# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_Ti16DHB4
_database_code_depnum_ccdc_archive 'CCDC 1849504'
_audit_update_record             
;
2018-07-25 deposited with the CCDC.
2018-07-31 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         'C47 H84 O27 Ti8'
_chemical_formula_sum            'C47 H84 O27 Ti8'
_chemical_formula_weight         1464.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 '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'

_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                   12.9587(3)
_cell_length_b                   19.2226(4)
_cell_length_c                   25.8490(5)
_cell_angle_alpha                90
_cell_angle_beta                 93.3590(10)
_cell_angle_gamma                90
_cell_volume                     6427.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9953
_cell_measurement_theta_min      2.87
_cell_measurement_theta_max      68.21

_exptl_crystal_description       rodlike
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_F_000             3032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    8.693
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5896
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37147
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         4.119
_diffrn_reflns_theta_max         68.284
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             11659
_reflns_number_gt                10041
_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       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'APEX3 (Bruker, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND. Version 3.2k. Crystal Impact'
_computing_publication_material  'Windows Word 2010'
_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)+(0.0902P)²+11.2452P] 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         11659
_refine_ls_number_parameters     787
_refine_ls_number_restraints     152
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0535
_refine_ls_wR_factor_ref         0.1552
_refine_ls_wR_factor_gt          0.1479
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.111
_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 0.33022(5) 0.77713(3) 0.65407(3) 0.02579(16) Uani 1 1 d . . . . .
Ti2 Ti 0.40294(5) 0.81491(3) 0.55065(3) 0.02648(16) Uani 1 1 d . . . . .
Ti3 Ti 0.15266(5) 0.74135(3) 0.57562(3) 0.02836(16) Uani 1 1 d . . . . .
Ti4 Ti 0.29964(5) 0.69517(3) 0.47725(2) 0.02439(15) Uani 1 1 d . . . . .
Ti5 Ti 0.55039(5) 0.68601(3) 0.52665(2) 0.02143(15) Uani 1 1 d . . . . .
Ti6 Ti 0.55388(5) 0.72830(3) 0.65381(3) 0.02732(16) Uani 1 1 d . . . . .
Ti7 Ti 0.43180(5) 0.60947(3) 0.70508(2) 0.02714(16) Uani 1 1 d . . . . .
Ti8 Ti 0.17062(5) 0.61764(3) 0.65234(3) 0.02822(16) Uani 1 1 d . . . . .
O1 O 0.2762(2) 0.80491(13) 0.58369(10) 0.0283(5) Uani 1 1 d . . . . .
O2 O 0.45988(19) 0.79909(13) 0.61981(10) 0.0283(5) Uani 1 1 d . . . . .
O3 O 0.18127(19) 0.71681(13) 0.51091(10) 0.0289(5) Uani 1 1 d . . . . .
O4 O 0.40025(18) 0.70654(12) 0.54411(9) 0.0213(5) Uani 1 1 d . . . . .
H4O H 0.381838 0.680114 0.568271 0.026 Uiso 1 1 d R U . . .
O5 O 0.60562(19) 0.70226(13) 0.59317(10) 0.0271(5) Uani 1 1 d . . . . .
O6 O 0.42012(19) 0.71196(13) 0.68651(10) 0.0277(5) Uani 1 1 d . . . . .
O7 O 0.21429(19) 0.71894(13) 0.64615(10) 0.0280(5) Uani 1 1 d . . . . .
O8 O 0.2921(2) 0.59876(14) 0.68982(10) 0.0316(6) Uani 1 1 d . . . . .
O9 O 0.0846(2) 0.62372(15) 0.70324(11) 0.0392(7) Uani 1 1 d . . . . .
O10 O 0.4322(2) 0.61483(16) 0.77415(10) 0.0390(7) Uani 1 1 d . . . . .
O11 O 0.5842(2) 0.64915(15) 0.70014(11) 0.0339(6) Uani 1 1 d . . . . .
O12 O 0.2481(2) 0.67854(15) 0.41429(11) 0.0365(6) Uani 1 1 d . . . . .
O13 O 0.06556(19) 0.66506(14) 0.59806(11) 0.0332(6) Uani 1 1 d . . . . .
O14 O 0.3048(2) 0.84458(15) 0.69784(12) 0.0407(7) Uani 1 1 d . . . . .
O15 O 0.6450(2) 0.78597(16) 0.68447(12) 0.0432(7) Uani 1 1 d D . . . .
O16 O 0.5371(2) 0.78810(12) 0.51691(10) 0.0278(5) Uani 1 1 d . . . . .
O17 O 0.3351(2) 0.79650(13) 0.47860(10) 0.0299(6) Uani 1 1 d . . . . .
O18 O 0.4147(2) 0.90643(14) 0.54583(13) 0.0422(7) Uani 1 1 d . . . . .
O19 O 0.0584(2) 0.80823(16) 0.57032(14) 0.0440(7) Uani 1 1 d . . . . .
O20 O 0.45113(19) 0.66987(12) 0.45934(9) 0.0235(5) Uani 1 1 d . . . . .
O21 O 0.47732(18) 0.41316(12) 0.45104(9) 0.0224(5) Uani 1 1 d . . . . .
O22 O 0.54438(19) 0.38803(12) 0.37650(9) 0.0248(5) Uani 1 1 d . . . . .
O23 O 0.5281(2) 0.48458(13) 0.30190(9) 0.0301(6) Uani 1 1 d . . . . .
O24 O 0.66301(19) 0.66265(12) 0.49263(10) 0.0264(5) Uani 1 1 d . . . . .
O25 O 0.71318(19) 0.40495(12) 0.49857(9) 0.0252(5) Uani 1 1 d . . . . .
O26 O 0.74954(19) 0.37926(12) 0.41809(9) 0.0247(5) Uani 1 1 d . . . . .
O27 O 0.85944(19) 0.47471(13) 0.37015(10) 0.0292(5) Uani 1 1 d . . . . .
C1 C -0.0095(9) 0.6030(6) 0.7761(4) 0.139(4) Uani 1 1 d . . . . .
H1A H -0.022749 0.557431 0.759989 0.209 Uiso 1 1 calc R U . . .
H1B H -0.074574 0.622613 0.786939 0.209 Uiso 1 1 calc R U . . .
H1C H 0.038952 0.597610 0.806374 0.209 Uiso 1 1 calc R U . . .
C2 C 0.0319(10) 0.6463(5) 0.7413(4) 0.138(4) Uani 1 1 d . U . . .
H2 H -0.033687 0.656127 0.720312 0.165 Uiso 1 1 calc R U . . .
C3 C 0.0577(12) 0.7219(5) 0.7557(5) 0.175(7) Uani 1 1 d . . . . .
H3A H 0.115462 0.722891 0.781869 0.263 Uiso 1 1 calc R U . . .
H3B H -0.002922 0.743985 0.769633 0.263 Uiso 1 1 calc R U . . .
H3C H 0.076880 0.747061 0.724726 0.263 Uiso 1 1 calc R U . . .
C4 C 0.3488(9) 0.7036(5) 0.8192(4) 0.130(4) Uani 1 1 d . . . . .
H4A H 0.409235 0.733404 0.826763 0.195 Uiso 1 1 calc R U . . .
H4B H 0.300065 0.709218 0.846457 0.195 Uiso 1 1 calc R U . . .
H4C H 0.315110 0.717000 0.785720 0.195 Uiso 1 1 calc R U . . .
C5 C 0.3817(9) 0.6311(5) 0.8171(3) 0.117(3) Uani 1 1 d . U . . .
H5 H 0.314530 0.606088 0.810736 0.141 Uiso 1 1 calc R U . . .
C6 C 0.4227(10) 0.5997(6) 0.8643(3) 0.137(4) Uani 1 1 d . . . . .
H6A H 0.438180 0.550608 0.858026 0.206 Uiso 1 1 calc R U . . .
H6B H 0.371767 0.603160 0.890731 0.206 Uiso 1 1 calc R U . . .
H6C H 0.486236 0.623864 0.876373 0.206 Uiso 1 1 calc R U . . .
C7 C 0.6810(5) 0.5922(5) 0.7706(3) 0.089(2) Uani 1 1 d . . . . .
H7A H 0.661061 0.628192 0.794987 0.133 Uiso 1 1 calc R U . . .
H7B H 0.749481 0.574068 0.781623 0.133 Uiso 1 1 calc R U . . .
H7C H 0.630405 0.554338 0.769978 0.133 Uiso 1 1 calc R U . . .
C8 C 0.6843(4) 0.6231(3) 0.71735(18) 0.0461(11) Uani 1 1 d . . . . .
H8 H 0.733438 0.663282 0.719411 0.055 Uiso 1 1 calc R U . . .
C9 C 0.7225(4) 0.5717(3) 0.6787(3) 0.0673(16) Uani 1 1 d . . . . .
H9A H 0.682181 0.528655 0.680063 0.101 Uiso 1 1 calc R U . . .
H9B H 0.795643 0.561418 0.687273 0.101 Uiso 1 1 calc R U . . .
H9C H 0.714618 0.591518 0.643812 0.101 Uiso 1 1 calc R U . . .
C10 C 0.1525(7) 0.5755(4) 0.3896(3) 0.103(3) Uani 1 1 d . . . . .
