 0.968578 0.692097 0.540321 0.257 Uiso 0.364(15) 1 d R U P B 1
H39B H 0.958538 0.665787 0.647502 0.257 Uiso 0.364(15) 1 d R U P B 1
H39C H 0.881078 0.699447 0.582111 0.257 Uiso 0.364(15) 1 d R U P B 1
C40A C 0.834(2) 0.6442(16) 0.436(2) 0.176(7) Uani 0.364(15) 1 d D U P B 1
H40A H 0.812551 0.612099 0.403184 0.264 Uiso 0.364(15) 1 calc R U P B 1
H40B H 0.784836 0.662864 0.452699 0.264 Uiso 0.364(15) 1 calc R U P B 1
H40C H 0.859637 0.663783 0.387005 0.264 Uiso 0.364(15) 1 calc R U P B 1
C38B C 0.9180(11) 0.6217(9) 0.5281(13) 0.172(6) Uani 0.636(15) 1 d D U P B 2
H38B H 0.937203 0.589295 0.501808 0.206 Uiso 0.636(15) 1 calc R U P B 2
C39B C 0.9986(10) 0.6364(7) 0.5728(13) 0.174(6) Uani 0.636(15) 1 d D U P B 2
H39D H 1.039830 0.621669 0.534841 0.261 Uiso 0.636(15) 1 calc R U P B 2
H39E H 1.013174 0.625339 0.646365 0.261 Uiso 0.636(15) 1 calc R U P B 2
H39F H 1.002161 0.673090 0.570091 0.261 Uiso 0.636(15) 1 calc R U P B 2
C40B C 0.8864(15) 0.6398(10) 0.4327(15) 0.192(7) Uani 0.636(15) 1 d D U P B 2
H40D H 0.883511 0.676253 0.440598 0.288 Uiso 0.636(15) 1 d R U P B 2
H40E H 0.827531 0.626463 0.406948 0.288 Uiso 0.636(15) 1 d R U P B 2
H40F H 0.922331 0.631753 0.382278 0.288 Uiso 0.636(15) 1 d R U P B 2


_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 1.720(3) . ?
Ti1 O1 1.847(2) . ?
Ti1 O12 2.009(3) . ?
Ti1 O16 2.016(3) . ?
Ti1 O4 2.041(3) . ?
Ti1 O8 2.369(3) . ?
Ti2 O11 1.767(3) . ?
Ti2 O3 1.935(3) 3_666 ?
Ti2 O10 1.998(3) . ?
Ti2 O7 2.002(3) . ?
Ti2 O12 2.016(3) . ?
Ti2 O1 2.022(2) . ?
Ti3 O9 1.762(3) . ?
Ti3 O2 1.920(3) 3_666 ?
Ti3 O5 1.954(3) . ?
Ti3 O10 2.007(3) . ?
Ti3 O1 2.011(2) . ?
Ti3 O6 2.054(3) . ?
Ti4 O13 1.750(4) . ?
Ti4 O14 1.750(4) . ?
Ti4 O15 1.894(3) . ?
Ti4 O8 1.985(3) . ?
Ti4 O16 2.146(3) . ?
P1 O6 1.514(3) . ?
P1 O7 1.521(3) . ?
P1 O8 1.549(3) . ?
P1 C1 1.787(5) . ?
P2 O3 1.513(3) . ?
P2 O5 1.514(3) . ?
P2 O4 1.531(3) . ?
P2 C7 1.788(4) . ?
O9 C23 1.415(6) . ?
O10 C26 1.456(5) . ?
O11 C29 1.389(6) . ?
O12 C32 1.446(5) . ?
O13 C35A 1.358(12) . ?
O13 C35B 1.365(12) . ?
O14 C38A 1.381(11) . ?
O14 C38B 1.384(10) . ?
O15 C14 1.336(5) . ?
O16 C13 1.369(5) . ?
C1 C2 1.365(8) . ?
C1 C6 1.371(7) . ?
C2 C3 1.400(10) . ?
C3 C4 1.339(11) . ?
C4 C5 1.334(11) . ?
C5 C6 1.391(8) . ?
C7 C12 1.366(6) . ?
C7 C8 1.376(6) . ?
C8 C9 1.377(7) . ?
C9 C10 1.350(9) . ?
C10 C11 1.368(9) . ?
C11 C12 1.380(6) . ?
C13 C22 1.348(6) . ?
C13 C14 1.424(6) . ?
C14 C15 1.367(7) . ?
C15 C16 1.401(7) . ?
C16 C17 1.398(8) . ?
C16 C21 1.412(7) . ?
C17 C18 1.353(10) . ?
C18 C19 1.399(11) . ?
C19 C20 1.345(9) . ?
C20 C21 1.395(8) . ?
C21 C22 1.422(7) . ?
C23 C24 1.350(10) . ?
C23 C25 1.404(7) . ?
C26 C27 1.499(7) . ?
C26 C28 1.514(8) . ?
C29 C31 1.423(8) . ?
C29 C30 1.435(8) . ?
C32 C33 1.447(8) . ?
C32 C34 1.513(9) . ?
C35A C37A 1.45(3) . ?
C35A C36A 1.46(3) . ?
C35B C36B 1.46(3) . ?
C35B C37B 1.46(3) . ?
C38A C40A 1.297(13) . ?
C38A C39A 1.299(13) . ?
C38B C40B 1.296(11) . ?
C38B C39B 1.307(11) . ?

