# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_pmeoobrticl2_sq
_database_code_depnum_ccdc_archive 'CCDC 1957864'
loop_
_audit_author_name
_audit_author_address
'Yutaka Ishida'
;Tokyo Institute of Technology
Japan
;
_audit_update_record             
;
2019-10-07 deposited with the CCDC.	2019-11-26 downloaded from the CCDC.
;
_audit_creation_date             2019-10-01
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_chemical_formula_moiety         'C33 H41 Br Cl2 O3 Ti, 0.5 (C4 H8 O)'
_chemical_formula_sum            'C35 H45 Br Cl2 O3.50 Ti'
_chemical_formula_weight         720.42

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.1016(2)
_cell_length_b                   13.3903(3)
_cell_length_c                   24.3259(5)
_cell_angle_alpha                78.765(2)
_cell_angle_beta                 80.424(2)
_cell_angle_gamma                89.325(2)
_cell_volume                     3496.62(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    26843
_cell_measurement_temperature    123
_cell_measurement_theta_max      30.9600
_cell_measurement_theta_min      2.4410
_exptl_absorpt_coefficient_mu    1.574
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93419
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'reddish brown'
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       plate
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0731
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            57804
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.560
_diffrn_reflns_theta_min         2.551
_diffrn_ambient_temperature      123.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.1429
_diffrn_detector_type            'Rigaku Saturn724+ area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50    2.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50    2.00    --  -20.00  45.00  90.00  360
  3  ω   -110.00  70.00   0.50    2.00    --  -20.00  45.00 180.00  360
  4  ω   -110.00  70.00   0.50    2.00    --  -20.00  45.00 270.00  360
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0005935000
_diffrn_orient_matrix_UB_12      0.0336240000
_diffrn_orient_matrix_UB_13      -0.0263726000
_diffrn_orient_matrix_UB_21      -0.0132950000
_diffrn_orient_matrix_UB_22      0.0410544000
_diffrn_orient_matrix_UB_23      0.0144232000
_diffrn_orient_matrix_UB_31      0.0634281000
_diffrn_orient_matrix_UB_32      0.0100971000
_diffrn_orient_matrix_UB_33      -0.0023775000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11177
_reflns_number_total             16124
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         16124
_refine_ls_number_restraints     149
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0500
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0378P)²+2.2938P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.1043
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap

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
Br1 Br -0.05635(3) 0.78968(3) 0.71810(2) 0.02651(9) Uani 1 1 d . . . . .
Ti1 Ti 0.15687(5) 0.72080(4) 0.53432(2) 0.01535(12) Uani 1 1 d . . . . .
Cl1 Cl -0.03910(7) 0.77001(6) 0.55905(3) 0.02812(18) Uani 1 1 d . . . . .
Cl2 Cl 0.18067(7) 0.59683(6) 0.48346(3) 0.02632(18) Uani 1 1 d . . . . .
O1 O 0.16359(17) 0.64423(14) 0.60195(8) 0.0170(4) Uani 1 1 d . . . . .
O2 O 0.28683(17) 0.80444(14) 0.53121(8) 0.0162(4) Uani 1 1 d . . . . .
O3 O 0.14413(18) 0.82306(14) 0.45401(8) 0.0193(4) Uani 1 1 d . U . . .
C1 C 0.2198(2) 0.8059(2) 0.65043(11) 0.0138(6) Uani 1 1 d . . . . .
H1 H 0.165868 0.812744 0.620864 0.017 Uiso 1 1 calc R . . . .
C2 C 0.1702(2) 0.6191(2) 0.65883(12) 0.0149(6) Uani 1 1 d . . . . .
C3 C 0.1460(3) 0.5180(2) 0.68855(12) 0.0167(6) Uani 1 1 d . . . . .
C4 C 0.1631(3) 0.4988(2) 0.74512(12) 0.0188(6) Uani 1 1 d . . . . .
H4 H 0.148943 0.431384 0.766509 0.023 Uiso 1 1 calc R . . . .
C5 C 0.2000(3) 0.5736(2) 0.77191(12) 0.0198(6) Uani 1 1 d . . . . .
C6 C 0.2164(3) 0.6727(2) 0.74135(12) 0.0176(6) Uani 1 1 d . . . . .
H6 H 0.238743 0.724829 0.759427 0.021 Uiso 1 1 calc R . . . .
C7 C 0.2009(2) 0.6972(2) 0.68508(12) 0.0141(6) Uani 1 1 d . . . . .
C8 C 0.1007(3) 0.4348(2) 0.66088(13) 0.0191(6) Uani 1 1 d . . . . .
C9 C 0.1984(3) 0.4124(2) 0.61232(14) 0.0257(7) Uani 1 1 d . . . . .
H9A H 0.224653 0.476102 0.585675 0.039 Uiso 1 1 calc GR . . . .
H9B H 0.164122 0.365605 0.592314 0.039 Uiso 1 1 calc GR . . . .
H9C H 0.268788 0.381163 0.628040 0.039 Uiso 1 1 calc GR . . . .
C10 C 0.0708(3) 0.3344(2) 0.70378(14) 0.0269(7) Uani 1 1 d . . . . .
H10A H 0.144087 0.310616 0.719535 0.040 Uiso 1 1 calc GR . . . .
H10B H 0.043145 0.283107 0.684621 0.040 Uiso 1 1 calc GR . . . .
H10C H 0.006063 0.345347 0.734579 0.040 Uiso 1 1 calc GR . . . .
C11 C -0.0180(3) 0.4691(2) 0.63843(13) 0.0235(7) Uani 1 1 d . . . . .
H11A H -0.080088 0.481105 0.669986 0.035 Uiso 1 1 calc GR . . . .
H11B H -0.047440 0.415794 0.621158 0.035 Uiso 1 1 calc GR . . . .
H11C H -0.001856 0.532062 0.609869 0.035 Uiso 1 1 calc GR . . . .
C12 C 0.2221(3) 0.5460(3) 0.83233(13) 0.0320(8) Uani 1 1 d . . . . .
H12A H 0.153058 0.504602 0.855723 0.048 Uiso 1 1 calc GR . . . .
H12B H 0.230364 0.608259 0.847026 0.048 Uiso 1 1 calc GR . . . .
H12C H 0.297253 0.507104 0.833585 0.048 Uiso 1 1 calc GR . . . .
C13 C 0.3806(3) 0.8115(2) 0.56121(12) 0.0148(6) Uani 1 1 d . . . . .
C14 C 0.5033(3) 0.8153(2) 0.53263(12) 0.0178(6) Uani 1 1 d . . . . .
C15 C 0.5924(3) 0.8189(2) 0.56651(13) 0.0202(7) Uani 1 1 d . . . . .
H15 H 0.675665 0.822227 0.548805 0.024 Uiso 1 1 calc R . . . .
C16 C 0.5670(3) 0.8178(2) 0.62444(13) 0.0209(7) Uani 1 1 d . . . . .
C17 C 0.4461(3) 0.8147(2) 0.64985(13) 0.0187(6) Uani 1 1 d . . . . .
H17 H 0.427087 0.812703 0.689597 0.022 Uiso 1 1 calc R . . . .
C18 C 0.3511(2) 0.8144(2) 0.61907(12) 0.0145(6) Uani 1 1 d . . . . .
C19 C 0.5395(3) 0.8116(2) 0.46932(13) 0.0216(7) Uani 1 1 d . . . . .
C20 C 0.4734(3) 0.8924(3) 0.43214(14) 0.0346(9) Uani 1 1 d . . . . .
H20A H 0.385174 0.878043 0.441269 0.052 Uiso 1 1 calc GR . . . .
H20B H 0.502177 0.890935 0.391980 0.052 Uiso 1 1 calc GR . . . .
H20C H 0.490454 0.959849 0.439400 0.052 Uiso 1 1 calc GR . . . .
C21 C 0.6776(3) 0.8311(3) 0.44877(14) 0.0307(8) Uani 1 1 d . . . . .
H21A H 0.700915 0.897221 0.455887 0.046 Uiso 1 1 calc GR . . . .
H21B H 0.696844 0.831292 0.407946 0.046 Uiso 1 1 calc GR . . . .
H21C H 0.722987 0.777237 0.469405 0.046 Uiso 1 1 calc GR . . . .
C22 C 0.5096(3) 0.7049(3) 0.46006(14) 0.0332(8) Uani 1 1 d . . . . .
H22A H 0.553835 0.653905 0.483271 0.050 Uiso 1 1 calc GR . . . .
H22B H 0.534323 0.701769 0.419842 0.050 Uiso 1 1 calc GR . . . .
H22C H 0.421516 0.690980 0.471152 0.050 Uiso 1 1 calc GR . . . .
C23 C 0.6687(3) 0.8177(3) 0.65853(14) 0.0326(8) Uani 1 1 d . . . . .
H23A H 0.728722 0.766827 0.649116 0.049 Uiso 1 1 calc GR . . . .
H23B H 0.635004 0.801094 0.699179 0.049 Uiso 1 1 calc GR . . . .
H23C H 0.708507 0.885252 0.649453 0.049 Uiso 1 1 calc GR . . . .
C24 C 0.1825(2) 0.8883(2) 0.68525(11) 0.0142(6) Uani 1 1 d . . . . .
C25 C 0.0657(3) 0.8888(2) 0.71727(12) 0.0176(6) Uani 1 1 d . . . . .
C26 C 0.0293(3) 0.9642(2) 0.74787(13) 0.0263(7) Uani 1 1 d . . . . .
H26 H -0.049952 0.960876 0.770174 0.032 Uiso 1 1 calc R . . . .
C27 C 0.1080(3) 1.0440(2) 0.74590(14) 0.0298(8) Uani 1 1 d . . . . .
H27 H 0.083382 1.096074 0.766643 0.036 Uiso 1 1 calc R . . . .
C28 C 0.2226(3) 1.0476(2) 0.71368(14) 0.0285(8) Uani 1 1 d . . . . .
H28 H 0.276997 1.102941 0.711713 0.034 Uiso 1 1 calc R . . . .
C29 C 0.2590(3) 0.9709(2) 0.68406(13) 0.0217(7) Uani 1 1 d . . . . .
H29 H 0.338665 0.974715 0.662201 0.026 Uiso 1 1 calc R . . . .
C30 C 0.1306(3) 0.9326(2) 0.45172(14) 0.0267(7) Uani 1 1 d . U . . .
H30A H 0.209524 0.969271 0.435907 0.032 Uiso 0.820(12) 1 calc R . P A 1
H30B H 0.101874 0.946662 0.490175 0.032 Uiso 0.820(12) 1 calc R . P A 1
H30C H 0.204892 0.964821 0.458830 0.032 Uiso 0.180(12) 1 calc R . P A 2
H30D H 0.058686 0.947963 0.478511 0.032 Uiso 0.180(12) 1 calc R . P A 2
C33 C 0.0828(4) 0.7948(3) 0.41045(15) 0.0417(10) Uani 1 1 d . U . . .