H10A H 0.212517 0.547674 0.401758 0.154 Uiso 1 1 calc R U . . .
H10B H 0.116693 0.552229 0.359935 0.154 Uiso 1 1 calc R U . . .
H10C H 0.105277 0.580417 0.417573 0.154 Uiso 1 1 calc R U . . .
C11 C 0.1877(5) 0.6456(4) 0.3735(2) 0.0697(17) Uani 1 1 d . . . . .
H11 H 0.230031 0.640775 0.342541 0.084 Uiso 1 1 calc R U . . .
C12 C 0.0966(9) 0.6914(5) 0.3600(6) 0.170(7) Uani 1 1 d . . . . .
H12A H 0.037085 0.675231 0.378439 0.255 Uiso 1 1 calc R U . . .
H12B H 0.079827 0.689416 0.322562 0.255 Uiso 1 1 calc R U . . .
H12C H 0.113128 0.739365 0.370183 0.255 Uiso 1 1 calc R U . . .
C13 C -0.0130(4) 0.5945(3) 0.5287(2) 0.0575(14) Uani 1 1 d . . . . .
H13A H 0.013048 0.626409 0.502874 0.086 Uiso 1 1 calc R U . . .
H13B H -0.078632 0.574309 0.515235 0.086 Uiso 1 1 calc R U . . .
H13C H 0.037476 0.557282 0.535854 0.086 Uiso 1 1 calc R U . . .
C14 C -0.0297(3) 0.6338(3) 0.5779(3) 0.0607(15) Uani 1 1 d . . . . .
H14 H -0.043580 0.596538 0.603560 0.073 Uiso 1 1 calc R U . . .
C15 C -0.1151(4) 0.6796(4) 0.5805(3) 0.090(3) Uani 1 1 d . . . . .
H15A H -0.114878 0.700214 0.615122 0.135 Uiso 1 1 calc R U . . .
H15B H -0.179475 0.653593 0.573402 0.135 Uiso 1 1 calc R U . . .
H15C H -0.109989 0.716512 0.554602 0.135 Uiso 1 1 calc R U . . .
C16 C 0.2440(10) 0.9405(5) 0.7448(4) 0.159(5) Uani 1 1 d D U . . .
H16A H 0.269118 0.980527 0.727261 0.239 Uiso 1 1 d R U . . .
H16B H 0.232208 0.952417 0.780031 0.239 Uiso 1 1 d R U . . .
H16C H 0.180428 0.925107 0.727571 0.239 Uiso 1 1 d R U . . .
C17 C 0.3071(7) 0.8835(4) 0.7421(3) 0.112(3) Uani 1 1 d D U . . .
H17 H 0.294967 0.852175 0.772048 0.134 Uiso 1 1 calc R U . . .
C18 C 0.4104(9) 0.9158(7) 0.7506(4) 0.175(5) Uani 1 1 d D U . . .
H18A H 0.435042 0.930967 0.717277 0.263 Uiso 1 1 calc DR U . . .
H18B H 0.458849 0.881747 0.766466 0.263 Uiso 1 1 calc DR U . . .
H18C H 0.405785 0.956035 0.773610 0.263 Uiso 1 1 calc R U . . .
C19A C 0.6448(11) 0.8996(8) 0.7182(9) 0.136(6) Uani 0.470(11) 1 d D U P A 1
H19A H 0.681404 0.928104 0.744795 0.204 Uiso 0.470(11) 1 calc R U P A 1
H19B H 0.652184 0.920546 0.684040 0.204 Uiso 0.470(11) 1 calc R U P A 1
H19C H 0.571340 0.897138 0.725174 0.204 Uiso 0.470(11) 1 calc DR U P A 1
C20A C 0.6860(11) 0.8337(7) 0.7190(7) 0.099(4) Uani 0.470(11) 1 d D U P A 1
H20A H 0.663524 0.815158 0.752667 0.119 Uiso 0.470(11) 1 calc R U P A 1
C21A C 0.7914(13) 0.8399(12) 0.7287(10) 0.128(5) Uani 0.470(11) 1 d D U P A 1
H21A H 0.815395 0.833146 0.694598 0.193 Uiso 0.470(11) 1 d R U P A 1
H21B H 0.834345 0.814116 0.753358 0.193 Uiso 0.470(11) 1 d R U P A 1
H21C H 0.794365 0.888445 0.737288 0.193 Uiso 0.470(11) 1 d R U P A 1
C19B C 0.7050(15) 0.9003(7) 0.6818(9) 0.125(5) Uani 0.530(11) 1 d D U P A 2
H19D H 0.630932 0.907854 0.673997 0.187 Uiso 0.530(11) 1 calc R U P A 2
H19E H 0.744533 0.925605 0.656684 0.187 Uiso 0.530(11) 1 calc R U P A 2
H19F H 0.724194 0.917100 0.716826 0.187 Uiso 0.530(11) 1 calc R U P A 2
C20B C 0.7264(8) 0.8307(6) 0.6788(6) 0.091(4) Uani 0.530(11) 1 d D U P A 2
H20B H 0.746170 0.823418 0.642407 0.110 Uiso 0.530(11) 1 calc R U P A 2
C21B C 0.8148(13) 0.8161(10) 0.7090(9) 0.128(5) Uani 0.530(11) 1 d D U P A 2
H21D H 0.796216 0.801028 0.743415 0.192 Uiso 0.530(11) 1 calc R U P A 2
H21E H 0.857999 0.857866 0.712210 0.192 Uiso 0.530(11) 1 calc R U P A 2
H21F H 0.853243 0.778867 0.692680 0.192 Uiso 0.530(11) 1 calc R U P A 2
C22 C 0.6946(8) 0.8473(6) 0.5302(5) 0.155(5) Uani 1 1 d . U . . .
H22A H 0.674094 0.843249 0.565939 0.232 Uiso 1 1 calc R U . . .
H22B H 0.723343 0.893743 0.524777 0.232 Uiso 1 1 calc R U . . .
H22C H 0.747005 0.812059 0.523769 0.232 Uiso 1 1 calc R U . . .
C23 C 0.6057(4) 0.8369(2) 0.4950(2) 0.0569(14) Uani 1 1 d . U . . .
H23 H 0.568400 0.882332 0.491525 0.068 Uiso 1 1 calc R U . . .
C24 C 0.6314(8) 0.8147(3) 0.4417(3) 0.112(3) Uani 1 1 d . U . . .
H24A H 0.680456 0.775882 0.444265 0.168 Uiso 1 1 calc R U . . .
H24B H 0.662322 0.853784 0.423871 0.168 Uiso 1 1 calc R U . . .
H24C H 0.568111 0.799848 0.422148 0.168 Uiso 1 1 calc R U . . .
C25 C 0.3392(10) 0.8338(5) 0.3905(3) 0.137(5) Uani 1 1 d . . . . .
H25A H 0.412792 0.821965 0.394663 0.205 Uiso 1 1 calc R U . . .
H25B H 0.330257 0.875013 0.368352 0.205 Uiso 1 1 calc R U . . .
H25C H 0.300855 0.794703 0.374532 0.205 Uiso 1 1 calc R U . . .
C26 C 0.2995(6) 0.8488(3) 0.4421(2) 0.0652(16) Uani 1 1 d . . . . .
H26 H 0.338076 0.891549 0.453838 0.078 Uiso 1 1 calc R U . . .
C27 C 0.1934(8) 0.8669(6) 0.4467(6) 0.170(5) Uani 1 1 d . U . . .
H27A H 0.154371 0.825390 0.455626 0.254 Uiso 1 1 calc R U . . .
H27B H 0.164844 0.885853 0.413700 0.254 Uiso 1 1 calc R U . . .
H27C H 0.188344 0.901963 0.473981 0.254 Uiso 1 1 calc R U . . .
C28 C 0.4900(12) 0.9950(5) 0.5965(4) 0.165(5) Uani 1 1 d . U . . .
H28A H 0.496967 1.045712 0.597796 0.247 Uiso 1 1 calc R U . . .
H28B H 0.553124 0.974560 0.583845 0.247 Uiso 1 1 calc R U . . .
H28C H 0.479120 0.977157 0.631245 0.247 Uiso 1 1 calc R U . . .
C29 C 0.3993(7) 0.9758(3) 0.5604(3) 0.090(2) Uani 1 1 d . U . . .
H29 H 0.402289 1.005213 0.528669 0.108 Uiso 1 1 calc R U . . .
C30 C 0.3038(9) 0.9874(4) 0.5812(5) 0.158(4) Uani 1 1 d . U . . .
H30A H 0.248238 0.977424 0.554938 0.237 Uiso 1 1 calc R U . . .
H30B H 0.299294 1.036042 0.592214 0.237 Uiso 1 1 calc R U . . .
H30C H 0.296845 0.956850 0.611203 0.237 Uiso 1 1 calc R U . . .
C31 C 0.0333(11) 0.8841(7) 0.6411(5) 0.163(5) Uani 1 1 d . . . . .
H31A H -0.012475 0.920516 0.653204 0.245 Uiso 1 1 calc R U . . .
H31B H 0.034437 0.844849 0.665327 0.245 Uiso 1 1 calc R U . . .
H31C H 0.103407 0.902832 0.639384 0.245 Uiso 1 1 calc R U . . .
