# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_PTC-75
_database_code_depnum_ccdc_archive 'CCDC 1583618'
_audit_update_record             
;
2017-12-01 deposited with the CCDC.
2017-12-05 downloaded from the CCDC.
;
_audit_creation_date             2017-11-28
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C21 H39 N O12 P Ti3'
_chemical_formula_sum            'C21 H39 N O12 P Ti3'
_chemical_formula_weight         672.20
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   12.9697(7)
_cell_length_b                   14.2366(6)
_cell_length_c                   16.8559(8)
_cell_angle_alpha                90
_cell_angle_beta                 99.380(5)
_cell_angle_gamma                90
_cell_volume                     3070.7(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5271
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.2650
_cell_measurement_theta_min      3.5580
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         3.405
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3503
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -44.00  36.00   1.00    3.28    --   11.76 -38.00 -60.00   80
  2  ω    -22.00  81.00   1.00    3.28    --   11.76  19.00 150.00  103
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0391694000
_diffrn_orient_matrix_UB_12      -0.0149322000
_diffrn_orient_matrix_UB_13      0.0318976000
_diffrn_orient_matrix_UB_21      0.0123330000
_diffrn_orient_matrix_UB_22      -0.0381421000
_diffrn_orient_matrix_UB_23      -0.0238458000
_diffrn_orient_matrix_UB_31      0.0372912000
_diffrn_orient_matrix_UB_32      0.0282950000
_diffrn_orient_matrix_UB_33      -0.0152717000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5568
_reflns_number_total             6783
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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    ?
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         6783
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0389
_refine_ls_restrained_S_all      1.086
_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)+(0.0487P)²+1.8099P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1078
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Same fragment restrains
{O1, C1B, C2B, C3B} sigma for 1-2: 0.02, 1-3: 0.04
as
{O1, C1A, C2A, C3A}
3. Others
 Sof(C1B)=Sof(H1B)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(H2BC)=Sof(C3B)=Sof(H3BA)=
 Sof(H3BB)=Sof(H3BC)=1-FVAR(1)
 Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=Sof(H3AA)=
 Sof(H3AB)=Sof(H3AC)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C1A(H1A), C1B(H1B), C00J(H00J), C00L(H00L), C00M(H00M), C00W(H00W)
4.b Aromatic/amide H refined with riding coordinates:
 C00N(H00N), C00O(H00O), C1AA(H1AA), C00T(H00T)
4.c Idealised Me refined as rotating group:
 C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,H3AC), C2B(H2BA,H2BB,H2BC), C3B(H3BA,H3BB,
 H3BC), C00Q(H00A,H00B,H00C), C00R(H00D,H00E,H00F), C00S(H00G,H00H,H00I),
 C00U(H00K,H00P,H00Q), C00V(H00R,H00S,H00U), C00X(H00V,H00X,H00Y), C00Z(H00Z,H,
 HA), C011(H01A,H01B,H01C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
O1 O 0.70443(13) 0.21494(10) 0.54978(9) 0.0195(3) Uani 1 1 d D . . . .
C1A C 0.7858(3) 0.1569(3) 0.5896(2) 0.0268(9) Uani 0.725(6) 1 d D . P A 1
H1A H 0.8524 0.1792 0.5763 0.032 Uiso 0.725(6) 1 calc R . P A 1
C2A C 0.7907(3) 0.1626(3) 0.6787(2) 0.0401(12) Uani 0.725(6) 1 d D . P A 1
H2AA H 0.7963 0.2271 0.6953 0.060 Uiso 0.725(6) 1 calc GR . P A 1
H2AB H 0.8506 0.1285 0.7049 0.060 Uiso 0.725(6) 1 calc GR . P A 1
H2AC H 0.7284 0.1358 0.6931 0.060 Uiso 0.725(6) 1 calc GR . P A 1
C3A C 0.7683(5) 0.0585(3) 0.5595(4) 0.076(2) Uani 0.725(6) 1 d D . P A 1
H3AA H 0.7060 0.0339 0.5758 0.115 Uiso 0.725(6) 1 calc GR . P A 1
H3AB H 0.8270 0.0203 0.5814 0.115 Uiso 0.725(6) 1 calc GR . P A 1
H3AC H 0.7605 0.0582 0.5019 0.115 Uiso 0.725(6) 1 calc GR . P A 1
C1B C 0.7456(8) 0.1217(7) 0.5543(7) 0.031(3) Uani 0.275(6) 1 d D . P A 2
H1B H 0.6956 0.0807 0.5209 0.037 Uiso 0.275(6) 1 calc R . P A 2
C2B C 0.7572(13) 0.0889(12) 0.6385(8) 0.079(5) Uiso 0.275(6) 1 d D . P A 2
H2BA H 0.7925 0.1360 0.6735 0.119 Uiso 0.275(6) 1 calc GR . P A 2
H2BB H 0.7972 0.0319 0.6442 0.119 Uiso 0.275(6) 1 calc GR . P A 2
H2BC H 0.6894 0.0774 0.6523 0.119 Uiso 0.275(6) 1 calc GR . P A 2
C3B C 0.8458(7) 0.1193(7) 0.5228(5) 0.030(3) Uani 0.275(6) 1 d D . P A 2
H3BA H 0.8363 0.1471 0.4702 0.045 Uiso 0.275(6) 1 calc GR . P A 2
H3BB H 0.8681 0.0553 0.5195 0.045 Uiso 0.275(6) 1 calc GR . P A 2
H3BC H 0.8978 0.1538 0.5582 0.045 Uiso 0.275(6) 1 calc GR . P A 2
Ti01 Ti 0.38658(3) 0.36537(3) 0.48421(2) 0.01458(11) Uani 1 1 d . . . . .
Ti02 Ti 0.40361(3) 0.54169(3) 0.62341(2) 0.01485(11) Uani 1 1 d . . . . .
Ti03 Ti 0.61890(3) 0.30673(3) 0.51207(2) 0.01517(11) Uani 1 1 d . . . . .
O005 O 0.51889(12) 0.39952(10) 0.45650(9) 0.0157(3) Uani 1 1 d . . . . .
O006 O 0.35589(12) 0.43746(10) 0.56145(9) 0.0180(3) Uani 1 1 d . . . . .
O007 O 0.70364(12) 0.37481(10) 0.44378(9) 0.0164(3) Uani 1 1 d . . . . .
O008 O 0.53627(12) 0.48332(10) 0.67132(9) 0.0183(3) Uani 1 1 d . . . . .
O009 O 0.48766(12) 0.27442(10) 0.54856(9) 0.0188(3) Uani 1 1 d . . . . .
O00A O 0.66281(12) 0.38500(10) 0.60634(9) 0.0191(3) Uani 1 1 d . . . . .
O00B O 0.68049(12) 0.56150(11) 0.60963(9) 0.0191(3) Uani 1 1 d . . . . .
O00C O 0.55040(13) 0.33221(10) 0.31218(9) 0.0194(3) Uani 1 1 d . . . . .
O00D O 0.56741(13) 0.22433(11) 0.41171(9) 0.0202(3) Uani 1 1 d . . . . .
O00E O 0.33890(12) 0.51807(11) 0.70664(9) 0.0189(3) Uani 1 1 d . . . . .
O00G O 0.29081(13) 0.27331(11) 0.45851(10) 0.0253(4) Uani 1 1 d . . . . .
N00K N 0.4258(2) 0.02393(17) 0.25419(19) 0.0483(7) Uani 1 1 d . . . . .
P04 P 0.64642(5) 0.47459(4) 0.65154(3) 0.01559(13) Uani 1 1 d . . . . .
C00H C 0.54095(18) 0.24920(15) 0.33870(13) 0.0178(5) Uani 1 1 d . . . . .
C00I C 0.50450(18) 0.17524(16) 0.27982(14) 0.0211(5) Uani 1 1 d . . . . .
C00J C 0.81309(18) 0.35906(18) 0.44177(14) 0.0242(5) Uani 1 1 d . . . . .
H00J H 0.8432 0.3264 0.4913 0.029 Uiso 1 1 calc R . . . .
C00L C 0.3289(2) 0.53394(18) 0.78778(14) 0.0258(5) Uani 1 1 d . . . . .
H00L H 0.3193 0.6014 0.7956 0.031 Uiso 1 1 calc R . . . .
C00M C 0.4736(2) 0.20161(17) 0.60555(16) 0.0304(6) Uani 1 1 d . . . . .
H00M H 0.5416 0.1919 0.6395 0.036 Uiso 1 1 calc R . . . .
C00N C 0.46303(19) 0.09350(17) 0.30513(16) 0.0274(6) Uani 1 1 d . . . . .
H00N H 0.4607 0.0860 0.3596 0.033 Uiso 1 1 calc R . . . .
C00O C 0.5072(2) 0.18652(18) 0.19842(16) 0.0296(6) Uani 1 1 d . . . . .
H00O H 0.5335 0.2417 0.1800 0.036 Uiso 1 1 calc R . . . .
C1AA C 0.4717(2) 0.1178(2) 0.14567(17) 0.0390(7) Uani 1 1 d . . . . .
H1AA H 0.4747 0.1239 0.0912 0.047 Uiso 1 1 calc R . . . .
C00Q C 0.8684(2) 0.4518(2) 0.43963(18) 0.0365(7) Uani 1 1 d . . . . .
H00A H 0.8415 0.4842 0.3906 0.055 Uiso 1 1 calc GR . . . .
H00B H 0.9419 0.4412 0.4422 0.055 Uiso 1 1 calc GR . . . .
H00C H 0.8569 0.4894 0.4847 0.055 Uiso 1 1 calc GR . . . .
C00R C 0.4459(2) 0.11150(18) 0.56133(18) 0.0360(7) Uani 1 1 d . . . . .
H00D H 0.3805 0.1188 0.5258 0.054 Uiso 1 1 calc GR . . . .
H00E H 0.4398 0.0623 0.5992 0.054 Uiso 1 1 calc GR . . . .
H00F H 0.4996 0.0957 0.5306 0.054 Uiso 1 1 calc GR . . . .
C00S C 0.2323(2) 0.4825(2) 0.80461(18) 0.0419(8) Uani 1 1 d . . . . .
H00G H 0.1720 0.5054 0.7692 0.063 Uiso 1 1 calc GR . . . .
H00H H 0.2236 0.4931 0.8594 0.063 Uiso 1 1 calc GR . . . .
H00I H 0.2401 0.4164 0.7959 0.063 Uiso 1 1 calc GR . . . .
C00T C 0.4314(2) 0.0389(2) 0.1753(2) 0.0469(9) Uani 1 1 d . . . . .
H00T H 0.4060 -0.0079 0.1388 0.056 Uiso 1 1 calc R . . . .
C00U C 0.4273(2) 0.5027(3) 0.84165(17) 0.0460(8) Uani 1 1 d . . . . .
H00K H 0.4386 0.4370 0.8334 0.069 Uiso 1 1 calc GR . . . .
H00P H 0.4204 0.5132 0.8968 0.069 Uiso 1 1 calc GR . . . .
H00Q H 0.4857 0.5379 0.8291 0.069 Uiso 1 1 calc GR . . . .
C00V C 0.8237(2) 0.2957(3) 0.37138(19) 0.0486(8) Uani 1 1 d . . . . .
H00R H 0.7914 0.2363 0.3782 0.073 Uiso 1 1 calc GR . . . .
H00S H 0.8964 0.2863 0.3689 0.073 Uiso 1 1 calc GR . . . .
H00U H 0.7901 0.3245 0.3224 0.073 Uiso 1 1 calc GR . . . .
C00W C 0.1845(2) 0.2633(2) 0.4257(2) 0.0465(8) Uani 1 1 d . . . . .
H00W H 0.1570 0.3263 0.4116 0.056 Uiso 1 1 calc R . . . .
C00X C 0.4000(3) 0.2333(2) 0.65967(19) 0.0443(8) Uani 1 1 d . . . . .
H00V H 0.4234 0.2923 0.6838 0.066 Uiso 1 1 calc GR . . . .
H00X H 0.3980 0.1873 0.7010 0.066 Uiso 1 1 calc GR . . . .
H00Y H 0.3313 0.2407 0.6290 0.066 Uiso 1 1 calc GR . . . .
C00Z C 0.1261(3) 0.2252(4) 0.4874(3) 0.0855(15) Uani 1 1 d . . . . .
H00Z H 0.1582 0.1678 0.5087 0.128 Uiso 1 1 calc GR . . . .
H H 0.0551 0.2130 0.4633 0.128 Uiso 1 1 calc GR . . . .
HA H 0.1272 0.2700 0.5300 0.128 Uiso 1 1 calc GR . . . .
C011 C 0.1712(4) 0.2084(5) 0.3523(3) 0.112(2) Uani 1 1 d . . . . .
H01A H 0.2099 0.2369 0.3148 0.168 Uiso 1 1 calc GR . . . .
H01B H 0.0984 0.2062 0.3294 0.168 Uiso 1 1 calc GR . . . .
H01C H 0.1964 0.1457 0.3643 0.168 Uiso 1 1 calc GR . . . .