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 O1 106.56(12) . . ?
O2 Ti1 O12 101.19(12) . . ?
O1 Ti1 O12 78.94(11) . . ?
O2 Ti1 O16 99.69(12) . . ?
O1 Ti1 O16 153.46(12) . . ?
O12 Ti1 O16 100.04(11) . . ?
O2 Ti1 O4 99.89(12) . . ?
O1 Ti1 O4 90.29(11) . . ?
O12 Ti1 O4 158.33(12) . . ?
O16 Ti1 O4 81.25(11) . . ?
O2 Ti1 O8 169.81(11) . . ?
O1 Ti1 O8 82.70(11) . . ?
O12 Ti1 O8 84.54(11) . . ?
O16 Ti1 O8 70.84(11) . . ?
O4 Ti1 O8 75.41(11) . . ?
O11 Ti2 O3 90.36(14) . 3_666 ?
O11 Ti2 O10 107.73(13) . . ?
O3 Ti2 O10 92.08(12) 3_666 . ?
O11 Ti2 O7 92.86(14) . . ?
O3 Ti2 O7 176.74(12) 3_666 . ?
O10 Ti2 O7 86.48(12) . . ?
O11 Ti2 O12 102.40(13) . . ?
O3 Ti2 O12 93.67(12) 3_666 . ?
O10 Ti2 O12 149.26(11) . . ?
O7 Ti2 O12 86.11(12) . . ?
O11 Ti2 O1 176.87(13) . . ?
O3 Ti2 O1 88.34(11) 3_666 . ?
O10 Ti2 O1 75.17(10) . . ?
O7 Ti2 O1 88.47(11) . . ?
O12 Ti2 O1 74.85(10) . . ?
O9 Ti3 O2 97.77(13) . 3_666 ?
O9 Ti3 O5 97.00(13) . . ?
O2 Ti3 O5 90.71(11) 3_666 . ?
O9 Ti3 O10 98.71(13) . . ?
O2 Ti3 O10 90.54(11) 3_666 . ?
O5 Ti3 O10 163.93(11) . . ?
O9 Ti3 O1 169.89(13) . . ?
O2 Ti3 O1 90.44(10) 3_666 . ?
O5 Ti3 O1 88.75(11) . . ?
O10 Ti3 O1 75.22(10) . . ?
O9 Ti3 O6 89.34(13) . . ?
O2 Ti3 O6 172.77(11) 3_666 . ?
O5 Ti3 O6 87.13(12) . . ?
O10 Ti3 O6 89.65(12) . . ?
O1 Ti3 O6 82.62(11) . . ?
O13 Ti4 O14 104.7(2) . . ?
O13 Ti4 O15 101.87(18) . . ?
O14 Ti4 O15 96.56(17) . . ?
O13 Ti4 O8 100.99(17) . . ?
O14 Ti4 O8 99.82(17) . . ?
O15 Ti4 O8 147.37(13) . . ?
O13 Ti4 O16 97.51(17) . . ?
O14 Ti4 O16 157.81(19) . . ?
O15 Ti4 O16 77.80(12) . . ?
O8 Ti4 O16 76.39(11) . . ?
O6 P1 O7 112.19(17) . . ?
O6 P1 O8 113.12(17) . . ?
O7 P1 O8 107.12(16) . . ?
O6 P1 C1 107.7(2) . . ?
O7 P1 C1 108.5(2) . . ?
O8 P1 C1 108.1(2) . . ?
O3 P2 O5 111.41(17) . . ?
O3 P2 O4 110.68(17) . . ?
O5 P2 O4 112.82(16) . . ?
O3 P2 C7 105.21(19) . . ?
O5 P2 C7 107.08(18) . . ?
O4 P2 C7 109.26(18) . . ?
Ti1 O1 Ti3 144.68(13) . . ?
Ti1 O1 Ti2 105.76(12) . . ?
Ti3 O1 Ti2 103.63(11) . . ?
Ti1 O2 Ti3 148.85(15) . 3_666 ?
P2 O3 Ti2 156.94(18) . 3_666 ?
P2 O4 Ti1 127.87(16) . . ?
P2 O5 Ti3 137.22(16) . . ?
P1 O6 Ti3 125.02(16) . . ?
P1 O7 Ti2 121.06(17) . . ?
P1 O8 Ti4 144.34(17) . . ?
P1 O8 Ti1 114.41(15) . . ?
Ti4 O8 Ti1 94.74(11) . . ?
C23 O9 Ti3 153.5(5) . . ?
C26 O10 Ti2 130.9(3) . . ?
C26 O10 Ti3 124.5(3) . . ?
Ti2 O10 Ti3 104.65(12) . . ?
C29 O11 Ti2 164.0(4) . . ?
C32 O12 Ti1 134.4(3) . . ?
C32 O12 Ti2 125.2(3) . . ?
Ti1 O12 Ti2 100.18(11) . . ?
C35A O13 Ti4 161(3) . . ?
C35B O13 Ti4 149(3) . . ?
C38A O14 Ti4 164.1(15) . . ?
C38B O14 Ti4 159.6(8) . . ?
C14 O15 Ti4 120.8(3) . . ?
C13 O16 Ti1 122.8(2) . . ?
C13 O16 Ti4 111.8(2) . . ?
Ti1 O16 Ti4 101.07(11) . . ?
C2 C1 C6 118.9(5) . . ?
C2 C1 P1 120.5(4) . . ?
C6 C1 P1 120.6(4) . . ?
C1 C2 C3 118.5(7) . . ?
C4 C3 C2 121.5(8) . . ?
C5 C4 C3 120.5(7) . . ?
C4 C5 C6 119.4(7) . . ?
C1 C6 C5 121.1(6) . . ?
C12 C7 C8 118.7(4) . . ?
C12 C7 P2 121.6(4) . . ?
C8 C7 P2 119.4(3) . . ?
C7 C8 C9 120.6(5) . . ?
C10 C9 C8 119.8(6) . . ?
C9 C10 C11 120.8(5) . . ?
C10 C11 C12 119.3(5) . . ?
C7 C12 C11 120.8(5) . . ?
C22 C13 O16 125.8(4) . . ?
C22 C13 C14 120.8(4) . . ?
O16 C13 C14 113.4(4) . . ?
O15 C14 C15 125.2(4) . . ?
O15 C14 C13 115.5(4) . . ?
C15 C14 C13 119.2(4) . . ?
C14 C15 C16 121.0(5) . . ?
C17 C16 C15 121.1(6) . . ?
C17 C16 C21 119.1(6) . . ?
C15 C16 C21 119.7(5) . . ?
C18 C17 C16 120.0(7) . . ?
C17 C18 C19 121.3(7) . . ?
C20 C19 C18 119.3(7) . . ?
C19 C20 C21 121.7(7) . . ?
C20 C21 C16 118.6(5) . . ?
C20 C21 C22 123.0(5) . . ?
C16 C21 C22 118.4(5) . . ?
C13 C22 C21 120.8(4) . . ?
C24 C23 C25 130.5(7) . . ?
C24 C23 O9 117.5(6) . . ?
C25 C23 O9 112.0(6) . . ?
O10 C26 C27 109.9(4) . . ?
O10 C26 C28 108.7(4) . . ?
C27 C26 C28 113.1(5) . . ?
O11 C29 C31 119.9(7) . . ?
O11 C29 C30 115.0(6) . . ?
C31 C29 C30 115.3(8) . . ?
O12 C32 C33 110.4(5) . . ?
O12 C32 C34 108.7(5) . . ?
C33 C32 C34 115.8(6) . . ?
O13 C35A C37A 115(3) . . ?
O13 C35A C36A 116(3) . . ?
C37A C35A C36A 93(3) . . ?
O13 C35B C36B 100(2) . . ?
O13 C35B C37B 112(3) . . ?
C36B C35B C37B 92(3) . . ?
C40A C38A C39A 116.4(17) . . ?
C40A C38A O14 107(2) . . ?
C39A C38A O14 117(2) . . ?
C40B C38B C39B 115.4(12) . . ?
C40B C38B O14 116.9(13) . . ?
C39B C38B O14 126.1(12) . . ?