C32 C -0.0058(7) 0.8597(4) 0.5878(4) 0.122(4) Uani 1 1 d D . . . .
H32 H -0.074303 0.837222 0.592279 0.146 Uiso 1 1 calc R U . . .
C33 C -0.0250(7) 0.9169(4) 0.5551(4) 0.123(4) Uani 1 1 d D . . . .
H33A H 0.040124 0.940978 0.549659 0.184 Uiso 1 1 calc R U . . .
H33B H -0.072710 0.948941 0.571026 0.184 Uiso 1 1 calc R U . . .
H33C H -0.055894 0.900807 0.521711 0.184 Uiso 1 1 calc R U . . .
C34 C 0.4700(3) 0.62386(18) 0.42007(13) 0.0232(7) Uani 1 1 d . . . . .
C35 C 0.4847(3) 0.64667(19) 0.36997(14) 0.0300(8) Uani 1 1 d . . . . .
H35 H 0.481393 0.694964 0.362247 0.036 Uiso 1 1 calc R U . . .
C36 C 0.5043(3) 0.5994(2) 0.33117(14) 0.0325(8) Uani 1 1 d . . . . .
H36 H 0.513458 0.615864 0.297107 0.039 Uiso 1 1 calc R U . . .
C37 C 0.5108(3) 0.52812(19) 0.34110(13) 0.0260(7) Uani 1 1 d . . . . .
C38 C 0.4964(3) 0.50519(17) 0.39196(13) 0.0216(7) Uani 1 1 d . . . . .
C39 C 0.4742(3) 0.55313(17) 0.43049(13) 0.0212(7) Uani 1 1 d . . . . .
H39 H 0.461850 0.536984 0.464301 0.025 Uiso 1 1 calc R U . . .
C40 C 0.5061(2) 0.43174(17) 0.40645(12) 0.0200(6) Uani 1 1 d . . . . .
C41 C 0.7153(3) 0.61616(18) 0.46391(14) 0.0252(7) Uani 1 1 d . . . . .
C42 C 0.7116(3) 0.54593(18) 0.47550(14) 0.0237(7) Uani 1 1 d . . . . .
H42 H 0.677376 0.530642 0.504962 0.028 Uiso 1 1 calc R U . . .
C43 C 0.7579(3) 0.49764(18) 0.44408(13) 0.0229(7) Uani 1 1 d . . . . .
C44 C 0.8132(3) 0.51920(19) 0.40140(14) 0.0258(7) Uani 1 1 d . . . . .
C45 C 0.8214(3) 0.5908(2) 0.39302(15) 0.0331(8) Uani 1 1 d . . . . .
H45 H 0.862207 0.606979 0.366130 0.040 Uiso 1 1 calc R U . . .
C46 C 0.7716(3) 0.63872(19) 0.42293(16) 0.0318(8) Uani 1 1 d . . . . .
H46 H 0.776004 0.686974 0.415437 0.038 Uiso 1 1 calc R U . . .
C47 C 0.7410(2) 0.42294(18) 0.45408(13) 0.0219(7) Uani 1 1 d . . . . .


_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 O14 1.764(3) . ?
Ti1 O7 1.875(3) . ?
Ti1 O6 1.875(3) . ?
Ti1 O1 1.984(3) . ?
Ti1 O2 1.990(3) . ?
Ti2 O18 1.771(3) . ?
Ti2 O1 1.905(3) . ?
Ti2 O2 1.918(3) . ?
Ti2 O17 2.043(3) . ?
Ti2 O16 2.055(3) . ?
Ti2 O4 2.090(2) . ?
Ti3 O19 1.773(3) . ?
Ti3 O3 1.797(3) . ?
Ti3 O13 1.959(3) . ?
Ti3 O7 1.994(3) . ?
Ti3 O1 2.015(3) . ?
Ti4 O12 1.752(3) . ?
Ti4 O3 1.855(3) . ?
Ti4 O17 2.001(3) . ?
Ti4 O25 2.033(2) 3_666 ?
Ti4 O20 2.100(2) . ?
Ti4 O4 2.114(2) . ?
Ti5 O24 1.804(2) . ?
Ti5 O5 1.850(3) . ?
Ti5 O16 1.985(2) . ?
Ti5 O21 2.030(2) 3_666 ?
Ti5 O4 2.061(2) . ?
Ti5 O20 2.125(3) . ?
Ti6 O15 1.772(3) . ?
Ti6 O5 1.811(3) . ?
Ti6 O11 1.962(3) . ?
Ti6 O2 1.996(3) . ?
Ti6 O6 1.997(3) . ?
Ti7 O10 1.788(3) . ?
Ti7 O8 1.842(3) . ?
Ti7 O23 1.893(3) 3_666 ?
Ti7 O6 2.031(3) . ?
Ti7 O11 2.127(3) . ?
Ti7 O22 2.149(2) 3_666 ?
Ti8 O9 1.777(3) . ?
Ti8 O8 1.836(3) . ?
Ti8 O27 1.901(3) 3_666 ?
Ti8 O7 2.037(3) . ?
Ti8 O13 2.105(3) . ?
Ti8 O26 2.147(2) 3_666 ?
O9 C2 1.305(8) . ?
O10 C5 1.357(8) . ?
O11 C8 1.437(5) . ?
O12 C11 1.425(6) . ?
O13 C14 1.443(5) . ?
O14 C17 1.367(7) . ?
O15 C20A 1.365(9) . ?
O15 C20B 1.375(10) . ?
O16 C23 1.432(5) . ?
O17 C26 1.437(5) . ?
O18 C29 1.403(6) . ?
O19 C32 1.387(8) . ?
O20 C34 1.379(4) . ?
O21 C40 1.283(4) . ?
O22 C40 1.263(4) . ?
O23 C37 1.343(4) . ?
O24 C41 1.367(4) . ?
O25 C47 1.273(4) . ?
O26 C47 1.263(4) . ?
O27 C44 1.341(4) . ?
C1 C2 1.358(12) . ?
C2 C3 1.531(13) . ?
C4 C5 1.460(11) . ?
C5 C6 1.436(12) . ?
C7 C8 1.502(8) . ?
C8 C9 1.509(7) . ?
C10 C11 1.490(11) . ?
C11 C12 1.497(11) . ?
C13 C14 1.506(7) . ?
C14 C15 1.419(8) . ?
C16 C17 1.371(8) . ?
C17 C18 1.480(8) . ?
C19A C20A 1.375(11) . ?
C20A C21A 1.379(11) . ?
C19B C20B 1.369(11) . ?
C20B C21B 1.376(11) . ?
C22 C23 1.440(11) . ?
C23 C24 1.497(9) . ?
C25 C26 1.484(11) . ?
C26 C27 1.431(12) . ?
C28 C29 1.502(14) . ?
C29 C30 1.396(12) . ?
C31 C32 1.515(15) . ?
C32 C33 1.400(8) . ?
C34 C39 1.386(5) . ?
C34 C35 1.391(5) . ?
C35 C36 1.388(5) . ?
C36 C37 1.395(5) . ?
C37 C38 1.409(5) . ?
C38 C39 1.399(5) . ?
C38 C40 1.464(5) . ?
C41 C42 1.384(5) . ?
C41 C46 1.391(5) . ?
C42 C43 1.393(5) . ?
C43 C44 1.412(5) . ?
C43 C47 1.478(5) . ?
C44 C45 1.398(5) . ?
C45 C46 1.386(5) . ?

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
O14 Ti1 O7 109.27(13) . . ?
O14 Ti1 O6 109.79(13) . . ?
O7 Ti1 O6 97.07(12) . . ?
O14 Ti1 O1 108.73(13) . . ?
O7 Ti1 O1 79.79(11) . . ?
O6 Ti1 O1 140.05(11) . . ?
O14 Ti1 O2 108.88(13) . . ?
O7 Ti1 O2 140.37(11) . . ?
O6 Ti1 O2 79.75(11) . . ?
O1 Ti1 O2 78.28(11) . . ?
O18 Ti2 O1 102.23(13) . . ?
O18 Ti2 O2 101.13(14) . . ?
O1 Ti2 O2 82.00(11) . . ?
O18 Ti2 O17 98.17(13) . . ?
O1 Ti2 O17 93.17(11) . . ?
O2 Ti2 O17 160.68(11) . . ?
O18 Ti2 O16 98.09(12) . . ?
O1 Ti2 O16 159.68(10) . . ?
O2 Ti2 O16 93.85(11) . . ?
O17 Ti2 O16 84.20(11) . . ?
O18 Ti2 O4 170.25(12) . . ?
O1 Ti2 O4 85.69(10) . . ?
O2 Ti2 O4 85.47(10) . . ?
O17 Ti2 O4 75.49(10) . . ?
O16 Ti2 O4 74.12(9) . . ?
O19 Ti3 O3 107.28(14) . . ?
O19 Ti3 O13 99.17(13) . . ?
O3 Ti3 O13 103.47(12) . . ?
O19 Ti3 O7 117.67(14) . . ?
O3 Ti3 O7 134.49(11) . . ?
O13 Ti3 O7 76.97(11) . . ?
O19 Ti3 O1 96.19(13) . . ?
O3 Ti3 O1 92.84(11) . . ?
O13 Ti3 O1 153.04(12) . . ?
O7 Ti3 O1 76.29(11) . . ?