_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
O1 C1A 1.420(4) . ?
O1 C1B 1.428(9) . ?
O1 Ti03 1.7643(15) . ?
C1A C2A 1.495(5) . ?
C1A C3A 1.494(6) . ?
C1B C2B 1.478(14) . ?
C1B C3B 1.482(11) . ?
Ti01 Ti03 3.0878(6) . ?
Ti01 O005 1.9132(15) . ?
Ti01 O006 1.7537(15) . ?
Ti01 O009 2.0269(16) . ?
Ti01 O00B 1.9733(16) 3_666 ?
Ti01 O00G 1.8092(16) . ?
Ti02 Ti03 3.1208(5) 3_666 ?
Ti02 O005 1.9916(15) 3_666 ?
Ti02 O006 1.8614(16) . ?
Ti02 O007 2.0290(15) 3_666 ?
Ti02 O008 1.9621(16) . ?
Ti02 O00C 2.1324(16) 3_666 ?
Ti02 O00E 1.7803(15) . ?
Ti03 Ti02 3.1208(5) 3_666 ?
Ti03 O005 1.9770(15) . ?
Ti03 O007 1.9711(15) . ?
Ti03 O009 1.9565(16) . ?
Ti03 O00A 1.9483(16) . ?
Ti03 O00D 2.0774(16) . ?
O005 Ti02 1.9916(15) 3_666 ?
O007 Ti02 2.0290(15) 3_666 ?
O007 C00J 1.443(3) . ?
O008 P04 1.5242(17) . ?
O009 C00M 1.445(3) . ?
O00A P04 1.5183(16) . ?
O00B Ti01 1.9733(16) 3_666 ?
O00B P04 1.5255(16) . ?
O00C Ti02 2.1324(16) 3_666 ?
O00C C00H 1.276(3) . ?
O00D C00H 1.273(3) . ?
O00E C00L 1.413(3) . ?
O00G C00W 1.407(3) . ?
N00K C00N 1.348(4) . ?
N00K C00T 1.361(5) . ?
C00H C00I 1.471(3) . ?
C00I C00N 1.378(3) . ?
C00I C00O 1.387(3) . ?
C00J C00Q 1.506(4) . ?
C00J C00V 1.514(4) . ?
C00L C00S 1.518(4) . ?
C00L C00U 1.508(4) . ?
C00M C00R 1.498(4) . ?
C00M C00X 1.494(4) . ?
C00O C1AA 1.352(4) . ?
C1AA C00T 1.366(5) . ?
C00W C00Z 1.485(5) . ?
C00W C011 1.449(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
C1A O1 Ti03 167.6(2) . . ?
C1B O1 Ti03 156.3(5) . . ?
O1 C1A C2A 110.5(3) . . ?
O1 C1A C3A 108.9(4) . . ?
C2A C1A C3A 111.8(4) . . ?
O1 C1B C2B 108.9(10) . . ?
O1 C1B C3B 110.2(7) . . ?
C3B C1B C2B 112.3(10) . . ?
O005 Ti01 Ti03 38.19(4) . . ?
O005 Ti01 O009 76.43(6) . . ?
O005 Ti01 O00B 88.05(6) . 3_666 ?
O006 Ti01 Ti03 112.29(6) . . ?
O006 Ti01 O005 110.72(7) . . ?
O006 Ti01 O009 100.48(7) . . ?
O006 Ti01 O00B 99.36(7) . 3_666 ?
O006 Ti01 O00G 111.82(8) . . ?
O009 Ti01 Ti03 38.36(4) . . ?
O00B Ti01 Ti03 123.80(5) 3_666 . ?
O00B Ti01 O009 158.15(7) 3_666 . ?
O00G Ti01 Ti03 117.09(6) . . ?
O00G Ti01 O005 137.20(7) . . ?
O00G Ti01 O009 91.39(7) . . ?
O00G Ti01 O00B 89.69(7) . 3_666 ?
O005 Ti02 Ti03 37.99(4) 3_666 3_666 ?
O005 Ti02 O007 75.64(6) 3_666 3_666 ?
O005 Ti02 O00C 81.98(6) 3_666 3_666 ?
O006 Ti02 Ti03 99.08(5) . 3_666 ?
O006 Ti02 O005 96.54(6) . 3_666 ?
O006 Ti02 O007 91.08(7) . 3_666 ?
O006 Ti02 O008 94.73(7) . . ?
O006 Ti02 O00C 175.35(7) . 3_666 ?
O007 Ti02 Ti03 38.06(4) 3_666 3_666 ?
O007 Ti02 O00C 84.28(6) 3_666 3_666 ?
O008 Ti02 Ti03 124.42(5) . 3_666 ?
O008 Ti02 O005 87.19(6) . 3_666 ?
O008 Ti02 O007 162.41(6) . 3_666 ?
O008 Ti02 O00C 89.61(6) . 3_666 ?
O00C Ti02 Ti03 77.02(4) 3_666 3_666 ?
O00E Ti02 Ti03 135.02(5) . 3_666 ?
O00E Ti02 O005 165.24(7) . 3_666 ?
O00E Ti02 O006 97.77(7) . . ?
O00E Ti02 O007 100.49(7) . 3_666 ?
O00E Ti02 O008 95.17(7) . . ?
O00E Ti02 O00C 83.47(7) . 3_666 ?
O1 Ti03 Ti01 142.72(6) . . ?
O1 Ti03 Ti02 138.95(5) . 3_666 ?
O1 Ti03 O005 172.33(7) . . ?
O1 Ti03 O007 101.36(7) . . ?
O1 Ti03 O009 103.93(7) . . ?
O1 Ti03 O00A 92.68(7) . . ?
O1 Ti03 O00D 88.56(7) . . ?
Ti01 Ti03 Ti02 74.288(14) . 3_666 ?
O005 Ti03 Ti01 36.75(4) . . ?
O005 Ti03 Ti02 38.32(4) . 3_666 ?
O005 Ti03 O00D 83.83(6) . . ?
O007 Ti03 Ti01 113.67(5) . . ?
O007 Ti03 Ti02 39.39(4) . 3_666 ?
O007 Ti03 O005 77.29(6) . . ?
O007 Ti03 O00D 86.44(6) . . ?
O009 Ti03 Ti01 40.01(4) . . ?
O009 Ti03 Ti02 114.22(5) . 3_666 ?
O009 Ti03 O005 76.64(6) . . ?
O009 Ti03 O007 153.59(7) . . ?
O009 Ti03 O00D 86.71(7) . . ?
O00A Ti03 Ti01 96.76(5) . . ?
O00A Ti03 Ti02 100.45(5) . 3_666 ?
O00A Ti03 O005 94.95(6) . . ?
O00A Ti03 O007 94.49(6) . . ?
O00A Ti03 O009 91.82(7) . . ?
O00A Ti03 O00D 178.27(7) . . ?
O00D Ti03 Ti01 81.53(5) . . ?
O00D Ti03 Ti02 79.36(4) . 3_666 ?
Ti01 O005 Ti02 147.51(9) . 3_666 ?
Ti01 O005 Ti03 105.06(7) . . ?
Ti03 O005 Ti02 103.70(7) . 3_666 ?
Ti01 O006 Ti02 142.00(9) . . ?
Ti03 O007 Ti02 102.55(7) . 3_666 ?
C00J O007 Ti02 131.72(14) . 3_666 ?
C00J O007 Ti03 125.56(13) . . ?
P04 O008 Ti02 137.29(10) . . ?
Ti03 O009 Ti01 101.63(7) . . ?
C00M O009 Ti01 132.33(15) . . ?
C00M O009 Ti03 126.03(15) . . ?
P04 O00A Ti03 147.52(10) . . ?
P04 O00B Ti01 132.54(10) . 3_666 ?
C00H O00C Ti02 129.49(14) . 3_666 ?
C00H O00D Ti03 129.08(14) . . ?
C00L O00E Ti02 149.55(16) . . ?
C00W O00G Ti01 139.32(17) . . ?
C00N N00K C00T 115.9(3) . . ?
O008 P04 O00B 112.81(9) . . ?
O00A P04 O008 113.03(9) . . ?
O00A P04 O00B 111.97(9) . . ?
O00C C00H C00I 117.71(19) . . ?
O00D C00H O00C 124.8(2) . . ?
O00D C00H C00I 117.35(19) . . ?
C00N C00I C00H 119.6(2) . . ?
C00N C00I C00O 118.5(2) . . ?
C00O C00I C00H 121.8(2) . . ?
O007 C00J C00Q 109.8(2) . . ?
O007 C00J C00V 109.1(2) . . ?
C00Q C00J C00V 113.5(2) . . ?
O00E C00L C00S 108.2(2) . . ?
O00E C00L C00U 109.5(2) . . ?
C00U C00L C00S 112.9(2) . . ?
O009 C00M C00R 109.2(2) . . ?
O009 C00M C00X 110.6(2) . . ?
C00X C00M C00R 115.9(2) . . ?
N00K C00N C00I 122.7(3) . . ?
C1AA C00O C00I 120.4(3) . . ?
C00O C1AA C00T 117.6(3) . . ?
N00K C00T C1AA 124.8(3) . . ?
O00G C00W C00Z 110.0(3) . . ?
O00G C00W C011 111.3(3) . . ?
C011 C00W C00Z 113.4(4) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.318
_oxdiff_exptl_absorpt_empirical_full_min 0.775
####################################################################### 
# 
# 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_PTC-78
_database_code_depnum_ccdc_archive 'CCDC 1583621'
_audit_update_record             
;
2017-12-01 deposited with the CCDC.
2017-12-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H53 O14 P S Ti3'
_chemical_formula_weight         808.42

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           163
_space_group_name_H-M_alt        'P -3 1 c'
_space_group_name_Hall           '-P 3 2c'

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

_cell_length_a                   18.9359(5)
_cell_length_b                   18.9359(5)
_cell_length_c                   49.4964(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     15370.1(9)
_cell_formula_units_Z            12
_cell_measurement_temperature    100.02(16)
_cell_measurement_reflns_used    6975
_cell_measurement_theta_min      4.4850
_cell_measurement_theta_max      52.3910

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.048
_exptl_crystal_F_000             5088
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    4.940
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.45915
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100.02(16)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22333
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_theta_min         3.572
_diffrn_reflns_theta_max         53.387
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.648
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.648
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.648
_reflns_number_total             6029
_reflns_number_gt                4222
_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.
 
 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.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014 (Sheldrick, 2014)'
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1773P)²+30.5774P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6029
_refine_ls_number_parameters     464
_refine_ls_number_restraints     192
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0968
_refine_ls_wR_factor_ref         0.3004
_refine_ls_wR_factor_gt          0.2842
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001