_refine_diff_density_max         0.944
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.071

####################################################################### 
# 
# 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 
# 
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# Please retain this information to preserve the provenance of 
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data_C3
_database_code_depnum_ccdc_archive 'CCDC 1841902'
_audit_update_record             
;
2018-05-22 deposited with the CCDC.
2018-06-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H50 N O12 P Ti3'
_chemical_formula_sum            'C30 H50 N O12 P Ti3'
_chemical_formula_weight         791.38

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'

_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                   14.5622(9)
_cell_length_b                   19.8886(8)
_cell_length_c                   14.7162(9)
_cell_angle_alpha                90
_cell_angle_beta                 110.627(7)
_cell_angle_gamma                90
_cell_volume                     3988.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2896
_cell_measurement_theta_min      2.9990
_cell_measurement_theta_max      24.8510

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_F_000             1656
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    0.679
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.41489
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1213
_diffrn_reflns_number            16063
_diffrn_reflns_av_unetI/netI     0.0912
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.958
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7827
_reflns_number_gt                4545
_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       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0546P)²+1.2583P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7827
_refine_ls_number_parameters     436
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_gt           0.0619
_refine_ls_wR_factor_ref         0.1548
_refine_ls_wR_factor_gt          0.1247
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.033
_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_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 0.73121(5) 0.51374(4) 0.55540(6) 0.0421(2) Uani 1 1 d . . . . .
Ti2 Ti 0.55252(5) 0.60757(4) 0.46511(6) 0.0399(2) Uani 1 1 d . . . . .
Ti3 Ti 0.57682(6) 0.43117(4) 0.38992(6) 0.0412(2) Uani 1 1 d . . . . .
P1 P 0.38601(8) 0.52661(6) 0.29504(8) 0.0420(3) Uani 1 1 d . . . . .
O1 O 0.59251(18) 0.51650(12) 0.46615(19) 0.0373(6) Uani 1 1 d . . . . .
O2 O 0.48351(19) 0.61976(12) 0.5414(2) 0.0427(7) Uani 1 1 d . . . . .
O3 O 0.3029(2) 0.51101(14) 0.3311(2) 0.0501(8) Uani 1 1 d . . . . .
O4 O 0.4435(2) 0.58790(13) 0.3452(2) 0.0470(7) Uani 1 1 d . . . . .
O5 O 0.4520(2) 0.46677(14) 0.3001(2) 0.0472(7) Uani 1 1 d . . . . .
O6 O 0.6497(2) 0.49022(14) 0.3152(2) 0.0518(8) Uani 1 1 d . . . . .
O7 O 0.7666(2) 0.54229(14) 0.4381(2) 0.0490(8) Uani 1 1 d . . . . .
O8 O 0.5860(2) 0.36644(14) 0.3087(2) 0.0518(8) Uani 1 1 d . . . . .
O9 O 0.70877(19) 0.42190(13) 0.4980(2) 0.0445(7) Uani 1 1 d . . . . .
O10 O 0.8570(2) 0.51386(14) 0.6254(2) 0.0535(8) Uani 1 1 d . . . . .
O11 O 0.6916(2) 0.60741(13) 0.5644(2) 0.0442(7) Uani 1 1 d . . . . .
O12 O 0.5748(2) 0.68420(16) 0.4124(3) 0.0711(10) Uani 1 1 d . . . . .
N1 N 0.8639(4) 0.6555(3) 0.0759(4) 0.0953(17) Uani 1 1 d . . . . .
C1 C 0.3304(4) 0.5489(2) 0.1697(3) 0.0517(12) Uani 1 1 d . . . . .
C2 C 0.2327(4) 0.5619(3) 0.1277(4) 0.092(2) Uani 1 1 d . . . . .
H2 H 0.192417 0.557792 0.164430 0.111 Uiso 1 1 calc R U . . .
C3 C 0.1924(6) 0.5812(4) 0.0317(5) 0.130(3) Uani 1 1 d . . . . .
H3 H 0.125593 0.590128 0.003715 0.156 Uiso 1 1 calc R U . . .
C4 C 0.2513(7) 0.5868(4) -0.0212(5) 0.115(3) Uani 1 1 d . . . . .
H4 H 0.224136 0.598970 -0.086239 0.138 Uiso 1 1 calc R U . . .
C5 C 0.3478(6) 0.5753(4) 0.0177(5) 0.109(2) Uani 1 1 d . . . . .
H5 H 0.387481 0.580854 -0.019343 0.130 Uiso 1 1 calc R U . . .
C6 C 0.3878(4) 0.5551(3) 0.1131(4) 0.0820(17) Uani 1 1 d . . . . .
H6 H 0.454467 0.545486 0.139666 0.098 Uiso 1 1 calc R U . . .
C7 C 0.7219(3) 0.5298(2) 0.3485(3) 0.0448(11) Uani 1 1 d . . . . .
C8 C 0.7576(3) 0.5641(2) 0.2772(4) 0.0479(11) Uani 1 1 d . . . . .
C9 C 0.7137(4) 0.5541(2) 0.1793(4) 0.0655(14) Uani 1 1 d . . . . .
H9 H 0.659619 0.525666 0.157202 0.079 Uiso 1 1 calc R U . . .
C10 C 0.7466(4) 0.5843(3) 0.1125(4) 0.0782(17) Uani 1 1 d . . . . .
H10 H 0.713720 0.576944 0.046512 0.094 Uiso 1 1 calc R U . . .
C11 C 0.8292(4) 0.6261(3) 0.1430(4) 0.0655(15) Uani 1 1 d . . . . .
C12 C 0.8738(4) 0.6370(2) 0.2421(4) 0.0611(14) Uani 1 1 d . . . . .
H12 H 0.928248 0.665041 0.264584 0.073 Uiso 1 1 calc R U . . .
C13 C 0.8389(3) 0.6070(2) 0.3074(4) 0.0528(12) Uani 1 1 d . . . . .
H13 H 0.869946 0.615454 0.373368 0.063 Uiso 1 1 calc R U . . .
C14 C 0.9514(5) 0.6964(3) 0.1078(5) 0.099(2) Uani 1 1 d . . . . .
H14A H 0.944680 0.730866 0.150672 0.148 Uiso 1 1 calc R U . . .
H14B H 0.960673 0.716760 0.052492 0.148 Uiso 1 1 calc R U . . .
H14C H 1.007065 0.668746 0.141407 0.148 Uiso 1 1 calc R U . . .
C15 C 0.8222(6) 0.6394(4) -0.0241(5) 0.150(3) Uani 1 1 d . . . . .
H15A H 0.829878 0.592214 -0.032880 0.225 Uiso 1 1 calc R U . . .
H15B H 0.854768 0.664595 -0.059526 0.225 Uiso 1 1 calc R U . . .
H15C H 0.753669 0.650602 -0.047607 0.225 Uiso 1 1 calc R U . . .
C16 C 0.5857(5) 0.3585(3) 0.2129(4) 0.0801(18) Uani 1 1 d . . . . .
H16 H 0.592635 0.403566 0.189105 0.096 Uiso 1 1 calc R U . . .
C17 C 0.6724(5) 0.3193(3) 0.2135(5) 0.110(2) Uani 1 1 d . . . . .
H17A H 0.730834 0.345201 0.243974 0.165 Uiso 1 1 calc R U . . .
H17B H 0.666647 0.308945 0.148022 0.165 Uiso 1 1 calc R U . . .
H17C H 0.675968 0.278272 0.249022 0.165 Uiso 1 1 calc R U . . .
C18 C 0.4906(6) 0.3323(4) 0.1490(5) 0.143(3) Uani 1 1 d . . . . .
H18A H 0.483320 0.286609 0.166396 0.214 Uiso 1 1 calc R U . . .
H18B H 0.487522 0.333992 0.082820 0.214 Uiso 1 1 calc R U . . .
H18C H 0.438756 0.359172 0.156099 0.214 Uiso 1 1 calc R U . . .
C19 C 0.7621(4) 0.3592(3) 0.5226(4) 0.0703(16) Uani 1 1 d . . . . .
H19 H 0.717630 0.324937 0.482619 0.084 Uiso 1 1 calc R U . . .
C20 C 0.7795(5) 0.3396(3) 0.6234(5) 0.111(2) Uani 1 1 d . . . . .
H20A H 0.830403 0.367212 0.666457 0.166 Uiso 1 1 calc R U . . .
H20B H 0.799138 0.293282 0.632607 0.166 Uiso 1 1 calc R U . . .
H20C H 0.720267 0.345505 0.637229 0.166 Uiso 1 1 calc R U . . .
C21 C 0.8475(4) 0.3587(3) 0.4925(5) 0.106(2) Uani 1 1 d . . . . .
H21A H 0.826442 0.364454 0.423387 0.158 Uiso 1 1 calc R U . . .
H21B H 0.881308 0.316607 0.510224 0.158 Uiso 1 1 calc R U . . .
H21C H 0.890778 0.394776 0.524037 0.158 Uiso 1 1 calc R U . . .
C22 C 0.9599(4) 0.5109(3) 0.6742(5) 0.0846(18) Uani 1 1 d . . . . .
H22 H 0.980723 0.465719 0.663068 0.101 Uiso 1 1 calc R U . . .
C23 C 0.9833(5) 0.5175(4) 0.7799(5) 0.130(3) Uani 1 1 d . . . . .
H23A H 0.959929 0.560022 0.793621 0.195 Uiso 1 1 calc R U . . .
H23B H 1.053063 0.514870 0.812481 0.195 Uiso 1 1 calc R U . . .
H23C H 0.952153 0.481824 0.802204 0.195 Uiso 1 1 calc R U . . .
C24 C 1.0112(5) 0.5584(4) 0.6329(7) 0.141(3) Uani 1 1 d . . . . .
H24A H 0.994808 0.549148 0.564947 0.212 Uiso 1 1 calc R U . . .
H24B H 1.080713 0.553781 0.665459 0.212 Uiso 1 1 calc R U . . .
H24C H 0.991660 0.603431 0.641035 0.212 Uiso 1 1 calc R U . . .
C25 C 0.7493(4) 0.6601(3) 0.6259(4) 0.0715(16) Uani 1 1 d . . . . .
H25 H 0.802243 0.637537 0.677545 0.086 Uiso 1 1 calc R U . . .
C26 C 0.6937(5) 0.6954(4) 0.6728(7) 0.169(4) Uani 1 1 d . . . . .
H26A H 0.633794 0.711273 0.625100 0.253 Uiso 1 1 calc R U . . .
H26B H 0.730985 0.733027 0.707788 0.253 Uiso 1 1 calc R U . . .
H26C H 0.678713 0.665870 0.717260 0.253 Uiso 1 1 calc R U . . .
C27 C 0.7983(5) 0.7013(3) 0.5703(5) 0.118(3) Uani 1 1 d . . . . .
H27A H 0.835863 0.672317 0.544617 0.178 Uiso 1 1 calc R U . . .
H27B H 0.840952 0.733775 0.612927 0.178 Uiso 1 1 calc R U . . .
H27C H 0.749250 0.724119 0.517988 0.178 Uiso 1 1 calc R U . . .
C28 C 0.5496(7) 0.7247(3) 0.3315(5) 0.137(3) Uani 1 1 d D U . . .
H28 H 0.488936 0.700037 0.297530 0.164 Uiso 1 1 calc DR U . . .
C29 C 0.5014(8) 0.7832(4) 0.3380(6) 0.206(4) Uani 1 1 d D U . . .
H29A H 0.544289 0.811237 0.388064 0.309 Uiso 1 1 calc R U . . .
H29B H 0.444187 0.772408 0.353260 0.309 Uiso 1 1 calc R U . . .
H29C H 0.481996 0.806527 0.277021 0.309 Uiso 1 1 calc R U . . .
C30 C 0.5904(7) 0.7106(5) 0.2623(6) 0.190(4) Uani 1 1 d D U . . .
H30A H 0.539730 0.709428 0.199324 0.285 Uiso 1 1 calc DR U . . .
H30B H 0.622633 0.667665 0.275843 0.285 Uiso 1 1 calc R U . . .
H30C H 0.637337 0.744744 0.263331 0.285 Uiso 1 1 calc R U . . .