O12 Ti4 O3 101.30(13) . . ?
O12 Ti4 O17 105.57(13) . . ?
O3 Ti4 O17 88.23(11) . . ?
O12 Ti4 O25 94.54(12) . 3_666 ?
O3 Ti4 O25 89.05(11) . 3_666 ?
O17 Ti4 O25 159.85(11) . 3_666 ?
O12 Ti4 O20 93.63(12) . . ?
O3 Ti4 O20 164.76(11) . . ?
O17 Ti4 O20 90.70(10) . . ?
O25 Ti4 O20 86.72(10) 3_666 . ?
O12 Ti4 O4 164.03(12) . . ?
O3 Ti4 O4 94.63(10) . . ?
O17 Ti4 O4 75.82(10) . . ?
O25 Ti4 O4 84.51(10) 3_666 . ?
O20 Ti4 O4 70.40(9) . . ?
O24 Ti5 O5 102.42(12) . . ?
O24 Ti5 O16 104.54(11) . . ?
O5 Ti5 O16 88.69(11) . . ?
O24 Ti5 O21 93.80(10) . 3_666 ?
O5 Ti5 O21 87.70(10) . 3_666 ?
O16 Ti5 O21 161.65(10) . 3_666 ?
O24 Ti5 O4 162.81(11) . . ?
O5 Ti5 O4 94.75(10) . . ?
O16 Ti5 O4 76.24(10) . . ?
O21 Ti5 O4 86.14(9) 3_666 . ?
O24 Ti5 O20 91.88(11) . . ?
O5 Ti5 O20 165.54(10) . . ?
O16 Ti5 O20 89.80(10) . . ?
O21 Ti5 O20 89.24(9) 3_666 . ?
O4 Ti5 O20 70.93(9) . . ?
O15 Ti6 O5 106.82(13) . . ?
O15 Ti6 O11 96.20(14) . . ?
O5 Ti6 O11 104.06(12) . . ?
O15 Ti6 O2 98.27(13) . . ?
O5 Ti6 O2 93.13(11) . . ?
O11 Ti6 O2 153.24(12) . . ?
O15 Ti6 O6 118.75(13) . . ?
O5 Ti6 O6 134.20(11) . . ?
O11 Ti6 O6 76.55(11) . . ?
O2 Ti6 O6 76.77(11) . . ?
O10 Ti7 O8 99.53(13) . . ?
O10 Ti7 O23 99.53(12) . 3_666 ?
O8 Ti7 O23 98.31(12) . 3_666 ?
O10 Ti7 O6 100.13(12) . . ?
O8 Ti7 O6 89.95(11) . . ?
O23 Ti7 O6 157.07(11) 3_666 . ?
O10 Ti7 O11 95.21(13) . . ?
O8 Ti7 O11 158.65(12) . . ?
O23 Ti7 O11 94.35(12) 3_666 . ?
O6 Ti7 O11 72.22(11) . . ?
O10 Ti7 O22 170.43(13) . 3_666 ?
O8 Ti7 O22 89.33(11) . 3_666 ?
O23 Ti7 O22 82.63(10) 3_666 3_666 ?
O6 Ti7 O22 76.09(9) . 3_666 ?
O11 Ti7 O22 75.29(10) . 3_666 ?
O9 Ti8 O8 100.26(14) . . ?
O9 Ti8 O27 99.30(12) . 3_666 ?
O8 Ti8 O27 97.52(12) . 3_666 ?
O9 Ti8 O7 100.63(12) . . ?
O8 Ti8 O7 89.82(11) . . ?
O27 Ti8 O7 157.15(11) 3_666 . ?
O9 Ti8 O13 93.19(13) . . ?
O8 Ti8 O13 159.84(12) . . ?
O27 Ti8 O13 95.02(12) 3_666 . ?
O7 Ti8 O13 72.87(11) . . ?
O9 Ti8 O26 168.57(13) . 3_666 ?
O8 Ti8 O26 90.69(11) . 3_666 ?
O27 Ti8 O26 82.35(10) 3_666 3_666 ?
O7 Ti8 O26 75.93(9) . 3_666 ?
O13 Ti8 O26 75.38(10) . 3_666 ?
Ti2 O1 Ti1 99.84(12) . . ?
Ti2 O1 Ti3 135.67(14) . . ?
Ti1 O1 Ti3 99.64(12) . . ?
Ti2 O2 Ti1 99.19(12) . . ?
Ti2 O2 Ti6 135.25(13) . . ?
Ti1 O2 Ti6 99.72(12) . . ?
Ti3 O3 Ti4 135.80(15) . . ?
Ti5 O4 Ti2 101.37(10) . . ?
Ti5 O4 Ti4 110.25(10) . . ?
Ti2 O4 Ti4 100.12(10) . . ?
Ti6 O5 Ti5 135.11(14) . . ?
Ti1 O6 Ti6 103.75(12) . . ?
Ti1 O6 Ti7 142.14(14) . . ?
Ti6 O6 Ti7 101.42(11) . . ?
Ti1 O7 Ti3 104.27(12) . . ?
Ti1 O7 Ti8 141.86(14) . . ?
Ti3 O7 Ti8 100.37(11) . . ?
Ti8 O8 Ti7 153.22(16) . . ?
C2 O9 Ti8 163.5(5) . . ?
C5 O10 Ti7 148.9(5) . . ?
C8 O11 Ti6 127.1(3) . . ?
C8 O11 Ti7 132.9(3) . . ?
Ti6 O11 Ti7 99.29(12) . . ?
C11 O12 Ti4 158.7(4) . . ?
C14 O13 Ti3 134.5(3) . . ?
C14 O13 Ti8 124.5(3) . . ?
Ti3 O13 Ti8 99.22(11) . . ?
C17 O14 Ti1 160.7(5) . . ?
C20A O15 Ti6 159.4(8) . . ?
C20B O15 Ti6 147.0(6) . . ?
C23 O16 Ti5 130.3(3) . . ?
C23 O16 Ti2 124.3(3) . . ?
Ti5 O16 Ti2 105.28(11) . . ?
C26 O17 Ti4 127.2(3) . . ?
C26 O17 Ti2 125.6(3) . . ?
Ti4 O17 Ti2 105.70(12) . . ?
C29 O18 Ti2 155.6(4) . . ?
C32 O19 Ti3 156.4(5) . . ?
C34 O20 Ti4 121.3(2) . . ?
C34 O20 Ti5 124.8(2) . . ?
Ti4 O20 Ti5 108.33(10) . . ?
C40 O21 Ti5 125.6(2) . 3_666 ?
C40 O22 Ti7 132.1(2) . 3_666 ?
C37 O23 Ti7 136.6(2) . 3_666 ?
C41 O24 Ti5 150.3(2) . . ?
C47 O25 Ti4 124.6(2) . 3_666 ?
C47 O26 Ti8 132.4(2) . 3_666 ?
C44 O27 Ti8 133.5(2) . 3_666 ?
O9 C2 C1 122.7(9) . . ?
O9 C2 C3 112.5(7) . . ?
C1 C2 C3 120.7(9) . . ?
O10 C5 C6 115.2(8) . . ?
O10 C5 C4 114.0(7) . . ?
C6 C5 C4 117.7(9) . . ?
O11 C8 C7 110.4(4) . . ?
O11 C8 C9 110.4(4) . . ?
C7 C8 C9 112.0(5) . . ?
O12 C11 C10 111.1(5) . . ?
O12 C11 C12 107.6(6) . . ?
C10 C11 C12 110.3(8) . . ?
C15 C14 O13 112.2(5) . . ?
C15 C14 C13 120.1(6) . . ?
O13 C14 C13 110.6(4) . . ?
O14 C17 C16 119.7(8) . . ?
O14 C17 C18 109.2(7) . . ?
C16 C17 C18 101.3(10) . . ?
O15 C20A C19A 118.3(13) . . ?
O15 C20A C21A 121.4(13) . . ?
C19A C20A C21A 107.6(12) . . ?
C19B C20B O15 116.5(12) . . ?
C19B C20B C21B 109.4(11) . . ?
O15 C20B C21B 115.5(13) . . ?
O16 C23 C22 109.5(6) . . ?
O16 C23 C24 110.7(5) . . ?
C22 C23 C24 114.1(8) . . ?
C27 C26 O17 112.9(6) . . ?
C27 C26 C25 120.5(9) . . ?
O17 C26 C25 109.9(6) . . ?
C30 C29 O18 113.5(6) . . ?
C30 C29 C28 113.6(10) . . ?
O18 C29 C28 106.4(7) . . ?
O19 C32 C33 116.9(8) . . ?
O19 C32 C31 110.0(8) . . ?
C33 C32 C31 110.2(9) . . ?
O20 C34 C39 119.5(3) . . ?
O20 C34 C35 121.5(3) . . ?
C39 C34 C35 118.9(3) . . ?
C36 C35 C34 120.5(3) . . ?
C35 C36 C37 121.5(3) . . ?
O23 C37 C36 118.9(3) . . ?
O23 C37 C38 123.1(3) . . ?
C36 C37 C38 118.0(3) . . ?
C39 C38 C37 120.1(3) . . ?
C39 C38 C40 118.1(3) . . ?
C37 C38 C40 121.7(3) . . ?
C34 C39 C38 121.0(3) . . ?