H33A H 0.008771 0.752514 0.428161 0.050 Uiso 0.820(12) 1 calc R . P A 1
H33B H 0.138065 0.755760 0.386536 0.050 Uiso 0.820(12) 1 calc R . P A 1
H33C H -0.005803 0.781171 0.423563 0.050 Uiso 0.180(12) 1 calc R . P A 2
H33D H 0.121132 0.736494 0.395225 0.050 Uiso 0.180(12) 1 calc R . P A 2
C31 C 0.0376(7) 0.9653(4) 0.4136(3) 0.0424(16) Uani 0.820(12) 1 d . U P A 1
H31A H -0.045740 0.962050 0.436036 0.051 Uiso 0.820(12) 1 calc R . P A 1
H31B H 0.055436 1.035612 0.391970 0.051 Uiso 0.820(12) 1 calc R . P A 1
C32 C 0.0493(8) 0.8927(5) 0.3754(3) 0.0498(18) Uani 0.820(12) 1 d . U P A 1
H32A H 0.113727 0.915501 0.342059 0.060 Uiso 0.820(12) 1 calc R . P A 1
H32B H -0.028875 0.884738 0.362031 0.060 Uiso 0.820(12) 1 calc R . P A 1
C31A C 0.112(3) 0.9638(16) 0.3893(11) 0.040(5) Uani 0.180(12) 1 d . U P A 2
H31C H 0.033613 0.999110 0.388807 0.048 Uiso 0.180(12) 1 calc R . P A 2
H31D H 0.177643 1.014009 0.369343 0.048 Uiso 0.180(12) 1 calc R . P A 2
C32A C 0.112(4) 0.905(2) 0.3652(13) 0.044(5) Uani 0.180(12) 1 d . U P A 2
H32C H 0.193092 0.902721 0.340929 0.053 Uiso 0.180(12) 1 calc R . P A 2
H32D H 0.049499 0.917517 0.340361 0.053 Uiso 0.180(12) 1 calc R . P A 2
Br2 Br 0.15290(3) 0.19030(3) 0.85063(2) 0.03404(10) Uani 1 1 d . . . . .
Ti04 Ti 0.56074(5) 0.30712(4) 0.76827(2) 0.01856(12) Uani 1 1 d . . . . .
Cl3 Cl 0.40000(8) 0.28007(6) 0.72550(4) 0.0321(2) Uani 1 1 d . . . . .
Cl4 Cl 0.74718(7) 0.26255(6) 0.72954(3) 0.02977(19) Uani 1 1 d . . . . .
O4 O 0.52935(19) 0.19569(15) 0.82216(9) 0.0239(5) Uani 1 1 d . . . . .
O5 O 0.54940(18) 0.39962(15) 0.81460(8) 0.0190(4) Uani 1 1 d . . . . .
O6 O 0.58962(18) 0.44245(15) 0.70052(8) 0.0210(5) Uani 1 1 d . . . . .
C34 C 0.3677(3) 0.2787(2) 0.89859(12) 0.0171(6) Uani 1 1 d . . . . .
H34 H 0.371561 0.300046 0.856570 0.021 Uiso 1 1 calc R . . . .
C35 C 0.4737(3) 0.1269(2) 0.86835(13) 0.0244(7) Uani 1 1 d . . . . .
C36 C 0.4978(3) 0.0226(3) 0.87417(15) 0.0349(8) Uani 1 1 d D . . . .
C37 C 0.4410(4) -0.0399(3) 0.92445(16) 0.0403(9) Uani 1 1 d . . . . .
H37 H 0.455641 -0.110913 0.929648 0.048 Uiso 1 1 calc R . . . .
C38 C 0.3642(3) -0.0040(2) 0.96738(14) 0.0303(8) Uani 1 1 d . . . . .
C39 C 0.3393(3) 0.0989(2) 0.95838(13) 0.0245(7) Uani 1 1 d . . . . .
H39 H 0.284510 0.124736 0.986413 0.029 Uiso 1 1 calc R . . . .
C40 C 0.3923(3) 0.1651(2) 0.90950(13) 0.0196(6) Uani 1 1 d . . . . .
C45 C 0.3088(4) -0.0766(3) 1.02083(16) 0.0417(10) Uani 1 1 d . . . . .
H45A H 0.282089 -0.139449 1.011034 0.063 Uiso 1 1 calc GR . . . .
H45B H 0.238468 -0.045071 1.040328 0.063 Uiso 1 1 calc GR . . . .
H45C H 0.369885 -0.092530 1.045897 0.063 Uiso 1 1 calc GR . . . .
C46 C 0.5571(3) 0.3959(2) 0.87085(12) 0.0176(6) Uani 1 1 d . . . . .
C47 C 0.6502(3) 0.4532(2) 0.88496(13) 0.0206(7) Uani 1 1 d . . . . .
C48 C 0.6583(3) 0.4399(2) 0.94235(13) 0.0222(7) Uani 1 1 d . . . . .
H48 H 0.720070 0.477178 0.952923 0.027 Uiso 1 1 calc R . . . .
C49 C 0.5813(3) 0.3750(2) 0.98527(13) 0.0213(7) Uani 1 1 d . . . . .
C50 C 0.4892(3) 0.3239(2) 0.96986(13) 0.0206(7) Uani 1 1 d . . . . .
H50 H 0.435465 0.279696 0.998536 0.025 Uiso 1 1 calc R . . . .
C51 C 0.4725(3) 0.3352(2) 0.91331(12) 0.0180(6) Uani 1 1 d . . . . .
C52 C 0.7365(3) 0.5275(3) 0.84049(13) 0.0271(8) Uani 1 1 d . . . . .
C53 C 0.6608(4) 0.6072(3) 0.80733(16) 0.0410(10) Uani 1 1 d . . . . .
H53A H 0.603912 0.572712 0.790023 0.062 Uiso 1 1 calc GR . . . .
H53B H 0.715538 0.652952 0.777489 0.062 Uiso 1 1 calc GR . . . .
H53C H 0.614610 0.646789 0.833357 0.062 Uiso 1 1 calc GR . . . .
C54 C 0.8209(4) 0.5862(3) 0.86782(15) 0.0458(11) Uani 1 1 d . . . . .
H54A H 0.771358 0.624087 0.893762 0.069 Uiso 1 1 calc GR . . . .
H54B H 0.873420 0.633925 0.838047 0.069 Uiso 1 1 calc GR . . . .
H54C H 0.871752 0.538051 0.889072 0.069 Uiso 1 1 calc GR . . . .
C55 C 0.8188(3) 0.4730(3) 0.79945(17) 0.0465(10) Uani 1 1 d . . . . .
H55A H 0.862238 0.418969 0.821051 0.070 Uiso 1 1 calc GR . . . .
H55B H 0.878133 0.521917 0.774099 0.070 Uiso 1 1 calc GR . . . .
H55C H 0.768912 0.443204 0.776859 0.070 Uiso 1 1 calc GR . . . .
C56 C 0.5976(3) 0.3647(3) 1.04651(13) 0.0304(8) Uani 1 1 d . . . . .
H56A H 0.680073 0.341009 1.050683 0.046 Uiso 1 1 calc GR . . . .
H56B H 0.537227 0.315379 1.070776 0.046 Uiso 1 1 calc GR . . . .
H56C H 0.586080 0.430946 1.057836 0.046 Uiso 1 1 calc GR . . . .
C57 C 0.2394(3) 0.3045(2) 0.92555(12) 0.0179(6) Uani 1 1 d . . . . .
C58 C 0.1362(3) 0.2703(2) 0.90791(12) 0.0219(7) Uani 1 1 d . . . . .
C59 C 0.0186(3) 0.2944(3) 0.92926(15) 0.0309(8) Uani 1 1 d . . . . .
H59 H -0.049068 0.268625 0.916599 0.037 Uiso 1 1 calc R . . . .
C60 C 0.0001(3) 0.3557(3) 0.96882(15) 0.0352(9) Uani 1 1 d . . . . .
H60 H -0.080562 0.372491 0.983774 0.042 Uiso 1 1 calc R . . . .
C61 C 0.0991(3) 0.3930(3) 0.98686(14) 0.0304(8) Uani 1 1 d . . . . .
H61 H 0.086862 0.436073 1.013969 0.036 Uiso 1 1 calc R . . . .
C62 C 0.2168(3) 0.3673(2) 0.96519(13) 0.0234(7) Uani 1 1 d . . . . .
H62 H 0.283980 0.393594 0.977932 0.028 Uiso 1 1 calc R . . . .
C63 C 0.6463(3) 0.4368(3) 0.64213(12) 0.0261(7) Uani 1 1 d . . . . .
H63A H 0.616879 0.375250 0.631032 0.031 Uiso 1 1 calc R . . . .
H63B H 0.736396 0.434776 0.638594 0.031 Uiso 1 1 calc R . . . .
C64 C 0.6079(3) 0.5318(3) 0.60567(14) 0.0364(9) Uani 1 1 d . . . . .
H64A H 0.605186 0.521566 0.566666 0.044 Uiso 1 1 calc R . . . .
H64B H 0.663679 0.589976 0.603719 0.044 Uiso 1 1 calc R . . . .
C65 C 0.4818(3) 0.5483(3) 0.63647(14) 0.0302(8) Uani 1 1 d . . . . .
H65A H 0.457119 0.619906 0.626009 0.036 Uiso 1 1 calc R . . . .
H65B H 0.420358 0.502725 0.628329 0.036 Uiso 1 1 calc R . . . .
C66 C 0.4978(3) 0.5223(2) 0.69741(14) 0.0270(7) Uani 1 1 d . . . . .
H66A H 0.526450 0.582861 0.709743 0.032 Uiso 1 1 calc R . . . .
H66B H 0.419716 0.497207 0.722047 0.032 Uiso 1 1 calc R . . . .
C41 C 0.5742(6) -0.0213(5) 0.8253(3) 0.0390(16) Uani 0.785(16) 1 d D U P B 1
C42 C 0.7056(6) 0.0201(5) 0.8171(3) 0.052(2) Uani 0.785(16) 1 d D U P B 1
H42A H 0.737010 0.001749 0.852954 0.078 Uiso 0.785(16) 1 calc R . P B 1
H42B H 0.757121 -0.009436 0.787764 0.078 Uiso 0.785(16) 1 calc R . P B 1
H42C H 0.706471 0.094373 0.805227 0.078 Uiso 0.785(16) 1 calc R . P B 1
C43 C 0.5791(9) -0.1390(4) 0.8405(3) 0.059(2) Uani 0.785(16) 1 d D U P B 1
H43A H 0.612480 -0.159282 0.875812 0.088 Uiso 0.785(16) 1 calc R . P B 1
H43B H 0.496460 -0.168175 0.845703 0.088 Uiso 0.785(16) 1 calc R . P B 1
H43C H 0.631422 -0.164123 0.809720 0.088 Uiso 0.785(16) 1 calc R . P B 1
C44 C 0.5216(8) 0.0057(6) 0.7701(3) 0.0479(19) Uani 0.785(16) 1 d D U P B 1
H44A H 0.437821 -0.021589 0.776461 0.072 Uiso 0.785(16) 1 calc R . P B 1
H44B H 0.521307 0.079903 0.757923 0.072 Uiso 0.785(16) 1 calc R . P B 1
H44C H 0.571958 -0.023907 0.740460 0.072 Uiso 0.785(16) 1 calc R . P B 1
C41A C 0.614(2) -0.0138(17) 0.8388(11) 0.052(5) Uani 0.215(16) 1 d D U P B 2
C42A C 0.738(2) 0.041(2) 0.8382(13) 0.069(6) Uani 0.215(16) 1 d D U P B 2
H42D H 0.757118 0.029185 0.876855 0.103 Uiso 0.215(16) 1 calc R . P B 2
H42E H 0.803183 0.013982 0.813153 0.103 Uiso 0.215(16) 1 calc R . P B 2
H42F H 0.731234 0.114299 0.824330 0.103 Uiso 0.215(16) 1 calc R . P B 2
C43A C 0.639(4) -0.1286(17) 0.8593(15) 0.087(8) Uani 0.215(16) 1 d D U P B 2
H43D H 0.665796 -0.138369 0.896340 0.131 Uiso 0.215(16) 1 calc R . P B 2
H43E H 0.563909 -0.168656 0.862710 0.131 Uiso 0.215(16) 1 calc R . P B 2
H43F H 0.702976 -0.151011 0.831654 0.131 Uiso 0.215(16) 1 calc R . P B 2
C44A C 0.573(4) -0.002(2) 0.7812(13) 0.067(7) Uani 0.215(16) 1 d D U P B 2
H44D H 0.556774 0.070027 0.767320 0.101 Uiso 0.215(16) 1 calc R . P B 2
H44E H 0.637330 -0.025013 0.754034 0.101 Uiso 0.215(16) 1 calc R . P B 2
H44F H 0.498263 -0.042659 0.785090 0.101 Uiso 0.215(16) 1 calc R . 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
Br1 C25 1.904(3) . ?