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
C1 C 0.1619(5) 0.4721(6) 0.68506(16) 0.074(2) Uani 1 1 d D U . . .
C4 C 0.2268(6) 0.4837(6) 0.73648(17) 0.080(3) Uani 1 1 d D U . . .
C2A C 0.2425(9) 0.5013(8) 0.6891(3) 0.099(5) Uani 0.656(9) 1 d D U P A 1
H2A H 0.2774 0.5170 0.6744 0.119 Uiso 0.656(9) 1 calc R U P A 1
C3A C 0.2739(9) 0.5083(9) 0.7146(3) 0.096(5) Uani 0.656(9) 1 d D U P A 1
H3A H 0.3299 0.5309 0.7167 0.115 Uiso 0.656(9) 1 calc R U P A 1
C5A C 0.1460(10) 0.4590(10) 0.7325(3) 0.111(5) Uani 0.656(9) 1 d D U P A 1
H5A H 0.1118 0.4464 0.7473 0.133 Uiso 0.656(9) 1 calc R U P A 1
C6A C 0.1144(10) 0.4523(10) 0.7068(3) 0.111(5) Uani 0.656(9) 1 d D U P A 1
H6A H 0.0590 0.4336 0.7048 0.133 Uiso 0.656(9) 1 calc R U P A 1
C2B C 0.1785(12) 0.4141(13) 0.6945(4) 0.095(6) Uani 0.344(9) 1 d D U P A 2
H2B H 0.1678 0.3698 0.6836 0.114 Uiso 0.344(9) 1 calc R U P A 2
C3B C 0.2111(12) 0.4206(13) 0.7202(4) 0.094(6) Uani 0.344(9) 1 d D U P A 2
H3B H 0.2223 0.3806 0.7262 0.113 Uiso 0.344(9) 1 calc R U P A 2
C5B C 0.2114(13) 0.5396(13) 0.7270(4) 0.092(6) Uani 0.344(9) 1 d D U P A 2
H5B H 0.2230 0.5844 0.7377 0.111 Uiso 0.344(9) 1 calc R U P A 2
C6B C 0.1787(13) 0.5337(12) 0.7017(3) 0.094(6) Uani 0.344(9) 1 d D U P A 2
H6B H 0.1680 0.5742 0.6961 0.113 Uiso 0.344(9) 1 calc R U P A 2
Ti1 Ti 0.16224(10) 0.47400(10) 0.58839(3) 0.0648(6) Uani 1 1 d . . . . .
Ti2 Ti -0.00564(11) 0.33344(11) 0.60597(4) 0.0844(7) Uani 1 1 d . . . . .
S3 S 0.11798(14) 0.45715(15) 0.65254(4) 0.0685(7) Uani 1 1 d . . . . .
Ti4 Ti -0.00312(10) 0.50064(11) 0.61757(3) 0.0735(6) Uani 1 1 d . . . . .
P5 P 0.18353(14) 0.64792(14) 0.60486(4) 0.0634(7) Uani 1 1 d . . . . .
O1 O 0.2044(3) 0.5912(4) 0.58978(10) 0.0677(15) Uani 1 1 d . . . . .
O2 O 0.0622(4) 0.3687(4) 0.64804(11) 0.0831(19) Uani 1 1 d . . . . .
O3 O 0.2714(3) 0.4870(3) 0.58990(10) 0.0640(15) Uani 1 1 d . . . . .
O4 O 0.0928(3) 0.6094(4) 0.61025(11) 0.0687(15) Uani 1 1 d . . . . .
O5 O -0.0450(4) 0.5344(4) 0.64356(12) 0.0816(18) Uani 1 1 d . . . . .
O6 O -0.0687(4) 0.3794(4) 0.62377(12) 0.0812(19) Uani 1 1 d . . . . .
O7 O 0.1540(4) 0.4712(4) 0.55295(10) 0.0815(19) Uani 1 1 d . . . . .
O8 O 0.1044(4) 0.3545(4) 0.59458(11) 0.0784(18) Uani 1 1 d . . . . .
O9 O -0.0596(4) 0.5061(4) 0.59001(12) 0.091(2) Uani 1 1 d . . . . .
C4BA C -0.1430(7) 0.3310(8) 0.6390(2) 0.104(4) Uani 1 1 d . . . . .
H4BA H -0.1624 0.2741 0.6340 0.125 Uiso 1 1 calc R U . . .
O11 O 0.0588(3) 0.4531(3) 0.59948(10) 0.0696(17) Uani 1 1 d . . . . .
O12 O -0.0473(4) 0.2356(4) 0.62074(16) 0.110(2) Uani 1 1 d . . . . .
O13 O -0.0578(4) 0.3055(5) 0.57440(15) 0.108(2) Uani 1 1 d . . . . .
C18 C -0.0348(7) 0.5673(9) 0.6698(2) 0.097(3) Uani 1 1 d . . . . .
H18 H -0.0187 0.5369 0.6820 0.116 Uiso 1 1 calc R U . . .
C19 C -0.0633(8) 0.3536(9) 0.5520(2) 0.110(4) Uani 1 1 d . . . . .
H19 H -0.0263 0.4118 0.5553 0.132 Uiso 1 1 calc R U . . .
O1AA O 0.1858(3) 0.4897(3) 0.63374(10) 0.0610(14) Uani 1 1 d . . . . .
O0AA O 0.0769(3) 0.5051(4) 0.65327(10) 0.0692(16) Uani 1 1 d . . . . .
C0AA C -0.2095(8) 0.3490(8) 0.6302(3) 0.119(4) Uani 1 1 d . . . . .
H0AA H -0.1944 0.4037 0.6353 0.179 Uiso 1 1 calc R U . . .
H0AB H -0.2599 0.3113 0.6389 0.179 Uiso 1 1 calc R U . . .
H0AC H -0.2162 0.3432 0.6110 0.179 Uiso 1 1 calc R U . . .
C9AA C 0.1926(9) 0.5291(9) 0.5309(2) 0.124(5) Uani 1 1 d . . . . .
H9AA H 0.2474 0.5712 0.5365 0.149 Uiso 1 1 calc R U . . .
C2BA C 0.1591(9) 0.3002(9) 0.5619(3) 0.137(5) Uani 1 1 d . . . . .
H2BA H 0.1284 0.3132 0.5494 0.206 Uiso 1 1 calc R U . . .
H2BB H 0.1558 0.2499 0.5566 0.206 Uiso 1 1 calc R U . . .
H2BC H 0.2150 0.3430 0.5618 0.206 Uiso 1 1 calc R U . . .
C0BA C 0.1248(7) 0.2915(7) 0.5895(3) 0.101(4) Uani 1 1 d . . . . .
H0BA H 0.0743 0.2387 0.5906 0.121 Uiso 1 1 calc R U . . .
C1BA C -0.0822(11) 0.5590(12) 0.5780(3) 0.160(7) Uani 1 1 d D . . . .
C4AA C -0.1277(8) 0.3362(9) 0.6688(3) 0.130(5) Uani 1 1 d . . . . .
H4AA H -0.0822 0.3285 0.6725 0.195 Uiso 1 1 calc R U . . .
H4AB H -0.1753 0.2946 0.6779 0.195 Uiso 1 1 calc R U . . .
H4AC H -0.1158 0.3888 0.6753 0.195 Uiso 1 1 calc R U . . .
C2AA C 0.0287(8) 0.6541(9) 0.6705(3) 0.127(4) Uani 1 1 d . . . . .
H2AA H 0.0795 0.6599 0.6645 0.190 Uiso 1 1 calc R U . . .
H2AB H 0.0347 0.6743 0.6886 0.190 Uiso 1 1 calc R U . . .
H2AC H 0.0132 0.6846 0.6588 0.190 Uiso 1 1 calc R U . . .
C5BA C -0.1530(9) 0.3358(11) 0.5515(3) 0.159(6) Uani 1 1 d . . . . .
H5BA H -0.1890 0.2792 0.5475 0.238 Uiso 1 1 calc R U . . .
H5BB H -0.1587 0.3689 0.5380 0.238 Uiso 1 1 calc R U . . .
H5BC H -0.1667 0.3482 0.5689 0.238 Uiso 1 1 calc R U . . .
C3BA C -0.0357(10) 0.5933(9) 0.5535(2) 0.134(5) Uani 1 1 d . . . . .
H3BA H 0.0149 0.6415 0.5579 0.201 Uiso 1 1 calc R U . . .
H3BB H -0.0663 0.6071 0.5413 0.201 Uiso 1 1 calc R U . . .
H3BC H -0.0247 0.5540 0.5452 0.201 Uiso 1 1 calc R U . . .
C1AA C -0.1163(8) 0.5564(10) 0.6793(3) 0.132(5) Uani 1 1 d . . . . .
H1AA H -0.1388 0.5746 0.6654 0.198 Uiso 1 1 calc R U . . .
H1AB H -0.1081 0.5878 0.6954 0.198 Uiso 1 1 calc R U . . .
H1AC H -0.1531 0.4998 0.6830 0.198 Uiso 1 1 calc R U . . .
C11 C -0.0371(11) 0.3271(10) 0.5257(3) 0.169(7) Uani 1 1 d . . . . .
H11A H 0.0195 0.3430 0.5268 0.254 Uiso 1 1 calc R U . . .
H11B H -0.0456 0.3530 0.5103 0.254 Uiso 1 1 calc R U . . .
H11C H -0.0692 0.2690 0.5237 0.254 Uiso 1 1 calc R U . . .
C12 C 0.1431(10) 0.5686(10) 0.5242(3) 0.138(5) Uani 1 1 d . . . . .
H12A H 0.0898 0.5277 0.5184 0.206 Uiso 1 1 calc R U . . .
H12B H 0.1695 0.6077 0.5100 0.206 Uiso 1 1 calc R U . . .
H12C H 0.1384 0.5956 0.5399 0.206 Uiso 1 1 calc R U . . .
C13 C 0.1799(9) 0.2938(8) 0.6110(3) 0.125(4) Uani 1 1 d . . . . .
H13A H 0.2281 0.3466 0.6113 0.187 Uiso 1 1 calc R U . . .
H13B H 0.1946 0.2530 0.6075 0.187 Uiso 1 1 calc R U . . .
H13C H 0.1528 0.2834 0.6281 0.187 Uiso 1 1 calc R U . . .
C3AA C 0.1996(11) 0.4788(12) 0.5083(2) 0.167(7) Uani 1 1 d . . . . .
H3AA H 0.1474 0.4312 0.5053 0.251 Uiso 1 1 calc R U . . .
H3AB H 0.2384 0.4626 0.5133 0.251 Uiso 1 1 calc R U . . .
H3AC H 0.2174 0.5109 0.4921 0.251 Uiso 1 1 calc R U . . .
C5AA C -0.0553(12) 0.1765(10) 0.6411(4) 0.162(5) Uani 1 1 d D U . . .
H5AA H -0.0335 0.2015 0.6587 0.195 Uiso 1 1 calc R U . . .
C7AA C -0.1456(11) 0.1164(13) 0.6418(4) 0.209(7) Uani 1 1 d D U . . .
H7AA H -0.1732 0.1337 0.6296 0.313 Uiso 1 1 calc R U . . .
H7AB H -0.1657 0.1139 0.6598 0.313 Uiso 1 1 calc R U . . .
H7AC H -0.1552 0.0635 0.6366 0.313 Uiso 1 1 calc R U . . .
C6AA C -0.0159(13) 0.1292(13) 0.6303(5) 0.217(7) Uani 1 1 d D U . . .
C8AA C -0.1396(19) 0.570(2) 0.5903(5) 0.36(2) Uani 1 1 d D . . . .
H8AA H -0.1632 0.5432 0.6064 0.430 Uiso 1 1 calc R U . . .
H8AB H -0.1555 0.6051 0.5827 0.430 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6B 1.331(14) . ?
C1 C6A 1.333(14) . ?
C1 C2A 1.355(15) . ?
C1 C2B 1.367(19) . ?
C1 S3 1.768(8) . ?
C4 C5B 1.317(19) . ?
C4 C3A 1.329(16) . ?
C4 C3B 1.35(2) . ?
C4 C5A 1.372(16) . ?
C4 C4 1.455(17) 5_556 ?
C2A C3A 1.372(17) . ?
C5A C6A 1.380(18) . ?
C2B C3B 1.39(2) . ?
C5B C6B 1.37(2) . ?
Ti1 O7 1.759(5) . ?
Ti1 O11 1.876(6) . ?
Ti1 O1 1.949(6) . ?
Ti1 O3 1.956(6) . ?
Ti1 O8 1.985(6) . ?
Ti1 O1AA 2.279(5) . ?
Ti1 Ti2 3.080(2) . ?
Ti2 O12 1.768(7) . ?
Ti2 O13 1.782(7) . ?
Ti2 O11 1.991(6) . ?
Ti2 O8 1.998(7) . ?
Ti2 O6 2.000(7) . ?
Ti2 O2 2.361(6) . ?
Ti2 Ti4 3.194(3) . ?
S3 O1AA 1.451(6) . ?
S3 O0AA 1.462(6) . ?
S3 O2 1.484(7) . ?
Ti4 O9 1.768(6) . ?
Ti4 O5 1.789(7) . ?
Ti4 O4 1.982(6) . ?
Ti4 O11 2.010(6) . ?
Ti4 O6 2.014(6) . ?
Ti4 O0AA 2.301(5) . ?
P5 O1 1.513(6) . ?
P5 O4 1.518(6) . ?
P5 O3 1.525(6) 3_565 ?
O3 P5 1.525(6) 2_665 ?
O5 C18 1.412(12) . ?
O6 C4BA 1.449(12) . ?
O7 C9AA 1.456(13) . ?
O8 C0BA 1.446(13) . ?
O9 C1BA 1.403(13) . ?
C4BA C4AA 1.498(16) . ?
C4BA C0AA 1.524(15) . ?
O12 C5AA 1.456(16) . ?
O13 C19 1.473(13) . ?
C18 C2AA 1.473(17) . ?
C18 C1AA 1.524(15) . ?
C19 C5BA 1.557(17) . ?
C19 C11 1.563(19) . ?
C9AA C12 1.499(18) . ?
C9AA C3AA 1.517(18) . ?
C2BA C0BA 1.490(18) . ?
C0BA C13 1.472(15) . ?
C1BA C8AA 1.352(15) . ?
C1BA C3BA 1.448(18) . ?
C5AA C7AA 1.51(2) . ?
C5AA C6AA 1.522(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
C6A C1 C2A 117.3(10) . . ?
C6B C1 C2B 116.2(13) . . ?
C6B C1 S3 126.4(10) . . ?
C6A C1 S3 119.6(8) . . ?
C2A C1 S3 123.0(8) . . ?
C2B C1 S3 117.4(10) . . ?
C5B C4 C3B 117.4(13) . . ?
C3A C4 C5A 116.0(10) . . ?
C5B C4 C4 124.9(11) . 5_556 ?
C3A C4 C4 123.7(11) . 5_556 ?
C3B C4 C4 117.6(10) . 5_556 ?
C5A C4 C4 120.3(11) . 5_556 ?
C1 C2A C3A 121.5(13) . . ?
C4 C3A C2A 122.2(13) . . ?
C4 C5A C6A 121.6(13) . . ?
C1 C6A C5A 121.1(14) . . ?
C1 C2B C3B 120.8(18) . . ?
C4 C3B C2B 121.1(18) . . ?
C4 C5B C6B 122.1(18) . . ?
C1 C6B C5B 122.5(18) . . ?
O7 Ti1 O11 102.6(3) . . ?
O7 Ti1 O1 92.8(3) . . ?
O11 Ti1 O1 91.1(3) . . ?
O7 Ti1 O3 96.5(3) . . ?
O11 Ti1 O3 160.2(2) . . ?
O1 Ti1 O3 92.9(2) . . ?
O7 Ti1 O8 97.5(3) . . ?
O11 Ti1 O8 78.0(3) . . ?
O1 Ti1 O8 166.4(3) . . ?
O3 Ti1 O8 94.8(3) . . ?
O7 Ti1 O1AA 174.0(3) . . ?
O11 Ti1 O1AA 81.7(2) . . ?
O1 Ti1 O1AA 82.8(2) . . ?
O3 Ti1 O1AA 79.6(2) . . ?
O8 Ti1 O1AA 87.5(2) . . ?
O7 Ti1 Ti2 102.6(2) . . ?
O11 Ti1 Ti2 38.51(19) . . ?
O1 Ti1 Ti2 129.21(18) . . ?
O3 Ti1 Ti2 131.83(18) . . ?
O8 Ti1 Ti2 39.5(2) . . ?
O1AA Ti1 Ti2 83.37(15) . . ?
O12 Ti2 O13 99.3(4) . . ?
O12 Ti2 O11 163.3(3) . . ?
O13 Ti2 O11 97.4(3) . . ?
O12 Ti2 O8 101.5(3) . . ?
O13 Ti2 O8 100.4(3) . . ?
O11 Ti2 O8 75.1(3) . . ?
O12 Ti2 O6 102.9(3) . . ?
O13 Ti2 O6 98.8(3) . . ?
O11 Ti2 O6 74.6(3) . . ?
O8 Ti2 O6 145.9(3) . . ?
O12 Ti2 O2 80.0(3) . . ?
O13 Ti2 O2 179.2(3) . . ?
O11 Ti2 O2 83.3(2) . . ?
O8 Ti2 O2 80.0(2) . . ?
O6 Ti2 O2 81.2(2) . . ?
O12 Ti2 Ti1 138.5(3) . . ?
O13 Ti2 Ti1 100.8(3) . . ?
O11 Ti2 Ti1 35.93(18) . . ?
O8 Ti2 Ti1 39.19(18) . . ?
O6 Ti2 Ti1 109.34(19) . . ?
O2 Ti2 Ti1 79.88(17) . . ?
O12 Ti2 Ti4 137.9(3) . . ?
O13 Ti2 Ti4 100.5(3) . . ?
O11 Ti2 Ti4 37.24(18) . . ?
O8 Ti2 Ti4 110.87(19) . . ?
O6 Ti2 Ti4 37.41(18) . . ?
O2 Ti2 Ti4 79.93(18) . . ?
Ti1 Ti2 Ti4 72.35(6) . . ?
O1AA S3 O0AA 112.7(3) . . ?
O1AA S3 O2 111.3(4) . . ?
O0AA S3 O2 113.9(4) . . ?
O1AA S3 C1 105.7(4) . . ?
O0AA S3 C1 103.4(4) . . ?
O2 S3 C1 109.3(4) . . ?
O9 Ti4 O5 98.3(3) . . ?
O9 Ti4 O4 93.7(3) . . ?
O5 Ti4 O4 95.7(3) . . ?
O9 Ti4 O11 100.8(3) . . ?
O5 Ti4 O11 160.5(2) . . ?
O4 Ti4 O11 87.0(2) . . ?
O9 Ti4 O6 97.9(3) . . ?
O5 Ti4 O6 99.6(3) . . ?
O4 Ti4 O6 159.1(3) . . ?
O11 Ti4 O6 73.9(3) . . ?
O9 Ti4 O0AA 175.3(3) . . ?
O5 Ti4 O0AA 80.6(2) . . ?
O4 Ti4 O0AA 81.8(2) . . ?
O11 Ti4 O0AA 80.7(2) . . ?
O6 Ti4 O0AA 86.8(2) . . ?
O9 Ti4 Ti2 102.1(3) . . ?
O5 Ti4 Ti2 133.9(2) . . ?
O4 Ti4 Ti2 123.27(18) . . ?
O11 Ti4 Ti2 36.82(17) . . ?
O6 Ti4 Ti2 37.1(2) . . ?
O0AA Ti4 Ti2 81.81(17) . . ?
O1 P5 O4 112.3(4) . . ?
O1 P5 O3 110.9(3) . 3_565 ?
O4 P5 O3 110.9(3) . 3_565 ?
P5 O1 Ti1 136.2(4) . . ?
S3 O2 Ti2 115.5(3) . . ?
P5 O3 Ti1 140.5(3) 2_665 . ?
P5 O4 Ti4 139.5(4) . . ?
C18 O5 Ti4 146.3(6) . . ?
C4BA O6 Ti2 123.8(7) . . ?
C4BA O6 Ti4 130.7(7) . . ?
Ti2 O6 Ti4 105.5(3) . . ?
C9AA O7 Ti1 136.0(7) . . ?
C0BA O8 Ti1 133.8(7) . . ?
C0BA O8 Ti2 124.5(6) . . ?
Ti1 O8 Ti2 101.3(3) . . ?
C1BA O9 Ti4 141.0(10) . . ?
O6 C4BA C4AA 112.2(9) . . ?
O6 C4BA C0AA 111.1(9) . . ?
C4AA C4BA C0AA 114.9(11) . . ?
Ti1 O11 Ti2 105.6(3) . . ?
Ti1 O11 Ti4 144.8(3) . . ?
Ti2 O11 Ti4 105.9(3) . . ?
C5AA O12 Ti2 155.7(9) . . ?
C19 O13 Ti2 132.7(7) . . ?
O5 C18 C2AA 111.6(10) . . ?
O5 C18 C1AA 108.5(9) . . ?
C2AA C18 C1AA 110.5(12) . . ?
O13 C19 C5BA 106.4(10) . . ?
O13 C19 C11 107.3(11) . . ?
C5BA C19 C11 113.9(11) . . ?
S3 O1AA Ti1 120.2(3) . . ?
S3 O0AA Ti4 120.2(3) . . ?
O7 C9AA C12 109.8(11) . . ?
O7 C9AA C3AA 104.3(12) . . ?
C12 C9AA C3AA 114.9(12) . . ?
O8 C0BA C13 109.1(10) . . ?
O8 C0BA C2BA 110.4(9) . . ?
C13 C0BA C2BA 113.3(12) . . ?
C8AA C1BA O9 118.6(15) . . ?
C8AA C1BA C3BA 131.5(15) . . ?
O9 C1BA C3BA 109.8(12) . . ?
O12 C5AA C7AA 103.8(14) . . ?
O12 C5AA C6AA 108.5(15) . . ?
C7AA C5AA C6AA 105.7(14) . . ?