O22 C40 O21 120.7(3) . . ?
O22 C40 C38 121.0(3) . . ?
O21 C40 C38 118.2(3) . . ?
O24 C41 C42 119.7(3) . . ?
O24 C41 C46 120.6(3) . . ?
C42 C41 C46 119.7(3) . . ?
C41 C42 C43 120.2(3) . . ?
C42 C43 C44 121.0(3) . . ?
C42 C43 C47 118.2(3) . . ?
C44 C43 C47 120.6(3) . . ?
O27 C44 C45 119.6(3) . . ?
O27 C44 C43 123.2(3) . . ?
C45 C44 C43 117.2(3) . . ?
C46 C45 C44 121.7(3) . . ?
C45 C46 C41 120.0(3) . . ?
O26 C47 O25 121.8(3) . . ?
O26 C47 C43 119.8(3) . . ?
O25 C47 C43 118.3(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4O O22 0.85 2.12 2.803(3) 136.7 3_666
O4 H4O O26 0.85 2.10 2.769(3) 135.6 3_666

_refine_diff_density_max         1.578
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.099

####################################################################### 
# 
# 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_Ti4DPPA4
_database_code_depnum_ccdc_archive 'CCDC 1849505'
_audit_update_record             
;
2018-07-25 deposited with the CCDC.
2018-07-31 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         'C63 H76 O17 P4 Ti4'
_chemical_formula_sum            'C63 H76 O17 P4 Ti4'
_chemical_formula_weight         1420.71

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                   12.6584(5)
_cell_length_b                   16.2449(6)
_cell_length_c                   33.8431(12)
_cell_angle_alpha                90
_cell_angle_beta                 96.617(3)
_cell_angle_gamma                90
_cell_volume                     6912.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    8378
_cell_measurement_theta_min      3.0800
_cell_measurement_theta_max      28.4890

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_F_000             2952
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    0.602
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.65916
_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            36582
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         2.860
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             13556
_reflns_number_gt                9302
_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 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND. Version 3.2k. Crystal Impact'
_computing_publication_material  'Windows Word 2010'
_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)+(0.0822P)²+9.7734P] 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         13556
_refine_ls_number_parameters     838
_refine_ls_number_restraints     203
_refine_ls_R_factor_all          0.1037
_refine_ls_R_factor_gt           0.0696
_refine_ls_wR_factor_ref         0.2000
_refine_ls_wR_factor_gt          0.1750
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.111
_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 0.67900(6) 0.81977(5) 0.08000(2) 0.0359(2) Uani 1 1 d . . . . .
Ti2 Ti 0.72138(6) 0.66437(5) 0.12028(2) 0.0349(2) Uani 1 1 d . . . . .
Ti3 Ti 0.87186(6) 0.71823(5) 0.05926(2) 0.0364(2) Uani 1 1 d . . . . .
Ti4 Ti 0.88957(6) 0.80196(5) 0.13516(2) 0.0382(2) Uani 1 1 d . . . . .
P1 P 0.74641(10) 0.82818(8) -0.00817(3) 0.0437(3) Uani 1 1 d . . . . .
P2 P 0.75829(11) 0.97048(8) 0.13638(4) 0.0463(3) Uani 1 1 d . . . . .
P3 P 0.85840(11) 0.67627(9) 0.20576(3) 0.0468(3) Uani 1 1 d . . . . .
P4 P 0.80806(11) 0.52918(8) 0.06358(3) 0.0441(3) Uani 1 1 d . . . . .
O1 O 0.7235(2) 0.78016(17) 0.13303(8) 0.0339(6) Uani 1 1 d . . . . .
O2 O 0.8493(2) 0.82543(17) 0.08048(8) 0.0343(6) Uani 1 1 d . . . . .
O3 O 0.7060(2) 0.70807(17) 0.06737(8) 0.0341(6) Uani 1 1 d . . . . .
O4 O 0.8841(2) 0.69094(17) 0.11507(8) 0.0352(6) Uani 1 1 d . . . . .
O5 O 1.0083(2) 0.7191(2) 0.05364(9) 0.0505(8) Uani 1 1 d . U . . .
O6 O 1.0276(3) 0.8233(2) 0.14117(10) 0.0547(8) Uani 1 1 d . U . . .
O7 O 0.5391(2) 0.8208(2) 0.07764(9) 0.0479(8) Uani 1 1 d . . . . .
O8 O 0.5888(3) 0.6422(2) 0.12826(9) 0.0489(8) Uani 1 1 d . . . . .
O9 O 0.6812(2) 0.8578(2) 0.02367(8) 0.0467(8) Uani 1 1 d . . . . .
O10 O 0.8200(3) 0.7573(2) 0.00395(8) 0.0446(8) Uani 1 1 d . . . . .
O11 O 0.6921(3) 0.93667(19) 0.09983(9) 0.0458(8) Uani 1 1 d . . . . .
O12 O 0.8509(3) 0.91679(19) 0.15249(9) 0.0462(8) Uani 1 1 d . . . . .
O13 O 0.8934(3) 0.7590(2) 0.19172(8) 0.0492(8) Uani 1 1 d . . . . .
O14 O 0.7776(3) 0.6316(2) 0.17708(8) 0.0447(8) Uani 1 1 d . . . . .
O15 O 0.8491(3) 0.60139(19) 0.04140(9) 0.0480(8) Uani 1 1 d . . . . .
O16 O 0.7564(3) 0.55121(19) 0.10037(9) 0.0450(8) Uani 1 1 d . . . . .
C1 C 0.8199(4) 0.9131(3) -0.02412(15) 0.0550(13) Uani 1 1 d . . . . .
C2 C 0.8219(5) 0.9869(4) -0.0046(2) 0.0703(16) Uani 1 1 d . . . . .
H2 H 0.784575 0.993395 0.017306 0.084 Uiso 1 1 calc R U . . .
C3 C 0.8798(6) 1.0518(4) -0.0176(3) 0.092(2) Uani 1 1 d . . . . .
H3 H 0.879990 1.102016 -0.004390 0.110 Uiso 1 1 calc R U . . .
C4 C 0.9354(7) 1.0442(6) -0.0487(3) 0.101(3) Uani 1 1 d . . . . .
H4 H 0.974447 1.088306 -0.056866 0.122 Uiso 1 1 calc R U . . .
C5 C 0.9340(7) 0.9717(6) -0.0681(3) 0.111(3) Uani 1 1 d . . . . .
H5 H 0.972076 0.966549 -0.089862 0.134 Uiso 1 1 calc R U . . .
C6 C 0.8781(6) 0.9051(5) -0.05652(19) 0.087(2) Uani 1 1 d . . . . .
H6 H 0.878939 0.855351 -0.070109 0.104 Uiso 1 1 calc R U . . .
C7 C 0.6571(4) 0.7963(4) -0.04977(14) 0.0577(14) Uani 1 1 d D . . . .
C8 C 0.5909(7) 0.8535(6) -0.0698(2) 0.120(3) Uani 1 1 d D . . . .
H8 H 0.596104 0.908555 -0.062300 0.144 Uiso 1 1 calc R U . . .
C9 C 0.5172(8) 0.8299(8) -0.1007(3) 0.167(6) Uani 1 1 d D . . . .
H9 H 0.473764 0.868946 -0.114529 0.201 Uiso 1 1 calc R U . . .
C10 C 0.5082(8) 0.7488(8) -0.1110(3) 0.156(6) Uani 1 1 d D . . . .
H10 H 0.456179 0.732483 -0.131170 0.187 Uiso 1 1 calc R U . . .
C11 C 0.5746(8) 0.6911(7) -0.0922(2) 0.140(4) Uani 1 1 d D . . . .
H11 H 0.569623 0.636175 -0.099845 0.167 Uiso 1 1 calc R U . . .
C12 C 0.6495(6) 0.7161(4) -0.06135(19) 0.086(2) Uani 1 1 d D . . . .
H12 H 0.695336 0.677430 -0.048400 0.103 Uiso 1 1 calc R U . . .
C13 C 0.7589(7) 1.1081(4) 0.0893(2) 0.083(2) Uani 1 1 d . . . . .
H13 H 0.703028 1.083323 0.073322 0.100 Uiso 1 1 calc R U . . .
C14 C 0.7963(10) 1.1833(5) 0.0796(3) 0.118(3) Uani 1 1 d . . . . .
H14 H 0.765243 1.209248 0.056682 0.142 Uiso 1 1 calc R U . . .
C15 C 0.8756(11) 1.2209(6) 0.1018(4) 0.136(4) Uani 1 1 d . . . . .
H15 H 0.898174 1.272681 0.094604 0.163 Uiso 1 1 calc R U . . .
C16 C 0.9234(8) 1.1835(5) 0.1351(4) 0.130(4) Uani 1 1 d . . . . .
H16 H 0.980183 1.209024 0.150173 0.156 Uiso 1 1 calc R U . . .
C17 C 0.8881(6) 1.1078(4) 0.1465(3) 0.093(2) Uani 1 1 d . . . . .
H17 H 0.919717 1.083010 0.169720 0.111 Uiso 1 1 calc R U . . .
C18 C 0.8061(5) 1.0689(3) 0.12359(18) 0.0640(15) Uani 1 1 d . . . . .