Ti1 Cl1 2.2835(9) . ?
Ti1 Cl2 2.2444(9) . ?
Ti1 O1 1.7734(19) . ?
Ti1 O2 1.8195(19) . ?
Ti1 O3 2.1810(19) . ?
O1 C2 1.373(3) . ?
O2 C13 1.381(3) . ?
O3 C30 1.464(3) . ?
O3 C33 1.460(4) . ?
C1 C7 1.531(4) . ?
C1 C18 1.524(4) . ?
C1 C24 1.531(4) . ?
C2 C3 1.411(4) . ?
C2 C7 1.399(4) . ?
C3 C4 1.394(4) . ?
C3 C8 1.538(4) . ?
C4 C5 1.397(4) . ?
C5 C6 1.386(4) . ?
C5 C12 1.504(4) . ?
C6 C7 1.383(4) . ?
C8 C9 1.539(4) . ?
C8 C10 1.535(4) . ?
C8 C11 1.540(4) . ?
C13 C14 1.419(4) . ?
C13 C18 1.399(4) . ?
C14 C15 1.396(4) . ?
C14 C19 1.536(4) . ?
C15 C16 1.388(4) . ?
C16 C17 1.378(4) . ?
C16 C23 1.508(4) . ?
C17 C18 1.392(4) . ?
C19 C20 1.533(4) . ?
C19 C21 1.540(4) . ?
C19 C22 1.538(4) . ?
C24 C25 1.397(4) . ?
C24 C29 1.395(4) . ?
C25 C26 1.386(4) . ?
C26 C27 1.377(5) . ?
C27 C28 1.375(5) . ?
C28 C29 1.385(4) . ?
C30 C31 1.505(6) . ?
C30 C31A 1.54(2) . ?
C33 C32 1.497(7) . ?
C33 C32A 1.66(3) . ?
C31 C32 1.460(9) . ?
C31A C32A 1.07(4) . ?
Br2 C58 1.901(3) . ?
Ti04 Cl3 2.2754(9) . ?
Ti04 Cl4 2.2514(9) . ?
Ti04 O4 1.779(2) . ?
Ti04 O5 1.820(2) . ?
Ti04 O6 2.186(2) . ?
O4 C35 1.368(4) . ?
O5 C46 1.376(3) . ?
O6 C63 1.471(3) . ?
O6 C66 1.468(4) . ?
C34 C40 1.522(4) . ?
C34 C51 1.523(4) . ?
C34 C57 1.531(4) . ?
C35 C36 1.403(4) . ?
C35 C40 1.403(4) . ?
C36 C37 1.397(5) . ?
C36 C41 1.551(6) . ?
C36 C41A 1.559(16) . ?
C37 C38 1.392(5) . ?
C38 C39 1.385(4) . ?
C38 C45 1.506(5) . ?
C39 C40 1.383(4) . ?
C46 C47 1.419(4) . ?
C46 C51 1.406(4) . ?
C47 C48 1.390(4) . ?
C47 C52 1.529(4) . ?
C48 C49 1.394(4) . ?
C49 C50 1.378(4) . ?
C49 C56 1.510(4) . ?
C50 C51 1.397(4) . ?
C52 C53 1.538(5) . ?
C52 C54 1.538(4) . ?
C52 C55 1.526(5) . ?
C57 C58 1.400(4) . ?
C57 C62 1.389(4) . ?
C58 C59 1.381(4) . ?
C59 C60 1.372(5) . ?
C60 C61 1.382(5) . ?
C61 C62 1.390(4) . ?
C63 C64 1.504(4) . ?
C64 C65 1.509(5) . ?
C65 C66 1.495(4) . ?
C41 C42 1.534(7) . ?
C41 C43 1.550(7) . ?
C41 C44 1.530(7) . ?
C41A C42A 1.561(14) . ?
C41A C43A 1.556(14) . ?
C41A C44A 1.526(14) . ?

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
Cl2 Ti1 Cl1 116.01(4) . . ?
O1 Ti1 Cl1 94.51(7) . . ?
O1 Ti1 Cl2 97.89(7) . . ?
O1 Ti1 O2 97.36(9) . . ?
O1 Ti1 O3 176.22(9) . . ?
O2 Ti1 Cl1 121.49(7) . . ?
O2 Ti1 Cl2 118.60(7) . . ?
O2 Ti1 O3 81.52(8) . . ?
O3 Ti1 Cl1 83.07(6) . . ?
O3 Ti1 Cl2 85.79(6) . . ?
C2 O1 Ti1 159.37(18) . . ?
C13 O2 Ti1 138.71(17) . . ?
C30 O3 Ti1 120.29(17) . . ?
C33 O3 Ti1 123.24(18) . . ?
C33 O3 C30 108.3(2) . . ?
C18 C1 C7 106.8(2) . . ?
C18 C1 C24 115.2(2) . . ?
C24 C1 C7 113.9(2) . . ?
O1 C2 C3 120.1(3) . . ?
O1 C2 C7 117.3(2) . . ?
C7 C2 C3 122.6(3) . . ?
C2 C3 C8 122.3(3) . . ?
C4 C3 C2 115.7(3) . . ?
C4 C3 C8 122.0(3) . . ?
C3 C4 C5 123.2(3) . . ?
C4 C5 C12 120.1(3) . . ?
C6 C5 C4 118.4(3) . . ?
C6 C5 C12 121.5(3) . . ?
C7 C6 C5 121.4(3) . . ?
C2 C7 C1 119.3(2) . . ?
C6 C7 C1 122.1(3) . . ?
C6 C7 C2 118.5(3) . . ?
C3 C8 C9 110.9(2) . . ?
C3 C8 C11 109.4(2) . . ?
C9 C8 C11 110.4(3) . . ?
C10 C8 C3 111.7(2) . . ?
C10 C8 C9 107.3(2) . . ?
C10 C8 C11 107.0(2) . . ?
O2 C13 C14 119.2(2) . . ?
O2 C13 C18 118.7(2) . . ?
C18 C13 C14 122.1(3) . . ?
C13 C14 C19 123.8(3) . . ?
C15 C14 C13 115.5(3) . . ?
C15 C14 C19 120.7(3) . . ?
C16 C15 C14 124.1(3) . . ?
C15 C16 C23 120.8(3) . . ?
C17 C16 C15 117.9(3) . . ?
C17 C16 C23 121.3(3) . . ?
C16 C17 C18 122.0(3) . . ?
C13 C18 C1 122.2(2) . . ?
C17 C18 C1 119.1(3) . . ?
C17 C18 C13 118.3(3) . . ?
C14 C19 C21 111.7(2) . . ?
C14 C19 C22 109.3(2) . . ?
C20 C19 C14 111.4(3) . . ?
C20 C19 C21 107.1(3) . . ?
C20 C19 C22 110.0(3) . . ?
C22 C19 C21 107.2(3) . . ?
C25 C24 C1 121.5(2) . . ?
C29 C24 C1 122.5(2) . . ?
C29 C24 C25 115.8(3) . . ?
C24 C25 Br1 121.8(2) . . ?
C26 C25 Br1 115.7(2) . . ?
C26 C25 C24 122.4(3) . . ?
C27 C26 C25 119.9(3) . . ?
C28 C27 C26 119.5(3) . . ?
C27 C28 C29 120.2(3) . . ?
C28 C29 C24 122.2(3) . . ?
O3 C30 C31 105.6(3) . . ?
O3 C30 C31A 98.3(9) . . ?
O3 C33 C32 106.1(4) . . ?
O3 C33 C32A 95.2(11) . . ?
C32 C31 C30 104.5(4) . . ?
C31 C32 C33 104.9(5) . . ?
C32A C31A C30 118(2) . . ?
C31A C32A C33 108(2) . . ?
Cl4 Ti04 Cl3 117.74(4) . . ?
O4 Ti04 Cl3 94.07(7) . . ?
O4 Ti04 Cl4 96.77(7) . . ?
O4 Ti04 O5 97.70(9) . . ?
O4 Ti04 O6 176.77(9) . . ?
O5 Ti04 Cl3 119.91(7) . . ?
O5 Ti04 Cl4 118.91(7) . . ?
O5 Ti04 O6 83.60(8) . . ?
O6 Ti04 Cl3 82.73(6) . . ?
O6 Ti04 Cl4 85.13(6) . . ?
C35 O4 Ti04 162.1(2) . . ?
C46 O5 Ti04 135.20(18) . . ?
C63 O6 Ti04 121.77(17) . . ?
C66 O6 Ti04 120.39(17) . . ?
C66 O6 C63 108.0(2) . . ?
C40 C34 C51 109.0(2) . . ?
C40 C34 C57 113.4(2) . . ?
C51 C34 C57 115.5(2) . . ?
O4 C35 C36 121.1(3) . . ?
O4 C35 C40 117.3(3) . . ?
C40 C35 C36 121.6(3) . . ?
C35 C36 C41 121.5(4) . . ?
C35 C36 C41A 120.0(9) . . ?
C37 C36 C35 116.2(3) . . ?
C37 C36 C41 122.1(4) . . ?
C37 C36 C41A 120.1(9) . . ?
C38 C37 C36 123.7(3) . . ?
C37 C38 C45 120.2(3) . . ?
C39 C38 C37 117.7(3) . . ?
C39 C38 C45 122.1(3) . . ?
C40 C39 C38 121.5(3) . . ?
C35 C40 C34 118.1(3) . . ?
C39 C40 C34 122.7(3) . . ?
C39 C40 C35 119.2(3) . . ?
O5 C46 C47 119.5(3) . . ?
O5 C46 C51 119.3(3) . . ?
C51 C46 C47 121.2(3) . . ?
C46 C47 C52 122.9(3) . . ?
C48 C47 C46 116.4(3) . . ?
C48 C47 C52 120.8(3) . . ?
C47 C48 C49 123.9(3) . . ?
C48 C49 C56 120.3(3) . . ?
C50 C49 C48 117.7(3) . . ?
C50 C49 C56 122.0(3) . . ?
C49 C50 C51 122.0(3) . . ?
C46 C51 C34 121.4(3) . . ?
C50 C51 C34 120.0(3) . . ?
C50 C51 C46 118.5(3) . . ?
C47 C52 C53 109.2(3) . . ?
C47 C52 C54 112.0(3) . . ?
C53 C52 C54 106.8(3) . . ?
C55 C52 C47 111.8(3) . . ?
C55 C52 C53 109.9(3) . . ?
C55 C52 C54 106.9(3) . . ?
C58 C57 C34 120.4(3) . . ?
C62 C57 C34 123.8(3) . . ?
C62 C57 C58 115.7(3) . . ?
C57 C58 Br2 120.6(2) . . ?
C59 C58 Br2 116.5(2) . . ?
C59 C58 C57 122.9(3) . . ?
C60 C59 C58 119.6(3) . . ?
C59 C60 C61 119.7(3) . . ?
C60 C61 C62 119.8(3) . . ?
C57 C62 C61 122.3(3) . . ?
O6 C63 C64 105.0(3) . . ?
C63 C64 C65 102.6(3) . . ?
C66 C65 C64 102.3(3) . . ?
O6 C66 C65 105.8(2) . . ?
C42 C41 C36 107.7(5) . . ?
C42 C41 C43 107.3(5) . . ?
C43 C41 C36 111.5(5) . . ?
C44 C41 C36 112.1(5) . . ?
C44 C41 C42 111.1(5) . . ?
C44 C41 C43 107.2(5) . . ?
C36 C41A C42A 117.2(16) . . ?