_refine_diff_density_max         0.834
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.105

_shelxl_version_number           2014-3


# SQUEEZE RESULTS (Version =  91117)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 0.000 773 12 ' '
2 -0.017 -0.008 0.250 1475 69 ' '
3 0.000 0.000 0.500 773 12 ' '
4 -0.016 -0.003 0.750 1475 69 ' '
5 0.333 0.667 0.048 71 -9 ' '
6 0.333 0.667 0.452 72 -9 ' '
7 0.333 0.666 0.650 23 -3 ' '
8 0.333 0.666 0.850 23 -3 ' '
9 0.667 0.333 0.548 71 -9 ' '
10 0.667 0.333 0.952 72 -9 ' '
11 0.667 0.333 0.150 23 -3 ' '
12 0.667 0.333 0.350 23 -3 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
0 1 0 2.694
0 1 1 2.839
0 0 2 1.785
0 1 2 3.233
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
;


####################################################################### 
# 
# 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_PTC-77
_database_code_depnum_ccdc_archive 'CCDC 1583620'
_audit_update_record             
;
2017-12-01 deposited with the CCDC.
2017-12-05 downloaded from the CCDC.
;
_audit_creation_date             2017-11-27
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C27 H53 Br0.33 Cu0.33 N O13 P Ti3'
_chemical_formula_sum            'C27 H46 Br0.33 Cu0.33 N O13 P Ti3'
_chemical_formula_weight         815.13
_chemical_melting_point          ?
_chemical_oxdiff_formula         COPTi
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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'
P P 0.2955 0.4335 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-y, x-y, z'
3 '-x+y, -x, z'
4 '-x, -y, -z'
5 'y, -x+y, -z'
6 'x-y, x, -z'