C19 C 0.6727(4) 0.9852(4) 0.17450(15) 0.0572(14) Uani 1 1 d . . . . .
C20 C 0.6425(6) 1.0614(4) 0.18683(18) 0.083(2) Uani 1 1 d . . . . .
H20 H 0.670262 1.108501 0.176282 0.100 Uiso 1 1 calc R U . . .
C21 C 0.5722(8) 1.0689(6) 0.2144(2) 0.113(3) Uani 1 1 d . . . . .
H21 H 0.549411 1.120675 0.221519 0.135 Uiso 1 1 calc R U . . .
C22 C 0.5359(7) 1.0009(7) 0.2313(2) 0.110(3) Uani 1 1 d . . . . .
H22 H 0.489130 1.006075 0.250382 0.131 Uiso 1 1 calc R U . . .
C23 C 0.5673(7) 0.9243(6) 0.2205(2) 0.116(3) Uani 1 1 d . . . . .
H23 H 0.541272 0.877708 0.232132 0.140 Uiso 1 1 calc R U . . .
C24 C 0.6367(6) 0.9161(4) 0.1927(2) 0.096(3) Uani 1 1 d . . . . .
H24 H 0.659829 0.864077 0.186094 0.115 Uiso 1 1 calc R U . . .
C25 C 0.8025(4) 0.6922(4) 0.25134(14) 0.0571(14) Uani 1 1 d . . . . .
C26 C 0.8059(8) 0.7676(6) 0.2685(2) 0.121(3) Uani 1 1 d . . . . .
H26 H 0.837649 0.811400 0.256626 0.145 Uiso 1 1 calc R U . . .
C27 C 0.7618(10) 0.7794(7) 0.3039(3) 0.161(5) Uani 1 1 d . . . . .
H27 H 0.762403 0.831790 0.315095 0.194 Uiso 1 1 calc R U . . .
C28 C 0.7194(8) 0.7182(8) 0.3219(2) 0.123(4) Uani 1 1 d . . . . .
H28 H 0.693596 0.726726 0.346238 0.148 Uiso 1 1 calc R U . . .
C29 C 0.7135(9) 0.6448(7) 0.3055(3) 0.128(4) Uani 1 1 d . . . . .
H29 H 0.681804 0.601998 0.318035 0.154 Uiso 1 1 calc R U . . .
C30 C 0.7539(8) 0.6299(5) 0.2696(2) 0.107(3) Uani 1 1 d . . . . .
H30 H 0.747860 0.577893 0.258071 0.128 Uiso 1 1 calc DR U . . .
C31 C 0.9705(4) 0.6122(4) 0.21606(14) 0.0701(16) Uani 1 1 d D U . . .
C32 C 0.9763(6) 0.5437(4) 0.2398(2) 0.136(3) Uani 1 1 d D U . . .
H32 H 0.916556 0.529625 0.252004 0.163 Uiso 1 1 calc DR U . . .
C33 C 1.0652(6) 0.4942(5) 0.2469(2) 0.145(3) Uani 1 1 d D U . . .
H33 H 1.063725 0.447978 0.263031 0.174 Uiso 1 1 calc R U . . .
C34 C 1.1557(6) 0.5130(5) 0.2301(2) 0.125(3) Uani 1 1 d D U . . .
H34 H 1.216819 0.481192 0.235258 0.150 Uiso 1 1 calc R U . . .
C35 C 1.1535(6) 0.5796(5) 0.2055(3) 0.165(3) Uani 1 1 d D U . . .
H35 H 1.212816 0.593118 0.192972 0.198 Uiso 1 1 calc R U . . .
C36 C 1.0618(5) 0.6271(5) 0.1993(2) 0.153(3) Uani 1 1 d D U . . .
H36 H 1.062621 0.672317 0.182513 0.184 Uiso 1 1 calc R U . . .
C37 C 0.9186(4) 0.4635(3) 0.07811(13) 0.0485(12) Uani 1 1 d D . . . .
C38 C 0.9584(5) 0.4549(4) 0.11725(15) 0.0775(19) Uani 1 1 d D . . . .
H38 H 0.925043 0.480606 0.137006 0.093 Uiso 1 1 calc R U . . .
C39 C 1.0480(6) 0.4081(5) 0.12721(19) 0.108(3) Uani 1 1 d D . . . .
H39 H 1.073884 0.401168 0.153848 0.130 Uiso 1 1 calc R U . . .
C40 C 1.0996(6) 0.3716(5) 0.09832(18) 0.089(2) Uani 1 1 d D . . . .
H40 H 1.161178 0.341275 0.105459 0.107 Uiso 1 1 calc R U . . .
C41 C 1.0610(5) 0.3796(4) 0.05908(16) 0.0742(18) Uani 1 1 d D . . . .
H41 H 1.094388 0.353703 0.039384 0.089 Uiso 1 1 calc R U . . .
C42 C 0.9720(5) 0.4265(4) 0.04947(15) 0.0629(15) Uani 1 1 d D . . . .
H42 H 0.946718 0.433805 0.022797 0.075 Uiso 1 1 calc R U . . .
C43 C 0.6646(5) 0.4043(5) 0.04219(18) 0.0793(19) Uani 1 1 d . . . . .
H43 H 0.682983 0.384575 0.067871 0.095 Uiso 1 1 calc R U . . .
C44 C 0.5889(6) 0.3634(6) 0.0172(3) 0.102(3) Uani 1 1 d . . . . .
H44 H 0.557335 0.316012 0.025806 0.123 Uiso 1 1 calc R U . . .
C45 C 0.5605(6) 0.3922(7) -0.0198(3) 0.105(3) Uani 1 1 d . . . . .
H45 H 0.508568 0.365099 -0.036649 0.126 Uiso 1 1 calc R U . . .
C46 C 0.6064(9) 0.4588(6) -0.0322(2) 0.116(3) Uani 1 1 d . . . . .
H46 H 0.586051 0.478073 -0.057814 0.139 Uiso 1 1 calc R U . . .
C47 C 0.6850(7) 0.5014(4) -0.00775(19) 0.089(2) Uani 1 1 d . . . . .
H47 H 0.717106 0.547800 -0.017151 0.107 Uiso 1 1 calc R U . . .
C48 C 0.7138(4) 0.4739(3) 0.02990(15) 0.0526(13) Uani 1 1 d . . . . .
C49 C 0.4218(7) 0.8762(7) 0.0249(2) 0.138(4) Uani 1 1 d . . . . .
H49A H 0.459056 0.925484 0.019205 0.208 Uiso 1 1 calc R U . . .
H49B H 0.346912 0.883837 0.017538 0.208 Uiso 1 1 calc R U . . .
H49C H 0.446473 0.831148 0.010094 0.208 Uiso 1 1 calc R U . . .
C50 C 0.4412(6) 0.8585(7) 0.0669(2) 0.117(3) Uani 1 1 d . . . . .
H50 H 0.395076 0.810210 0.067781 0.141 Uiso 1 1 calc R U . . .
C51 C 0.4032(8) 0.9048(7) 0.0961(3) 0.150(4) Uani 1 1 d . . . . .
H51A H 0.421769 0.878880 0.121449 0.225 Uiso 1 1 calc R U . . .
H51B H 0.327256 0.909087 0.090874 0.225 Uiso 1 1 calc R U . . .
H51C H 0.434079 0.958807 0.096429 0.225 Uiso 1 1 calc R U . . .
C52 C 0.4971(9) 0.7007(7) 0.1768(3) 0.163(5) Uani 1 1 d . . . . .
H52A H 0.540256 0.682027 0.200243 0.245 Uiso 1 1 calc R U . . .
H52B H 0.425203 0.707974 0.182505 0.245 Uiso 1 1 calc R U . . .
H52C H 0.524259 0.752084 0.168255 0.245 Uiso 1 1 calc R U . . .
C53 C 0.4994(8) 0.6437(7) 0.1473(3) 0.155(5) Uani 1 1 d . . . . .
H53 H 0.450396 0.670075 0.126598 0.186 Uiso 1 1 calc R U . . .
C54 C 0.4473(8) 0.5666(7) 0.1494(3) 0.158(5) Uani 1 1 d . . . . .
H54A H 0.446623 0.538535 0.124378 0.237 Uiso 1 1 calc R U . . .
H54B H 0.375606 0.575459 0.155012 0.237 Uiso 1 1 calc R U . . .
H54C H 0.484561 0.533824 0.170080 0.237 Uiso 1 1 calc R U . . .
C55 C 1.1731(6) 0.7165(5) 0.0279(3) 0.110(3) Uani 1 1 d . U . . .
H55A H 1.183528 0.775008 0.027301 0.164 Uiso 1 1 d R U . . .
H55B H 1.136368 0.698728 0.002951 0.164 Uiso 1 1 d R U . . .
H55C H 1.240848 0.689478 0.032341 0.164 Uiso 1 1 d R U . . .
C56 C 1.1113(6) 0.6961(6) 0.0594(2) 0.110(2) Uani 1 1 d . U . . .
H56 H 1.136355 0.741249 0.077293 0.132 Uiso 1 1 calc R U . . .
C57 C 1.1392(7) 0.6326(7) 0.0858(3) 0.144(4) Uani 1 1 d . U . . .
H57A H 1.097446 0.635944 0.107707 0.216 Uiso 1 1 calc R U . . .
