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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_earlyy2
_database_code_depnum_ccdc_archive 'CCDC 1905879'
loop_
_audit_author_name
_audit_author_address
'Kelly E Aldrich'
;Michigan State University
United States of America
;
_audit_update_record             
;
2019-03-27 deposited with the CCDC.	2019-05-07 downloaded from the CCDC.
;
_audit_creation_date             2019-03-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H19 N3 Ti'
_chemical_formula_sum            'C18 H19 N3 Ti'
_chemical_formula_weight         325.26
_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 0.0181 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'
N N 0.0311 0.0180 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.7583(3)
_cell_length_b                   9.5204(4)
_cell_length_c                   11.4421(4)
_cell_angle_alpha                70.673(2)
_cell_angle_beta                 88.342(3)
_cell_angle_gamma                84.629(3)
_cell_volume                     794.01(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4939
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      70.01
_cell_measurement_theta_min      4.09
_shelx_estimated_absorpt_T_max   0.605
_shelx_estimated_absorpt_T_min   0.276
_exptl_absorpt_coefficient_mu    4.546
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.4906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0828 before and 0.0535 after correction. The Ratio of minimum to maximum transmission is 0.6513. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.381
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.123
_exptl_special_details           
;
Data was collected using a BRUKER CCD (charge coupled device) based
diffractometer equipped with an Oxford low-temperature apparatus operating at
173 K.  A suitable crystal was chosen and mounted on a nylon loop using 
Paratone oil.  Data  were measured using omega and phi scans of 1.0° per frame 
for 30 s. The total number of images were based on 
results from the program COSMO where redundancy was expected to be 4 and 
completeness to 0.83Å to 100%. Cell parameters were
retrieved using APEX II software and refined using SAINT on all observed
reflections.Data reduction was performed using the SAINT software which 
corrects for Lp. Scaling and absorption corrections were applied using SADABS6 
multi-scan technique, supplied by George Sheldrick.  The structure was solved 
by the direct method using the SHELXT program and refined by least squares 
method on F2, SHELXL, incorporated in OLEX2. 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0877
_diffrn_reflns_av_unetI/netI     0.0758
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6753
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.373
_diffrn_reflns_theta_min         4.094
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean 8.36
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2244
_reflns_number_total             2787
_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       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         2787
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0613
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1004P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1524
_refine_ls_wR_factor_ref         0.1600
_refine_special_details          
;
The structure was refined by Least Squares using version 2018/3 
of XL (Sheldrick, 2015) incorporated in Olex2 (Dolomanov et al., 2009). 
All non-hydrogen atoms were refined anisotropically. 
Hydrogen atom positions were calculated geometrically and refined using the 
riding model, except for the hydrogen atom(s) on the non-carbon atom(s) 
which was found by difference Fourier methods and refined isotropically.
;
_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.a Ternary CH refined with riding coordinates:
 C007(H007), C00B(H00B), C00G(H00G)
2.b Aromatic/amide H refined with riding coordinates:
 C008(H008), C009(H009), C00E(H00E), C00H(H00H), C00I(H00I), C00J(H00J),
 C00K(H00K)
2.c Idealised Me refined as rotating group:
 C00D(H00A,H00C,H00D), C00L(H00F,H00L,H00M), C00M(H00N,H00O,H00P)
;
_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
Ti01 Ti 0.49120(8) 0.57642(6) 0.58642(5) 0.0297(2) Uani 1 1 d . . . . .
N002 N 0.4260(4) 0.3912(3) 0.5808(3) 0.0326(6) Uani 1 1 d . . . . .
N003 N 0.6971(4) 0.5304(3) 0.6965(3) 0.0369(7) Uani 1 1 d . . . . .
C004 C 0.7189(5) 0.5970(4) 0.7853(3) 0.0343(8) Uani 1 1 d . . . . .
N005 N 0.4236(5) 0.8231(4) 0.5817(3) 0.0430(8) Uani 1 1 d . . . . .
C006 C 0.3453(4) 0.2702(4) 0.6619(3) 0.0304(7) Uani 1 1 d . . . . .
C007 C 0.3163(5) 0.6342(4) 0.7362(3) 0.0348(8) Uani 1 1 d . . . . .
H007 H 0.293691 0.564836 0.821229 0.042 Uiso 1 1 calc R . . . .
C008 C 0.3841(5) 0.2172(4) 0.7885(3) 0.0332(7) Uani 1 1 d . . . . .
H008 H 0.465002 0.264314 0.820433 0.040 Uiso 1 1 calc R . . . .
C009 C 0.3060(5) 0.0971(4) 0.8674(3) 0.0375(8) Uani 1 1 d . . . . .
H009 H 0.334294 0.063313 0.953083 0.045 Uiso 1 1 calc R . . . .
C00A C 0.4414(5) 0.7334(4) 0.7046(3) 0.0338(8) Uani 1 1 d . . . . .
C00B C 0.2124(5) 0.6633(4) 0.6329(4) 0.0413(9) Uani 1 1 d . . . . .
H00B H 0.102669 0.617324 0.629751 0.050 Uiso 1 1 calc R . . . .
C00C C 0.1884(5) 0.0250(4) 0.8257(4) 0.0386(8) Uani 1 1 d . . . . .
C00D C 0.5378(6) 0.7126(5) 0.9186(4) 0.0470(10) Uani 1 1 d . . . . .
H00A H 0.471873 0.624842 0.950684 0.071 Uiso 1 1 calc GR . . . .
H00C H 0.464702 0.802048 0.919353 0.071 Uiso 1 1 calc GR . . . .
H00D H 0.639867 0.699764 0.970847 0.071 Uiso 1 1 calc GR . . . .
C00E C 0.1514(5) 0.0769(4) 0.6995(4) 0.0413(9) Uani 1 1 d . . . . .
H00E H 0.072526 0.027892 0.667760 0.050 Uiso 1 1 calc R . . . .
C00F C 0.5956(5) 0.7302(4) 0.7852(3) 0.0353(8) Uani 1 1 d . . . . .
C00G C 0.2777(5) 0.7788(4) 0.5389(4) 0.0381(8) Uani 1 1 d . . . . .
H00G H 0.222890 0.828958 0.455681 0.046 Uiso 1 1 calc R . . . .
C00H C 0.2264(5) 0.1975(4) 0.6199(3) 0.0380(8) Uani 1 1 d . . . . .
H00H H 0.196297 0.231707 0.534509 0.046 Uiso 1 1 calc R . . . .
C00I C 0.9301(5) 0.4127(5) 0.8098(4) 0.0467(9) Uani 1 1 d . . . . .
H00I H 1.029076 0.345300 0.841301 0.056 Uiso 1 1 calc R . . . .
C00J C 0.8303(5) 0.4161(4) 0.7146(4) 0.0420(9) Uani 1 1 d . . . . .
H00J H 0.847792 0.350905 0.667159 0.050 Uiso 1 1 calc R . . . .
C00K C 0.8607(6) 0.5280(5) 0.8546(4) 0.0479(10) Uani 1 1 d . . . . .
H00K H 0.905283 0.552571 0.921126 0.057 Uiso 1 1 calc R . . . .
C00L C 0.1071(6) -0.1094(5) 0.9129(4) 0.0528(11) Uani 1 1 d . . . . .
H00F H 0.168998 -0.144474 0.992252 0.079 Uiso 1 1 calc GR . . . .
H00L H 0.114415 -0.189516 0.876461 0.079 Uiso 1 1 calc GR . . . .
H00M H -0.014627 -0.081017 0.926464 0.079 Uiso 1 1 calc GR . . . .
C00M C 0.6840(6) 0.8752(4) 0.7311(4) 0.0485(10) Uani 1 1 d . . . . .
H00N H 0.781911 0.873632 0.783887 0.073 Uiso 1 1 calc GR . . . .
H00O H 0.600801 0.960706 0.727194 0.073 Uiso 1 1 calc GR . . . .
H00P H 0.725947 0.884169 0.647508 0.073 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
Ti01 Ti01 2.8105(11) 2_666 ?
Ti01 N002 1.935(3) 2_666 ?
Ti01 N002 1.901(3) . ?
Ti01 N003 1.988(3) . ?
Ti01 N005 2.341(3) . ?
Ti01 C007 2.331(4) . ?
Ti01 C00A 2.326(3) . ?
Ti01 C00B 2.353(4) . ?
Ti01 C00G 2.348(4) . ?
N002 C006 1.405(4) . ?
N003 C004 1.386(5) . ?
N003 C00J 1.395(5) . ?
C004 C00F 1.514(5) . ?
C004 C00K 1.357(6) . ?
N005 C00A 1.386(5) . ?
N005 C00G 1.399(5) . ?
C006 C008 1.399(5) . ?
C006 C00H 1.388(5) . ?
C007 C00A 1.374(5) . ?
C007 C00B 1.386(6) . ?
C008 C009 1.380(5) . ?
C009 C00C 1.376(5) . ?
C00A C00F 1.523(5) . ?
C00B C00G 1.382(6) . ?
C00C C00E 1.391(6) . ?
C00C C00L 1.517(5) . ?
C00D C00F 1.538(5) . ?
C00E C00H 1.375(5) . ?
C00F C00M 1.532(5) . ?
C00I C00J 1.344(6) . ?
C00I C00K 1.415(6) . ?

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
N002 Ti01 Ti01 42.41(8) 2_666 2_666 ?
N002 Ti01 Ti01 43.36(9) . 2_666 ?
N002 Ti01 N002 85.77(12) . 2_666 ?
N002 Ti01 N003 107.50(13) 2_666 . ?
N002 Ti01 N003 107.04(13) . . ?
N002 Ti01 N005 151.56(13) . . ?