C43A C41A C36 112.5(17) . . ?
C43A C41A C42A 104.1(17) . . ?
C44A C41A C36 99.9(18) . . ?
C44A C41A C42A 115.2(17) . . ?
C44A C41A C43A 107.9(17) . . ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.000 -0.000 0.000 292 86 ' '
2 0.117 0.785 0.167 9 0 ' '
3 0.183 0.375 0.483 7 0 ' '
4 0.246 0.760 0.122 7 0 ' '
5 0.770 0.237 0.872 9 0 ' '
6 0.817 0.625 0.517 7 0 ' '
7 0.901 0.212 0.827 7 0 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The unit cell contains 2 THF molecules which have been treated
as a diffuse contribution to the overall scattering without 
specific atom positions by SQUEEZE/PLATON.
;


####################################################################### 
# 
# 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_o2ccti_thf
_database_code_depnum_ccdc_archive 'CCDC 1957865'
loop_
_audit_author_name
_audit_author_address
'Yutaka Ishida'
;Tokyo Institute of Technology
Japan
;
_audit_update_record             
;
2019-10-07 deposited with the CCDC.	2019-11-26 downloaded from the CCDC.
;
_audit_creation_date             2019-10-01
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_chemical_formula_moiety         'C43 H60 O4 Ti'
_chemical_formula_sum            'C43 H60 O4 Ti'
_chemical_formula_weight         688.81

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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'

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                   9.8645(2)
_cell_length_b                   17.6446(5)
_cell_length_c                   21.7498(5)
_cell_angle_alpha                90
_cell_angle_beta                 89.382(2)
_cell_angle_gamma                90
_cell_volume                     3785.45(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    17534
_cell_measurement_temperature    123
_cell_measurement_theta_max      31.2420
_cell_measurement_theta_min      2.1890
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73915
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       Rod
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31095
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.556
_diffrn_reflns_theta_min         2.536
_diffrn_ambient_temperature      123
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.1429
_diffrn_detector_type            'Rigaku Saturn724+ area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50    8.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50    8.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0686537000
_diffrn_orient_matrix_UB_12      0.0090117000
_diffrn_orient_matrix_UB_13      -0.0060115000
_diffrn_orient_matrix_UB_21      -0.0026359000
_diffrn_orient_matrix_UB_22      -0.0297280000
_diffrn_orient_matrix_UB_23      -0.0219011000
_diffrn_orient_matrix_UB_31      -0.0211622000
_diffrn_orient_matrix_UB_32      -0.0255283000
_diffrn_orient_matrix_UB_33      0.0234085000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6919
_reflns_number_total             8740
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         8740
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0433
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0491P)²+1.7711P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1080
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap

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 0.72108(3) 0.48488(2) 0.32839(2) 0.01372(8) Uani 1 1 d . . . . .
O1 O 0.62537(11) 0.48718(6) 0.25156(5) 0.0160(2) Uani 1 1 d . . . . .
O2 O 0.81879(11) 0.40820(6) 0.37102(5) 0.0177(2) Uani 1 1 d . . . . .
O3 O 0.91111(11) 0.49016(7) 0.27823(5) 0.0192(2) Uani 1 1 d . . . . .
O4 O 0.76332(13) 0.61092(7) 0.30900(5) 0.0218(3) Uani 1 1 d . . . . .
C1 C 0.53179(16) 0.43370(9) 0.23710(7) 0.0143(3) Uani 1 1 d . . . . .
C2 C 0.46932(16) 0.42860(9) 0.17911(7) 0.0147(3) Uani 1 1 d . . . . .
C3 C 0.38711(16) 0.36538(9) 0.16966(7) 0.0152(3) Uani 1 1 d . . . . .
H3 H 0.345370 0.360074 0.130737 0.018 Uiso 1 1 calc R . . . .
C4 C 0.36221(15) 0.30925(9) 0.21392(7) 0.0146(3) Uani 1 1 d . . . . .
C5 C 0.41911(15) 0.31924(9) 0.27171(7) 0.0145(3) Uani 1 1 d . . . . .
H5 H 0.401708 0.283027 0.303146 0.017 Uiso 1 1 calc R . . . .
C6 C 0.50103(15) 0.38147(9) 0.28406(7) 0.0138(3) Uani 1 1 d . . . . .
C7 C 0.49044(17) 0.48955(9) 0.12966(7) 0.0170(3) Uani 1 1 d . . . . .
C8 C 0.4511(2) 0.56726(10) 0.15611(8) 0.0257(4) Uani 1 1 d . . . . .
H8A H 0.353663 0.568096 0.165305 0.039 Uiso 1 1 calc GR . . . .
H8B H 0.472909 0.606843 0.125977 0.039 Uiso 1 1 calc GR . . . .
H8C H 0.501699 0.576443 0.193919 0.039 Uiso 1 1 calc GR . . . .
C9 C 0.63897(18) 0.49077(12) 0.10790(8) 0.0272(4) Uani 1 1 d . . . . .
H9A H 0.697504 0.502756 0.142697 0.041 Uiso 1 1 calc GR . . . .
H9B H 0.650642 0.529350 0.075869 0.041 Uiso 1 1 calc GR . . . .
H9C H 0.663586 0.440967 0.091244 0.041 Uiso 1 1 calc GR . . . .
C10 C 0.40157(18) 0.47649(10) 0.07338(7) 0.0217(4) Uani 1 1 d . . . . .
H10A H 0.428277 0.429055 0.053193 0.032 Uiso 1 1 calc GR . . . .
H10B H 0.413213 0.518718 0.044536 0.032 Uiso 1 1 calc GR . . . .
H10C H 0.306309 0.473347 0.086394 0.032 Uiso 1 1 calc GR . . . .
C11 C 0.27443(17) 0.24044(10) 0.19809(8) 0.0192(3) Uani 1 1 d . . . . .
C12 C 0.1276(2) 0.26499(12) 0.18707(11) 0.0357(5) Uani 1 1 d . . . . .
H12A H 0.090201 0.287869 0.224648 0.054 Uiso 1 1 calc GR . . . .
H12B H 0.073233 0.220667 0.175921 0.054 Uiso 1 1 calc GR . . . .
H12C H 0.125387 0.302124 0.153585 0.054 Uiso 1 1 calc GR . . . .
C13 C 0.2707(2) 0.18176(10) 0.24982(8) 0.0249(4) Uani 1 1 d . . . . .
H13A H 0.363245 0.165234 0.258817 0.037 Uiso 1 1 calc GR . . . .
H13B H 0.216638 0.138026 0.237042 0.037 Uiso 1 1 calc GR . . . .
H13C H 0.229859 0.204410 0.286753 0.037 Uiso 1 1 calc GR . . . .
C14 C 0.3284(2) 0.20199(11) 0.13954(8) 0.0315(5) Uani 1 1 d . . . . .
H14A H 0.319032 0.236610 0.104607 0.047 Uiso 1 1 calc GR . . . .
H14B H 0.276387 0.155685 0.131832 0.047 Uiso 1 1 calc GR . . . .
H14C H 0.424200 0.189085 0.144745 0.047 Uiso 1 1 calc GR . . . .
C15 C 0.56757(15) 0.40069(9) 0.34315(7) 0.0135(3) Uani 1 1 d . . . . .
C16 C 0.75734(16) 0.34714(9) 0.39761(7) 0.0152(3) Uani 1 1 d . . . . .
C17 C 0.82467(16) 0.29449(9) 0.43519(7) 0.0163(3) Uani 1 1 d . . . . .
C18 C 0.74481(16) 0.23558(9) 0.45935(7) 0.0165(3) Uani 1 1 d . . . . .
H18 H 0.787863 0.198565 0.484134 0.020 Uiso 1 1 calc R . . . .
C19 C 0.60629(17) 0.22804(9) 0.44923(7) 0.0161(3) Uani 1 1 d . . . . .
C20 C 0.54468(16) 0.28156(9) 0.41130(7) 0.0158(3) Uani 1 1 d . . . . .
H20 H 0.450199 0.278137 0.403750 0.019 Uiso 1 1 calc R . . . .
C21 C 0.61952(16) 0.33965(9) 0.38449(7) 0.0144(3) Uani 1 1 d . . . . .
C22 C 0.97679(16) 0.30111(10) 0.44791(8) 0.0196(4) Uani 1 1 d . . . . .
C23 C 1.00604(18) 0.37595(11) 0.48158(9) 0.0259(4) Uani 1 1 d . . . . .
H23A H 0.972222 0.418510 0.457194 0.039 Uiso 1 1 calc GR . . . .
H23B H 1.104007 0.381413 0.487145 0.039 Uiso 1 1 calc GR . . . .
H23C H 0.960510 0.375591 0.521853 0.039 Uiso 1 1 calc GR . . . .
C24 C 1.02891(18) 0.23587(11) 0.48784(9) 0.0269(4) Uani 1 1 d . . . . .
H24A H 0.981377 0.236355 0.527638 0.040 Uiso 1 1 calc GR . . . .
H24B H 1.126451 0.242049 0.494313 0.040 Uiso 1 1 calc GR . . . .
H24C H 1.012202 0.187520 0.467081 0.040 Uiso 1 1 calc GR . . . .
C25 C 1.05605(18) 0.29855(11) 0.38636(8) 0.0262(4) Uani 1 1 d . . . . .
H25A H 1.038645 0.250214 0.365705 0.039 Uiso 1 1 calc GR . . . .
H25B H 1.153288 0.303441 0.394232 0.039 Uiso 1 1 calc GR . . . .
H25C H 1.026529 0.340385 0.360055 0.039 Uiso 1 1 calc GR . . . .
C26 C 0.51838(18) 0.16574(10) 0.47892(8) 0.0209(4) Uani 1 1 d . . . . .
C27 C 0.41733(19) 0.20333(12) 0.52372(10) 0.0339(5) Uani 1 1 d . . . . .
H27A H 0.467139 0.229594 0.556128 0.051 Uiso 1 1 calc GR . . . .
H27B H 0.358815 0.164462 0.542219 0.051 Uiso 1 1 calc GR . . . .
H27C H 0.361610 0.239908 0.501386 0.051 Uiso 1 1 calc GR . . . .
C28 C 0.60125(19) 0.10859(10) 0.51532(9) 0.0260(4) Uani 1 1 d . . . . .
H28A H 0.664320 0.082260 0.487515 0.039 Uiso 1 1 calc GR . . . .
H28B H 0.540224 0.071628 0.534728 0.039 Uiso 1 1 calc GR . . . .
H28C H 0.652470 0.135147 0.547106 0.039 Uiso 1 1 calc GR . . . .
C29 C 0.4416(3) 0.12251(13) 0.42914(10) 0.0469(6) Uani 1 1 d . . . . .
H29A H 0.383063 0.157687 0.406815 0.070 Uiso 1 1 calc GR . . . .
H29B H 0.385963 0.082843 0.448341 0.070 Uiso 1 1 calc GR . . . .
H29C H 0.506605 0.099333 0.400407 0.070 Uiso 1 1 calc GR . . . .
C30 C 0.50438(16) 0.46532(9) 0.37998(7) 0.0151(3) Uani 1 1 d . . . . .
C31 C 0.59474(17) 0.52137(9) 0.39907(7) 0.0169(3) Uani 1 1 d . . . . .
C32 C 0.54561(18) 0.57691(9) 0.44017(7) 0.0205(4) Uani 1 1 d . . . . .
H32 H 0.605774 0.614336 0.455418 0.025 Uiso 1 1 calc R . . . .
C33 C 0.41133(19) 0.57770(10) 0.45859(7) 0.0227(4) Uani 1 1 d . . . . .
H33 H 0.379805 0.615353 0.486507 0.027 Uiso 1 1 calc R . . . .
C34 C 0.32164(18) 0.52320(10) 0.43625(8) 0.0224(4) Uani 1 1 d . . . . .