H57B H 1.213295 0.637021 0.095589 0.216 Uiso 1 1 calc R U . . .
H57C H 1.126381 0.580783 0.072497 0.216 Uiso 1 1 calc R U . . .
C58 C 1.1228(8) 0.9429(4) 0.1713(3) 0.147(3) Uani 1 1 d D U . . .
H58A H 1.192376 0.952872 0.184926 0.221 Uiso 1 1 calc R U . . .
H58B H 1.112292 0.976372 0.147812 0.221 Uiso 1 1 calc R U . . .
H58C H 1.070080 0.956345 0.188505 0.221 Uiso 1 1 calc R U . . .
C59 C 1.1128(5) 0.8539(4) 0.1598(3) 0.1170(19) Uani 1 1 d D U . . .
H59 H 1.085941 0.843380 0.185399 0.140 Uiso 1 1 d R U . . .
C60 C 1.2136(6) 0.8053(5) 0.1681(3) 0.138(3) Uani 1 1 d D U . . .
H60A H 1.267497 0.839114 0.182257 0.207 Uiso 1 1 calc R U . . .
H60B H 1.201042 0.758000 0.183880 0.207 Uiso 1 1 calc R U . . .
H60C H 1.236764 0.787782 0.143406 0.207 Uiso 1 1 calc R U . . .
O17A O 0.6379(19) 0.3384(11) 0.2109(5) 0.257(7) Uani 0.646(10) 1 d D U P A 1
H17A H 0.662861 0.331480 0.234133 0.309 Uiso 0.646(10) 1 d R U P A 1
C61A C 0.7010(19) 0.4705(8) 0.2109(4) 0.175(7) Uani 0.646(10) 1 d D U P A 1
H61A H 0.635008 0.498197 0.202847 0.262 Uiso 0.646(10) 1 calc R U P A 1
H61B H 0.758760 0.502389 0.202926 0.262 Uiso 0.646(10) 1 calc R U P A 1
H61C H 0.709949 0.463977 0.239253 0.262 Uiso 0.646(10) 1 calc DR U P A 1
C62A C 0.700(2) 0.3930(10) 0.1928(4) 0.227(6) Uani 0.646(10) 1 d D U P A 1
H62A H 0.772332 0.372464 0.199767 0.272 Uiso 0.646(10) 1 calc R U P A 1
C63A C 0.685(2) 0.3876(12) 0.1513(4) 0.223(7) Uani 0.646(10) 1 d D U P A 1
H63A H 0.729414 0.426921 0.140146 0.334 Uiso 0.646(10) 1 calc R U P A 1
H63B H 0.702165 0.333169 0.143223 0.334 Uiso 0.646(10) 1 calc R U P A 1
H63C H 0.611478 0.399156 0.141998 0.334 Uiso 0.646(10) 1 calc R U P A 1
O17B O 0.728(3) 0.2902(16) 0.1999(9) 0.266(8) Uani 0.354(10) 1 d D U P A 2
H17B H 0.663563 0.289757 0.193823 0.320 Uiso 0.354(10) 1 calc R U P A 2
C61B C 0.871(2) 0.377(2) 0.2078(11) 0.253(11) Uani 0.354(10) 1 d D U P A 2
H61D H 0.878395 0.433647 0.216058 0.379 Uiso 0.354(10) 1 calc DR U P A 2
H61E H 0.921901 0.365417 0.189441 0.379 Uiso 0.354(10) 1 calc R U P A 2
H61F H 0.884680 0.341959 0.230588 0.379 Uiso 0.354(10) 1 calc R U P A 2
C62B C 0.768(3) 0.3634(16) 0.1892(10) 0.232(7) Uani 0.354(10) 1 d D U P A 2
H62B H 0.781133 0.352872 0.161651 0.279 Uiso 0.354(10) 1 calc R U P A 2
C63B C 0.690(3) 0.425(2) 0.1845(11) 0.220(7) Uani 0.354(10) 1 d D U P A 2
H63D H 0.643003 0.419171 0.204559 0.331 Uiso 0.354(10) 1 calc R U P A 2
H63E H 0.650590 0.420543 0.158655 0.331 Uiso 0.354(10) 1 calc R U P A 2
H63F H 0.723748 0.478311 0.187067 0.331 Uiso 0.354(10) 1 calc R U P A 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 O7 1.764(3) . ?
Ti1 O3 1.904(3) . ?
Ti1 O1 1.929(3) . ?
Ti1 O9 2.007(3) . ?
Ti1 O11 2.015(3) . ?
Ti1 O2 2.156(3) . ?
Ti2 O8 1.767(3) . ?
Ti2 O3 1.915(3) . ?
Ti2 O1 1.929(3) . ?
Ti2 O16 2.025(3) . ?
Ti2 O14 2.042(3) . ?
Ti2 O4 2.132(3) . ?
Ti3 O5 1.759(3) . ?
Ti3 O2 1.918(3) . ?
Ti3 O4 1.929(3) . ?
Ti3 O15 2.003(3) . ?
Ti3 O10 2.013(3) . ?
Ti3 O3 2.154(3) . ?
Ti4 O6 1.770(3) . ?
Ti4 O2 1.901(3) . ?
Ti4 O4 1.926(3) . ?
Ti4 O12 2.032(3) . ?
Ti4 O13 2.033(3) . ?
Ti4 O1 2.125(3) . ?
P1 O10 1.508(3) . ?
P1 O9 1.510(3) . ?
P1 C7 1.778(5) . ?
P1 C1 1.782(6) . ?
P2 O12 1.512(3) . ?
P2 O11 1.515(3) . ?
P2 C18 1.781(6) . ?
P2 C19 1.794(5) . ?
P3 O13 1.509(4) . ?
P3 O14 1.512(3) . ?
P3 C31 1.761(5) . ?
P3 C25 1.788(5) . ?
P4 O16 1.515(3) . ?
P4 O15 1.516(3) . ?
P4 C37 1.783(5) . ?
P4 C48 1.793(5) . ?
O5 C56 1.349(7) . ?
O6 C59 1.285(6) . ?
O7 C50 1.392(7) . ?
O8 C53 1.365(7) . ?
C1 C2 1.367(8) . ?
C1 C6 1.396(8) . ?
C2 C3 1.385(9) . ?
C3 C4 1.338(11) . ?
C4 C5 1.346(12) . ?
C5 C6 1.375(10) . ?
C7 C12 1.360(7) . ?
C7 C8 1.376(7) . ?
C8 C9 1.374(8) . ?
C9 C10 1.365(9) . ?
C10 C11 1.366(9) . ?
C11 C12 1.387(7) . ?
C13 C14 1.364(10) . ?
C13 C18 1.396(9) . ?
C14 C15 1.331(14) . ?
C15 C16 1.358(14) . ?
C16 C17 1.380(11) . ?
C17 C18 1.376(9) . ?
C19 C20 1.375(8) . ?
C19 C24 1.383(9) . ?
C20 C21 1.368(9) . ?
C21 C22 1.347(12) . ?
C22 C23 1.368(12) . ?
C23 C24 1.365(9) . ?
C25 C26 1.355(9) . ?
C25 C30 1.367(9) . ?
C26 C27 1.395(10) . ?
C27 C28 1.313(12) . ?
C28 C29 1.315(12) . ?
C29 C30 1.392(9) . ?
C31 C36 1.367(5) . ?
C31 C32 1.370(4) . ?
C32 C33 1.382(5) . ?
C33 C34 1.370(5) . ?
C34 C35 1.363(5) . ?
C35 C36 1.389(5) . ?
C37 C38 1.369(6) . ?
C37 C42 1.382(6) . ?
C38 C39 1.374(7) . ?
C39 C40 1.372(7) . ?
C40 C41 1.368(6) . ?
C41 C42 1.368(6) . ?
C43 C44 1.374(9) . ?
C43 C48 1.379(8) . ?
C44 C45 1.346(12) . ?
C45 C46 1.320(12) . ?
C46 C47 1.401(11) . ?
C47 C48 1.360(8) . ?
C49 C50 1.442(10) . ?
C50 C51 1.373(10) . ?
C52 C53 1.363(11) . ?
C53 C54 1.420(12) . ?
C55 C56 1.433(9) . ?
C56 C57 1.383(10) . ?
C58 C59 1.4983(10) . ?
C59 C60 1.4985(10) . ?
O17A C62A 1.375(10) . ?
C61A C62A 1.399(10) . ?
C62A C63A 1.398(10) . ?
O17B C62B 1.360(10) . ?
C61B C62B 1.399(10) . ?
C62B C63B 1.406(10) . ?

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
O7 Ti1 O3 101.81(14) . . ?
O7 Ti1 O1 103.27(13) . . ?
O3 Ti1 O1 81.38(12) . . ?
O7 Ti1 O9 94.46(14) . . ?
O3 Ti1 O9 93.32(13) . . ?
O1 Ti1 O9 162.18(13) . . ?
O7 Ti1 O11 92.84(15) . . ?
O3 Ti1 O11 164.37(13) . . ?
O1 Ti1 O11 90.03(12) . . ?
O9 Ti1 O11 90.93(13) . . ?
O7 Ti1 O2 176.30(13) . . ?
O3 Ti1 O2 80.62(11) . . ?
O1 Ti1 O2 79.78(11) . . ?
O9 Ti1 O2 82.57(12) . . ?