_cell_length_a                   19.0415(6)
_cell_length_b                   19.0415(6)
_cell_length_c                   20.0613(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6299.3(3)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    5654
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.0530
_cell_measurement_theta_min      4.6380
_exptl_absorpt_coefficient_mu    6.088
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15147
_diffrn_reflns_theta_full        74.37
_diffrn_reflns_theta_max         74.37
_diffrn_reflns_theta_min         3.47
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3503
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     39.00  66.00   1.00    1.00    --   40.84-125.00-120.00   27
  2  ω     26.00  68.00   1.00    3.96    --  108.54 -95.00 -90.00   42
  3  ω     42.00 134.00   1.00    3.96    --  108.54 -61.00  60.00   92
  4  ω    131.00 177.00   1.00    3.96    --  108.54  45.00 -90.00   46
  5  ω     81.00 171.00   1.00    3.96    --  108.54  30.00-180.00   90
  6  ω   -120.00 -16.00   1.00    1.00    --  -40.84 -19.00-120.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0621302000
_diffrn_orient_matrix_UB_12      -0.0745277000
_diffrn_orient_matrix_UB_13      -0.0398146000
_diffrn_orient_matrix_UB_21      0.0693360000
_diffrn_orient_matrix_UB_22      0.0023575000
_diffrn_orient_matrix_UB_23      -0.0411958000
_diffrn_orient_matrix_UB_31      0.0074202000
_diffrn_orient_matrix_UB_32      -0.0564492000
_diffrn_orient_matrix_UB_33      0.0511190000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                6622
_reflns_number_total             8349
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.388
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         8349
_refine_ls_number_restraints     237
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0808
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1710P)²+1.7620P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2314
_refine_ls_wR_factor_ref         0.2480
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2-C016
 1.45 with sigma of 0.02
 C1-C016
 1.45 with sigma of 0.02
 C1-C2
 2.5 with sigma of 0.02
3. Rigid bond restraints
 C016
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C016: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C00J \\sim C00K \\sim C00L \\sim C00M \\sim C00N \\sim C00O \\sim C00R \\sim
C00S \\sim C00T \\sim C00U \\sim C00V \\sim C00W \\sim C00X \\sim C00Y \\sim
C00Z \\sim C010 \\sim C011 \\sim C012 \\sim C013 \\sim C014 \\sim C015 \\sim
C016 \\sim C017 \\sim C3 \\sim C4 \\sim C1 \\sim C2: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C016) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Ternary CH refined with riding coordinates:
 C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), C00Z(H00Z), C011(H011),
 C016(H016)
5.b Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N)
5.c Idealised Me refined as rotating group:
 C00R(H00A,H00B,H00C), C00W(H00D,H00E,H00F), C00X(H00G,H00H,H00I), C00Y(H00J,
 H00O,H00P), C010(H01A,H01B,H01C), C012(H01D,H01E,H01F), C013(H01G,H01H,H01I),
 C014(H01J,H01K,H01L), C015(H01M,H01N,H01O), C017(H01P,H01Q,H01R), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Br01 Br 0.6667 0.3333 0.34360(4) 0.0428(2) Uani 1 d . . 3 S T P
Cu02 Cu 0.6667 0.3333 0.46769(5) 0.0308(3) Uani 1 d . . 3 S T P
Ti03 Ti 0.64487(5) 0.50327(5) 0.79891(4) 0.0311(2) Uani 1 d . . 1 . . .
Ti04 Ti 0.67258(6) 0.67032(5) 0.75370(4) 0.0386(2) Uani 1 d . . 1 . . .
Ti05 Ti 0.83658(6) 0.67069(5) 0.74037(5) 0.0427(3) Uani 1 d . . 1 . . .
P006 P 0.51818(7) 0.31367(7) 0.75870(5) 0.0347(3) Uani 1 d . . 1 . . .
O007 O 0.73094(19) 0.60929(18) 0.77964(15) 0.0348(6) Uani 1 d . . 1 . . .
O008 O 0.54847(19) 0.3945(2) 0.79279(16) 0.0358(6) Uani 1 d . . 1 . . .
O009 O 0.6434(2) 0.48750(19) 0.69189(15) 0.0348(6) Uani 1 d . . 1 . . .
O00A O 0.54050(19) 0.25911(19) 0.79737(16) 0.0351(6) Uani 1 d . . 1 . . .
O00B O 0.5840(2) 0.5609(2) 0.78271(16) 0.0364(7) Uani 1 d . . 1 . . .
O00C O 0.6420(2) 0.5045(2) 0.88760(16) 0.0410(7) Uani 1 d . . 1 . . .
O00D O 0.6573(2) 0.6063(2) 0.65891(16) 0.0426(8) Uani 1 d . . 1 . . .
O00E O 0.7858(3) 0.7384(2) 0.72091(19) 0.0479(8) Uani 1 d . . 1 . . .
O00F O 0.4274(2) 0.2729(2) 0.7453(2) 0.0499(9) Uani 1 d . . 1 . . .
O00G O 0.6172(3) 0.7112(2) 0.7141(2) 0.0532(9) Uani 1 d . . 1 . . .
O00H O 0.6854(2) 0.7182(2) 0.83344(18) 0.0473(8) Uani 1 d . . 1 . . .
N00I N 0.6376(2) 0.4187(2) 0.49535(17) 0.0310(7) Uani 1 d . . 1 . . .
C00J C 0.6354(3) 0.5095(3) 0.5767(2) 0.0355(8) Uani 1 d . . 1 . U .
C00K C 0.6440(3) 0.4445(3) 0.5583(2) 0.0338(8) Uani 1 d . . 1 . U .
H00K H 0.6550 0.4171 0.5914 0.041 Uiso 1 calc . . 1 R . .
C00L C 0.6177(3) 0.4570(3) 0.4487(2) 0.0399(9) Uani 1 d . . 1 . U .
H00L H 0.6099 0.4382 0.4050 0.048 Uiso 1 calc . . 1 R . .
C00M C 0.6180(3) 0.5496(3) 0.5280(2) 0.0405(9) Uani 1 d . . 1 . U .
H00M H 0.6128 0.5943 0.5386 0.049 Uiso 1 calc . . 1 R . .
C00N C 0.6084(3) 0.5219(3) 0.4628(2) 0.0439(10) Uani 1 d . . 1 . U .
H00N H 0.5958 0.5474 0.4291 0.053 Uiso 1 calc . . 1 R . .
C00O C 0.6461(3) 0.5373(3) 0.6486(2) 0.0346(8) Uani 1 d . . 1 . U .
O00P O 0.9119(3) 0.7300(3) 0.7990(3) 0.0824(16) Uani 1 d . . 1 . . .
O00Q O 0.8811(5) 0.6895(4) 0.6590(3) 0.095(2) Uani 1 d . . 1 . . .
C00R C 0.4582(4) 0.4941(4) 0.7223(4) 0.0589(14) Uani 1 d . . 1 . U .
H00A H 0.4860 0.5289 0.6852 0.088 Uiso 1 calc . . 1 GR . .
H00B H 0.4027 0.4815 0.7225 0.088 Uiso 1 calc . . 1 GR . .
H00C H 0.4604 0.4450 0.7185 0.088 Uiso 1 calc . . 1 GR . .
C00S C 0.4987(4) 0.5369(4) 0.7867(3) 0.0594(14) Uani 1 d . . 1 . U .
H00S H 0.4968 0.5874 0.7871 0.071 Uiso 1 calc . . 1 R . .
C00T C 0.6434(5) 0.4604(5) 0.9439(3) 0.0715(19) Uani 1 d . . 1 . U .
H00T H 0.6656 0.4253 0.9323 0.086 Uiso 1 calc . . 1 R . .
C00U C 0.9273(5) 0.6684(5) 0.6169(4) 0.0686(17) Uani 1 d . . 1 . U .
H00U H 0.9576 0.6510 0.6452 0.082 Uiso 1 calc . . 1 R . .
C00V C 0.5586(5) 0.7256(5) 0.6844(4) 0.0670(16) Uani 1 d . . 1 . U .
H00V H 0.5052 0.6807 0.6971 0.080 Uiso 1 calc . . 1 R . .
C00W C 0.5651(5) 0.7234(6) 0.6105(4) 0.080(2) Uani 1 d . . 1 . U .
H00D H 0.6148 0.7696 0.5960 0.120 Uiso 1 calc . . 1 GR . .
H00E H 0.5200 0.7246 0.5902 0.120 Uiso 1 calc . . 1 GR . .
H00F H 0.5646 0.6746 0.5976 0.120 Uiso 1 calc . . 1 GR . .
C00X C 0.7976(6) 0.7964(5) 0.6100(4) 0.081(2) Uani 1 d . . 1 . U .
H00G H 0.8309 0.7763 0.5920 0.121 Uiso 1 calc . . 1 GR . .
H00H H 0.8090 0.8453 0.5873 0.121 Uiso 1 calc . . 1 GR . .
H00I H 0.7415 0.7564 0.6041 0.121 Uiso 1 calc . . 1 GR . .
C00Y C 0.8702(5) 0.5965(7) 0.5733(4) 0.095(3) Uani 1 d . . 1 . U .
H00J H 0.8371 0.5506 0.6012 0.142 Uiso 1 calc . . 1 GR . .
H00O H 0.9014 0.5833 0.5437 0.142 Uiso 1 calc . . 1 GR . .
H00P H 0.8362 0.6104 0.5478 0.142 Uiso 1 calc . . 1 GR . .
C00Z C 0.8153(6) 0.8138(4) 0.6836(5) 0.085(2) Uani 1 d . . 1 . U .
H00Z H 0.7811 0.8359 0.6981 0.102 Uiso 1 calc . . 1 R . .
C010 C 0.4632(6) 0.4965(7) 0.8490(5) 0.090(2) Uani 1 d . . 1 . U .
H01A H 0.4671 0.4483 0.8526 0.134 Uiso 1 calc . . 1 GR . .
H01B H 0.4072 0.4822 0.8504 0.134 Uiso 1 calc . . 1 GR . .
H01C H 0.4917 0.5322 0.8855 0.134 Uiso 1 calc . . 1 GR . .
C011 C 0.7009(7) 0.7102(6) 0.9005(4) 0.088(3) Uani 1 d . . 1 . U .
H011 H 0.6886 0.6545 0.9088 0.106 Uiso 1 calc . . 1 R . .
C012 C 0.9875(7) 0.7413(6) 0.5787(6) 0.101(3) Uani 1 d . . 1 . U .
H01D H 0.9610 0.7500 0.5415 0.151 Uiso 1 calc . . 1 GR . .
H01E H 1.0302 0.7327 0.5629 0.151 Uiso 1 calc . . 1 GR . .
H01F H 1.0099 0.7880 0.6073 0.151 Uiso 1 calc . . 1 GR . .
C013 C 0.6941(8) 0.5207(8) 0.9981(5) 0.119(4) Uani 1 d . . 1 . U .
H01G H 0.7463 0.5591 0.9803 0.178 Uiso 1 calc . . 1 GR . .
H01H H 0.7009 0.4922 1.0347 0.178 Uiso 1 calc . . 1 GR . .
H01I H 0.6670 0.5488 1.0133 0.178 Uiso 1 calc . . 1 GR . .
C014 C 0.5587(7) 0.4114(8) 0.9715(5) 0.115(4) Uani 1 d . . 1 . U .
H01J H 0.5399 0.4474 0.9857 0.173 Uiso 1 calc . . 1 GR . .
H01K H 0.5590 0.3799 1.0087 0.173 Uiso 1 calc . . 1 GR . .
H01L H 0.5232 0.3758 0.9375 0.173 Uiso 1 calc . . 1 GR . .
C015 C 0.8918(7) 0.8706(6) 0.7012(7) 0.109(3) Uani 1 d . . 1 . U .
H01M H 0.8921 0.8867 0.7465 0.163 Uiso 1 calc . . 1 GR . .
H01N H 0.9104 0.9169 0.6725 0.163 Uiso 1 calc . . 1 GR . .
H01O H 0.9271 0.8484 0.6968 0.163 Uiso 1 calc . . 1 GR . .
C016 C 0.9883(8) 0.7604(10) 0.8237(8) 0.140(5) Uani 1 d . . 1 D U .
H016 H 0.9815 0.7843 0.8647 0.168 Uiso 1 calc . . 1 R . .
C017 C 0.5655(8) 0.8014(7) 0.7123(6) 0.111(3) Uani 1 d . . 1 . U .
H01P H 0.5752 0.8036 0.7594 0.166 Uiso 1 calc . . 1 GR . .
H01Q H 0.5160 0.8018 0.7042 0.166 Uiso 1 calc . . 1 GR . .
H01R H 0.6097 0.8476 0.6911 0.166 Uiso 1 calc . . 1 GR . .
C3 C 0.6451(10) 0.7269(12) 0.9407(6) 0.167(6) Uani 1 d . . 1 . U .
H3A H 0.6018 0.7219 0.9129 0.250 Uiso 1 calc . . 1 GR . .
H3B H 0.6745 0.7809 0.9584 0.250 Uiso 1 calc . . 1 GR . .
H3C H 0.6230 0.6887 0.9767 0.250 Uiso 1 calc . . 1 GR . .
C4 C 0.7880(8) 0.7676(11) 0.9170(6) 0.143(5) Uani 1 d . . 1 . U .
H4A H 0.8212 0.7480 0.8981 0.214 Uiso 1 calc . . 1 GR . .
H4B H 0.7947 0.7715 0.9646 0.214 Uiso 1 calc . . 1 GR . .
H4C H 0.8038 0.8202 0.8990 0.214 Uiso 1 calc . . 1 GR . .
C1 C 1.0065(12) 0.7029(12) 0.8536(12) 0.209(8) Uani 1 d . . 1 D U .
H1A H 0.9828 0.6890 0.8973 0.314 Uiso 1 calc . . 1 GR . .
H1B H 1.0642 0.7262 0.8570 0.314 Uiso 1 calc . . 1 GR . .
H1C H 0.9845 0.6549 0.8265 0.314 Uiso 1 calc . . 1 GR . .
C2 C 1.0498(13) 0.8298(13) 0.7958(13) 0.241(9) Uani 1 d . . 1 D U .
H2A H 1.0450 0.8263 0.7481 0.362 Uiso 1 calc . . 1 GR . .
H2B H 1.1011 0.8359 0.8087 0.362 Uiso 1 calc . . 1 GR . .
H2C H 1.0463 0.8757 0.8111 0.362 Uiso 1 calc . . 1 GR . .


_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
Br01 Cu02 2.4895(12) . ?
Cu02 N00I 2.039(4) . ?
Cu02 N00I 2.039(4) 3_665 ?
Cu02 N00I 2.039(4) 2_655 ?
Ti03 Ti04 3.0889(11) . ?
Ti03 O007 1.898(3) . ?
Ti03 O008 1.967(3) . ?
Ti03 O009 2.166(3) . ?
Ti03 O00A 1.959(3) 3_665 ?
Ti03 O00B 1.981(3) . ?
Ti03 O00C 1.781(3) . ?
Ti04 Ti05 3.1308(13) . ?
Ti04 O007 2.037(3) . ?
Ti04 O00B 2.002(3) . ?
Ti04 O00D 2.198(3) . ?
Ti04 O00E 1.992(4) . ?
Ti04 O00G 1.781(4) . ?
Ti04 O00H 1.796(3) . ?
Ti05 O007 1.919(3) . ?
Ti05 O00E 2.000(4) . ?
Ti05 O00F 1.961(4) 3_665 ?
Ti05 O00P 1.759(5) . ?
Ti05 O00Q 1.791(5) . ?
P006 O008 1.511(3) . ?
P006 O00A 1.518(3) . ?
P006 O00F 1.524(4) . ?
O009 C00O 1.269(6) . ?
O00A Ti03 1.959(3) 2_655 ?
O00B C00S 1.452(7) . ?
O00C C00T 1.416(7) . ?
O00D C00O 1.238(6) . ?
O00E C00Z 1.459(8) . ?
O00F Ti05 1.961(4) 2_655 ?
O00G C00V 1.407(8) . ?
O00H C011 1.402(9) . ?
N00I C00K 1.338(6) . ?
N00I C00L 1.352(6) . ?
C00J C00K 1.378(7) . ?
C00J C00M 1.377(7) . ?
C00J C00O 1.514(6) . ?
C00L C00N 1.363(7) . ?
C00M C00N 1.388(7) . ?
O00P C016 1.362(13) . ?
O00Q C00U 1.415(8) . ?
C00R C00S 1.515(9) . ?
C00S C010 1.448(12) . ?
C00T C013 1.524(13) . ?
C00T C014 1.508(14) . ?
C00U C00Y 1.527(13) . ?
C00U C012 1.494(12) . ?
C00V C00W 1.490(12) . ?
C00V C017 1.491(11) . ?
C00X C00Z 1.514(13) . ?
C00Z C015 1.357(15) . ?
C011 C3 1.488(18) . ?
C011 C4 1.497(16) . ?
C016 C1 1.436(15) . ?
C016 C2 1.372(15) . ?