H34 H 0.228835 0.524754 0.448321 0.027 Uiso 1 1 calc R . . . .
C35 C 0.36667(17) 0.46728(10) 0.39689(7) 0.0191(3) Uani 1 1 d . . . . .
H35 H 0.305447 0.430555 0.381397 0.023 Uiso 1 1 calc R . . . .
C36 C 1.03973(17) 0.50516(11) 0.30910(8) 0.0241(4) Uani 1 1 d . . . . .
H36A H 1.041249 0.480251 0.349875 0.029 Uiso 1 1 calc R . . . .
H36B H 1.053055 0.560320 0.314799 0.029 Uiso 1 1 calc R . . . .
C37 C 1.14897(18) 0.47278(11) 0.26741(9) 0.0268(4) Uani 1 1 d . . . . .
H37A H 1.175749 0.421311 0.280735 0.032 Uiso 1 1 calc R . . . .
H37B H 1.230125 0.505776 0.266409 0.032 Uiso 1 1 calc R . . . .
C38 C 1.0807(2) 0.47073(12) 0.20535(9) 0.0330(5) Uani 1 1 d . . . . .
H38A H 1.082084 0.521136 0.185363 0.040 Uiso 1 1 calc R . . . .
H38B H 1.124023 0.433158 0.177622 0.040 Uiso 1 1 calc R . . . .
C39 C 0.9382(2) 0.44729(13) 0.22298(9) 0.0338(5) Uani 1 1 d . . . . .
H39A H 0.873303 0.460534 0.190264 0.041 Uiso 1 1 calc R . . . .
H39B H 0.932995 0.392130 0.231009 0.041 Uiso 1 1 calc R . . . .
C40 C 0.73858(19) 0.67609(10) 0.34859(8) 0.0242(4) Uani 1 1 d . . . . .
H40A H 0.799980 0.675104 0.384291 0.029 Uiso 1 1 calc R . . . .
H40B H 0.643714 0.676014 0.363920 0.029 Uiso 1 1 calc R . . . .
C41 C 0.7656(2) 0.74580(10) 0.30934(9) 0.0294(4) Uani 1 1 d . . . . .
H41A H 0.705081 0.788194 0.321285 0.035 Uiso 1 1 calc R . . . .
H41B H 0.861084 0.762493 0.312550 0.035 Uiso 1 1 calc R . . . .
C42 C 0.7348(2) 0.71771(11) 0.24509(9) 0.0309(4) Uani 1 1 d . . . . .
H42A H 0.636120 0.717919 0.237262 0.037 Uiso 1 1 calc R . . . .
H42B H 0.781541 0.748710 0.213401 0.037 Uiso 1 1 calc R . . . .
C43 C 0.79029(19) 0.63793(10) 0.24668(8) 0.0247(4) Uani 1 1 d . . . . .
H43A H 0.744156 0.605538 0.216188 0.030 Uiso 1 1 calc R . . . .
H43B H 0.888845 0.637772 0.237598 0.030 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O1 1.9286(11) . ?
Ti1 O2 1.9075(11) . ?
Ti1 O3 2.1607(11) . ?
Ti1 O4 2.3008(12) . ?
Ti1 C15 2.1429(16) . ?
Ti1 C31 2.0711(16) . ?
O1 C1 1.3593(19) . ?
O2 C16 1.3620(19) . ?
O3 C36 1.466(2) . ?
O3 C39 1.443(2) . ?
O4 C40 1.456(2) . ?
O4 C43 1.459(2) . ?
C1 C2 1.413(2) . ?
C1 C6 1.407(2) . ?
C2 C3 1.396(2) . ?
C2 C7 1.534(2) . ?
C3 C4 1.401(2) . ?
C4 C5 1.393(2) . ?
C4 C11 1.533(2) . ?
C5 C6 1.391(2) . ?
C6 C15 1.489(2) . ?
C7 C8 1.535(2) . ?
C7 C9 1.535(2) . ?
C7 C10 1.531(2) . ?
C11 C12 1.534(3) . ?
C11 C13 1.529(2) . ?
C11 C14 1.533(2) . ?
C15 C21 1.497(2) . ?
C15 C30 1.523(2) . ?
C16 C17 1.409(2) . ?
C16 C21 1.398(2) . ?
C17 C18 1.403(2) . ?
C17 C22 1.533(2) . ?
C18 C19 1.393(2) . ?
C19 C20 1.397(2) . ?
C19 C26 1.538(2) . ?
C20 C21 1.388(2) . ?
C22 C23 1.539(2) . ?
C22 C24 1.534(2) . ?
C22 C25 1.544(2) . ?
C26 C27 1.537(3) . ?
C26 C28 1.525(2) . ?
C26 C29 1.531(3) . ?
C30 C31 1.398(2) . ?
C30 C35 1.404(2) . ?
C31 C32 1.409(2) . ?
C32 C33 1.380(3) . ?
C33 C34 1.398(3) . ?
C34 C35 1.377(2) . ?
C36 C37 1.513(2) . ?
C37 C38 1.515(3) . ?
C38 C39 1.511(3) . ?
C40 C41 1.519(2) . ?
C41 C42 1.516(3) . ?
C42 C43 1.511(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 O3 89.53(5) . . ?
O1 Ti1 O4 84.85(4) . . ?
O1 Ti1 C15 78.04(5) . . ?
O1 Ti1 C31 109.89(6) . . ?
O2 Ti1 O1 133.69(5) . . ?
O2 Ti1 O3 80.55(5) . . ?
O2 Ti1 O4 133.09(5) . . ?
O2 Ti1 C15 78.20(5) . . ?
O2 Ti1 C31 99.38(6) . . ?
O3 Ti1 O4 73.22(4) . . ?
C15 Ti1 O3 135.51(5) . . ?
C15 Ti1 O4 145.46(5) . . ?
C31 Ti1 O3 150.82(6) . . ?
C31 Ti1 O4 86.66(5) . . ?
C31 Ti1 C15 71.68(6) . . ?
C1 O1 Ti1 121.73(9) . . ?
C16 O2 Ti1 122.85(10) . . ?
C36 O3 Ti1 121.80(10) . . ?
C39 O3 Ti1 123.34(11) . . ?
C39 O3 C36 108.85(13) . . ?
C40 O4 Ti1 128.78(10) . . ?
C40 O4 C43 108.62(12) . . ?
C43 O4 Ti1 121.13(10) . . ?
O1 C1 C2 123.70(14) . . ?
O1 C1 C6 115.37(13) . . ?
C6 C1 C2 120.93(14) . . ?
C1 C2 C7 121.61(14) . . ?
C3 C2 C1 116.25(14) . . ?
C3 C2 C7 122.14(14) . . ?
C2 C3 C4 124.18(14) . . ?
C3 C4 C11 120.07(14) . . ?
C5 C4 C3 117.46(14) . . ?
C5 C4 C11 122.48(14) . . ?
C6 C5 C4 120.96(14) . . ?
C1 C6 C15 112.59(14) . . ?
C5 C6 C1 119.88(14) . . ?
C5 C6 C15 127.52(14) . . ?
C2 C7 C8 109.37(13) . . ?
C2 C7 C9 110.37(14) . . ?
C9 C7 C8 109.85(15) . . ?
C10 C7 C2 112.37(13) . . ?
C10 C7 C8 106.83(14) . . ?
C10 C7 C9 107.98(13) . . ?
C4 C11 C12 110.39(14) . . ?
C4 C11 C14 110.20(14) . . ?
C13 C11 C4 112.35(13) . . ?
C13 C11 C12 106.92(15) . . ?
C13 C11 C14 108.47(15) . . ?
C14 C11 C12 108.37(16) . . ?
C6 C15 Ti1 110.24(10) . . ?
C6 C15 C21 120.77(13) . . ?
C6 C15 C30 116.29(13) . . ?
C21 C15 Ti1 110.05(10) . . ?
C21 C15 C30 111.32(12) . . ?
C30 C15 Ti1 81.05(9) . . ?
O2 C16 C17 123.89(14) . . ?
O2 C16 C21 114.66(14) . . ?
C21 C16 C17 121.45(15) . . ?
C16 C17 C22 121.54(14) . . ?
C18 C17 C16 116.08(15) . . ?
C18 C17 C22 122.38(14) . . ?
C19 C18 C17 124.02(15) . . ?
C18 C19 C20 117.54(15) . . ?
C18 C19 C26 123.48(14) . . ?
C20 C19 C26 118.96(14) . . ?
C21 C20 C19 120.95(15) . . ?
C16 C21 C15 113.23(14) . . ?
C20 C21 C15 126.84(14) . . ?
C20 C21 C16 119.87(14) . . ?
C17 C22 C23 109.88(14) . . ?
C17 C22 C24 112.31(14) . . ?
C17 C22 C25 109.19(14) . . ?
C23 C22 C25 110.00(15) . . ?
C24 C22 C23 107.99(14) . . ?
C24 C22 C25 107.42(14) . . ?
C27 C26 C19 108.46(14) . . ?
C28 C26 C19 112.81(14) . . ?
C28 C26 C27 107.69(14) . . ?
C28 C26 C29 108.04(16) . . ?
C29 C26 C19 109.88(15) . . ?
C29 C26 C27 109.93(18) . . ?
C31 C30 C15 115.30(14) . . ?
C31 C30 C35 121.55(15) . . ?
C35 C30 C15 123.07(14) . . ?
C30 C31 Ti1 86.57(10) . . ?
C30 C31 C32 117.68(15) . . ?
C32 C31 Ti1 152.54(13) . . ?
C33 C32 C31 120.92(16) . . ?
C32 C33 C34 120.10(16) . . ?
C35 C34 C33 120.54(16) . . ?
C34 C35 C30 119.03(16) . . ?
O3 C36 C37 105.76(14) . . ?
C36 C37 C38 102.86(14) . . ?
C39 C38 C37 101.64(15) . . ?
O3 C39 C38 103.36(15) . . ?
O4 C40 C41 106.25(14) . . ?
C42 C41 C40 102.56(15) . . ?
C43 C42 C41 101.96(15) . . ?
O4 C43 C42 105.26(14) . . ?



####################################################################### 
# 
# 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_oocpticl
_database_code_depnum_ccdc_archive 'CCDC 1957866'
loop_
_audit_author_name
_audit_author_address
'Yutaka Ishida'
;Tokyo Institute of Technology
Japan
;
_audit_update_record             
;
2019-10-07 deposited with the CCDC.	2019-11-26 downloaded from the CCDC.
;
_audit_creation_date             2019-10-01
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_chemical_formula_moiety         'C52 H59 Cl N O2 P Ti, 1(C7 H8)'
_chemical_formula_sum            'C59 H67 Cl N O2 P Ti'
_chemical_formula_weight         936.45

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'
Cl Cl 0.1484 0.1585 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.9944(2)
_cell_length_b                   13.2152(2)
_cell_length_c                   17.0702(3)
_cell_angle_alpha                79.141(1)
_cell_angle_beta                 80.483(1)
_cell_angle_gamma                84.749(1)
_cell_volume                     2615.65(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    20127
_cell_measurement_temperature    123
_cell_measurement_theta_max      31.2050
_cell_measurement_theta_min      2.2450
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.287
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95063
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'reddish brown'
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       block
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32698
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.560
_diffrn_reflns_theta_min         2.674
_diffrn_ambient_temperature      123
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.1429
_diffrn_detector_type            'Rigaku Saturn724+ area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50    8.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50    8.00    --  -20.00  45.00  90.00  360
  3  ω   -110.00  70.00   0.50    8.00    --  -20.00  45.00 180.00  360
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0101110000
_diffrn_orient_matrix_UB_12      0.0076187000
_diffrn_orient_matrix_UB_13      -0.0427687000
_diffrn_orient_matrix_UB_21      -0.0126812000
_diffrn_orient_matrix_UB_22      0.0537831000
_diffrn_orient_matrix_UB_23      -0.0016782000
_diffrn_orient_matrix_UB_31      0.0578476000
_diffrn_orient_matrix_UB_32      0.0069139000
_diffrn_orient_matrix_UB_33      0.0003755000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9547
_reflns_number_total             12066
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         12066
_refine_ls_number_restraints     348
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0407
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0532P)²+0.9368P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1083

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap

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 0.40994(2) 0.32693(2) 0.22043(2) 0.01797(8) Uani 1 1 d . . . . .