N002 Ti01 N005 100.80(12) 2_666 . ?
N002 Ti01 C007 106.13(12) . . ?
N002 Ti01 C007 154.04(13) 2_666 . ?
N002 Ti01 C00A 139.72(13) . . ?
N002 Ti01 C00A 132.81(12) 2_666 . ?
N002 Ti01 C00B 95.29(13) . . ?
N002 Ti01 C00B 123.38(14) 2_666 . ?
N002 Ti01 C00G 97.04(13) 2_666 . ?
N002 Ti01 C00G 117.40(13) . . ?
N003 Ti01 Ti01 113.90(9) . 2_666 ?
N003 Ti01 N005 97.39(12) . . ?
N003 Ti01 C007 91.28(13) . . ?
N003 Ti01 C00A 75.67(13) . . ?
N003 Ti01 C00B 125.62(13) . . ?
N003 Ti01 C00G 130.38(12) . . ?
N005 Ti01 Ti01 136.36(9) . 2_666 ?
N005 Ti01 C00B 57.90(13) . . ?
N005 Ti01 C00G 34.72(12) . . ?
C007 Ti01 Ti01 143.79(9) . 2_666 ?
C007 Ti01 N005 58.08(12) . . ?
C007 Ti01 C00B 34.42(14) . . ?
C007 Ti01 C00G 57.01(13) . . ?
C00A Ti01 Ti01 169.69(10) . 2_666 ?
C00A Ti01 N005 34.55(12) . . ?
C00A Ti01 C007 34.33(13) . . ?
C00A Ti01 C00B 56.74(13) . . ?
C00A Ti01 C00G 56.47(13) . . ?
C00B Ti01 Ti01 116.18(10) . 2_666 ?
C00G Ti01 Ti01 113.30(10) . 2_666 ?
C00G Ti01 C00B 34.21(14) . . ?
Ti01 N002 Ti01 94.23(12) . 2_666 ?
C006 N002 Ti01 129.9(2) . 2_666 ?
C006 N002 Ti01 135.9(2) . . ?
C004 N003 Ti01 123.7(3) . . ?
C004 N003 C00J 106.6(3) . . ?
C00J N003 Ti01 129.1(2) . . ?
N003 C004 C00F 118.6(3) . . ?
C00K C004 N003 108.9(3) . . ?
C00K C004 C00F 132.4(3) . . ?
C00A N005 Ti01 72.13(19) . . ?
C00A N005 C00G 105.1(3) . . ?
C00G N005 Ti01 72.90(19) . . ?
C008 C006 N002 120.9(3) . . ?
C00H C006 N002 121.6(3) . . ?
C00H C006 C008 117.5(3) . . ?
C00A C007 Ti01 72.7(2) . . ?
C00A C007 C00B 107.3(3) . . ?
C00B C007 Ti01 73.7(2) . . ?
C009 C008 C006 120.6(3) . . ?
C00C C009 C008 121.9(3) . . ?
N005 C00A Ti01 73.32(19) . . ?
N005 C00A C00F 123.6(3) . . ?
C007 C00A Ti01 73.0(2) . . ?
C007 C00A N005 110.5(3) . . ?
C007 C00A C00F 125.2(3) . . ?
C00F C00A Ti01 113.0(2) . . ?
C007 C00B Ti01 71.9(2) . . ?
C00G C00B Ti01 72.7(2) . . ?
C00G C00B C007 107.5(3) . . ?
C009 C00C C00E 117.4(3) . . ?
C009 C00C C00L 121.3(4) . . ?
C00E C00C C00L 121.3(4) . . ?
C00H C00E C00C 121.5(3) . . ?
C004 C00F C00A 107.1(3) . . ?
C004 C00F C00D 109.4(3) . . ?
C004 C00F C00M 110.4(3) . . ?
C00A C00F C00D 110.8(3) . . ?
C00A C00F C00M 109.7(3) . . ?
C00M C00F C00D 109.4(3) . . ?
N005 C00G Ti01 72.4(2) . . ?
C00B C00G Ti01 73.1(2) . . ?
C00B C00G N005 109.5(3) . . ?
C00E C00H C006 121.2(4) . . ?
C00J C00I C00K 107.5(4) . . ?
C00I C00J N003 109.4(3) . . ?
C004 C00K C00I 107.6(4) . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'


# start Validation Reply Form
_vrf_PLAT029_earlyy2             
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.957 Why?
RESPONSE: This is low due to the three circle geometry combined with 
the requested 
and integrated data out 0.81 Angstroms using Copper radiation.  
This results in 
lower reported measured fraction, but when calculated the value 
tends to be 
higher than 97% collected.  Occasionally falling to 96% for
 triiclinic systems.  
;
# end Validation Reply Form


####################################################################### 
# 
# 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_finalka
_database_code_depnum_ccdc_archive 'CCDC 1905882'
loop_
_audit_author_name
_audit_author_address
'Kelly E Aldrich'
;Michigan State University
United States of America
;
_audit_update_record             
;
2019-03-27 deposited with the CCDC.	2019-05-07 downloaded from the CCDC.
;
_audit_creation_date             2019-03-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C40 H52 O4 Ti'
_chemical_formula_sum            'C40 H52 O4 Ti'
_chemical_formula_weight         644.71
_chemical_absolute_configuration ?
_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 0.0181 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'
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      tetragonal
_space_group_IT_number           114
_space_group_name_H-M_alt        'P -4 21 c'
_space_group_name_Hall           'P -4 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   15.2024(18)
_cell_length_b                   15.2024(18)
_cell_length_c                   7.9195(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1830.3(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1979
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      70.61
_cell_measurement_theta_min      5.82
_shelx_estimated_absorpt_T_max   0.859
_shelx_estimated_absorpt_T_min   0.644
_exptl_absorpt_coefficient_mu    2.267
_exptl_absorpt_correction_T_max  0.7535
_exptl_absorpt_correction_T_min  0.5640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1013 before and 0.0689 after correction. The Ratio of minimum to maximum transmission is 0.7485. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.069
_exptl_special_details           
;
Data was collected using a BRUKER CCD (charge coupled device) based
diffractometer equipped with an Oxford low-temperature apparatus operating at
173 K.  A suitable crystal was chosen and mounted on a nylon loop using 
Paratone oil.  Data  were measured using omega and phi scans of 1.0° per frame 
for 30 s. The total number of images were based on 
results from the program COSMO where redundancy was expected to be 4 and 
completeness to 0.83Å to 100%. Cell parameters were
retrieved using APEX II software and refined using SAINT on all observed
reflections.Data reduction was performed using the SAINT software which 
corrects for Lp. Scaling and absorption corrections were applied using SADABS6 
multi-scan technique, supplied by George Sheldrick.  The structure was solved 
by the direct method using the SHELXT program and refined by least squares 
method on F2, SHELXL, incorporated in OLEX2. 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_unetI/netI     0.0837
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6299
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.308
_diffrn_reflns_theta_min         4.112
_diffrn_ambient_temperature      173.02
_diffrn_detector_area_resol_mean 8.36
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.685
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.913
_reflns_number_gt                1284
_reflns_number_total             1680
_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       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 
;
 Flack x determined using 445 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.030(13)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         1680
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0515
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+1.5714P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1263
_refine_special_details          
;
The structure was refined by Least Squares using version 2018/3 
of XL (Sheldrick, 2015) incorporated in Olex2 (Dolomanov et al., 2009). 
All non-hydrogen atoms were refined anisotropically. 
Hydrogen atom positions were calculated geometrically and refined using the 
riding model, except for the hydrogen atom(s) on the non-carbon atom(s) 
which was found by difference Fourier methods and refined isotropically.
;
_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.a Aromatic/amide H refined with riding coordinates:
 C005(H005), C007(H007), C009(H009), C00B(H00G)
2.b Idealised Me refined as rotating group:
 C008(H00A,H00B,H00C), C00A(H00D,H00E,H00F), C00C(H00H,H00I,H00J)
;
_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
Ti01 Ti 0.5000 0.5000 0.5000 0.0246(4) Uani 1 4 d S T P . .
O002 O 0.4027(2) 0.4939(3) 0.3724(4) 0.0363(9) Uani 1 1 d . . . . .
C003 C 0.3444(3) 0.5316(3) 0.2621(7) 0.0268(12) Uani 1 1 d . . . . .
C004 C 0.2530(3) 0.5194(3) 0.2849(6) 0.0258(12) Uani 1 1 d . . . . .
C005 C 0.2008(4) 0.5608(4) 0.1656(7) 0.0362(14) Uani 1 1 d . . . . .
H005 H 0.1388 0.5554 0.1758 0.043 Uiso 1 1 calc R . . . .
C006 C 0.2154(4) 0.4648(4) 0.4317(7) 0.0325(13) Uani 1 1 d . . . . .
C007 C 0.3792(4) 0.5809(4) 0.1288(8) 0.0376(15) Uani 1 1 d . . . . .
H007 H 0.4410 0.5872 0.1170 0.045 Uiso 1 1 calc R . . . .
C008 C 0.2413(3) 0.5068(4) 0.6023(6) 0.0351(12) Uani 1 1 d . . . . .
H00A H 0.3054 0.5054 0.6149 0.053 Uiso 1 1 calc GR . . . .
H00B H 0.2141 0.4736 0.6947 0.053 Uiso 1 1 calc GR . . . .
H00C H 0.2208 0.5679 0.6057 0.053 Uiso 1 1 calc GR . . . .
C009 C 0.3236(4) 0.6201(4) 0.0154(8) 0.0458(15) Uani 1 1 d . . . . .
H009 H 0.3469 0.6544 -0.0744 0.055 Uiso 1 1 calc R . . . .