_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 O10 1.757(3) . ?
Ti1 O3 1.965(3) 3_666 ?
Ti1 O11 1.968(3) . ?
Ti1 O1 1.985(3) . ?
Ti1 O9 1.991(3) . ?
Ti1 O7 2.048(3) . ?
Ti2 O2 1.768(3) . ?
Ti2 O12 1.790(3) . ?
Ti2 O1 1.901(3) . ?
Ti2 O4 1.953(3) . ?
Ti2 O11 2.038(3) . ?
Ti3 O8 1.793(3) . ?
Ti3 O2 1.856(3) 3_666 ?
Ti3 O5 1.964(3) . ?
Ti3 O1 2.002(3) . ?
Ti3 O9 2.025(3) . ?
Ti3 O6 2.129(3) . ?
P1 O4 1.515(3) . ?
P1 O5 1.515(3) . ?
P1 O3 1.516(3) . ?
P1 C1 1.789(5) . ?
O6 C7 1.267(5) . ?
O7 C7 1.273(5) . ?
O8 C16 1.417(6) . ?
O9 C19 1.447(5) . ?
O10 C22 1.416(6) . ?
O11 C25 1.446(5) . ?
O12 C28 1.375(6) . ?
N1 C11 1.388(6) . ?
N1 C15 1.416(8) . ?
N1 C14 1.443(7) . ?
C1 C2 1.362(6) . ?
C1 C6 1.377(7) . ?
C2 C3 1.380(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.351(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.336(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.377(8) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.490(6) . ?
C8 C9 1.369(6) . ?
C8 C13 1.399(6) . ?
C9 C10 1.375(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.399(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.389(7) . ?
C12 C13 1.372(6) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C18 1.468(8) . ?
C16 C17 1.482(7) . ?
C16 H16 0.9800 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C21 1.460(7) . ?
C19 C20 1.467(7) . ?
C19 H19 0.9800 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C24 1.464(8) . ?
C22 C23 1.475(8) . ?
C22 H22 0.9800 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C26 1.421(8) . ?
C25 C27 1.503(8) . ?
C25 H25 0.9800 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C30 1.378(7) . ?
C28 C29 1.380(7) . ?
C28 H28 0.9800 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?