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
N00I Cu02 Br01 105.79(10) 2_655 . ?
N00I Cu02 Br01 105.79(10) . . ?
N00I Cu02 Br01 105.79(10) 3_665 . ?
N00I Cu02 N00I 112.89(8) 2_655 . ?
N00I Cu02 N00I 112.89(9) 3_665 . ?
N00I Cu02 N00I 112.89(8) 3_665 2_655 ?
O007 Ti03 Ti04 39.90(10) . . ?
O007 Ti03 O008 164.10(14) . . ?
O007 Ti03 O009 83.68(13) . . ?
O007 Ti03 O00A 91.60(14) . 3_665 ?
O007 Ti03 O00B 79.08(14) . . ?
O008 Ti03 Ti04 130.88(10) . . ?
O008 Ti03 O009 81.48(13) . . ?
O008 Ti03 O00B 94.38(14) . . ?
O009 Ti03 Ti04 80.53(9) . . ?
O00A Ti03 Ti04 130.08(10) 3_665 . ?
O00A Ti03 O008 92.37(14) 3_665 . ?
O00A Ti03 O009 83.54(13) 3_665 . ?
O00A Ti03 O00B 167.25(14) 3_665 . ?
O00B Ti03 Ti04 39.41(10) . . ?
O00B Ti03 O009 86.78(13) . . ?
O00C Ti03 Ti04 105.67(12) . . ?
O00C Ti03 O007 101.83(16) . . ?
O00C Ti03 O008 93.32(16) . . ?
O00C Ti03 O009 173.68(15) . . ?
O00C Ti03 O00A 93.14(15) . 3_665 ?
O00C Ti03 O00B 97.25(15) . . ?
Ti03 Ti04 Ti05 71.58(3) . . ?
O007 Ti04 Ti03 36.71(9) . . ?
O007 Ti04 Ti05 36.38(9) . . ?
O007 Ti04 O00D 82.14(13) . . ?
O00B Ti04 Ti03 38.91(9) . . ?
O00B Ti04 Ti05 110.33(9) . . ?
O00B Ti04 O007 75.40(13) . . ?
O00B Ti04 O00D 82.26(14) . . ?
O00D Ti04 Ti03 77.04(9) . . ?
O00D Ti04 Ti05 77.45(11) . . ?
O00E Ti04 Ti03 109.84(11) . . ?
O00E Ti04 Ti05 38.42(11) . . ?
O00E Ti04 O007 74.58(14) . . ?
O00E Ti04 O00B 147.97(14) . . ?
O00E Ti04 O00D 82.85(15) . . ?
O00G Ti04 Ti03 138.42(15) . . ?
O00G Ti04 Ti05 140.25(16) . . ?
O00G Ti04 O007 167.15(15) . . ?
O00G Ti04 O00B 102.13(18) . . ?
O00G Ti04 O00D 85.03(16) . . ?
O00G Ti04 O00E 104.62(19) . . ?
O00G Ti04 O00H 97.81(18) . . ?
O00H Ti04 Ti03 99.83(13) . . ?
O00H Ti04 Ti05 101.08(13) . . ?
O00H Ti04 O007 94.99(16) . . ?
O00H Ti04 O00B 95.70(16) . . ?
O00H Ti04 O00D 176.81(16) . . ?
O00H Ti04 O00E 97.77(18) . . ?
O007 Ti05 Ti04 39.01(10) . . ?
O007 Ti05 O00E 77.03(15) . . ?
O007 Ti05 O00F 87.88(15) . 3_665 ?
O00E Ti05 Ti04 38.24(11) . . ?
O00F Ti05 Ti04 123.73(12) 3_665 . ?
O00F Ti05 O00E 157.60(18) 3_665 . ?
O00P Ti05 Ti04 115.9(2) . . ?
O00P Ti05 O007 112.7(2) . . ?
O00P Ti05 O00E 102.6(2) . . ?
O00P Ti05 O00F 98.4(2) . 3_665 ?
O00P Ti05 O00Q 109.1(4) . . ?
O00Q Ti05 Ti04 116.8(2) . . ?
O00Q Ti05 O007 138.0(3) . . ?
O00Q Ti05 O00E 91.5(2) . . ?
O00Q Ti05 O00F 88.74(19) . 3_665 ?
O008 P006 O00A 111.81(18) . . ?
O008 P006 O00F 110.9(2) . . ?
O00A P006 O00F 112.1(2) . . ?
Ti03 O007 Ti04 103.39(15) . . ?
Ti03 O007 Ti05 144.72(17) . . ?
Ti05 O007 Ti04 104.61(15) . . ?
P006 O008 Ti03 141.3(2) . . ?
C00O O009 Ti03 125.6(3) . . ?
P006 O00A Ti03 133.2(2) . 2_655 ?
Ti03 O00B Ti04 101.68(15) . . ?
C00S O00B Ti03 133.5(4) . . ?
C00S O00B Ti04 124.8(3) . . ?
C00T O00C Ti03 141.2(4) . . ?
C00O O00D Ti04 129.7(3) . . ?
Ti04 O00E Ti05 103.33(16) . . ?
C00Z O00E Ti04 124.7(5) . . ?
C00Z O00E Ti05 131.4(5) . . ?
P006 O00F Ti05 141.9(2) . 2_655 ?
C00V O00G Ti04 167.0(5) . . ?
C011 O00H Ti04 141.6(5) . . ?
C00K N00I Cu02 122.5(3) . . ?
C00K N00I C00L 117.0(4) . . ?
C00L N00I Cu02 120.2(3) . . ?
C00K C00J C00O 120.9(4) . . ?
C00M C00J C00K 118.5(4) . . ?
C00M C00J C00O 120.6(4) . . ?
N00I C00K C00J 123.5(4) . . ?
N00I C00L C00N 123.0(4) . . ?
C00J C00M C00N 118.8(4) . . ?
C00L C00N C00M 119.1(4) . . ?
O009 C00O C00J 116.3(4) . . ?
O00D C00O O009 126.8(4) . . ?
O00D C00O C00J 116.9(4) . . ?
C016 O00P Ti05 150.6(10) . . ?
C00U O00Q Ti05 141.9(5) . . ?
O00B C00S C00R 108.1(5) . . ?
C010 C00S O00B 111.5(6) . . ?
C010 C00S C00R 118.3(7) . . ?
O00C C00T C013 108.3(7) . . ?
O00C C00T C014 109.1(7) . . ?
C014 C00T C013 106.4(8) . . ?
O00Q C00U C00Y 109.4(7) . . ?
O00Q C00U C012 109.9(6) . . ?
C012 C00U C00Y 114.3(8) . . ?
O00G C00V C00W 109.3(6) . . ?
O00G C00V C017 109.6(7) . . ?
C00W C00V C017 115.6(8) . . ?
O00E C00Z C00X 110.5(6) . . ?
C015 C00Z O00E 112.6(9) . . ?
C015 C00Z C00X 117.4(9) . . ?
O00H C011 C3 106.7(10) . . ?
O00H C011 C4 110.4(9) . . ?
C3 C011 C4 111.9(9) . . ?
O00P C016 C1 116.2(13) . . ?
O00P C016 C2 118.5(14) . . ?
C2 C016 C1 119.4(16) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.480
_oxdiff_exptl_absorpt_empirical_full_min 0.377
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 0.000 206 18 ' '
2 0.000 0.000 0.500 123 19 ' '
3 0.333 0.667 0.849 137 32 ' '
4 0.333 0.667 0.318 7 1 ' '
5 0.667 0.333 0.151 137 32 ' '
6 0.666 0.333 0.682 7 1 ' '
_platon_squeeze_details          
;
;

####################################################################### 
# 
# 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_PTC-76
_database_code_depnum_ccdc_archive 'CCDC 1583619'
_audit_update_record             
;
2017-12-01 deposited with the CCDC.
2017-12-05 downloaded from the CCDC.
;
_audit_creation_date             2017-11-24
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C27 H49 Cl0.33 Cu0.33 N O13 P Ti3'
_chemical_formula_sum            'C27 H49 Cl0.33 Cu0.33 N O13 P Ti3'
_chemical_formula_weight         803.34
_chemical_melting_point          ?
_chemical_oxdiff_formula         COTi
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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'
P P 0.2955 0.4335 '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'