C00A C 0.2488(4) 0.3695(4) 0.4225(8) 0.0489(17) Uani 1 1 d . . . . .
H00D H 0.2252 0.3411 0.3211 0.073 Uiso 1 1 calc GR . . . .
H00E H 0.2293 0.3373 0.5229 0.073 Uiso 1 1 calc GR . . . .
H00F H 0.3132 0.3694 0.4176 0.073 Uiso 1 1 calc GR . . . .
C00B C 0.2342(5) 0.6098(4) 0.0315(7) 0.0463(16) Uani 1 1 d . . . . .
H00G H 0.1955 0.6359 -0.0482 0.056 Uiso 1 1 calc R . . . .
C00C C 0.1139(4) 0.4626(5) 0.4240(9) 0.0518(19) Uani 1 1 d . . . . .
H00H H 0.0909 0.5226 0.4338 0.078 Uiso 1 1 calc GR . . . .
H00I H 0.0912 0.4268 0.5171 0.078 Uiso 1 1 calc GR . . . .
H00J H 0.0951 0.4371 0.3162 0.078 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
Ti01 O002 1.794(3) 3_566 ?
Ti01 O002 1.794(3) 2_665 ?
Ti01 O002 1.794(3) 4_656 ?
Ti01 O002 1.794(3) . ?
O002 C003 1.370(6) . ?
C003 C004 1.414(7) . ?
C003 C007 1.398(7) . ?
C004 C005 1.384(7) . ?
C004 C006 1.538(7) . ?
C005 C00B 1.393(8) . ?
C006 C008 1.545(7) . ?
C006 C00A 1.537(8) . ?
C006 C00C 1.545(7) . ?
C007 C009 1.369(8) . ?
C009 C00B 1.374(9) . ?

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
O002 Ti01 O002 111.4(2) 3_566 4_656 ?
O002 Ti01 O002 108.50(11) 4_656 . ?
O002 Ti01 O002 108.50(11) 3_566 . ?
O002 Ti01 O002 108.50(11) 3_566 2_665 ?
O002 Ti01 O002 108.50(11) 4_656 2_665 ?
O002 Ti01 O002 111.4(2) 2_665 . ?
C003 O002 Ti01 150.6(4) . . ?
O002 C003 C004 120.0(5) . . ?
O002 C003 C007 117.5(5) . . ?
C007 C003 C004 122.6(5) . . ?
C003 C004 C006 122.2(4) . . ?
C005 C004 C003 114.6(5) . . ?
C005 C004 C006 123.3(5) . . ?
C004 C005 C00B 123.7(6) . . ?
C004 C006 C008 110.2(4) . . ?
C004 C006 C00C 110.7(5) . . ?
C008 C006 C00C 107.3(4) . . ?
C00A C006 C004 110.5(4) . . ?
C00A C006 C008 110.3(5) . . ?
C00A C006 C00C 107.9(5) . . ?
C009 C007 C003 119.7(6) . . ?
C007 C009 C00B 120.0(6) . . ?
C009 C00B C005 119.5(6) . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_uc_a
_database_code_depnum_ccdc_archive 'CCDC 1905883'
loop_
_audit_author_name
_audit_author_address
'Kelly E Aldrich'
;Michigan State University
United States of America
;
_audit_update_record             
;
2019-03-27 deposited with the CCDC.	2019-05-07 downloaded from the CCDC.
;
_audit_creation_date             2019-03-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C56 H84 O4 Ti'
_chemical_formula_sum            'C56 H84 O4 Ti'
_chemical_formula_weight         869.13
_chemical_absolute_configuration ?
_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 0.0181 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'
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      tetragonal
_space_group_IT_number           114
_space_group_name_H-M_alt        'P -4 21 c'
_space_group_name_Hall           'P -4 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   12.3120(3)
_cell_length_b                   12.3120(3)
_cell_length_c                   17.7572(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2691.73(18)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4498
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.22
_cell_measurement_theta_min      4.37
_shelx_estimated_absorpt_T_max   0.734
_shelx_estimated_absorpt_T_min   0.625
_exptl_absorpt_coefficient_mu    1.650
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6280
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0836 before and 0.0680 after correction. The Ratio of minimum to maximum transmission is 0.8339. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
Data was collected using a BRUKER CCD (charge coupled device) based
diffractometer equipped with an Oxford low-temperature apparatus operating at
173 K.  A suitable crystal was chosen and mounted on a nylon loop using 
Paratone oil.  Data  were measured using omega and phi scans of 1.0° per frame 
for 30 s. The total number of images were based on 
results from the program COSMO where redundancy was expected to be 4 and 
completeness to 0.83Å to 100%. Cell parameters were
retrieved using APEX II software and refined using SAINT on all observed
reflections.Data reduction was performed using the SAINT software which 
corrects for Lp. Scaling and absorption corrections were applied using SADABS6 
multi-scan technique, supplied by George Sheldrick.  The structure was solved 
by the direct method using the SHELXT program and refined by least squares 
method on F2, SHELXL, incorporated in OLEX2. 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9725
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.288
_diffrn_reflns_theta_min         3.590
_diffrn_ambient_temperature      172.99
_diffrn_detector_area_resol_mean 8.36
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.764
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2223
_reflns_number_total             2462
_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       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.132
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details 
;
 Flack x determined using 874 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.013(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2462
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0350
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0388P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0868
_refine_special_details          
;
The structure was refined by Least Squares using version 2018/3 
of XL (Sheldrick, 2015) incorporated in Olex2 (Dolomanov et al., 2009). 
All non-hydrogen atoms were refined anisotropically. 
Hydrogen atom positions were calculated geometrically and refined using the 
riding model, except for the hydrogen atom(s) on the non-carbon atom(s) 
which was found by difference Fourier methods and refined isotropically.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.994(12)
 0.006(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C006(H006), C007(H007), C008(H008)
3.b Idealised Me refined as rotating group:
 C009(H00A,H00B,H00C), C00A(H00D,H00E,H00F), C00D(H00G,H00H,H00I), C00E(H00J,
 H00K,H00L), C00F(H00M,H00N,H00O), C00G(H00P,H00Q,H00R)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
Ti01 Ti 0.5000 0.5000 0.5000 0.0212(2) Uani 1 4 d S T P . .
O002 O 0.55377(16) 0.60487(15) 0.56080(10) 0.0311(4) Uani 1 1 d . . . . .
C003 C 0.5934(2) 0.7087(2) 0.55748(16) 0.0262(6) Uani 1 1 d . . . . .
C004 C 0.6280(2) 0.7617(2) 0.62328(15) 0.0258(6) Uani 1 1 d . . . . .
C005 C 0.6707(2) 0.9217(2) 0.54509(15) 0.0265(6) Uani 1 1 d . . . . .
C006 C 0.6360(2) 0.8659(2) 0.48184(15) 0.0294(6) Uani 1 1 d . . . . .
H006 H 0.6379 0.9002 0.4339 0.035 Uiso 1 1 calc R . . . .
C007 C 0.6658(2) 0.8675(2) 0.61377(15) 0.0266(6) Uani 1 1 d . . . . .
H007 H 0.6900 0.9054 0.6573 0.032 Uiso 1 1 calc R . . . .
C008 C 0.5982(2) 0.7598(2) 0.48822(15) 0.0284(6) Uani 1 1 d . . . . .
H008 H 0.5753 0.7219 0.4444 0.034 Uiso 1 1 calc R . . . .
C009 C 0.6986(3) 0.6051(3) 0.69985(17) 0.0451(8) Uani 1 1 d . . . . .
H00A H 0.6705 0.5528 0.6631 0.068 Uiso 1 1 calc GR . . . .
H00B H 0.6992 0.5719 0.7500 0.068 Uiso 1 1 calc GR . . . .
H00C H 0.7726 0.6262 0.6859 0.068 Uiso 1 1 calc GR . . . .
C00A C 0.6673(3) 0.7814(3) 0.76318(16) 0.0457(8) Uani 1 1 d . . . . .
H00D H 0.7422 0.8031 0.7519 0.069 Uiso 1 1 calc GR . . . .
H00E H 0.6653 0.7430 0.8115 0.069 Uiso 1 1 calc GR . . . .
H00F H 0.6213 0.8462 0.7660 0.069 Uiso 1 1 calc GR . . . .
C00B C 0.7129(2) 1.0389(2) 0.54212(16) 0.0316(6) Uani 1 1 d . . . . .
C00C C 0.6253(2) 0.7063(2) 0.70078(15) 0.0328(6) Uani 1 1 d . . . . .
C00D C 0.8306(2) 1.0418(2) 0.57136(18) 0.0384(7) Uani 1 1 d . . . . .
H00G H 0.8326 1.0148 0.6233 0.058 Uiso 1 1 calc GR . . . .
H00H H 0.8576 1.1167 0.5700 0.058 Uiso 1 1 calc GR . . . .
H00I H 0.8764 0.9959 0.5394 0.058 Uiso 1 1 calc GR . . . .
C00E C 0.6417(2) 1.1113(2) 0.59250(19) 0.0377(7) Uani 1 1 d . . . . .
H00J H 0.5660 1.1070 0.5757 0.057 Uiso 1 1 calc GR . . . .
H00K H 0.6669 1.1867 0.5891 0.057 Uiso 1 1 calc GR . . . .
H00L H 0.6469 1.0864 0.6448 0.057 Uiso 1 1 calc GR . . . .
C00F C 0.7110(3) 1.0852(2) 0.46228(18) 0.0465(8) Uani 1 1 d . . . . .
H00M H 0.7586 1.0418 0.4298 0.070 Uiso 1 1 calc GR . . . .
H00N H 0.7366 1.1606 0.4632 0.070 Uiso 1 1 calc GR . . . .