Cl1 Cl 0.41017(4) 0.50058(3) 0.15056(2) 0.02766(10) Uani 1 1 d . . . . .
P1 P 0.45561(3) 0.41637(3) 0.33094(2) 0.01842(9) Uani 1 1 d . . . . .
O1 O 0.56361(9) 0.26788(8) 0.20810(6) 0.0208(2) Uani 1 1 d . . . . .
O2 O 0.25291(9) 0.31208(9) 0.25573(6) 0.0217(2) Uani 1 1 d . . . . .
N1 N 0.37700(12) 0.28875(11) 0.10309(8) 0.0219(3) Uani 1 1 d . . . . .
C1 C 0.53095(13) 0.17022(12) 0.21661(9) 0.0194(3) Uani 1 1 d . . . . .
C2 C 0.57953(14) 0.09956(13) 0.16539(10) 0.0221(3) Uani 1 1 d . . . . .
C3 C 0.52142(15) 0.01213(13) 0.17072(10) 0.0242(3) Uani 1 1 d . . . . .
H3 H 0.552137 -0.036015 0.136739 0.029 Uiso 1 1 calc R . . . .
C4 C 0.41953(15) -0.01013(12) 0.22335(10) 0.0225(3) Uani 1 1 d . . . . .
C5 C 0.38061(14) 0.05533(12) 0.27763(9) 0.0210(3) Uani 1 1 d . . . . .
H5 H 0.314384 0.040252 0.315706 0.025 Uiso 1 1 calc R . . . .
C6 C 0.43724(13) 0.14362(12) 0.27743(9) 0.0183(3) Uani 1 1 d . . . . .
C7 C 0.69205(15) 0.11992(14) 0.10904(11) 0.0279(4) Uani 1 1 d . . . . .
C8 C 0.78126(16) 0.14016(17) 0.15850(12) 0.0366(5) Uani 1 1 d . . . . .
H8A H 0.756212 0.201279 0.183083 0.055 Uiso 1 1 calc GR . . . .
H8B H 0.853631 0.151864 0.122970 0.055 Uiso 1 1 calc GR . . . .
H8C H 0.790787 0.080218 0.200966 0.055 Uiso 1 1 calc GR . . . .
C9 C 0.67691(16) 0.21253(16) 0.04219(11) 0.0346(4) Uani 1 1 d . . . . .
H9A H 0.616908 0.200647 0.012969 0.052 Uiso 1 1 calc GR . . . .
H9B H 0.748031 0.221524 0.004726 0.052 Uiso 1 1 calc GR . . . .
H9C H 0.656078 0.274834 0.066009 0.052 Uiso 1 1 calc GR . . . .
C10 C 0.73668(18) 0.02665(17) 0.06881(14) 0.0445(5) Uani 1 1 d . . . . .
H10A H 0.746285 -0.034213 0.110459 0.067 Uiso 1 1 calc GR . . . .
H10B H 0.809782 0.041033 0.034958 0.067 Uiso 1 1 calc GR . . . .
H10C H 0.682478 0.013556 0.035307 0.067 Uiso 1 1 calc GR . . . .
C11 C 0.35331(16) -0.10345(13) 0.22121(10) 0.0273(4) Uani 1 1 d . . . . .
C12 C 0.32350(19) -0.16475(15) 0.30639(11) 0.0371(5) Uani 1 1 d . . . . .
H12A H 0.393150 -0.187546 0.329381 0.056 Uiso 1 1 calc GR . . . .
H12B H 0.283147 -0.225123 0.304162 0.056 Uiso 1 1 calc GR . . . .
H12C H 0.275107 -0.120907 0.340242 0.056 Uiso 1 1 calc GR . . . .
C13 C 0.24316(19) -0.06365(17) 0.18731(14) 0.0439(5) Uani 1 1 d . . . . .
H13A H 0.199046 -0.017336 0.221119 0.066 Uiso 1 1 calc GR . . . .
H13B H 0.198674 -0.122218 0.187187 0.066 Uiso 1 1 calc GR . . . .
H13C H 0.261613 -0.026045 0.132047 0.066 Uiso 1 1 calc GR . . . .
C14 C 0.4191(2) -0.17736(16) 0.16806(13) 0.0436(5) Uani 1 1 d . . . . .
H14A H 0.436267 -0.140489 0.112452 0.065 Uiso 1 1 calc GR . . . .
H14B H 0.373116 -0.235401 0.169308 0.065 Uiso 1 1 calc GR . . . .
H14C H 0.489898 -0.203365 0.188494 0.065 Uiso 1 1 calc GR . . . .
C15 C 0.40647(13) 0.21466(12) 0.33713(9) 0.0183(3) Uani 1 1 d . . . . .
C16 C 0.20778(14) 0.26150(12) 0.32924(9) 0.0199(3) Uani 1 1 d . . . . .
C17 C 0.09066(14) 0.25921(13) 0.35646(10) 0.0231(3) Uani 1 1 d . . . . .
C18 C 0.05877(15) 0.21176(13) 0.43692(10) 0.0254(4) Uani 1 1 d . . . . .
H18 H -0.019793 0.209186 0.457188 0.030 Uiso 1 1 calc R . . . .
C19 C 0.13546(15) 0.16819(12) 0.48887(10) 0.0242(4) Uani 1 1 d . . . . .
C20 C 0.25053(14) 0.16808(12) 0.45795(10) 0.0217(3) Uani 1 1 d . . . . .
H20 H 0.304622 0.137357 0.491580 0.026 Uiso 1 1 calc R . . . .
C21 C 0.28685(14) 0.21260(12) 0.37825(9) 0.0195(3) Uani 1 1 d . . . . .
C22 C 0.00387(14) 0.30829(14) 0.30197(11) 0.0288(4) Uani 1 1 d . . . . .
C23 C 0.02277(17) 0.2614(2) 0.22456(13) 0.0438(5) Uani 1 1 d . . . . .
H23A H 0.095689 0.281022 0.192582 0.066 Uiso 1 1 calc GR . . . .
H23B H -0.038258 0.287306 0.192893 0.066 Uiso 1 1 calc GR . . . .
H23C H 0.022926 0.186016 0.238868 0.066 Uiso 1 1 calc GR . . . .
C24 C 0.01610(17) 0.42527(16) 0.28040(14) 0.0425(5) Uani 1 1 d . . . . .
H24A H -0.000268 0.455260 0.329689 0.064 Uiso 1 1 calc GR . . . .
H24B H -0.037256 0.456446 0.243624 0.064 Uiso 1 1 calc GR . . . .
H24C H 0.093630 0.438803 0.254099 0.064 Uiso 1 1 calc GR . . . .
C25 C -0.11857(15) 0.29107(16) 0.34237(13) 0.0365(4) Uani 1 1 d . . . . .
H25A H -0.128919 0.216835 0.357234 0.055 Uiso 1 1 calc GR . . . .
H25B H -0.170559 0.322824 0.304750 0.055 Uiso 1 1 calc GR . . . .
H25C H -0.134470 0.322559 0.390952 0.055 Uiso 1 1 calc GR . . . .
C26 C 0.09524(15) 0.12388(14) 0.57812(10) 0.0280(4) Uani 1 1 d D . . . .
C27 C 0.1443(3) 0.0180(2) 0.59880(19) 0.0392(9) Uani 0.622(3) 1 d D . P A 1
H27A H 0.121223 -0.025372 0.564390 0.059 Uiso 0.622(3) 1 calc R . P A 1
H27B H 0.227093 0.018512 0.590278 0.059 Uiso 0.622(3) 1 calc R . P A 1
H27C H 0.117302 -0.009617 0.655511 0.059 Uiso 0.622(3) 1 calc R . P A 1
C28 C -0.0384(3) 0.1201(3) 0.59577(19) 0.0394(9) Uani 0.622(3) 1 d D . P A 1
H28A H -0.073404 0.189891 0.582458 0.059 Uiso 0.622(3) 1 calc R . P A 1
H28B H -0.062532 0.075382 0.562762 0.059 Uiso 0.622(3) 1 calc R . P A 1
H28C H -0.062025 0.092605 0.653019 0.059 Uiso 0.622(3) 1 calc R . P A 1
C29 C 0.1248(3) 0.1981(3) 0.62711(19) 0.0427(10) Uani 0.622(3) 1 d D . P A 1
H29A H 0.089056 0.266614 0.609779 0.064 Uiso 0.622(3) 1 calc R . P A 1
H29B H 0.097383 0.174021 0.684368 0.064 Uiso 0.622(3) 1 calc R . P A 1
H29C H 0.207174 0.202151 0.619135 0.064 Uiso 0.622(3) 1 calc R . P A 1
C28A C 0.0315(5) 0.2031(4) 0.6222(3) 0.0361(14) Uani 0.378(3) 1 d D . P A 2
H28D H 0.075774 0.264133 0.613053 0.054 Uiso 0.378(3) 1 calc R . P A 2
H28E H -0.041113 0.222493 0.602604 0.054 Uiso 0.378(3) 1 calc R . P A 2
H28F H 0.017927 0.174856 0.680076 0.054 Uiso 0.378(3) 1 calc R . P A 2
C29A C 0.2017(4) 0.0834(4) 0.6293(3) 0.0368(14) Uani 0.378(3) 1 d D . P A 2
H29D H 0.249224 0.030193 0.604366 0.055 Uiso 0.378(3) 1 calc R . P A 2
H29E H 0.247128 0.141654 0.628612 0.055 Uiso 0.378(3) 1 calc R . P A 2
H29F H 0.171659 0.054521 0.685206 0.055 Uiso 0.378(3) 1 calc R . P A 2
C27A C 0.0335(5) 0.0270(4) 0.5888(3) 0.0443(16) Uani 0.378(3) 1 d D . P A 2
H27D H 0.079421 -0.022144 0.558419 0.066 Uiso 0.378(3) 1 calc R . P A 2
H27E H 0.019904 -0.003807 0.646118 0.066 Uiso 0.378(3) 1 calc R . P A 2
H27F H -0.039136 0.043830 0.568646 0.066 Uiso 0.378(3) 1 calc R . P A 2
C30 C 0.49379(13) 0.21801(12) 0.39007(9) 0.0190(3) Uani 1 1 d . . . . .
C31 C 0.52207(13) 0.31567(12) 0.39807(9) 0.0191(3) Uani 1 1 d . . . . .
C32 C 0.59834(14) 0.32639(13) 0.44874(10) 0.0227(3) Uani 1 1 d . . . . .
H32 H 0.617060 0.393100 0.453397 0.027 Uiso 1 1 calc R . . . .
C33 C 0.64666(15) 0.23926(14) 0.49224(10) 0.0261(4) Uani 1 1 d . . . . .
H33 H 0.698310 0.245983 0.527294 0.031 Uiso 1 1 calc R . . . .
C34 C 0.61971(15) 0.14199(14) 0.48470(10) 0.0267(4) Uani 1 1 d . . . . .
H34 H 0.652905 0.082460 0.515005 0.032 Uiso 1 1 calc R . . . .
C35 C 0.54481(14) 0.13049(13) 0.43340(10) 0.0239(3) Uani 1 1 d . . . . .
H35 H 0.528341 0.063484 0.427794 0.029 Uiso 1 1 calc R . . . .