_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      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   18.9783(12)
_cell_length_b                   18.9783(12)
_cell_length_c                   19.9218(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6214.0(8)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    4511
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      74.1470
_cell_measurement_theta_min      4.6680
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.993
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2510
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0729
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15005
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.413
_diffrn_reflns_theta_min         3.486
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3503
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     24.00  54.00   1.00    1.57    --   40.72-125.00-120.00   30
  2  ω     35.00  62.00   1.00    1.57    --   40.72-125.00  90.00   27
  3  ω     63.00 174.00   1.00    6.29    --  108.54  15.00  30.00  111
  4  ω    109.00 172.00   1.00    6.29    --  108.54  45.00  60.00   63
  5  ω    105.00 154.00   1.00    6.29    --  108.54 125.00 -30.00   49
  6  ω    106.00 156.00   1.00    6.29    --  108.54 125.00 -60.00   50
  7  ω    -93.00  -6.00   1.00    1.57    --  -40.72 125.00-120.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0300545000
_diffrn_orient_matrix_UB_12      -0.0442087000
_diffrn_orient_matrix_UB_13      0.0467048000
_diffrn_orient_matrix_UB_21      -0.0784601000
_diffrn_orient_matrix_UB_22      -0.0811017000
_diffrn_orient_matrix_UB_23      -0.0139464000
_diffrn_orient_matrix_UB_31      0.0416058000
_diffrn_orient_matrix_UB_32      -0.0153854000
_diffrn_orient_matrix_UB_33      -0.0601288000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6087
_reflns_number_total             8193
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_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 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.203
_refine_diff_density_min         -1.211
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         8193
_refine_ls_number_restraints     244
_refine_ls_R_factor_all          0.1574
_refine_ls_R_factor_gt           0.1342
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1250P)²+65.4400P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3239
_refine_ls_wR_factor_ref         0.3378
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 O00I, C00X
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C012, C018
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O00Q, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
C00J \\sim C00K \\sim C00L \\sim C00M \\sim C00N \\sim C00P \\sim C00R \\sim
C00S \\sim C00T \\sim C00U \\sim C00V \\sim C00W \\sim C00X \\sim C00Y \\sim
C00Z \\sim C010 \\sim C011 \\sim C012 \\sim C013 \\sim C015 \\sim C016 \\sim
C017 \\sim C018 \\sim C2 \\sim C5 \\sim C15 \\sim C3: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O00Q) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C00S(H00S), C00T(H00T), C00V(H00V), C00X(H00X), C010(H010), C012(H012)
4.b Aromatic/amide H refined with riding coordinates:
 C00J(H00J), C00M(H00M), C00N(H00N), C00P(H00P)
4.c Idealised Me refined as rotating group:
 C00R(H00A,H00B,H00C), C00U(H00D,H00E,H00F), C00W(H00G,H00H,H00I), C00Y(H00K,
 H00L,H00O), C00Z(H00Q,H00R,H00U), C011(H01A,H01B,H01C), C013(H01D,H01E,H01F),
 C015(H01G,H01H,H01I), C016(H01J,H01K,H01L), C017(H01M,H01N,H01O), C018(H01P,
 H01Q,H01R), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Cu01 Cu 0.3333 0.6667 0.46741(5) 0.0395(3) Uani 1 3 d S T P . .
Ti02 Ti 0.50356(5) 0.64470(5) 0.79961(4) 0.0401(2) Uani 1 1 d . . . . .
Ti03 Ti 0.67107(5) 0.67265(6) 0.75447(5) 0.0478(2) Uani 1 1 d . . . . .
Ti04 Ti 0.67188(6) 0.83688(6) 0.74087(5) 0.0551(3) Uani 1 1 d . . . . .
Cl05 Cl 0.3333 0.6667 0.34901(9) 0.0501(5) Uani 1 3 d S T P . .
P06 P 0.48170(8) 0.79491(8) 0.75871(6) 0.0449(3) Uani 1 1 d . . . . .
O007 O 0.4527(2) 0.8464(2) 0.79295(16) 0.0457(9) Uani 1 1 d . . . . .
O008 O 0.61110(18) 0.73194(19) 0.78016(15) 0.0421(8) Uani 1 1 d . . . . .
O009 O 0.45976(19) 0.71800(19) 0.79742(16) 0.0453(9) Uani 1 1 d . . . . .
O00A O 0.48718(18) 0.64242(19) 0.69194(16) 0.0434(9) Uani 1 1 d . . . . .
O00B O 0.5034(2) 0.6414(2) 0.88805(17) 0.0491(10) Uani 1 1 d . . . . .
O00C O 0.5602(2) 0.5831(2) 0.78257(17) 0.0468(9) Uani 1 1 d . . . . .
O00D O 0.5723(2) 0.8448(2) 0.74449(19) 0.0530(10) Uani 1 1 d . . . . .
O00E O 0.6072(2) 0.6573(2) 0.65899(16) 0.0574(10) Uani 1 1 d . . . . .
O00F O 0.7201(2) 0.6851(2) 0.83418(18) 0.0559(10) Uani 1 1 d . . . . .
O00G O 0.7400(2) 0.7868(2) 0.7223(2) 0.0588(11) Uani 1 1 d . . . . .
N00H N 0.4193(2) 0.6384(2) 0.49471(17) 0.0369(9) Uani 1 1 d . . . . .
O00I O 0.7128(2) 0.6184(2) 0.7138(2) 0.0753(12) Uani 1 1 d . U . . .
C00J C 0.4449(3) 0.6451(3) 0.5582(2) 0.0444(11) Uani 1 1 d . U . . .
H00J H 0.4182 0.6570 0.5917 0.053 Uiso 1 1 calc R . . . .
C00K C 0.5382(3) 0.6466(3) 0.6482(2) 0.0454(11) Uani 1 1 d . U . . .
C00L C 0.5097(3) 0.6349(3) 0.5757(2) 0.0454(11) Uani 1 1 d . U . . .
C00M C 0.5228(3) 0.6097(3) 0.4618(2) 0.0479(12) Uani 1 1 d . U . . .
H00M H 0.5475 0.5960 0.4279 0.058 Uiso 1 1 calc R . . . .
C00N C 0.5514(3) 0.6190(3) 0.5277(2) 0.0474(11) Uani 1 1 d . U . . .
H00N H 0.5968 0.6147 0.5384 0.057 Uiso 1 1 calc R . . . .
O00O O 0.6922(3) 0.8827(3) 0.6602(3) 0.1186(16) Uani 1 1 d . . . . .
C00P C 0.4583(3) 0.6207(3) 0.4468(2) 0.0461(12) Uani 1 1 d . U . . .
H00P H 0.4410 0.6158 0.4025 0.055 Uiso 1 1 calc R . . . .
O00Q O 0.7290(3) 0.9092(3) 0.8018(3) 0.1030(17) Uani 1 1 d . U . . .
C00R C 0.4932(3) 0.4568(3) 0.7229(3) 0.0633(15) Uani 1 1 d . U . . .
H00A H 0.4403 0.4516 0.7221 0.095 Uiso 1 1 calc GR . . . .
H00B H 0.4878 0.4038 0.7200 0.095 Uiso 1 1 calc GR . . . .
H00C H 0.5245 0.4892 0.6855 0.095 Uiso 1 1 calc GR . . . .
C00S C 0.5356(4) 0.4971(4) 0.7872(3) 0.0739(17) Uani 1 1 d . U . . .
H00S H 0.5867 0.4960 0.7863 0.089 Uiso 1 1 calc R . . . .
C00T C 0.4586(5) 0.6424(4) 0.9453(3) 0.082(2) Uani 1 1 d . U . . .
H00T H 0.4246 0.6661 0.9335 0.098 Uiso 1 1 calc R . . . .
C00U C 0.7174(5) 0.5591(5) 0.6139(4) 0.097(2) Uani 1 1 d . U . . .
H00D H 0.6613 0.5319 0.6007 0.145 Uiso 1 1 calc GR . . . .
H00E H 0.7443 0.5336 0.5926 0.145 Uiso 1 1 calc GR . . . .
H00F H 0.7432 0.6152 0.6007 0.145 Uiso 1 1 calc GR . . . .
C00V C 0.6714(4) 0.9267(4) 0.6155(4) 0.087(2) Uani 1 1 d . U . . .
H00V H 0.6528 0.9570 0.6431 0.104 Uiso 1 1 calc R . . . .
C00W C 0.7999(5) 0.7973(6) 0.6113(5) 0.115(3) Uani 1 1 d . U . . .
H00G H 0.7520 0.7452 0.6049 0.173 Uiso 1 1 calc GR . . . .
H00H H 0.8457 0.7973 0.5910 0.173 Uiso 1 1 calc GR . . . .
H00I H 0.7920 0.8387 0.5910 0.173 Uiso 1 1 calc GR . . . .
C00X C 0.7227(5) 0.5542(5) 0.6838(4) 0.092(2) Uani 1 1 d . U . . .
H00X H 0.6768 0.5020 0.6984 0.110 Uiso 1 1 calc R . . . .
C00Y C 0.4047(6) 0.5535(6) 0.9711(4) 0.110(3) Uani 1 1 d . U . . .
H00K H 0.3676 0.5208 0.9364 0.165 Uiso 1 1 calc GR . . . .
H00L H 0.3745 0.5535 1.0098 0.165 Uiso 1 1 calc GR . . . .
H00O H 0.4388 0.5314 0.9831 0.165 Uiso 1 1 calc GR . . . .
C00Z C 0.5983(6) 0.8678(5) 0.5722(4) 0.098(3) Uani 1 1 d . U . . .
H00Q H 0.6147 0.8392 0.5420 0.146 Uiso 1 1 calc GR . . . .
H00R H 0.5792 0.8980 0.5468 0.146 Uiso 1 1 calc GR . . . .
H00U H 0.5554 0.8295 0.6006 0.146 Uiso 1 1 calc GR . . . .
C010 C 0.8158(5) 0.8146(7) 0.6876(6) 0.123(3) Uani 1 1 d . U . . .
H010 H 0.8369 0.7798 0.7033 0.148 Uiso 1 1 calc R . . . .
C011 C 0.5011(6) 0.4644(5) 0.8494(5) 0.104(3) Uani 1 1 d . U . . .
H01A H 0.5288 0.5043 0.8838 0.156 Uiso 1 1 calc GR . . . .
H01B H 0.5060 0.4174 0.8582 0.156 Uiso 1 1 calc GR . . . .
H01C H 0.4446 0.4491 0.8491 0.156 Uiso 1 1 calc GR . . . .
C012 C 0.7072(8) 0.6963(6) 0.9020(4) 0.131(3) Uani 1 1 d . U . . .
H012 H 0.6503 0.6806 0.9101 0.157 Uiso 1 1 calc R . . . .
C013 C 0.5170(6) 0.6907(6) 0.9987(4) 0.108(3) Uani 1 1 d . U . . .
H01D H 0.5410 0.6607 1.0168 0.162 Uiso 1 1 calc GR . . . .
H01E H 0.4891 0.7018 1.0337 0.162 Uiso 1 1 calc GR . . . .
H01F H 0.5589 0.7411 0.9802 0.162 Uiso 1 1 calc GR . . . .
C015 C 0.7431(5) 0.9868(5) 0.5801(4) 0.113(3) Uani 1 1 d . U . . .
H01G H 0.7799 1.0267 0.6114 0.170 Uiso 1 1 calc GR . . . .
H01H H 0.7275 1.0128 0.5467 0.170 Uiso 1 1 calc GR . . . .
H01I H 0.7693 0.9606 0.5588 0.170 Uiso 1 1 calc GR . . . .
C016 C 0.7646(8) 0.7873(6) 0.9181(5) 0.153(4) Uani 1 1 d . U . . .
H01J H 0.8168 0.8051 0.8980 0.230 Uiso 1 1 calc GR . . . .
H01K H 0.7707 0.7946 0.9659 0.230 Uiso 1 1 calc GR . . . .
H01L H 0.7419 0.8187 0.9005 0.230 Uiso 1 1 calc GR . . . .
C017 C 0.8755(6) 0.8937(7) 0.7028(7) 0.146(4) Uani 1 1 d . U . . .
H01M H 0.8605 0.9311 0.6846 0.219 Uiso 1 1 calc GR . . . .
H01N H 0.9264 0.9044 0.6837 0.219 Uiso 1 1 calc GR . . . .
H01O H 0.8810 0.9002 0.7507 0.219 Uiso 1 1 calc GR . . . .
C018 C 0.7311(9) 0.6463(7) 0.9428(4) 0.169(4) Uani 1 1 d . U . . .
H01P H 0.7234 0.6002 0.9171 0.253 Uiso 1 1 calc GR . . . .
H01Q H 0.6980 0.6278 0.9825 0.253 Uiso 1 1 calc GR . . . .
H01R H 0.7873 0.6785 0.9554 0.253 Uiso 1 1 calc GR . . . .
C2 C 0.7743(8) 1.0021(7) 0.8143(8) 0.155(3) Uani 1 1 d . U . . .
C5 C 0.7098(9) 1.0108(8) 0.8502(9) 0.194(4) Uani 1 1 d . U . . .
H5A H 0.6639 0.9941 0.8210 0.291 Uiso 1 1 calc GR . . . .
H5B H 0.7310 1.0666 0.8628 0.291 Uiso 1 1 calc GR . . . .
H5C H 0.6933 0.9773 0.8896 0.291 Uiso 1 1 calc GR . . . .
C15 C 0.8355(10) 1.0108(9) 0.8697(10) 0.200(5) Uani 1 1 d . U . . .
C3 C 0.8009(6) 0.5619(7) 0.7145(6) 0.137(4) Uani 1 1 d . U . . .
H3A H 0.8067 0.5167 0.7003 0.205 Uiso 1 1 calc GR . . . .
H3B H 0.7975 0.5620 0.7626 0.205 Uiso 1 1 calc GR . . . .
H3C H 0.8471 0.6117 0.6998 0.205 Uiso 1 1 calc GR . . . .