H00O H 0.6367 1.0828 0.4426 0.070 Uiso 1 1 calc GR . . . .
C00G C 0.5081(3) 0.6742(3) 0.72119(16) 0.0455(7) Uani 1 1 d . . . . .
H00P H 0.4619 0.7390 0.7209 0.068 Uiso 1 1 calc GR . . . .
H00Q H 0.5070 0.6413 0.7714 0.068 Uiso 1 1 calc GR . . . .
H00R H 0.4808 0.6218 0.6842 0.068 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
Ti01 O002 1.8086(18) . ?
Ti01 O002 1.8087(18) 4_656 ?
Ti01 O002 1.8087(18) 3_566 ?
Ti01 O002 1.8087(18) 2_665 ?
O002 C003 1.370(3) . ?
C003 C004 1.404(4) . ?
C003 C008 1.383(4) . ?
C004 C007 1.394(4) . ?
C004 C00C 1.536(4) . ?
C005 C006 1.384(4) . ?
C005 C007 1.391(4) . ?
C005 C00B 1.534(4) . ?
C006 H006 0.9500 . ?
C006 C008 1.392(4) . ?
C007 H007 0.9500 . ?
C008 H008 0.9500 . ?
C009 H00A 0.9800 . ?
C009 H00B 0.9800 . ?
C009 H00C 0.9800 . ?
C009 C00C 1.538(4) . ?
C00A H00D 0.9800 . ?
C00A H00E 0.9800 . ?
C00A H00F 0.9800 . ?
C00A C00C 1.533(4) . ?
C00B C00D 1.539(4) . ?
C00B C00E 1.538(4) . ?
C00B C00F 1.528(4) . ?
C00C C00G 1.540(4) . ?
C00D H00G 0.9800 . ?
C00D H00H 0.9800 . ?
C00D H00I 0.9800 . ?
C00E H00J 0.9800 . ?
C00E H00K 0.9800 . ?
C00E H00L 0.9800 . ?
C00F H00M 0.9800 . ?
C00F H00N 0.9800 . ?
C00F H00O 0.9800 . ?
C00G H00P 0.9800 . ?
C00G H00Q 0.9800 . ?
C00G H00R 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O002 Ti01 O002 110.88(6) . 4_656 ?
O002 Ti01 O002 110.88(6) . 3_566 ?
O002 Ti01 O002 110.88(6) 4_656 2_665 ?
O002 Ti01 O002 110.88(6) 2_665 3_566 ?
O002 Ti01 O002 106.70(12) 4_656 3_566 ?
O002 Ti01 O002 106.70(12) . 2_665 ?
C003 O002 Ti01 140.45(18) . . ?
O002 C003 C004 120.4(2) . . ?
O002 C003 C008 118.5(2) . . ?
C008 C003 C004 121.1(2) . . ?
C003 C004 C00C 122.2(2) . . ?
C007 C004 C003 115.8(2) . . ?
C007 C004 C00C 122.0(2) . . ?
C006 C005 C007 117.4(2) . . ?
C006 C005 C00B 122.9(3) . . ?
C007 C005 C00B 119.7(3) . . ?
C005 C006 H006 119.9 . . ?
C005 C006 C008 120.2(2) . . ?
C008 C006 H006 119.9 . . ?
C004 C007 H007 117.7 . . ?
C005 C007 C004 124.7(2) . . ?
C005 C007 H007 117.7 . . ?
C003 C008 C006 120.9(2) . . ?
C003 C008 H008 119.6 . . ?
C006 C008 H008 119.6 . . ?
H00A C009 H00B 109.5 . . ?
H00A C009 H00C 109.5 . . ?
H00B C009 H00C 109.5 . . ?
C00C C009 H00A 109.5 . . ?
C00C C009 H00B 109.5 . . ?
C00C C009 H00C 109.5 . . ?
H00D C00A H00E 109.5 . . ?
H00D C00A H00F 109.5 . . ?
H00E C00A H00F 109.5 . . ?
C00C C00A H00D 109.5 . . ?
C00C C00A H00E 109.5 . . ?
C00C C00A H00F 109.5 . . ?
C005 C00B C00D 109.2(2) . . ?
C005 C00B C00E 109.4(2) . . ?
C00E C00B C00D 109.1(2) . . ?
C00F C00B C005 112.2(2) . . ?
C00F C00B C00D 108.6(3) . . ?
C00F C00B C00E 108.3(2) . . ?
C004 C00C C009 109.7(2) . . ?
C004 C00C C00G 110.2(2) . . ?
C009 C00C C00G 110.1(3) . . ?
C00A C00C C004 111.9(2) . . ?
C00A C00C C009 107.4(3) . . ?
C00A C00C C00G 107.5(3) . . ?
C00B C00D H00G 109.5 . . ?
C00B C00D H00H 109.5 . . ?
C00B C00D H00I 109.5 . . ?
H00G C00D H00H 109.5 . . ?
H00G C00D H00I 109.5 . . ?
H00H C00D H00I 109.5 . . ?
C00B C00E H00J 109.5 . . ?
C00B C00E H00K 109.5 . . ?
C00B C00E H00L 109.5 . . ?
H00J C00E H00K 109.5 . . ?
H00J C00E H00L 109.5 . . ?
H00K C00E H00L 109.5 . . ?
C00B C00F H00M 109.5 . . ?
C00B C00F H00N 109.5 . . ?
C00B C00F H00O 109.5 . . ?
H00M C00F H00N 109.5 . . ?
H00M C00F H00O 109.5 . . ?
H00N C00F H00O 109.5 . . ?
C00C C00G H00P 109.5 . . ?
C00C C00G H00Q 109.5 . . ?
C00C C00G H00R 109.5 . . ?
H00P C00G H00Q 109.5 . . ?
H00P C00G H00R 109.5 . . ?
H00Q C00G H00R 109.5 . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.994(12)
2 0.006(12)

####################################################################### 
# 
# 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_dk_22may
_database_code_depnum_ccdc_archive 'CCDC 1905887'
loop_
_audit_author_name
_audit_author_address
'Kelly E Aldrich'
;Michigan State University
United States of America
;
_audit_update_record             
;
2019-03-27 deposited with the CCDC.	2019-05-07 downloaded from the CCDC.
;
_audit_creation_date             2019-03-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C40 H48 F4 O4 Ti'
_chemical_formula_sum            'C40 H48 F4 O4 Ti'
_chemical_formula_weight         716.68
_chemical_absolute_configuration ?
_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 0.0181 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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      tetragonal
_space_group_IT_number           114
_space_group_name_H-M_alt        'P -4 21 c'
_space_group_name_Hall           'P -4 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   15.2973(16)
_cell_length_b                   15.2973(16)
_cell_length_c                   8.263(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1933.5(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3953
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      69.55
_cell_measurement_theta_min      4.09
_shelx_estimated_absorpt_T_max   0.772
_shelx_estimated_absorpt_T_min   0.465
_exptl_absorpt_coefficient_mu    2.352
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.5521
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1150 before and 0.0756 after correction. The Ratio of minimum to maximum transmission is 0.7329. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             756
_exptl_crystal_recrystallization_method 'used as received'
_exptl_crystal_size_max          0.384
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.116
_exptl_special_details           
'Data was collected using a BRUKER CCD (charge coupled device) based diffractometer equipped with an Oxford low-temperature apparatus operating at 173 K. A suitable crystal was chosen and mounted on a nylon loop using Paratone oil. Data were measured using omega and phi scans of 1.0° per frame for 30 s. The total number of images were based on results from the program COSMO where redundancy was expected to be 4 and completeness to 0.83Α to 100. Cell parameters were retrieved using APEX II software and refined using SAINT on all observed reflections.Data reduction was performed using the SAINT software which corrects for Lp. Scaling and absorption corrections were applied using SADABS6 multi-scan technique, supplied by George Sheldrick. The structure was solved by the direct method using the SHELXT program and refined by least squares method on F2, SHELXL, incorporated in OLEX2.'
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0818
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8947
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.385
_diffrn_reflns_theta_min         2.889
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'sealed tube'
_reflns_Friedel_coverage         0.741
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.972
_reflns_number_gt                1337
_reflns_number_total             1757
_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       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
'SHELXT (Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8)'
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 
;
 Flack x determined using 445 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.041(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1757
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0756
_refine_ls_restrained_S_all      1.147
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1012P)²+2.9140P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2282
_refine_ls_wR_factor_ref         0.2410
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.28(5)
 0.72(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C7(H7)
3.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_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
Ti1 Ti 0.5000 0.5000 0.0000 0.0411(7) Uani 1 4 d S T P . .
O1 O 0.4035(4) 0.4916(5) 0.1252(7) 0.0546(16) Uani 1 1 d . . . . .
C2 C 0.3844(6) 0.5757(6) 0.3639(12) 0.050(2) Uani 1 1 d . . . . .
H2 H 0.4458 0.5847 0.3667 0.060 Uiso 1 1 calc R . . . .
C3 C 0.2572(5) 0.5122(5) 0.2268(10) 0.0417(19) Uani 1 1 d . . . . .
F4 F 0.1907(5) 0.6331(5) 0.5891(8) 0.096(3) Uani 1 1 d . . . . .
C5 C 0.3485(5) 0.5270(5) 0.2400(11) 0.0405(19) Uani 1 1 d . . . . .
C6 C 0.2074(6) 0.5508(7) 0.3492(13) 0.057(3) Uani 1 1 d . . . . .
H6 H 0.1456 0.5442 0.3472 0.068 Uiso 1 1 calc R . . . .
C7 C 0.3321(7) 0.6123(6) 0.4855(13) 0.063(3) Uani 1 1 d . . . . .
H7 H 0.3567 0.6451 0.5719 0.076 Uiso 1 1 calc R . . . .