C36 C 0.33141(14) 0.46878(12) 0.39039(10) 0.0211(3) Uani 1 1 d . . . . .
C37 C 0.30600(15) 0.43872(14) 0.47368(11) 0.0276(4) Uani 1 1 d . . . . .
H37 H 0.355152 0.389646 0.501657 0.033 Uiso 1 1 calc R . . . .
C38 C 0.20905(16) 0.48019(15) 0.51605(12) 0.0336(4) Uani 1 1 d . . . . .
H38 H 0.192759 0.460042 0.572973 0.040 Uiso 1 1 calc R . . . .
C39 C 0.13639(16) 0.55042(15) 0.47594(12) 0.0327(4) Uani 1 1 d . . . . .
H39 H 0.070083 0.578570 0.505042 0.039 Uiso 1 1 calc R . . . .
C40 C 0.16051(17) 0.57967(16) 0.39316(13) 0.0390(5) Uani 1 1 d . . . . .
H40 H 0.110429 0.627982 0.365421 0.047 Uiso 1 1 calc R . . . .
C41 C 0.25721(16) 0.53908(15) 0.35023(12) 0.0332(4) Uani 1 1 d . . . . .
H41 H 0.272815 0.559316 0.293281 0.040 Uiso 1 1 calc R . . . .
C42 C 0.55530(14) 0.51827(12) 0.30620(9) 0.0211(3) Uani 1 1 d . . . . .
C43 C 0.54075(16) 0.60526(13) 0.34289(11) 0.0288(4) Uani 1 1 d . . . . .
H43 H 0.475932 0.614222 0.381841 0.035 Uiso 1 1 calc R . . . .
C44 C 0.62116(17) 0.67883(15) 0.32242(13) 0.0367(5) Uani 1 1 d . . . . .
H44 H 0.611214 0.738095 0.347466 0.044 Uiso 1 1 calc R . . . .
C45 C 0.71587(17) 0.66609(16) 0.26560(12) 0.0364(5) Uani 1 1 d . . . . .
H45 H 0.770804 0.716459 0.251937 0.044 Uiso 1 1 calc R . . . .
C46 C 0.73044(16) 0.58014(16) 0.22878(12) 0.0343(4) Uani 1 1 d . . . . .
H46 H 0.795303 0.571514 0.189783 0.041 Uiso 1 1 calc R . . . .
C47 C 0.65028(15) 0.50648(14) 0.24881(11) 0.0278(4) Uani 1 1 d . . . . .
H47 H 0.660287 0.447691 0.223213 0.033 Uiso 1 1 calc R . . . .
C48 C 0.41920(15) 0.34040(14) 0.02995(10) 0.0258(4) Uani 1 1 d . . . . .
H48 H 0.470091 0.392434 0.027154 0.031 Uiso 1 1 calc R . . . .
C49 C 0.39189(15) 0.32120(14) -0.04131(10) 0.0291(4) Uani 1 1 d . . . . .
H49 H 0.423724 0.358915 -0.091856 0.035 Uiso 1 1 calc R . . . .
C50 C 0.31757(16) 0.24626(15) -0.03743(11) 0.0307(4) Uani 1 1 d . . . . .
H50 H 0.296144 0.232172 -0.085252 0.037 Uiso 1 1 calc R . . . .
C51 C 0.27465(16) 0.19186(14) 0.03726(10) 0.0283(4) Uani 1 1 d . . . . .
H51 H 0.224087 0.139156 0.041424 0.034 Uiso 1 1 calc R . . . .
C52 C 0.30618(14) 0.21509(13) 0.10558(10) 0.0243(4) Uani 1 1 d . . . . .
H52 H 0.276410 0.177254 0.156626 0.029 Uiso 1 1 calc R . . . .
C53 C 0.0909(7) 0.6238(6) 0.0255(5) 0.0552(15) Uani 0.535(11) 1 d D U P B 1
C54 C 0.0127(9) 0.7046(7) 0.0111(5) 0.0515(15) Uani 0.535(11) 1 d D U P B 1
H54 H -0.016596 0.719025 -0.038543 0.062 Uiso 0.535(11) 1 calc R . P B 1
C55 C -0.0239(11) 0.7664(8) 0.0708(6) 0.0597(18) Uani 0.535(11) 1 d D U P B 1
H55 H -0.081340 0.819903 0.061878 0.072 Uiso 0.535(11) 1 calc R . P B 1
C56 C 0.0197(7) 0.7519(7) 0.1386(5) 0.0594(16) Uani 0.535(11) 1 d D U P B 1
H56 H -0.003010 0.797502 0.176078 0.071 Uiso 0.535(11) 1 calc R . P B 1
C57 C 0.0978(7) 0.6710(8) 0.1551(5) 0.0675(18) Uani 0.535(11) 1 d D U P B 1
H57 H 0.127602 0.658148 0.204530 0.081 Uiso 0.535(11) 1 calc R . P B 1
C58 C 0.1327(7) 0.6073(6) 0.0961(6) 0.0677(17) Uani 0.535(11) 1 d D U P B 1
H58 H 0.187036 0.551384 0.106522 0.081 Uiso 0.535(11) 1 calc R . P B 1
C59 C 0.1355(6) 0.5543(5) -0.0387(5) 0.067(2) Uani 0.535(11) 1 d D U P B 1
H59A H 0.096704 0.576462 -0.085858 0.100 Uiso 0.535(11) 1 calc R . P B 1
H59B H 0.217213 0.560470 -0.055171 0.100 Uiso 0.535(11) 1 calc R . P B 1
H59C H 0.120773 0.482254 -0.015505 0.100 Uiso 0.535(11) 1 calc R . P B 1
C53A C 0.0938(9) 0.6207(8) 0.0551(7) 0.0640(17) Uani 0.465(11) 1 d D U P B 2
C54A C 0.0185(12) 0.6927(9) 0.0251(7) 0.0606(19) Uani 0.465(11) 1 d D U P B 2
H54A H -0.007418 0.683870 -0.022687 0.073 Uiso 0.465(11) 1 calc R . P B 2
C55A C -0.0244(13) 0.7787(10) 0.0578(7) 0.0562(18) Uani 0.465(11) 1 d D U P B 2
H55A H -0.069395 0.830961 0.028973 0.067 Uiso 0.465(11) 1 calc R . P B 2
C56A C -0.0024(9) 0.7880(8) 0.1300(6) 0.0565(17) Uani 0.465(11) 1 d D U P B 2
H56A H -0.033611 0.844265 0.155652 0.068 Uiso 0.465(11) 1 calc R . P B 2
C57A C 0.0686(9) 0.7105(8) 0.1654(6) 0.0691(19) Uani 0.465(11) 1 d D U P B 2
H57A H 0.081476 0.713091 0.218441 0.083 Uiso 0.465(11) 1 calc R . P B 2
C58A C 0.1229(8) 0.6289(8) 0.1295(7) 0.0653(19) Uani 0.465(11) 1 d D U P B 2
H58A H 0.176644 0.581571 0.154294 0.078 Uiso 0.465(11) 1 calc R . P B 2
C59A C 0.1503(8) 0.5364(7) 0.0107(9) 0.096(3) Uani 0.465(11) 1 d D U P B 2
H59D H 0.201995 0.492480 0.043463 0.145 Uiso 0.465(11) 1 calc R . P B 2
H59E H 0.092513 0.494626 0.000682 0.145 Uiso 0.465(11) 1 calc R . P B 2
H59F H 0.193144 0.567556 -0.040868 0.145 Uiso 0.465(11) 1 calc R . 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 Cl1 2.3785(5) . ?
Ti1 P1 2.5605(5) . ?
Ti1 O1 1.9290(12) . ?
Ti1 O2 1.8966(11) . ?
Ti1 N1 2.2586(14) . ?
Ti1 C1 2.4226(16) . ?
Ti1 C15 2.2454(15) . ?
P1 C31 1.8036(16) . ?
P1 C36 1.8180(17) . ?
P1 C42 1.8262(16) . ?
O1 C1 1.3576(19) . ?
O2 C16 1.3565(18) . ?
N1 C48 1.347(2) . ?
N1 C52 1.340(2) . ?
C1 C2 1.420(2) . ?
C1 C6 1.419(2) . ?
C2 C3 1.384(2) . ?
C2 C7 1.536(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.411(2) . ?
C4 C5 1.382(2) . ?
C4 C11 1.536(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.402(2) . ?
C6 C15 1.493(2) . ?
C7 C8 1.538(3) . ?
C7 C9 1.528(3) . ?
C7 C10 1.534(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.528(2) . ?
C11 C13 1.539(3) . ?
C11 C14 1.535(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C21 1.490(2) . ?
C15 C30 1.501(2) . ?
C16 C17 1.406(2) . ?
C16 C21 1.401(2) . ?
C17 C18 1.404(2) . ?
C17 C22 1.529(2) . ?
C18 H18 0.9500 . ?
C18 C19 1.394(3) . ?
C19 C20 1.394(2) . ?
C19 C26 1.539(2) . ?
C20 H20 0.9500 . ?
C20 C21 1.391(2) . ?
C22 C23 1.538(3) . ?
C22 C24 1.535(3) . ?
C22 C25 1.533(2) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.470(4) . ?
C26 C28 1.585(3) . ?
C26 C29 1.503(4) . ?
C26 C28A 1.485(5) . ?
C26 C29A 1.658(5) . ?
C26 C27A 1.504(5) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C28A H28D 0.9800 . ?
C28A H28E 0.9800 . ?
C28A H28F 0.9800 . ?
C29A H29D 0.9800 . ?
C29A H29E 0.9800 . ?
C29A H29F 0.9800 . ?
C27A H27D 0.9800 . ?
C27A H27E 0.9800 . ?
C27A H27F 0.9800 . ?
C30 C31 1.400(2) . ?
C30 C35 1.399(2) . ?
C31 C32 1.392(2) . ?
C32 H32 0.9500 . ?
C32 C33 1.382(2) . ?
C33 H33 0.9500 . ?
C33 C34 1.388(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.390(2) . ?
C35 H35 0.9500 . ?
C36 C37 1.392(2) . ?
C36 C41 1.391(2) . ?
C37 H37 0.9500 . ?
C37 C38 1.389(3) . ?
C38 H38 0.9500 . ?
C38 C39 1.378(3) . ?
C39 H39 0.9500 . ?
C39 C40 1.382(3) . ?
C40 H40 0.9500 . ?
C40 C41 1.387(3) . ?
C41 H41 0.9500 . ?
C42 C43 1.394(2) . ?
C42 C47 1.392(2) . ?
C43 H43 0.9500 . ?
C43 C44 1.389(3) . ?
C44 H44 0.9500 . ?
C44 C45 1.386(3) . ?
C45 H45 0.9500 . ?
C45 C46 1.383(3) . ?
C46 H46 0.9500 . ?
C46 C47 1.388(3) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C48 C49 1.384(2) . ?
C49 H49 0.9500 . ?
C49 C50 1.377(3) . ?
C50 H50 0.9500 . ?
C50 C51 1.383(2) . ?
C51 H51 0.9500 . ?
C51 C52 1.378(2) . ?
C52 H52 0.9500 . ?
C53 C54 1.369(8) . ?
C53 C58 1.355(7) . ?
C53 C59 1.558(8) . ?
C54 H54 0.9500 . ?
C54 C55 1.414(9) . ?
C55 H55 0.9500 . ?
C55 C56 1.323(9) . ?
C56 H56 0.9500 . ?
C56 C57 1.375(8) . ?
C57 H57 0.9500 . ?
C57 C58 1.419(8) . ?
C58 H58 0.9500 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C53A C54A 1.341(10) . ?
C53A C58A 1.396(9) . ?
C53A C59A 1.511(10) . ?
C54A H54A 0.9500 . ?
C54A C55A 1.380(10) . ?