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
O10 Ti1 O3 91.49(13) . 3_666 ?
O10 Ti1 O11 103.23(13) . . ?
O3 Ti1 O11 90.72(12) 3_666 . ?
O10 Ti1 O1 174.68(13) . . ?
O3 Ti1 O1 93.81(11) 3_666 . ?
O11 Ti1 O1 76.37(11) . . ?
O10 Ti1 O9 103.38(13) . . ?
O3 Ti1 O9 94.48(12) 3_666 . ?
O11 Ti1 O9 152.72(12) . . ?
O1 Ti1 O9 76.58(11) . . ?
O10 Ti1 O7 88.48(13) . . ?
O3 Ti1 O7 178.40(12) 3_666 . ?
O11 Ti1 O7 87.73(12) . . ?
O1 Ti1 O7 86.21(11) . . ?
O9 Ti1 O7 87.08(12) . . ?
O2 Ti2 O12 112.86(15) . . ?
O2 Ti2 O1 111.51(12) . . ?
O12 Ti2 O1 135.47(15) . . ?
O2 Ti2 O4 97.96(13) . . ?
O12 Ti2 O4 89.59(13) . . ?
O1 Ti2 O4 88.03(11) . . ?
O2 Ti2 O11 100.89(13) . . ?
O12 Ti2 O11 91.48(13) . . ?
O1 Ti2 O11 76.61(11) . . ?
O4 Ti2 O11 159.04(12) . . ?
O8 Ti3 O2 97.58(13) . 3_666 ?
O8 Ti3 O5 94.54(13) . . ?
O2 Ti3 O5 93.43(12) 3_666 . ?
O8 Ti3 O1 163.96(12) . . ?
O2 Ti3 O1 98.05(11) 3_666 . ?
O5 Ti3 O1 88.13(11) . . ?
O8 Ti3 O9 100.65(13) . . ?
O2 Ti3 O9 91.32(12) 3_666 . ?
O5 Ti3 O9 163.34(11) . . ?
O1 Ti3 O9 75.40(11) . . ?
O8 Ti3 O6 83.35(12) . . ?
O2 Ti3 O6 178.24(13) 3_666 . ?
O5 Ti3 O6 87.99(12) . . ?
O1 Ti3 O6 80.94(11) . . ?
O9 Ti3 O6 87.03(12) . . ?
O8 Ti3 Ti2 116.37(10) . 3_666 ?
O2 Ti3 Ti2 19.96(8) 3_666 3_666 ?
O5 Ti3 Ti2 85.30(8) . 3_666 ?
O1 Ti3 Ti2 79.59(8) . 3_666 ?
O9 Ti3 Ti2 93.95(8) . 3_666 ?
O6 Ti3 Ti2 159.58(8) . 3_666 ?
O4 P1 O5 112.07(17) . . ?
O4 P1 O3 111.49(17) . . ?
O5 P1 O3 113.16(16) . . ?
O4 P1 C1 105.95(19) . . ?
O5 P1 C1 107.1(2) . . ?
O3 P1 C1 106.6(2) . . ?
Ti2 O1 Ti1 105.62(12) . . ?
Ti2 O1 Ti3 145.97(15) . . ?
Ti1 O1 Ti3 103.65(11) . . ?
Ti2 O2 Ti3 139.03(15) . 3_666 ?
P1 O3 Ti1 145.22(19) . 3_666 ?
P1 O4 Ti2 137.31(17) . . ?
P1 O5 Ti3 137.48(18) . . ?
C7 O6 Ti3 129.8(3) . . ?
C7 O7 Ti1 129.2(3) . . ?
C16 O8 Ti3 140.2(3) . . ?
C19 O9 Ti1 133.8(3) . . ?
C19 O9 Ti3 123.5(3) . . ?
Ti1 O9 Ti3 102.60(12) . . ?
C22 O10 Ti1 174.6(4) . . ?
C25 O11 Ti1 127.5(3) . . ?
C25 O11 Ti2 131.3(3) . . ?
Ti1 O11 Ti2 101.19(12) . . ?
C28 O12 Ti2 147.1(5) . . ?
C11 N1 C15 120.9(5) . . ?
C11 N1 C14 120.5(5) . . ?
C15 N1 C14 118.1(5) . . ?
C2 C1 C6 117.9(5) . . ?
C2 C1 P1 122.4(4) . . ?
C6 C1 P1 119.7(4) . . ?
C1 C2 C3 121.1(6) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 H2 119.5 . . ?
C4 C3 C2 119.1(7) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C5 C4 C3 121.6(7) . . ?
C5 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
C4 C5 C6 119.3(6) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C5 C6 C1 120.9(6) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
O6 C7 O7 124.9(4) . . ?
O6 C7 C8 117.4(4) . . ?
O7 C7 C8 117.6(4) . . ?
C9 C8 C13 116.9(4) . . ?
C9 C8 C7 121.7(4) . . ?
C13 C8 C7 121.4(4) . . ?
C8 C9 C10 122.5(5) . . ?
C8 C9 H9 118.7 . . ?
C10 C9 H9 118.7 . . ?
C9 C10 C11 120.4(5) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
N1 C11 C12 121.9(5) . . ?
N1 C11 C10 120.6(5) . . ?
C12 C11 C10 117.5(5) . . ?
C13 C12 C11 121.1(5) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C12 C13 C8 121.5(5) . . ?
C12 C13 H13 119.2 . . ?
C8 C13 H13 119.2 . . ?
N1 C14 H14A 109.5 . . ?
N1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O8 C16 C18 110.4(5) . . ?
O8 C16 C17 110.4(5) . . ?
C18 C16 C17 115.3(6) . . ?
O8 C16 H16 106.8 . . ?
C18 C16 H16 106.8 . . ?
C17 C16 H16 106.8 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O9 C19 C21 111.6(4) . . ?
O9 C19 C20 111.6(4) . . ?
C21 C19 C20 116.3(5) . . ?
O9 C19 H19 105.4 . . ?
C21 C19 H19 105.4 . . ?
C20 C19 H19 105.4 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O10 C22 C24 111.4(5) . . ?
O10 C22 C23 110.0(5) . . ?
C24 C22 C23 114.7(6) . . ?
O10 C22 H22 106.7 . . ?
C24 C22 H22 106.7 . . ?
C23 C22 H22 106.7 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 O11 111.0(5) . . ?
C26 C25 C27 117.1(6) . . ?
O11 C25 C27 109.7(5) . . ?
C26 C25 H25 106.1 . . ?
O11 C25 H25 106.1 . . ?
C27 C25 H25 106.1 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O12 C28 C30 117.9(6) . . ?
O12 C28 C29 114.9(6) . . ?
C30 C28 C29 125.8(7) . . ?
O12 C28 H28 93.8 . . ?
C30 C28 H28 93.8 . . ?
C29 C28 H28 93.8 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