C8 C 0.2175(6) 0.4595(6) 0.0858(13) 0.056(3) Uani 1 1 d . . . . .
C9 C 0.2455(7) 0.5986(7) 0.4742(14) 0.064(3) Uani 1 1 d . . . . .
C10 C 0.1164(7) 0.4547(9) 0.0992(16) 0.082(4) Uani 1 1 d . . . . .
H10A H 0.1003 0.4291 0.2038 0.123 Uiso 1 1 calc GR . . . .
H10B H 0.0933 0.4182 0.0116 0.123 Uiso 1 1 calc GR . . . .
H10C H 0.0919 0.5137 0.0909 0.123 Uiso 1 1 calc GR . . . .
C11 C 0.2381(6) 0.5007(8) -0.0820(12) 0.062(2) Uani 1 1 d . . . . .
H11A H 0.2184 0.5616 -0.0833 0.093 Uiso 1 1 calc GR . . . .
H11B H 0.2076 0.4678 -0.1668 0.093 Uiso 1 1 calc GR . . . .
H11C H 0.3012 0.4985 -0.1016 0.093 Uiso 1 1 calc GR . . . .
C12 C 0.2530(8) 0.3643(6) 0.0858(15) 0.075(3) Uani 1 1 d . . . . .
H12A H 0.3170 0.3654 0.0795 0.112 Uiso 1 1 calc GR . . . .
H12B H 0.2295 0.3327 -0.0078 0.112 Uiso 1 1 calc GR . . . .
H12C H 0.2350 0.3348 0.1856 0.112 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
Ti1 O1 1.807(6) . ?
Ti1 O1 1.807(6) 2_565 ?
Ti1 O1 1.807(6) 3_665 ?
Ti1 O1 1.807(6) 4_655 ?
O1 C5 1.378(10) . ?
C2 H2 0.9500 . ?
C2 C5 1.380(12) . ?
C2 C7 1.401(14) . ?
C3 C5 1.419(10) . ?
C3 C6 1.397(13) . ?
C3 C8 1.542(13) . ?
F4 C9 1.373(12) . ?
C6 H6 0.9500 . ?
C6 C9 1.393(15) . ?
C7 H7 0.9500 . ?
C7 C9 1.345(15) . ?
C8 C10 1.552(13) . ?
C8 C11 1.555(14) . ?
C8 C12 1.554(13) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 O1 110.2(4) . 3_665 ?
O1 Ti1 O1 110.2(4) 4_655 2_565 ?
O1 Ti1 O1 109.13(18) . 2_565 ?
O1 Ti1 O1 109.13(18) . 4_655 ?
O1 Ti1 O1 109.13(18) 3_665 4_655 ?
O1 Ti1 O1 109.13(18) 3_665 2_565 ?
C5 O1 Ti1 149.9(6) . . ?
C5 C2 H2 119.3 . . ?
C5 C2 C7 121.4(9) . . ?
C7 C2 H2 119.3 . . ?
C5 C3 C8 122.0(8) . . ?
C6 C3 C5 114.5(8) . . ?
C6 C3 C8 123.6(8) . . ?
O1 C5 C2 118.7(8) . . ?
O1 C5 C3 119.0(8) . . ?
C2 C5 C3 122.3(8) . . ?
C3 C6 H6 119.0 . . ?
C9 C6 C3 122.0(8) . . ?
C9 C6 H6 119.0 . . ?
C2 C7 H7 121.6 . . ?
C9 C7 C2 116.8(10) . . ?
C9 C7 H7 121.6 . . ?
C3 C8 C10 111.3(9) . . ?
C3 C8 C11 112.5(7) . . ?
C3 C8 C12 110.6(8) . . ?
C10 C8 C11 106.5(8) . . ?
C10 C8 C12 107.7(9) . . ?
C12 C8 C11 108.0(10) . . ?
F4 C9 C6 117.4(9) . . ?
C7 C9 F4 119.6(10) . . ?
C7 C9 C6 123.1(10) . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C12 H12A 109.5 . . ?
C8 C12 H12B 109.5 . . ?
C8 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.28(5)
2 0.72(5)

####################################################################### 
# 
# 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_p21_c_a
_database_code_depnum_ccdc_archive 'CCDC 1905881'
loop_
_audit_author_name
_audit_author_address
'Kelly E Aldrich'
;Michigan State University
United States of America
;
_audit_update_record             
;
2019-03-27 deposited with the CCDC.	2019-05-07 downloaded from the CCDC.
;
_audit_creation_date             2019-03-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.67(C46 H60 O4 Ti), 0.5(C5 H11), 0.5(C5 H12)'
_chemical_formula_sum            'C35.67 H51.50 O2.67 Ti0.67'
_chemical_formula_weight         554.87
_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 0.0181 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'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.9534(4)
_cell_length_b                   21.2798(5)
_cell_length_c                   19.3799(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.805(2)
_cell_angle_gamma                90
_cell_volume                     5279.0(2)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    2667
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.04
_cell_measurement_theta_min      3.10
_shelx_estimated_absorpt_T_max   0.824
_shelx_estimated_absorpt_T_min   0.739
_exptl_absorpt_coefficient_mu    1.665
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0721 before and 0.0558 after correction. The Ratio of minimum to maximum transmission is 0.8878. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.047
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       cube
_exptl_crystal_F_000             1809
_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.121
_exptl_special_details           
;
Data was collected using a BRUKER CCD (charge coupled device) based
diffractometer equipped with an Oxford low-temperature apparatus operating at
173 K.  A suitable crystal was chosen and mounted on a nylon loop using 
Paratone oil.  Data  were measured using omega and phi scans of 1.0° per frame 
for 30 s. The total number of images were based on 
results from the program COSMO where redundancy was expected to be 4 and 
completeness to 0.83Å to 100%. Cell parameters were
retrieved using APEX II software and refined using SAINT on all observed
reflections.Data reduction was performed using the SAINT software which 
corrects for Lp. Scaling and absorption corrections were applied using SADABS6 
multi-scan technique, supplied by George Sheldrick.  The structure was solved 
by the direct method using the SHELXT program and refined by least squares 
method on F2, SHELXL, incorporated in OLEX2. 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1608
_diffrn_reflns_av_unetI/netI     0.1946
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29158
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.441
_diffrn_reflns_theta_min         3.104
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean 8.36
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω and φ'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3996
_reflns_number_total             9480
_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       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         9480
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1797
_refine_ls_R_factor_gt           0.0791
_refine_ls_restrained_S_all      0.892
_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)+(0.0942P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1903
_refine_ls_wR_factor_ref         0.2350
_refine_special_details          
;
The structure was refined by Least Squares using version 2018/3 
of XL (Sheldrick, 2015) incorporated in Olex2 (Dolomanov et al., 2009). 
All non-hydrogen atoms were refined anisotropically. 
Hydrogen atom positions were calculated geometrically and refined using the 
riding model, except for the hydrogen atom(s) on the non-carbon atom(s) 
which was found by difference Fourier methods and refined isotropically.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C01G(0.75) H2AA(0.75) C01I(0.75) H3AA(0.75) HH(0.75) HI(0.75)
 C5(0.75) H5A(0.75) H5B(0.75) C7(0.75) H7A(0.75) H7B(0.75) H7C(0.75) C1(0.75)
 H1A(0.75) H1B(0.75) C2(0.75) H2A(0.75) H2B(0.75) H2C(0.75) C3(0.75) H3A(0.75)
 H3B(0.75) C4(0.75) H4A(0.75) H4B(0.75) C0AA(0.75) H0AB(0.75) H0AC(0.75)
 C1AA(0.75) H1AA(0.75) H1AB(0.75) H1AC(0.75)
3.a Secondary CH2 refined with riding coordinates:
 C00G(H00A,H00B), C00M(H00H,H00I), C5(H5A,H5B), C1(H1A,H1B), C3(H3A,H3B),
 C4(H4A,H4B), C0AA(H0AB,H0AC)
3.b Aromatic/amide H refined with riding coordinates:
 C009(H009), C00D(H00D), C00F(H00F), C00R(H00R), C00V(H00V), C00X(H00X),
 C00Z(H00Z), C013(H013), C01G(H2AA)
3.c Idealised Me refined as rotating group:
 C00L(H00C,H00E,H00G), C00P(H00J,H00K,H00L), C00Q(H00M,H00N,H00O), C00W(H00P,
 H00Q,H00S), C011(H01A,H01B,H01C), C012(H01D,H01E,H01F), C014(H01G,H01H,H01I),
 C017(H01J,H01K,H01L), C018(H01M,H01N,H01O), C019(H01P,H01Q,H01R), C01A(H01S,
 H01T,H01U), C01B(H01V,H01W,H01X), C01C(H01Y,H,HA), C01D(H01Z,HB,HC), C01E(H01,
 HD,HE), C01F(H0AA,HF,HG), C01I(H3AA,HH,HI), C7(H7A,H7B,H7C), C2(H2A,H2B,H2C),
 C1AA(H1AA,H1AB,H1AC)
;
_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
Ti01 Ti 0.56513(8) 0.51722(5) 0.31302(5) 0.0275(2) Uani 1 1 d . . . . .
O002 O 0.5203(3) 0.54475(15) 0.39227(17) 0.0298(8) Uani 1 1 d . . . . .
O003 O 0.5480(3) 0.43358(15) 0.30723(18) 0.0313(9) Uani 1 1 d . . . . .
O004 O 0.7014(3) 0.53310(16) 0.31387(17) 0.0326(9) Uani 1 1 d . . . . .
O005 O 0.4872(3) 0.55765(17) 0.24146(17) 0.0336(9) Uani 1 1 d . . . . .