O11 Ti1 O2 85.03(12) . . ?
O8 Ti2 O3 102.86(14) . . ?
O8 Ti2 O1 98.81(14) . . ?
O3 Ti2 O1 81.08(11) . . ?
O8 Ti2 O16 96.56(14) . . ?
O3 Ti2 O16 91.60(12) . . ?
O1 Ti2 O16 164.10(13) . . ?
O8 Ti2 O14 92.12(14) . . ?
O3 Ti2 O14 164.50(13) . . ?
O1 Ti2 O14 92.82(12) . . ?
O16 Ti2 O14 90.62(13) . . ?
O8 Ti2 O4 175.98(13) . . ?
O3 Ti2 O4 80.94(11) . . ?
O1 Ti2 O4 80.35(11) . . ?
O16 Ti2 O4 84.58(12) . . ?
O14 Ti2 O4 84.00(12) . . ?
O5 Ti3 O2 102.92(15) . . ?
O5 Ti3 O4 97.96(14) . . ?
O2 Ti3 O4 80.83(12) . . ?
O5 Ti3 O15 94.83(15) . . ?
O2 Ti3 O15 162.02(13) . . ?
O4 Ti3 O15 94.02(12) . . ?
O5 Ti3 O10 96.65(14) . . ?
O2 Ti3 O10 90.87(12) . . ?
O4 Ti3 O10 164.50(12) . . ?
O15 Ti3 O10 89.89(13) . . ?
O5 Ti3 O3 175.92(14) . . ?
O2 Ti3 O3 80.35(11) . . ?
O4 Ti3 O3 80.05(11) . . ?
O15 Ti3 O3 81.80(12) . . ?
O10 Ti3 O3 85.68(12) . . ?
O6 Ti4 O2 102.90(14) . . ?
O6 Ti4 O4 102.61(15) . . ?
O2 Ti4 O4 81.34(12) . . ?
O6 Ti4 O12 93.14(15) . . ?
O2 Ti4 O12 92.88(12) . . ?
O4 Ti4 O12 164.06(13) . . ?
O6 Ti4 O13 92.44(15) . . ?
O2 Ti4 O13 163.82(13) . . ?
O4 Ti4 O13 90.40(13) . . ?
O12 Ti4 O13 91.37(13) . . ?
O6 Ti4 O1 175.06(14) . . ?
O2 Ti4 O1 81.20(11) . . ?
O4 Ti4 O1 80.61(11) . . ?
O12 Ti4 O1 83.84(12) . . ?
O13 Ti4 O1 83.75(12) . . ?
O10 P1 O9 114.88(17) . . ?
O10 P1 C7 108.0(2) . . ?
O9 P1 C7 108.0(2) . . ?
O10 P1 C1 110.2(2) . . ?
O9 P1 C1 108.4(2) . . ?
C7 P1 C1 107.0(3) . . ?
O12 P2 O11 114.72(18) . . ?
O12 P2 C18 109.6(3) . . ?
O11 P2 C18 107.4(3) . . ?
O12 P2 C19 109.0(2) . . ?
O11 P2 C19 108.2(2) . . ?
C18 P2 C19 107.8(3) . . ?
O13 P3 O14 115.25(18) . . ?
O13 P3 C31 109.2(2) . . ?
O14 P3 C31 108.3(2) . . ?
O13 P3 C25 107.6(2) . . ?
O14 P3 C25 108.5(2) . . ?
C31 P3 C25 107.7(2) . . ?
O16 P4 O15 115.41(18) . . ?
O16 P4 C37 108.3(2) . . ?
O15 P4 C37 107.3(2) . . ?
O16 P4 C48 108.8(2) . . ?
O15 P4 C48 108.3(2) . . ?
C37 P4 C48 108.6(2) . . ?
Ti1 O1 Ti2 97.02(12) . . ?
Ti1 O1 Ti4 99.08(12) . . ?
Ti2 O1 Ti4 99.11(12) . . ?
Ti4 O2 Ti3 98.49(13) . . ?
Ti4 O2 Ti1 98.90(12) . . ?
Ti3 O2 Ti1 98.66(12) . . ?
Ti1 O3 Ti2 98.33(12) . . ?
Ti1 O3 Ti3 99.12(12) . . ?
Ti2 O3 Ti3 98.76(12) . . ?
Ti4 O4 Ti3 97.24(13) . . ?
Ti4 O4 Ti2 98.97(12) . . ?
Ti3 O4 Ti2 99.09(12) . . ?
C56 O5 Ti3 157.9(4) . . ?
C59 O6 Ti4 153.3(5) . . ?
C50 O7 Ti1 151.1(5) . . ?
C53 O8 Ti2 157.2(5) . . ?
P1 O9 Ti1 130.40(19) . . ?
P1 O10 Ti3 128.21(18) . . ?
P2 O11 Ti1 129.07(19) . . ?
P2 O12 Ti4 128.92(19) . . ?
P3 O13 Ti4 128.78(19) . . ?
P3 O14 Ti2 128.02(19) . . ?
P4 O15 Ti3 129.02(18) . . ?
P4 O16 Ti2 128.32(18) . . ?
C2 C1 C6 118.6(6) . . ?
C2 C1 P1 120.9(4) . . ?
C6 C1 P1 120.4(5) . . ?
C1 C2 C3 119.7(7) . . ?
C4 C3 C2 121.7(8) . . ?
C3 C4 C5 119.0(8) . . ?
C4 C5 C6 121.9(8) . . ?
C5 C6 C1 119.0(8) . . ?
C12 C7 C8 119.1(6) . . ?
C12 C7 P1 121.6(4) . . ?
C8 C7 P1 119.2(5) . . ?
C9 C8 C7 120.5(8) . . ?
C10 C9 C8 119.6(9) . . ?
C9 C10 C11 120.9(10) . . ?
C10 C11 C12 118.8(10) . . ?
C7 C12 C11 121.1(8) . . ?
C14 C13 C18 118.7(8) . . ?
C15 C14 C13 122.4(10) . . ?
C14 C15 C16 119.8(9) . . ?
C15 C16 C17 120.3(9) . . ?
C18 C17 C16 119.8(8) . . ?
C17 C18 C13 118.9(6) . . ?
C17 C18 P2 122.0(5) . . ?
C13 C18 P2 119.1(5) . . ?
C20 C19 C24 118.6(5) . . ?
C20 C19 P2 123.4(5) . . ?
C24 C19 P2 118.1(4) . . ?
C21 C20 C19 120.8(7) . . ?
C22 C21 C20 119.8(8) . . ?
C21 C22 C23 120.6(7) . . ?
C24 C23 C22 120.1(8) . . ?
C23 C24 C19 120.0(7) . . ?
C26 C25 C30 118.0(6) . . ?
C26 C25 P3 120.2(5) . . ?
C30 C25 P3 121.7(5) . . ?
C25 C26 C27 119.8(8) . . ?
C28 C27 C26 121.4(9) . . ?
C27 C28 C29 119.8(7) . . ?
C28 C29 C30 121.2(8) . . ?
C25 C30 C29 119.7(7) . . ?
C36 C31 C32 113.4(6) . . ?
C36 C31 P3 120.9(4) . . ?
C32 C31 P3 125.7(5) . . ?
C31 C32 C33 124.2(8) . . ?
C34 C33 C32 120.1(8) . . ?
C35 C34 C33 118.1(8) . . ?
C34 C35 C36 119.4(8) . . ?
C31 C36 C35 124.9(7) . . ?
C38 C37 C42 118.6(5) . . ?
C38 C37 P4 121.2(4) . . ?
C42 C37 P4 119.9(4) . . ?
C37 C38 C39 119.7(5) . . ?
C40 C39 C38 120.8(6) . . ?
C41 C40 C39 120.3(6) . . ?
C40 C41 C42 118.4(5) . . ?
C41 C42 C37 122.1(5) . . ?
C44 C43 C48 121.2(7) . . ?
C45 C44 C43 119.9(8) . . ?
C46 C45 C44 120.0(8) . . ?
C45 C46 C47 121.7(8) . . ?
C48 C47 C46 119.1(8) . . ?
C47 C48 C43 118.1(6) . . ?
C47 C48 P4 121.2(5) . . ?
C43 C48 P4 120.7(4) . . ?
C51 C50 O7 115.3(7) . . ?
C51 C50 C49 124.4(8) . . ?
O7 C50 C49 113.0(6) . . ?
C52 C53 O8 116.5(8) . . ?
C52 C53 C54 120.9(8) . . ?
O8 C53 C54 115.0(8) . . ?
O5 C56 C57 118.2(7) . . ?
O5 C56 C55 115.4(6) . . ?
C57 C56 C55 122.2(7) . . ?
O6 C59 C58 122.8(5) . . ?
O6 C59 C60 122.4(6) . . ?
C58 C59 C60 114.5(5) . . ?
O17A C62A C63A 112.9(14) . . ?
O17A C62A C61A 111.3(13) . . ?
C63A C62A C61A 119.3(11) . . ?
O17B C62B C61B 112.2(14) . . ?
O17B C62B C63B 112.1(14) . . ?
C61B C62B C63B 123.0(13) . . ?

_refine_diff_density_max         0.709
_refine_diff_density_min         -1.075
_refine_diff_density_rms         0.079