_refine_diff_density_max         0.418
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.066

####################################################################### 
# 
# 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_C4
_database_code_depnum_ccdc_archive 'CCDC 1841903'
_audit_update_record             
;
2018-05-22 deposited with the CCDC.
2018-06-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H44 N O12 P Ti3'
_chemical_formula_sum            'C29 H44 N O12 P Ti3'
_chemical_formula_weight         773.32

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'

_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                   14.0170(6)
_cell_length_b                   15.6940(8)
_cell_length_c                   17.5353(8)
_cell_angle_alpha                90
_cell_angle_beta                 97.147(5)
_cell_angle_gamma                90
_cell_volume                     3827.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3849
_cell_measurement_theta_min      3.2840
_cell_measurement_theta_max      26.7160

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_F_000             1608
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    0.707
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.57107
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1213
_diffrn_reflns_number            16664
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.908
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7507
_reflns_number_gt                4894
_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       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7507
_refine_ls_number_parameters     436
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0599
_refine_ls_wR_factor_ref         0.1955
_refine_ls_wR_factor_gt          0.1622
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_restrained_S_all      1.160
_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_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 0.38075(5) 0.47893(5) 0.64048(4) 0.0457(2) Uani 1 1 d . . . . .
Ti2 Ti 0.33187(5) 0.51740(4) 0.46787(4) 0.0420(2) Uani 1 1 d . . . . .
Ti3 Ti 0.49140(5) 0.34351(4) 0.55309(4) 0.0452(2) Uani 1 1 d . . . . .
P1 P 0.55581(7) 0.61544(7) 0.62974(6) 0.0446(3) Uani 1 1 d . . . . .
O1 O 0.41657(17) 0.45223(16) 0.53762(14) 0.0401(6) Uani 1 1 d . . . . .
O2 O 0.38589(18) 0.61098(16) 0.43700(15) 0.0473(7) Uani 1 1 d . . . . .
O3 O 0.2732(2) 0.38699(19) 0.61139(16) 0.0563(7) Uani 1 1 d . . . . .
O4 O 0.3491(2) 0.29300(18) 0.54419(18) 0.0598(8) Uani 1 1 d . . . . .
O5 O 0.47866(19) 0.56624(18) 0.66508(15) 0.0532(7) Uani 1 1 d . . . . .
O6 O 0.63683(19) 0.55658(19) 0.61468(15) 0.0530(7) Uani 1 1 d . . . . .
O7 O 0.51542(19) 0.66553(16) 0.55877(15) 0.0491(7) Uani 1 1 d . . . . .
O8 O 0.2074(2) 0.5101(2) 0.4312(2) 0.0715(9) Uani 1 1 d . . . . .
O9 O 0.30224(18) 0.55775(17) 0.57255(15) 0.0485(7) Uani 1 1 d . . . . .
O10 O 0.3330(2) 0.4899(2) 0.72773(16) 0.0623(8) Uani 1 1 d . . . . .
O11 O 0.4699(2) 0.38102(18) 0.65956(15) 0.0526(7) Uani 1 1 d . . . . .
O12 O 0.5273(2) 0.23663(18) 0.57433(18) 0.0646(8) Uani 1 1 d . . . . .
N1 N -0.1265(5) 0.0746(4) 0.5186(6) 0.189(4) Uani 1 1 d . . . . .
C1 C 0.2773(3) 0.3203(3) 0.5727(3) 0.0562(11) Uani 1 1 d . . . . .
C2 C 0.1873(3) 0.2677(3) 0.5591(3) 0.0608(12) Uani 1 1 d . . . . .
C3 C 0.1094(4) 0.2872(4) 0.5954(4) 0.097(2) Uani 1 1 d . . . . .
H3 H 0.111731 0.333982 0.628156 0.117 Uiso 1 1 calc R U . . .
C4 C 0.0272(4) 0.2382(4) 0.5838(5) 0.119(3) Uani 1 1 d . . . . .
H4 H -0.025499 0.251636 0.608853 0.143 Uiso 1 1 calc R U . . .
C5 C 0.0234(4) 0.1694(4) 0.5350(4) 0.0931(18) Uani 1 1 d . . . . .
C6 C 0.1006(4) 0.1490(4) 0.4985(3) 0.0872(17) Uani 1 1 d . . . . .
H6 H 0.098451 0.101768 0.466377 0.105 Uiso 1 1 calc R U . . .
C7 C 0.1813(4) 0.1988(3) 0.5097(3) 0.0739(14) Uani 1 1 d . . . . .
H7 H 0.233154 0.186019 0.483366 0.089 Uiso 1 1 calc R U . . .
C8 C -0.0605(5) 0.1164(5) 0.5252(5) 0.134(3) Uani 1 1 d . . . . .
C9 C 0.6091(3) 0.6906(3) 0.6986(2) 0.0636(12) Uani 1 1 d D U . . .
C10 C 0.6221(6) 0.7726(4) 0.6786(4) 0.127(2) Uani 1 1 d D U . . .
H10 H 0.598146 0.791060 0.629541 0.153 Uiso 1 1 calc R U . . .
C11 C 0.6711(7) 0.8302(5) 0.7304(5) 0.164(3) Uani 1 1 d D U . . .
H11 H 0.677363 0.887016 0.716828 0.196 Uiso 1 1 calc R U . . .
C12 C 0.7089(6) 0.8020(5) 0.8001(4) 0.134(3) Uani 1 1 d D U . . .
H12 H 0.741684 0.840038 0.834605 0.161 Uiso 1 1 calc R U . . .
C13 C 0.7007(5) 0.7212(5) 0.8210(4) 0.116(2) Uani 1 1 d D U . . .
H13 H 0.727445 0.702598 0.869346 0.139 Uiso 1 1 calc R U . . .
C14 C 0.6515(4) 0.6655(4) 0.7693(3) 0.0999(18) Uani 1 1 d D U . . .
H14 H 0.646986 0.608644 0.783298 0.120 Uiso 1 1 calc R U . . .
C15 C 0.1434(5) 0.4747(5) 0.3728(5) 0.132(3) Uani 1 1 d . . . . .
H15 H 0.174652 0.484442 0.326617 0.158 Uiso 1 1 calc R U . . .
C16 C 0.0559(5) 0.5250(6) 0.3590(6) 0.161(4) Uani 1 1 d . . . . .
H16A H 0.033034 0.537688 0.407072 0.241 Uiso 1 1 calc R U . . .
H16B H 0.007806 0.493361 0.326986 0.241 Uiso 1 1 calc R U . . .
H16C H 0.069158 0.577155 0.333697 0.241 Uiso 1 1 calc R U . . .
C17 C 0.1324(5) 0.3874(5) 0.3741(5) 0.136(3) Uani 1 1 d . . . . .
H17A H 0.194297 0.360993 0.385722 0.204 Uiso 1 1 calc R U . . .
H17B H 0.102787 0.368214 0.324827 0.204 Uiso 1 1 calc R U . . .
H17C H 0.092577 0.372290 0.412770 0.204 Uiso 1 1 calc R U . . .
C18 C 0.2427(4) 0.6279(4) 0.5935(4) 0.0863(17) Uani 1 1 d D U . . .
H18A H 0.264676 0.642260 0.647229 0.104 Uiso 0.518(11) 1 d R U P A 1
C19A C 0.2560(10) 0.7033(7) 0.5511(8) 0.113(4) Uani 0.518(11) 1 d D U P A 1
H19A H 0.223626 0.697463 0.499830 0.169 Uiso 0.518(11) 1 calc R U P A 1
H19B H 0.323406 0.712225 0.549183 0.169 Uiso 0.518(11) 1 calc R U P A 1
H19C H 0.229911 0.751083 0.575719 0.169 Uiso 0.518(11) 1 calc R U P A 1
H18B H 0.239807 0.658689 0.543930 0.135 Uiso 0.482(11) 1 d R U P A 2
C19B C 0.2961(9) 0.6940(8) 0.6348(10) 0.112(5) Uani 0.482(11) 1 d D U P A 2
H19D H 0.252824 0.736852 0.648994 0.168 Uiso 0.482(11) 1 calc R U P A 2
H19E H 0.339636 0.718897 0.602917 0.168 Uiso 0.482(11) 1 calc R U P A 2
H19F H 0.331994 0.670718 0.680237 0.168 Uiso 0.482(11) 1 calc R U P A 2
C20 C 0.1449(5) 0.6016(6) 0.5908(6) 0.164(4) Uani 1 1 d . U . . .
H20A H 0.123311 0.611299 0.639879 0.247 Uiso 1 1 calc R U . . .
H20B H 0.139845 0.542070 0.578424 0.247 Uiso 1 1 calc R U . . .
H20C H 0.105859 0.633811 0.552149 0.247 Uiso 1 1 calc R U . . .
C21 C 0.2845(6) 0.4869(5) 0.7941(4) 0.121(3) Uani 1 1 d . . . . .
H21 H 0.331678 0.463949 0.834824 0.145 Uiso 1 1 calc R U . . .
C22 C 0.2647(9) 0.5724(8) 0.8186(6) 0.235(6) Uani 1 1 d . . . . .
H22A H 0.320431 0.607437 0.816496 0.353 Uiso 1 1 calc R U . . .
H22B H 0.248983 0.570841 0.870287 0.353 Uiso 1 1 calc R U . . .
H22C H 0.211541 0.595515 0.785182 0.353 Uiso 1 1 calc R U . . .
C23 C 0.2060(7) 0.4279(7) 0.7876(5) 0.177(4) Uani 1 1 d . . . . .
H23A H 0.152469 0.451545 0.754885 0.266 Uiso 1 1 calc R U . . .
H23B H 0.187430 0.417270 0.837625 0.266 Uiso 1 1 calc R U . . .
H23C H 0.225330 0.375450 0.765976 0.266 Uiso 1 1 calc R U . . .
C24 C 0.5173(4) 0.3427(4) 0.7290(3) 0.0801(16) Uani 1 1 d . . . . .
H24 H 0.565229 0.303004 0.713413 0.096 Uiso 1 1 calc R U . . .
C25 C 0.4458(6) 0.2905(5) 0.7653(4) 0.136(3) Uani 1 1 d . . . . .
H25A H 0.409568 0.326808 0.795063 0.204 Uiso 1 1 calc R U . . .
H25B H 0.478934 0.248193 0.798090 0.204 Uiso 1 1 calc R U . . .
H25C H 0.402925 0.262958 0.725851 0.204 Uiso 1 1 calc R U . . .
C26 C 0.5716(5) 0.4096(5) 0.7781(3) 0.121(2) Uani 1 1 d . . . . .
H26A H 0.608283 0.443832 0.746919 0.181 Uiso 1 1 calc R U . . .
H26B H 0.614283 0.382544 0.817951 0.181 Uiso 1 1 calc R U . . .
H26C H 0.527058 0.445101 0.800816 0.181 Uiso 1 1 calc R U . . .
C27 C 0.5096(7) 0.1482(4) 0.5641(6) 0.130(3) Uani 1 1 d . . . . .
H27 H 0.441699 0.138528 0.545206 0.156 Uiso 1 1 calc R U . . .
C28 C 0.5349(9) 0.1029(5) 0.6335(6) 0.182(4) Uani 1 1 d . . . . .
H28A H 0.598575 0.118955 0.655398 0.272 Uiso 1 1 calc R U . . .
H28B H 0.533283 0.042795 0.623124 0.272 Uiso 1 1 calc R U . . .
H28C H 0.490158 0.116164 0.668943 0.272 Uiso 1 1 calc R U . . .
C29 C 0.5729(11) 0.1168(6) 0.5049(8) 0.235(7) Uani 1 1 d . . . . .
H29A H 0.607592 0.164013 0.487012 0.353 Uiso 1 1 calc R U . . .
H29B H 0.533246 0.091475 0.462278 0.353 Uiso 1 1 calc R U . . .
H29C H 0.617583 0.075207 0.528163 0.353 Uiso 1 1 calc R U . . .