C006 C 0.4442(4) 0.5881(2) 0.4008(3) 0.0274(12) Uani 1 1 d . . . . .
C007 C 0.3040(4) 0.5442(2) 0.2334(3) 0.0321(13) Uani 1 1 d . . . . .
C008 C 0.3902(4) 0.5606(2) 0.2021(3) 0.0314(13) Uani 1 1 d . . . . .
C009 C 0.2054(5) 0.5436(3) 0.1938(3) 0.0398(14) Uani 1 1 d . . . . .
H009 H 0.1468 0.5313 0.2147 0.048 Uiso 1 1 calc R . . . .
C00A C 0.3469(4) 0.5826(2) 0.3599(3) 0.0302(12) Uani 1 1 d . . . . .
C00B C 0.5733(4) 0.6388(2) 0.4993(3) 0.0320(13) Uani 1 1 d . . . . .
C00C C 0.8211(4) 0.4702(3) 0.3897(3) 0.0329(13) Uani 1 1 d . . . . .
C00D C 0.9859(4) 0.5408(3) 0.3563(3) 0.0386(14) Uani 1 1 d . . . . .
H00D H 1.0427 0.5651 0.3452 0.046 Uiso 1 1 calc R . . . .
C00E C 0.5758(5) 0.3304(2) 0.2632(3) 0.0366(14) Uani 1 1 d . . . . .
C00F C 0.9248(5) 0.4563(3) 0.4181(3) 0.0392(14) Uani 1 1 d . . . . .
H00F H 0.9384 0.4220 0.4495 0.047 Uiso 1 1 calc R . . . .
C00G C 0.3178(4) 0.5282(2) 0.3104(3) 0.0336(13) Uani 1 1 d . . . . .
H00A H 0.2518 0.5097 0.3209 0.040 Uiso 1 1 calc R . . . .
H00B H 0.3727 0.4957 0.3200 0.040 Uiso 1 1 calc R . . . .
C00H C 0.8021(4) 0.5208(3) 0.3431(3) 0.0325(12) Uani 1 1 d . . . . .
C00I C 0.4680(4) 0.6359(2) 0.4515(3) 0.0291(12) Uani 1 1 d . . . . .
C00J C 0.6083(4) 0.3807(2) 0.3096(3) 0.0319(13) Uani 1 1 d . . . . .
C00K C 0.6985(4) 0.3774(2) 0.3588(3) 0.0336(13) Uani 1 1 d . . . . .
C00L C 0.5473(5) 0.5454(3) 0.0943(3) 0.0489(16) Uani 1 1 d . . . . .
H00C H 0.5744 0.5311 0.1417 0.073 Uiso 1 1 calc GR . . . .
H00E H 0.6055 0.5585 0.0707 0.073 Uiso 1 1 calc GR . . . .
H00G H 0.5091 0.5111 0.0681 0.073 Uiso 1 1 calc GR . . . .
C00M C 0.7323(4) 0.4306(3) 0.4093(3) 0.0346(13) Uani 1 1 d . . . . .
H00H H 0.7545 0.4126 0.4564 0.042 Uiso 1 1 calc R . . . .
H00I H 0.6715 0.4581 0.4119 0.042 Uiso 1 1 calc R . . . .
C00N C 0.8848(4) 0.5578(3) 0.3257(3) 0.0363(14) Uani 1 1 d . . . . .
C00O C 0.4739(5) 0.3332(3) 0.2110(3) 0.0427(15) Uani 1 1 d . . . . .
C00P C 0.6649(4) 0.6452(3) 0.4577(3) 0.0382(14) Uani 1 1 d . . . . .
H00J H 0.6704 0.6069 0.4305 0.057 Uiso 1 1 calc GR . . . .
H00K H 0.7300 0.6516 0.4901 0.057 Uiso 1 1 calc GR . . . .
H00L H 0.6527 0.6813 0.4261 0.057 Uiso 1 1 calc GR . . . .
C00Q C 0.5881(5) 0.5785(3) 0.5445(3) 0.0420(15) Uani 1 1 d . . . . .
H00M H 0.5311 0.5750 0.5722 0.063 Uiso 1 1 calc GR . . . .
H00N H 0.6550 0.5806 0.5758 0.063 Uiso 1 1 calc GR . . . .
H00O H 0.5875 0.5417 0.5141 0.063 Uiso 1 1 calc GR . . . .
C00R C 0.2720(4) 0.6283(3) 0.3666(3) 0.0386(14) Uani 1 1 d . . . . .
H00R H 0.2053 0.6254 0.3385 0.046 Uiso 1 1 calc R . . . .
C00S C 0.3788(5) 0.5802(3) 0.1321(3) 0.0350(13) Uani 1 1 d . . . . .
C00T C 0.1911(5) 0.5607(3) 0.1239(3) 0.0486(17) Uani 1 1 d . . . . .
C00U C 1.0081(4) 0.4911(3) 0.4015(3) 0.0389(14) Uani 1 1 d . . . . .
C00V C 0.2782(5) 0.5789(3) 0.0941(3) 0.0426(15) Uani 1 1 d . . . . .
H00V H 0.2686 0.5909 0.0463 0.051 Uiso 1 1 calc R . . . .
C00W C 1.1178(4) 0.4726(3) 0.4313(3) 0.0495(17) Uani 1 1 d . . . . .
H00P H 1.1443 0.4425 0.4001 0.074 Uiso 1 1 calc GR . . . .
H00Q H 1.1183 0.4534 0.4773 0.074 Uiso 1 1 calc GR . . . .
H00S H 1.1624 0.5101 0.4361 0.074 Uiso 1 1 calc GR . . . .
C00X C 0.3903(5) 0.6798(3) 0.4556(3) 0.0385(14) Uani 1 1 d . . . . .
H00X H 0.4038 0.7128 0.4888 0.046 Uiso 1 1 calc R . . . .
C00Y C 0.8643(5) 0.6136(3) 0.2754(3) 0.0404(14) Uani 1 1 d . . . . .
C00Z C 0.6427(5) 0.2781(3) 0.2674(3) 0.0472(16) Uani 1 1 d . . . . .
H00Z H 0.6243 0.2439 0.2365 0.057 Uiso 1 1 calc R . . . .
C010 C 0.4723(5) 0.6021(3) 0.0981(3) 0.0402(14) Uani 1 1 d . . . . .
C011 C 0.7907(5) 0.6616(3) 0.3015(3) 0.0504(17) Uani 1 1 d . . . . .
H01A H 0.7222 0.6422 0.3021 0.076 Uiso 1 1 calc GR . . . .
H01B H 0.7830 0.6981 0.2703 0.076 Uiso 1 1 calc GR . . . .
H01C H 0.8200 0.6751 0.3489 0.076 Uiso 1 1 calc GR . . . .
C012 C 0.5793(5) 0.6962(3) 0.5490(3) 0.0483(17) Uani 1 1 d . . . . .
H01D H 0.5664 0.7347 0.5214 0.072 Uiso 1 1 calc GR . . . .
H01E H 0.6488 0.6981 0.5771 0.072 Uiso 1 1 calc GR . . . .
H01F H 0.5264 0.6919 0.5798 0.072 Uiso 1 1 calc GR . . . .
C013 C 0.7610(5) 0.3238(3) 0.3609(3) 0.0423(15) Uani 1 1 d . . . . .
H013 H 0.8226 0.3210 0.3944 0.051 Uiso 1 1 calc R . . . .
C014 C 0.4391(6) 0.6249(3) 0.0227(3) 0.061(2) Uani 1 1 d . . . . .
H01G H 0.5005 0.6401 0.0038 0.091 Uiso 1 1 calc GR . . . .
H01H H 0.3884 0.6591 0.0222 0.091 Uiso 1 1 calc GR . . . .
H01I H 0.4072 0.5901 -0.0060 0.091 Uiso 1 1 calc GR . . . .
C015 C 0.2923(5) 0.6778(3) 0.4130(3) 0.0436(15) Uani 1 1 d . . . . .
C016 C 0.7338(5) 0.2740(3) 0.3145(4) 0.0534(18) Uani 1 1 d . . . . .
C017 C 0.8163(5) 0.5900(3) 0.2026(3) 0.0551(18) Uani 1 1 d . . . . .
H01J H 0.8666 0.5630 0.1839 0.083 Uiso 1 1 calc GR . . . .
H01K H 0.7990 0.6260 0.1714 0.083 Uiso 1 1 calc GR . . . .
H01L H 0.7527 0.5661 0.2061 0.083 Uiso 1 1 calc GR . . . .
C018 C 0.3807(5) 0.3396(3) 0.2498(3) 0.0528(18) Uani 1 1 d . . . . .
H01M H 0.3750 0.3018 0.2778 0.079 Uiso 1 1 calc GR . . . .
H01N H 0.3168 0.3447 0.2160 0.079 Uiso 1 1 calc GR . . . .
H01O H 0.3904 0.3765 0.2804 0.079 Uiso 1 1 calc GR . . . .
C019 C 0.5300(5) 0.6563(3) 0.1405(3) 0.0491(17) Uani 1 1 d . . . . .
H01P H 0.5536 0.6423 0.1885 0.074 Uiso 1 1 calc GR . . . .
H01Q H 0.4827 0.6921 0.1409 0.074 Uiso 1 1 calc GR . . . .
H01R H 0.5906 0.6689 0.1191 0.074 Uiso 1 1 calc GR . . . .
C01A C 0.0848(5) 0.5594(4) 0.0798(4) 0.071(2) Uani 1 1 d . . . . .
H01S H 0.0636 0.5158 0.0698 0.107 Uiso 1 1 calc GR . . . .
H01T H 0.0875 0.5817 0.0359 0.107 Uiso 1 1 calc GR . . . .