C55A H55A 0.9500 . ?
C55A C56A 1.332(9) . ?
C56A H56A 0.9500 . ?
C56A C57A 1.384(9) . ?
C57A H57A 0.9500 . ?
C57A C58A 1.398(9) . ?
C58A H58A 0.9500 . ?
C59A H59D 0.9800 . ?
C59A H59E 0.9800 . ?
C59A H59F 0.9800 . ?

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
Cl1 Ti1 P1 80.337(16) . . ?
Cl1 Ti1 C1 137.02(4) . . ?
O1 Ti1 Cl1 108.12(4) . . ?
O1 Ti1 P1 89.05(4) . . ?
O1 Ti1 N1 93.32(5) . . ?
O1 Ti1 C1 34.02(5) . . ?
O1 Ti1 C15 79.50(5) . . ?
O2 Ti1 Cl1 101.43(4) . . ?
O2 Ti1 P1 99.59(4) . . ?
O2 Ti1 O1 150.22(5) . . ?
O2 Ti1 N1 85.56(5) . . ?
O2 Ti1 C1 117.24(5) . . ?
O2 Ti1 C15 76.97(5) . . ?
N1 Ti1 Cl1 84.97(4) . . ?
N1 Ti1 P1 165.12(4) . . ?
N1 Ti1 C1 80.31(5) . . ?
C1 Ti1 P1 109.06(4) . . ?
C15 Ti1 Cl1 149.17(4) . . ?
C15 Ti1 P1 69.79(4) . . ?
C15 Ti1 N1 125.09(5) . . ?
C15 Ti1 C1 63.67(5) . . ?
C31 P1 Ti1 104.80(5) . . ?
C31 P1 C36 107.16(7) . . ?
C31 P1 C42 104.11(7) . . ?
C36 P1 Ti1 113.96(5) . . ?
C36 P1 C42 105.33(8) . . ?
C42 P1 Ti1 120.40(5) . . ?
C1 O1 Ti1 93.34(9) . . ?
C16 O2 Ti1 124.71(10) . . ?
C48 N1 Ti1 123.60(11) . . ?
C52 N1 Ti1 118.81(11) . . ?
C52 N1 C48 117.46(14) . . ?
O1 C1 Ti1 52.64(7) . . ?
O1 C1 C2 123.80(14) . . ?
O1 C1 C6 115.64(14) . . ?
C2 C1 Ti1 142.77(12) . . ?
C6 C1 Ti1 74.06(9) . . ?
C6 C1 C2 120.40(14) . . ?
C1 C2 C7 120.67(14) . . ?
C3 C2 C1 116.44(15) . . ?
C3 C2 C7 122.87(15) . . ?
C2 C3 H3 117.9 . . ?
C2 C3 C4 124.24(15) . . ?
C4 C3 H3 117.9 . . ?
C3 C4 C11 121.83(15) . . ?
C5 C4 C3 117.58(15) . . ?
C5 C4 C11 120.59(15) . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 121.09(15) . . ?
C6 C5 H5 119.5 . . ?
C1 C6 C15 115.79(13) . . ?
C5 C6 C1 119.29(14) . . ?
C5 C6 C15 124.92(14) . . ?
C2 C7 C8 109.17(14) . . ?
C9 C7 C2 110.54(15) . . ?
C9 C7 C8 110.03(16) . . ?
C9 C7 C10 107.77(16) . . ?
C10 C7 C2 111.47(15) . . ?
C10 C7 C8 107.81(16) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C4 C11 C13 108.44(15) . . ?
C12 C11 C4 110.14(14) . . ?
C12 C11 C13 109.00(16) . . ?
C12 C11 C14 107.93(15) . . ?
C14 C11 C4 113.10(15) . . ?
C14 C11 C13 108.16(16) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C6 C15 Ti1 79.03(9) . . ?
C6 C15 C30 115.21(13) . . ?
C21 C15 Ti1 107.57(10) . . ?
C21 C15 C6 114.77(13) . . ?
C21 C15 C30 115.70(13) . . ?
C30 C15 Ti1 119.34(10) . . ?
O2 C16 C17 123.49(15) . . ?
O2 C16 C21 115.10(14) . . ?
C21 C16 C17 121.40(14) . . ?
C16 C17 C22 121.65(15) . . ?
C18 C17 C16 115.99(16) . . ?
C18 C17 C22 122.34(15) . . ?
C17 C18 H18 118.0 . . ?
C19 C18 C17 123.95(15) . . ?
C19 C18 H18 118.0 . . ?
C18 C19 C26 121.40(15) . . ?
C20 C19 C18 117.88(15) . . ?
C20 C19 C26 120.71(16) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 C19 120.56(16) . . ?
C21 C20 H20 119.7 . . ?
C16 C21 C15 114.07(13) . . ?
C20 C21 C15 125.94(15) . . ?
C20 C21 C16 119.99(15) . . ?
C17 C22 C23 109.97(15) . . ?
C17 C22 C24 109.38(15) . . ?
C17 C22 C25 112.71(15) . . ?
C24 C22 C23 109.86(17) . . ?
C25 C22 C23 107.32(16) . . ?
C25 C22 C24 107.54(16) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C19 C26 C28 111.01(18) . . ?
C19 C26 C29A 112.7(2) . . ?
C27 C26 C19 110.25(17) . . ?
C27 C26 C28 107.8(2) . . ?
C27 C26 C29 114.5(3) . . ?
C29 C26 C19 107.05(17) . . ?
C29 C26 C28 106.3(2) . . ?
C28A C26 C19 112.2(2) . . ?
C28A C26 C29A 103.4(3) . . ?
C28A C26 C27A 113.2(4) . . ?
C27A C26 C19 112.6(2) . . ?
C27A C26 C29A 101.9(3) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C26 C28A H28D 109.5 . . ?
C26 C28A H28E 109.5 . . ?
C26 C28A H28F 109.5 . . ?
H28D C28A H28E 109.5 . . ?
H28D C28A H28F 109.5 . . ?
H28E C28A H28F 109.5 . . ?
C26 C29A H29D 109.5 . . ?
C26 C29A H29E 109.5 . . ?
C26 C29A H29F 109.5 . . ?
H29D C29A H29E 109.5 . . ?
H29D C29A H29F 109.5 . . ?
H29E C29A H29F 109.5 . . ?
C26 C27A H27D 109.5 . . ?
C26 C27A H27E 109.5 . . ?
C26 C27A H27F 109.5 . . ?
H27D C27A H27E 109.5 . . ?
H27D C27A H27F 109.5 . . ?
H27E C27A H27F 109.5 . . ?
C31 C30 C15 117.06(14) . . ?
C35 C30 C15 124.15(14) . . ?
C35 C30 C31 118.75(15) . . ?
C30 C31 P1 111.14(12) . . ?
C32 C31 P1 127.61(13) . . ?
C32 C31 C30 121.11(15) . . ?
C31 C32 H32 120.2 . . ?
C33 C32 C31 119.52(16) . . ?
C33 C32 H32 120.2 . . ?
C32 C33 H33 120.0 . . ?
C32 C33 C34 120.00(16) . . ?
C34 C33 H33 120.0 . . ?
C33 C34 H34 119.6 . . ?
C33 C34 C35 120.89(16) . . ?
C35 C34 H34 119.6 . . ?
C30 C35 H35 120.1 . . ?
C34 C35 C30 119.71(15) . . ?
C34 C35 H35 120.1 . . ?
C37 C36 P1 122.63(13) . . ?
C41 C36 P1 118.28(13) . . ?
C41 C36 C37 119.06(16) . . ?
C36 C37 H37 119.9 . . ?
C38 C37 C36 120.26(17) . . ?
C38 C37 H37 119.9 . . ?
C37 C38 H38 119.8 . . ?
C39 C38 C37 120.35(18) . . ?
C39 C38 H38 119.8 . . ?
C38 C39 H39 120.2 . . ?
C38 C39 C40 119.64(17) . . ?
C40 C39 H39 120.2 . . ?
C39 C40 H40 119.7 . . ?
C39 C40 C41 120.55(18) . . ?
C41 C40 H40 119.7 . . ?
C36 C41 H41 119.9 . . ?
C40 C41 C36 120.13(18) . . ?
C40 C41 H41 119.9 . . ?
C43 C42 P1 122.90(13) . . ?
C47 C42 P1 117.66(13) . . ?
C47 C42 C43 119.43(16) . . ?
C42 C43 H43 120.0 . . ?
C44 C43 C42 119.91(18) . . ?
C44 C43 H43 120.0 . . ?
C43 C44 H44 119.9 . . ?
C45 C44 C43 120.25(18) . . ?
C45 C44 H44 119.9 . . ?
C44 C45 H45 120.0 . . ?
C46 C45 C44 120.05(17) . . ?
C46 C45 H45 120.0 . . ?
C45 C46 H46 120.0 . . ?
C45 C46 C47 119.98(18) . . ?
C47 C46 H46 120.0 . . ?
C42 C47 H47 119.8 . . ?
C46 C47 C42 120.37(17) . . ?
C46 C47 H47 119.8 . . ?
N1 C48 H48 118.5 . . ?
N1 C48 C49 123.06(16) . . ?
C49 C48 H48 118.5 . . ?
C48 C49 H49 120.7 . . ?
C50 C49 C48 118.61(16) . . ?
C50 C49 H49 120.7 . . ?
C49 C50 H50 120.6 . . ?
C49 C50 C51 118.88(16) . . ?
C51 C50 H50 120.6 . . ?
C50 C51 H51 120.4 . . ?
C52 C51 C50 119.15(17) . . ?
C52 C51 H51 120.4 . . ?
N1 C52 C51 122.82(15) . . ?
N1 C52 H52 118.6 . . ?
C51 C52 H52 118.6 . . ?
C54 C53 C59 121.4(6) . . ?
C58 C53 C54 118.6(6) . . ?
C58 C53 C59 119.9(6) . . ?
C53 C54 H54 120.4 . . ?
C53 C54 C55 119.3(6) . . ?
C55 C54 H54 120.4 . . ?
C54 C55 H55 119.1 . . ?
C56 C55 C54 121.9(7) . . ?
C56 C55 H55 119.1 . . ?
C55 C56 H56 119.9 . . ?
C55 C56 C57 120.1(7) . . ?
C57 C56 H56 119.9 . . ?
C56 C57 H57 121.0 . . ?
C56 C57 C58 118.1(6) . . ?
C58 C57 H57 121.0 . . ?
C53 C58 C57 122.0(6) . . ?
C53 C58 H58 119.0 . . ?
C57 C58 H58 119.0 . . ?
C53 C59 H59A 109.5 . . ?
C53 C59 H59B 109.5 . . ?
C53 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C54A C53A C58A 116.8(8) . . ?
C54A C53A C59A 123.0(8) . . ?
C58A C53A C59A 120.1(9) . . ?
C53A C54A H54A 117.3 . . ?
C53A C54A C55A 125.4(10) . . ?
C55A C54A H54A 117.3 . . ?
C54A C55A H55A 120.2 . . ?
C56A C55A C54A 119.7(9) . . ?
C56A C55A H55A 120.2 . . ?
C55A C56A H56A 122.1 . . ?
C55A C56A C57A 115.9(8) . . ?
C57A C56A H56A 122.1 . . ?
C56A C57A H57A 117.4 . . ?
C56A C57A C58A 125.3(9) . . ?
C58A C57A H57A 117.4 . . ?
C53A C58A C57A 116.3(8) . . ?
C53A C58A H58A 121.8 . . ?
C57A C58A H58A 121.8 . . ?
C53A C59A H59D 109.5 . . ?
C53A C59A H59E 109.5 . . ?
C53A C59A H59F 109.5 . . ?
H59D C59A H59E 109.5 . . ?
H59D C59A H59F 109.5 . . ?
H59E C59A H59F 109.5 . . ?