_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 O10 1.753(3) . ?
Ti1 O5 1.949(3) . ?
Ti1 O9 1.958(3) . ?
Ti1 O1 1.977(2) . ?
Ti1 O11 1.983(3) . ?
Ti1 O3 2.103(3) . ?
Ti2 O2 1.768(3) . ?
Ti2 O8 1.787(3) . ?
Ti2 O1 1.895(3) . ?
Ti2 O6 1.948(3) 3_666 ?
Ti2 O9 2.033(3) . ?
Ti3 O12 1.777(3) . ?
Ti3 O2 1.850(3) 3_666 ?
Ti3 O7 1.957(3) 3_666 ?
Ti3 O1 2.004(3) . ?
Ti3 O11 2.016(3) . ?
Ti3 O4 2.134(3) . ?
P1 O6 1.512(3) . ?
P1 O7 1.521(3) . ?
P1 O5 1.522(3) . ?
P1 C9 1.784(4) . ?
O3 C1 1.252(5) . ?
O4 C1 1.254(5) . ?
O8 C15 1.390(8) . ?
O9 C18 1.456(5) . ?
O10 C21 1.419(6) . ?
O11 C24 1.444(5) . ?
O12 C27 1.417(7) . ?
N1 C8 1.129(7) . ?
C1 C2 1.501(6) . ?
C2 C3 1.365(6) . ?
C2 C7 1.383(6) . ?
C3 C4 1.380(7) . ?
C4 C5 1.374(8) . ?
C5 C6 1.361(8) . ?
C5 C8 1.434(8) . ?
C6 C7 1.369(7) . ?
C9 C10 1.353(6) . ?
C9 C14 1.365(6) . ?
C10 C11 1.398(7) . ?
C11 C12 1.346(8) . ?
C12 C13 1.329(7) . ?
C13 C14 1.380(6) . ?
C15 C17 1.378(9) . ?
C15 C16 1.453(9) . ?
C18 C19B 1.423(10) . ?
C18 C19A 1.422(10) . ?
C18 C20 1.427(9) . ?
C21 C23 1.433(10) . ?
C21 C22 1.445(11) . ?
C24 C25 1.497(8) . ?
C24 C26 1.503(8) . ?
C27 C28 1.416(11) . ?
C27 C29 1.529(12) . ?