H01U H 0.0341 0.5800 0.1050 0.107 Uiso 1 1 calc GR . . . .
C01B C 0.4774(6) 0.3880(3) 0.1608(3) 0.060(2) Uani 1 1 d . . . . .
H01V H 0.4847 0.4275 0.1872 0.090 Uiso 1 1 calc GR . . . .
H01W H 0.4127 0.3889 0.1272 0.090 Uiso 1 1 calc GR . . . .
H01X H 0.5371 0.3829 0.1358 0.090 Uiso 1 1 calc GR . . . .
C01C C 0.9673(5) 0.6491(3) 0.2677(4) 0.0570(19) Uani 1 1 d . . . . .
H01Y H 1.0012 0.6634 0.3137 0.085 Uiso 1 1 calc GR . . . .
H H 0.9511 0.6854 0.2368 0.085 Uiso 1 1 calc GR . . . .
HA H 1.0144 0.6207 0.2476 0.085 Uiso 1 1 calc GR . . . .
C01D C 0.4596(6) 0.2729(3) 0.1664(4) 0.072(2) Uani 1 1 d . . . . .
H01Z H 0.5192 0.2679 0.1412 0.108 Uiso 1 1 calc GR . . . .
HB H 0.3951 0.2761 0.1327 0.108 Uiso 1 1 calc GR . . . .
HC H 0.4554 0.2365 0.1967 0.108 Uiso 1 1 calc GR . . . .
C01E C 0.2133(6) 0.7293(3) 0.4181(4) 0.072(2) Uani 1 1 d . . . . .
H01 H 0.1437 0.7148 0.3972 0.109 Uiso 1 1 calc GR . . . .
HD H 0.2322 0.7666 0.3932 0.109 Uiso 1 1 calc GR . . . .
HE H 0.2130 0.7399 0.4673 0.109 Uiso 1 1 calc GR . . . .
C01F C 0.8038(6) 0.2171(3) 0.3137(5) 0.090(3) Uani 1 1 d . . . . .
H0AA H 0.7607 0.1796 0.3022 0.134 Uiso 1 1 calc GR . . . .
HF H 0.8460 0.2119 0.3598 0.134 Uiso 1 1 calc GR . . . .
HG H 0.8499 0.2231 0.2786 0.134 Uiso 1 1 calc GR . . . .
C01G C 0.9345(14) 0.7737(8) 0.4692(9) 0.148(6) Uiso 0.75 1 d . . P . .
H2AA H 0.9637 0.7872 0.4296 0.178 Uiso 0.75 1 calc R . P . .
C01I C 0.7842(11) 0.9029(6) 0.4853(7) 0.120(5) Uiso 0.75 1 d . . P . .
H3AA H 0.8288 0.9262 0.5221 0.179 Uiso 0.75 1 calc GR . P . .
HH H 0.7342 0.8774 0.5062 0.179 Uiso 0.75 1 calc GR . P . .
HI H 0.7464 0.9325 0.4520 0.179 Uiso 0.75 1 calc GR . P . .
C5 C 0.8681(11) 0.8035(6) 0.4969(7) 0.101(4) Uiso 0.75 1 d . . P . .
H5A H 0.8963 0.8141 0.5459 0.122 Uiso 0.75 1 calc R . P . .
H5B H 0.8039 0.7781 0.4964 0.122 Uiso 0.75 1 calc R . P . .
C7 C 0.9610(11) 0.7132(6) 0.5082(7) 0.128(5) Uiso 0.75 1 d . . P . .
H7A H 0.9279 0.7127 0.5504 0.191 Uiso 0.75 1 calc GR . P . .
H7B H 1.0370 0.7099 0.5212 0.191 Uiso 0.75 1 calc GR . P . .
H7C H 0.9355 0.6776 0.4782 0.191 Uiso 0.75 1 calc GR . P . .
C1 C 0.9538(17) 0.3771(8) 0.2138(10) 0.149(7) Uiso 0.75 1 d . . P . .
H1A H 0.9600 0.3443 0.1784 0.178 Uiso 0.75 1 calc R . P . .
H1B H 0.9193 0.3549 0.2489 0.178 Uiso 0.75 1 calc R . P . .
C2 C 0.7983(13) 0.4159(7) 0.1391(9) 0.141(6) Uiso 0.75 1 d . . P . .
H2A H 0.8220 0.4336 0.0975 0.212 Uiso 0.75 1 calc GR . P . .
H2B H 0.7554 0.4469 0.1591 0.212 Uiso 0.75 1 calc GR . P . .
H2C H 0.7568 0.3780 0.1260 0.212 Uiso 0.75 1 calc GR . P . .
C3 C 0.875(2) 0.4022(11) 0.1825(12) 0.217(11) Uiso 0.75 1 d . . P . .
H3A H 0.9038 0.4453 0.1862 0.261 Uiso 0.75 1 calc R . P . .
H3B H 0.8350 0.3998 0.2223 0.261 Uiso 0.75 1 calc R . P . .
C4 C 1.0479(19) 0.3724(10) 0.2466(12) 0.198(9) Uiso 0.75 1 d . . P . .
H4A H 1.0907 0.3715 0.2084 0.238 Uiso 0.75 1 calc R . P . .
H4B H 1.0609 0.4143 0.2686 0.238 Uiso 0.75 1 calc R . P . .
C0AA C 0.8437(11) 0.8653(6) 0.4521(7) 0.112(5) Uiso 0.75 1 d . . P . .
H0AB H 0.9096 0.8870 0.4466 0.135 Uiso 0.75 1 calc R . P . .
H0AC H 0.8063 0.8547 0.4051 0.135 Uiso 0.75 1 calc R . P . .
C1AA C 1.0935(13) 0.3378(8) 0.2889(8) 0.146(7) Uiso 0.75 1 d . . P . .
H1AA H 1.0529 0.3319 0.3271 0.219 Uiso 0.75 1 calc GR . P . .
H1AB H 1.1618 0.3558 0.3073 0.219 Uiso 0.75 1 calc GR . P . .
H1AC H 1.1033 0.2971 0.2671 0.219 Uiso 0.75 1 calc GR . P . .


_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
Ti01 O002 1.820(3) . ?
Ti01 O003 1.795(3) . ?
Ti01 O004 1.795(3) . ?
Ti01 O005 1.804(3) . ?
O002 C006 1.379(6) . ?
O003 C00J 1.366(6) . ?
O004 C00H 1.366(6) . ?
O005 C008 1.367(6) . ?
C006 C00A 1.387(7) . ?
C006 C00I 1.415(7) . ?
C007 C008 1.394(7) . ?
C007 C009 1.386(8) . ?
C007 C00G 1.515(7) . ?
C008 C00S 1.406(7) . ?
C009 H009 0.9500 . ?
C009 C00T 1.387(8) . ?
C00A C00G 1.513(7) . ?
C00A C00R 1.394(7) . ?
C00B C00I 1.529(7) . ?
C00B C00P 1.539(7) . ?
C00B C00Q 1.550(7) . ?
C00B C012 1.548(7) . ?
C00C C00F 1.403(8) . ?
C00C C00H 1.402(7) . ?
C00C C00M 1.520(7) . ?
C00D H00D 0.9500 . ?
C00D C00N 1.400(8) . ?
C00D C00U 1.375(8) . ?
C00E C00J 1.422(7) . ?
C00E C00O 1.536(8) . ?
C00E C00Z 1.405(8) . ?
C00F H00F 0.9500 . ?
C00F C00U 1.386(8) . ?
C00G H00A 0.9900 . ?
C00G H00B 0.9900 . ?
C00H C00N 1.412(7) . ?
C00I C00X 1.385(7) . ?
C00J C00K 1.392(8) . ?
C00K C00M 1.516(7) . ?
C00K C013 1.397(7) . ?
C00L H00C 0.9800 . ?
C00L H00E 0.9800 . ?
C00L H00G 0.9800 . ?
C00L C010 1.557(8) . ?
C00M H00H 0.9900 . ?
C00M H00I 0.9900 . ?
C00N C00Y 1.534(8) . ?
C00O C018 1.522(8) . ?
C00O C01B 1.524(8) . ?
C00O C01D 1.542(7) . ?
C00P H00J 0.9800 . ?
C00P H00K 0.9800 . ?
C00P H00L 0.9800 . ?
C00Q H00M 0.9800 . ?
C00Q H00N 0.9800 . ?
C00Q H00O 0.9800 . ?
C00R H00R 0.9500 . ?
C00R C015 1.383(8) . ?
C00S C00V 1.395(8) . ?
C00S C010 1.537(8) . ?
C00T C00V 1.400(8) . ?
C00T C01A 1.505(8) . ?
C00U C00W 1.502(7) . ?
C00V H00V 0.9500 . ?
C00W H00P 0.9800 . ?
C00W H00Q 0.9800 . ?
C00W H00S 0.9800 . ?
C00X H00X 0.9500 . ?
C00X C015 1.405(8) . ?
C00Y C011 1.536(8) . ?
C00Y C017 1.536(8) . ?
C00Y C01C 1.560(8) . ?
C00Z H00Z 0.9500 . ?
C00Z C016 1.380(9) . ?
C010 C014 1.538(7) . ?
C010 C019 1.542(8) . ?
C011 H01A 0.9800 . ?
C011 H01B 0.9800 . ?
C011 H01C 0.9800 . ?
C012 H01D 0.9800 . ?
C012 H01E 0.9800 . ?
C012 H01F 0.9800 . ?
C013 H013 0.9500 . ?
C013 C016 1.399(8) . ?
C014 H01G 0.9800 . ?
C014 H01H 0.9800 . ?
C014 H01I 0.9800 . ?
C015 C01E 1.513(8) . ?
C016 C01F 1.514(8) . ?