_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
Cu01 Cl05 2.359(2) . ?
Cu01 N00H 2.030(4) . ?
Cu01 N00H 2.030(4) 2_665 ?
Cu01 N00H 2.030(4) 3_565 ?
Ti02 Ti03 3.0837(14) . ?
Ti02 O007 1.981(4) 3_565 ?
Ti02 O008 1.918(3) . ?
Ti02 O009 1.945(4) . ?
Ti02 O00A 2.165(3) . ?
Ti02 O00B 1.763(3) . ?
Ti02 O00C 1.973(4) . ?
Ti03 Ti04 3.1210(16) . ?
Ti03 O008 2.026(4) . ?
Ti03 O00C 2.014(3) . ?
Ti03 O00E 2.195(3) . ?
Ti03 O00F 1.795(4) . ?
Ti03 O00G 1.995(4) . ?
Ti03 O00I 1.778(5) . ?
Ti04 O008 1.901(3) . ?
Ti04 O00D 1.971(4) . ?
Ti04 O00G 1.984(5) . ?
Ti04 O00O 1.775(5) . ?
Ti04 O00Q 1.745(6) . ?
P06 O007 1.504(4) . ?
P06 O009 1.513(4) . ?
P06 O00D 1.518(4) . ?
O007 Ti02 1.981(4) 2_665 ?
O00A C00K 1.274(6) . ?
O00B C00T 1.429(8) . ?
O00C C00S 1.459(8) . ?
O00E C00K 1.240(7) . ?
O00F C012 1.408(9) . ?
O00G C010 1.438(10) . ?
N00H C00J 1.339(6) . ?
N00H C00P 1.349(7) . ?
O00I C00X 1.451(10) . ?
C00J H00J 0.9300 . ?
C00J C00L 1.381(8) . ?
C00K C00L 1.519(6) . ?
C00L C00N 1.369(8) . ?
C00M H00M 0.9300 . ?
C00M C00N 1.397(7) . ?
C00M C00P 1.374(8) . ?
C00N H00N 0.9300 . ?
O00O C00V 1.406(9) . ?
C00P H00P 0.9300 . ?
O00Q C2 1.546(13) . ?
C00R H00A 0.9600 . ?
C00R H00B 0.9600 . ?
C00R H00C 0.9600 . ?
C00R C00S 1.504(9) . ?
C00S H00S 0.9800 . ?
C00S C011 1.394(11) . ?
C00T H00T 0.9800 . ?
C00T C00Y 1.560(11) . ?
C00T C013 1.478(10) . ?
C00U H00D 0.9600 . ?
C00U H00E 0.9600 . ?
C00U H00F 0.9600 . ?
C00U C00X 1.402(11) . ?
C00V H00V 0.9800 . ?
C00V C00Z 1.538(10) . ?
C00V C015 1.448(10) . ?
C00W H00G 0.9600 . ?
C00W H00H 0.9600 . ?
C00W H00I 0.9600 . ?
C00W C010 1.552(15) . ?
C00X H00X 0.9800 . ?
C00X C3 1.544(15) . ?
C00Y H00K 0.9600 . ?
C00Y H00L 0.9600 . ?
C00Y H00O 0.9600 . ?
C00Z H00Q 0.9600 . ?
C00Z H00R 0.9600 . ?
C00Z H00U 0.9600 . ?
C010 H010 0.9800 . ?
C010 C017 1.389(14) . ?
C011 H01A 0.9600 . ?
C011 H01B 0.9600 . ?
C011 H01C 0.9600 . ?
C012 H012 0.9800 . ?
C012 C016 1.546(13) . ?
C012 C018 1.483(18) . ?
C013 H01D 0.9600 . ?
C013 H01E 0.9600 . ?
C013 H01F 0.9600 . ?
C015 H01G 0.9600 . ?
C015 H01H 0.9600 . ?
C015 H01I 0.9600 . ?
C016 H01J 0.9600 . ?
C016 H01K 0.9600 . ?
C016 H01L 0.9600 . ?
C017 H01M 0.9600 . ?
C017 H01N 0.9600 . ?
C017 H01O 0.9600 . ?
C018 H01P 0.9600 . ?
C018 H01Q 0.9600 . ?
C018 H01R 0.9600 . ?
C2 C5 1.50(2) . ?
C2 C15 1.55(2) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N00H Cu01 Cl05 105.54(10) 2_665 . ?
N00H Cu01 Cl05 105.54(10) 3_565 . ?
N00H Cu01 Cl05 105.54(10) . . ?
N00H Cu01 N00H 113.10(9) 2_665 3_565 ?
N00H Cu01 N00H 113.10(9) 3_565 . ?
N00H Cu01 N00H 113.10(9) 2_665 . ?
O007 Ti02 Ti03 130.87(10) 3_565 . ?
O007 Ti02 O00A 80.87(12) 3_565 . ?
O008 Ti02 Ti03 39.83(12) . . ?
O008 Ti02 O007 163.93(14) . 3_565 ?
O008 Ti02 O009 91.66(15) . . ?
O008 Ti02 O00A 84.11(12) . . ?
O008 Ti02 O00C 79.46(15) . . ?
O009 Ti02 Ti03 130.00(9) . . ?
O009 Ti02 O007 92.22(13) . 3_565 ?
O009 Ti02 O00A 83.32(15) . . ?
O009 Ti02 O00C 166.88(14) . . ?
O00A Ti02 Ti03 80.79(10) . . ?
O00B Ti02 Ti03 106.29(14) . . ?
O00B Ti02 O007 92.97(14) . 3_565 ?
O00B Ti02 O008 102.38(14) . . ?
O00B Ti02 O009 93.10(17) . . ?
O00B Ti02 O00A 172.72(16) . . ?
O00B Ti02 O00C 98.19(18) . . ?
O00C Ti02 Ti03 39.81(9) . . ?
O00C Ti02 O007 93.82(13) . 3_565 ?
O00C Ti02 O00A 86.16(15) . . ?
Ti02 Ti03 Ti04 71.76(3) . . ?
O008 Ti03 Ti02 37.32(8) . . ?
O008 Ti03 Ti04 35.99(8) . . ?
O008 Ti03 O00E 82.32(15) . . ?
O00C Ti03 Ti02 38.86(12) . . ?
O00C Ti03 Ti04 110.39(13) . . ?
O00C Ti03 O008 76.02(15) . . ?
O00C Ti03 O00E 81.61(13) . . ?
O00E Ti03 Ti02 77.08(10) . . ?
O00E Ti03 Ti04 77.53(12) . . ?
O00F Ti03 Ti02 100.74(14) . . ?
O00F Ti03 Ti04 101.63(14) . . ?
O00F Ti03 O008 95.81(18) . . ?
O00F Ti03 O00C 96.85(15) . . ?
O00F Ti03 O00E 177.81(18) . . ?
O00F Ti03 O00G 97.21(16) . . ?
O00G Ti03 Ti02 109.87(13) . . ?
O00G Ti03 Ti04 38.22(13) . . ?
O00G Ti03 O008 73.92(15) . . ?
O00G Ti03 O00C 147.87(18) . . ?
O00G Ti03 O00E 83.38(15) . . ?
O00I Ti03 Ti02 138.84(12) . . ?
O00I Ti03 Ti04 139.26(15) . . ?
O00I Ti03 O008 166.83(18) . . ?
O00I Ti03 O00C 102.60(17) . . ?
O00I Ti03 O00E 84.52(19) . . ?
O00I Ti03 O00F 97.4(2) . . ?
O00I Ti03 O00G 104.05(19) . . ?
O008 Ti04 Ti03 38.77(12) . . ?
O008 Ti04 O00D 87.84(16) . . ?
O008 Ti04 O00G 76.94(16) . . ?
O00D Ti04 Ti03 123.17(11) . . ?
O00D Ti04 O00G 157.28(15) . . ?
O00G Ti04 Ti03 38.46(10) . . ?
O00O Ti04 Ti03 117.3(2) . . ?
O00O Ti04 O008 139.1(2) . . ?
O00O Ti04 O00D 88.7(2) . . ?
O00O Ti04 O00G 91.9(2) . . ?
O00Q Ti04 Ti03 114.6(2) . . ?
O00Q Ti04 O008 110.5(2) . . ?
O00Q Ti04 O00D 99.0(3) . . ?
O00Q Ti04 O00G 102.1(3) . . ?
O00Q Ti04 O00O 110.3(3) . . ?
O007 P06 O009 112.4(2) . . ?
O007 P06 O00D 110.4(2) . . ?
O009 P06 O00D 112.1(2) . . ?
P06 O007 Ti02 140.8(2) . 2_665 ?
Ti02 O008 Ti03 102.85(16) . . ?
Ti04 O008 Ti02 144.5(2) . . ?
Ti04 O008 Ti03 105.24(15) . . ?
P06 O009 Ti02 133.7(2) . . ?
C00K O00A Ti02 125.4(3) . . ?
C00T O00B Ti02 141.9(4) . . ?
Ti02 O00C Ti03 101.33(16) . . ?
C00S O00C Ti02 133.5(4) . . ?
C00S O00C Ti03 125.2(4) . . ?
P06 O00D Ti04 142.1(3) . . ?
C00K O00E Ti03 129.8(3) . . ?
C012 O00F Ti03 138.7(6) . . ?
Ti04 O00G Ti03 103.31(17) . . ?
C010 O00G Ti03 123.0(6) . . ?
C010 O00G Ti04 133.3(6) . . ?
C00J N00H Cu01 122.0(4) . . ?
C00J N00H C00P 118.3(5) . . ?
C00P N00H Cu01 119.3(3) . . ?
C00X O00I Ti03 163.0(4) . . ?
N00H C00J H00J 119.0 . . ?
N00H C00J C00L 122.1(5) . . ?
C00L C00J H00J 119.0 . . ?
O00A C00K C00L 115.9(5) . . ?
O00E C00K O00A 126.8(4) . . ?
O00E C00K C00L 117.2(4) . . ?
C00J C00L C00K 119.7(5) . . ?
C00N C00L C00J 120.5(4) . . ?
C00N C00L C00K 119.7(5) . . ?
C00N C00M H00M 119.9 . . ?
C00P C00M H00M 119.9 . . ?
C00P C00M C00N 120.3(5) . . ?
C00L C00N C00M 117.0(5) . . ?
C00L C00N H00N 121.5 . . ?
C00M C00N H00N 121.5 . . ?
C00V O00O Ti04 143.9(5) . . ?
N00H C00P C00M 121.7(4) . . ?
N00H C00P H00P 119.1 . . ?
C00M C00P H00P 119.1 . . ?
C2 O00Q Ti04 141.4(7) . . ?
H00A C00R H00B 109.5 . . ?
H00A C00R H00C 109.5 . . ?
H00B C00R H00C 109.5 . . ?
C00S C00R H00A 109.5 . . ?
C00S C00R H00B 109.5 . . ?
C00S C00R H00C 109.5 . . ?
O00C C00S C00R 107.8(5) . . ?
O00C C00S H00S 104.9 . . ?
C00R C00S H00S 104.9 . . ?
C011 C00S O00C 111.7(6) . . ?
C011 C00S C00R 121.2(6) . . ?
C011 C00S H00S 104.9 . . ?
O00B C00T H00T 110.4 . . ?
O00B C00T C00Y 108.8(7) . . ?
O00B C00T C013 108.3(7) . . ?
C00Y C00T H00T 110.4 . . ?
C013 C00T H00T 110.4 . . ?
C013 C00T C00Y 108.4(6) . . ?
H00D C00U H00E 109.5 . . ?
H00D C00U H00F 109.5 . . ?
H00E C00U H00F 109.5 . . ?
C00X C00U H00D 109.5 . . ?
C00X C00U H00E 109.5 . . ?
C00X C00U H00F 109.5 . . ?
O00O C00V H00V 106.4 . . ?
O00O C00V C00Z 110.1(6) . . ?
O00O C00V C015 110.1(7) . . ?
C00Z C00V H00V 106.4 . . ?
C015 C00V H00V 106.4 . . ?
C015 C00V C00Z 116.7(6) . . ?
H00G C00W H00H 109.5 . . ?
H00G C00W H00I 109.5 . . ?
H00H C00W H00I 109.5 . . ?
C010 C00W H00G 109.5 . . ?
C010 C00W H00H 109.5 . . ?
C010 C00W H00I 109.5 . . ?
O00I C00X H00X 107.7 . . ?
O00I C00X C3 106.2(7) . . ?
C00U C00X O00I 108.0(7) . . ?
C00U C00X H00X 107.7 . . ?
C00U C00X C3 119.0(8) . . ?
C3 C00X H00X 107.7 . . ?
C00T C00Y H00K 109.5 . . ?
C00T C00Y H00L 109.5 . . ?
C00T C00Y H00O 109.5 . . ?
H00K C00Y H00L 109.5 . . ?
H00K C00Y H00O 109.5 . . ?
H00L C00Y H00O 109.5 . . ?
C00V C00Z H00Q 109.5 . . ?
C00V C00Z H00R 109.5 . . ?
C00V C00Z H00U 109.5 . . ?
H00Q C00Z H00R 109.5 . . ?
H00Q C00Z H00U 109.5 . . ?
H00R C00Z H00U 109.5 . . ?
O00G C010 C00W 109.9(7) . . ?
O00G C010 H010 105.7 . . ?
C00W C010 H010 105.7 . . ?
C017 C010 O00G 114.7(11) . . ?
C017 C010 C00W 114.2(9) . . ?
C017 C010 H010 105.7 . . ?
C00S C011 H01A 109.5 . . ?
C00S C011 H01B 109.5 . . ?
C00S C011 H01C 109.5 . . ?
H01A C011 H01B 109.5 . . ?
H01A C011 H01C 109.5 . . ?
H01B C011 H01C 109.5 . . ?
O00F C012 H012 111.1 . . ?
O00F C012 C016 106.8(7) . . ?
O00F C012 C018 107.4(10) . . ?
C016 C012 H012 111.1 . . ?
C018 C012 H012 111.1 . . ?
C018 C012 C016 109.3(9) . . ?
C00T C013 H01D 109.5 . . ?
C00T C013 H01E 109.5 . . ?
C00T C013 H01F 109.5 . . ?
H01D C013 H01E 109.5 . . ?
H01D C013 H01F 109.5 . . ?
H01E C013 H01F 109.5 . . ?
C00V C015 H01G 109.5 . . ?
C00V C015 H01H 109.5 . . ?
C00V C015 H01I 109.5 . . ?
H01G C015 H01H 109.5 . . ?
H01G C015 H01I 109.5 . . ?
H01H C015 H01I 109.5 . . ?
C012 C016 H01J 109.5 . . ?
C012 C016 H01K 109.5 . . ?
C012 C016 H01L 109.5 . . ?
H01J C016 H01K 109.5 . . ?
H01J C016 H01L 109.5 . . ?
H01K C016 H01L 109.5 . . ?
C010 C017 H01M 109.5 . . ?
C010 C017 H01N 109.5 . . ?
C010 C017 H01O 109.5 . . ?
H01M C017 H01N 109.5 . . ?
H01M C017 H01O 109.5 . . ?
H01N C017 H01O 109.5 . . ?
C012 C018 H01P 109.5 . . ?
C012 C018 H01Q 109.5 . . ?
C012 C018 H01R 109.5 . . ?
H01P C018 H01Q 109.5 . . ?
H01P C018 H01R 109.5 . . ?
H01Q C018 H01R 109.5 . . ?
C5 C2 O00Q 100.6(9) . . ?
C5 C2 C15 105.0(14) . . ?
C15 C2 O00Q 101.3(11) . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C00X C3 H3A 109.5 . . ?
C00X C3 H3B 109.5 . . ?
C00X C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.131
_oxdiff_exptl_absorpt_empirical_full_min 0.663

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 0.000 182 29 ' '
2 0.000 0.000 0.500 116 15 ' '
3 0.333 0.667 0.148 122 38 ' '
4 0.333 0.667 0.682 7 1 ' '
5 0.667 0.333 0.852 122 38 ' '
6 0.667 0.333 0.318 7 1 ' '
_platon_squeeze_details          
;
;