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
O10 Ti1 O5 94.17(13) . . ?
O10 Ti1 O9 102.86(14) . . ?
O5 Ti1 O9 91.00(12) . . ?
O10 Ti1 O1 170.13(13) . . ?
O5 Ti1 O1 95.69(11) . . ?
O9 Ti1 O1 76.47(11) . . ?
O10 Ti1 O11 103.28(14) . . ?
O5 Ti1 O11 95.49(12) . . ?
O9 Ti1 O11 152.50(12) . . ?
O1 Ti1 O11 76.30(11) . . ?
O10 Ti1 O3 86.51(12) . . ?
O5 Ti1 O3 178.34(13) . . ?
O9 Ti1 O3 87.37(12) . . ?
O1 Ti1 O3 83.63(11) . . ?
O11 Ti1 O3 85.82(12) . . ?
O2 Ti2 O8 112.30(15) . . ?
O2 Ti2 O1 112.85(11) . . ?
O8 Ti2 O1 134.67(15) . . ?
O2 Ti2 O6 97.07(12) . 3_666 ?
O8 Ti2 O6 89.67(13) . 3_666 ?
O1 Ti2 O6 88.68(11) . 3_666 ?
O2 Ti2 O9 99.27(12) . . ?
O8 Ti2 O9 92.58(13) . . ?
O1 Ti2 O9 76.54(11) . . ?
O6 Ti2 O9 161.25(12) 3_666 . ?
O12 Ti3 O2 96.24(14) . 3_666 ?
O12 Ti3 O7 96.82(13) . 3_666 ?
O2 Ti3 O7 92.92(11) 3_666 3_666 ?
O12 Ti3 O1 164.15(13) . . ?
O2 Ti3 O1 98.56(11) 3_666 . ?
O7 Ti3 O1 88.08(11) 3_666 . ?
O12 Ti3 O11 98.78(13) . . ?
O2 Ti3 O11 92.56(12) 3_666 . ?
O7 Ti3 O11 162.79(12) 3_666 . ?
O1 Ti3 O11 74.97(10) . . ?
O12 Ti3 O4 84.41(14) . . ?
O2 Ti3 O4 178.49(12) 3_666 . ?
O7 Ti3 O4 88.34(12) 3_666 . ?
O1 Ti3 O4 80.65(11) . . ?
O11 Ti3 O4 86.00(12) . . ?
O12 Ti3 Ti2 116.29(11) . 3_666 ?
O2 Ti3 Ti2 21.43(8) 3_666 3_666 ?
O7 Ti3 Ti2 83.23(8) 3_666 3_666 ?
O1 Ti3 Ti2 79.19(7) . 3_666 ?
O11 Ti3 Ti2 96.25(8) . 3_666 ?
O4 Ti3 Ti2 158.37(9) . 3_666 ?
O6 P1 O7 112.59(15) . . ?
O6 P1 O5 110.38(17) . . ?
O7 P1 O5 112.61(16) . . ?
O6 P1 C9 105.18(19) . . ?
O7 P1 C9 107.11(19) . . ?
O5 P1 C9 108.57(19) . . ?
Ti2 O1 Ti1 105.35(12) . . ?
Ti2 O1 Ti3 145.34(14) . . ?
Ti1 O1 Ti3 104.19(11) . . ?
Ti2 O2 Ti3 136.09(15) . 3_666 ?
C1 O3 Ti1 128.7(3) . . ?
C1 O4 Ti3 129.3(3) . . ?
P1 O5 Ti1 141.53(17) . . ?
P1 O6 Ti2 137.50(17) . 3_666 ?
P1 O7 Ti3 138.56(16) . 3_666 ?
C15 O8 Ti2 143.4(4) . . ?
C18 O9 Ti1 128.3(3) . . ?
C18 O9 Ti2 130.7(3) . . ?
Ti1 O9 Ti2 100.96(12) . . ?
C21 O10 Ti1 170.4(4) . . ?
C24 O11 Ti1 132.8(3) . . ?
C24 O11 Ti3 123.6(3) . . ?
Ti1 O11 Ti3 103.52(12) . . ?
C27 O12 Ti3 149.0(5) . . ?
O3 C1 O4 126.5(4) . . ?
O3 C1 C2 116.8(4) . . ?
O4 C1 C2 116.7(4) . . ?
C3 C2 C7 118.5(4) . . ?
C3 C2 C1 120.5(4) . . ?
C7 C2 C1 120.9(4) . . ?
C2 C3 C4 120.5(5) . . ?
C5 C4 C3 119.8(6) . . ?
C6 C5 C4 120.4(5) . . ?
C6 C5 C8 119.7(6) . . ?
C4 C5 C8 119.9(6) . . ?
C5 C6 C7 119.3(5) . . ?
C6 C7 C2 121.4(5) . . ?
N1 C8 C5 179.0(11) . . ?
C10 C9 C14 116.9(5) . . ?
C10 C9 P1 120.8(4) . . ?
C14 C9 P1 121.6(4) . . ?
C9 C10 C11 121.2(7) . . ?
C12 C11 C10 118.9(8) . . ?
C13 C12 C11 121.8(7) . . ?
C12 C13 C14 118.4(7) . . ?
C9 C14 C13 122.7(6) . . ?
C17 C15 O8 116.6(7) . . ?
C17 C15 C16 116.7(7) . . ?
O8 C15 C16 111.1(7) . . ?
C19B C18 C20 132.1(7) . . ?
C19A C18 C20 114.2(9) . . ?
C19B C18 O9 113.4(7) . . ?
C19A C18 O9 112.4(5) . . ?
C20 C18 O9 110.6(5) . . ?
O10 C21 C23 113.5(6) . . ?
O10 C21 C22 110.1(7) . . ?
C23 C21 C22 116.7(8) . . ?
O11 C24 C25 108.9(5) . . ?
O11 C24 C26 109.9(4) . . ?
C25 C24 C26 117.2(6) . . ?
O12 C27 C28 111.2(8) . . ?
O12 C27 C29 107.1(6) . . ?
C28 C27 C29 108.5(8) . . ?

_refine_diff_density_max         0.727
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.075