C017 H01J 0.9800 . ?
C017 H01K 0.9800 . ?
C017 H01L 0.9800 . ?
C018 H01M 0.9800 . ?
C018 H01N 0.9800 . ?
C018 H01O 0.9800 . ?
C019 H01P 0.9800 . ?
C019 H01Q 0.9800 . ?
C019 H01R 0.9800 . ?
C01A H01S 0.9800 . ?
C01A H01T 0.9800 . ?
C01A H01U 0.9800 . ?
C01B H01V 0.9800 . ?
C01B H01W 0.9800 . ?
C01B H01X 0.9800 . ?
C01C H01Y 0.9800 . ?
C01C H 0.9800 . ?
C01C HA 0.9800 . ?
C01D H01Z 0.9800 . ?
C01D HB 0.9800 . ?
C01D HC 0.9800 . ?
C01E H01 0.9800 . ?
C01E HD 0.9800 . ?
C01E HE 0.9800 . ?
C01F H0AA 0.9800 . ?
C01F HF 0.9800 . ?
C01F HG 0.9800 . ?
C01G H2AA 0.9500 . ?
C01G C5 1.254(17) . ?
C01G C7 1.505(17) . ?
C01I H3AA 0.9800 . ?
C01I HH 0.9800 . ?
C01I HI 0.9800 . ?
C01I C0AA 1.340(15) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C0AA 1.582(15) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C3 1.23(2) . ?
C1 C4 1.29(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C2 C3 1.23(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C1AA 1.19(2) . ?
C0AA H0AB 0.9900 . ?
C0AA H0AC 0.9900 . ?
C1AA H1AA 0.9800 . ?
C1AA H1AB 0.9800 . ?
C1AA H1AC 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O003 Ti01 O002 108.64(16) . . ?
O003 Ti01 O005 112.06(17) . . ?
O004 Ti01 O002 111.83(16) . . ?
O004 Ti01 O003 107.42(17) . . ?
O004 Ti01 O005 110.56(17) . . ?
O005 Ti01 O002 106.37(16) . . ?
C006 O002 Ti01 130.0(3) . . ?
C00J O003 Ti01 138.5(3) . . ?
C00H O004 Ti01 147.5(3) . . ?
C008 O005 Ti01 144.0(4) . . ?
O002 C006 C00A 118.6(5) . . ?
O002 C006 C00I 118.7(5) . . ?
C00A C006 C00I 122.7(5) . . ?
C008 C007 C00G 120.2(5) . . ?
C009 C007 C008 119.6(5) . . ?
C009 C007 C00G 120.2(5) . . ?
O005 C008 C007 118.4(5) . . ?
O005 C008 C00S 120.3(5) . . ?
C007 C008 C00S 121.3(5) . . ?
C007 C009 H009 119.6 . . ?
C007 C009 C00T 120.8(6) . . ?
C00T C009 H009 119.6 . . ?
C006 C00A C00G 122.9(5) . . ?
C006 C00A C00R 118.2(5) . . ?
C00R C00A C00G 118.9(5) . . ?
C00I C00B C00P 112.0(4) . . ?
C00I C00B C00Q 109.3(4) . . ?
C00I C00B C012 111.3(5) . . ?
C00P C00B C00Q 109.3(5) . . ?
C00P C00B C012 106.6(5) . . ?
C012 C00B C00Q 108.2(4) . . ?
C00F C00C C00M 120.0(5) . . ?
C00H C00C C00F 118.5(5) . . ?
C00H C00C C00M 121.5(5) . . ?
C00N C00D H00D 118.0 . . ?
C00U C00D H00D 118.0 . . ?
C00U C00D C00N 124.0(5) . . ?
C00J C00E C00O 121.9(5) . . ?
C00Z C00E C00J 116.1(6) . . ?
C00Z C00E C00O 122.0(5) . . ?
C00C C00F H00F 119.0 . . ?
C00U C00F C00C 121.9(5) . . ?
C00U C00F H00F 119.0 . . ?
C007 C00G H00A 108.4 . . ?
C007 C00G H00B 108.4 . . ?
C00A C00G C007 115.7(4) . . ?
C00A C00G H00A 108.4 . . ?
C00A C00G H00B 108.4 . . ?
H00A C00G H00B 107.4 . . ?
O004 C00H C00C 118.5(5) . . ?
O004 C00H C00N 120.3(5) . . ?
C00C C00H C00N 121.2(5) . . ?
C006 C00I C00B 122.0(5) . . ?
C00X C00I C006 116.2(5) . . ?
C00X C00I C00B 121.8(5) . . ?
O003 C00J C00E 119.1(5) . . ?
O003 C00J C00K 118.8(5) . . ?
C00K C00J C00E 122.1(5) . . ?
C00J C00K C00M 122.3(5) . . ?
C00J C00K C013 118.9(5) . . ?
C013 C00K C00M 118.8(5) . . ?
H00C C00L H00E 109.5 . . ?
H00C C00L H00G 109.5 . . ?
H00E C00L H00G 109.5 . . ?
C010 C00L H00C 109.5 . . ?
C010 C00L H00E 109.5 . . ?
C010 C00L H00G 109.5 . . ?
C00C C00M H00H 108.8 . . ?
C00C C00M H00I 108.8 . . ?
C00K C00M C00C 114.0(4) . . ?
C00K C00M H00H 108.8 . . ?
C00K C00M H00I 108.8 . . ?
H00H C00M H00I 107.7 . . ?
C00D C00N C00H 116.7(5) . . ?
C00D C00N C00Y 121.9(5) . . ?
C00H C00N C00Y 121.4(5) . . ?
C00E C00O C01D 110.7(5) . . ?
C018 C00O C00E 110.2(5) . . ?
C018 C00O C01B 110.5(5) . . ?
C018 C00O C01D 108.4(5) . . ?
C01B C00O C00E 110.1(5) . . ?
C01B C00O C01D 106.9(5) . . ?
C00B C00P H00J 109.5 . . ?
C00B C00P H00K 109.5 . . ?
C00B C00P H00L 109.5 . . ?
H00J C00P H00K 109.5 . . ?
H00J C00P H00L 109.5 . . ?
H00K C00P H00L 109.5 . . ?
C00B C00Q H00M 109.5 . . ?
C00B C00Q H00N 109.5 . . ?
C00B C00Q H00O 109.5 . . ?
H00M C00Q H00N 109.5 . . ?
H00M C00Q H00O 109.5 . . ?
H00N C00Q H00O 109.5 . . ?
C00A C00R H00R 119.1 . . ?
C015 C00R C00A 121.7(6) . . ?
C015 C00R H00R 119.1 . . ?
C008 C00S C010 122.0(5) . . ?
C00V C00S C008 117.2(6) . . ?
C00V C00S C010 120.9(5) . . ?
C009 C00T C00V 118.7(6) . . ?
C009 C00T C01A 121.6(6) . . ?
C00V C00T C01A 119.8(6) . . ?
C00D C00U C00F 117.7(5) . . ?
C00D C00U C00W 122.6(5) . . ?
C00F C00U C00W 119.7(6) . . ?
C00S C00V C00T 122.3(5) . . ?
C00S C00V H00V 118.8 . . ?
C00T C00V H00V 118.8 . . ?
C00U C00W H00P 109.5 . . ?
C00U C00W H00Q 109.5 . . ?
C00U C00W H00S 109.5 . . ?
H00P C00W H00Q 109.5 . . ?
H00P C00W H00S 109.5 . . ?
H00Q C00W H00S 109.5 . . ?
C00I C00X H00X 118.5 . . ?
C00I C00X C015 123.0(5) . . ?
C015 C00X H00X 118.5 . . ?
C00N C00Y C011 111.2(5) . . ?
C00N C00Y C017 109.7(5) . . ?
C00N C00Y C01C 111.6(5) . . ?
C011 C00Y C017 109.6(5) . . ?
C011 C00Y C01C 107.1(5) . . ?
C017 C00Y C01C 107.6(5) . . ?
C00E C00Z H00Z 118.5 . . ?
C016 C00Z C00E 123.1(6) . . ?
C016 C00Z H00Z 118.5 . . ?
C00S C010 C00L 108.9(5) . . ?
C00S C010 C014 112.2(5) . . ?
C00S C010 C019 110.4(5) . . ?
C014 C010 C00L 106.6(5) . . ?
C014 C010 C019 108.2(5) . . ?
C019 C010 C00L 110.5(5) . . ?
C00Y C011 H01A 109.5 . . ?
C00Y C011 H01B 109.5 . . ?
C00Y C011 H01C 109.5 . . ?
H01A C011 H01B 109.5 . . ?
H01A C011 H01C 109.5 . . ?
H01B C011 H01C 109.5 . . ?
C00B C012 H01D 109.5 . . ?
C00B C012 H01E 109.5 . . ?
C00B C012 H01F 109.5 . . ?
H01D C012 H01E 109.5 . . ?
H01D C012 H01F 109.5 . . ?
H01E C012 H01F 109.5 . . ?
C00K C013 H013 119.6 . . ?
C00K C013 C016 120.8(6) . . ?
C016 C013 H013 119.6 . . ?
C010 C014 H01G 109.5 . . ?
C010 C014 H01H 109.5 . . ?
C010 C014 H01I 109.5 . . ?
H01G C014 H01H 109.5 . . ?
H01G C014 H01I 109.5 . . ?
H01H C014 H01I 109.5 . . ?
C00R C015 C00X 118.1(5) . . ?
C00R C015 C01E 122.1(6) . . ?
C00X C015 C01E 119.8(6) . . ?
C00Z C016 C013 118.9(6) . . ?
C00Z C016 C01F 119.8(7) . . ?
C013 C016 C01F 121.3(7) . . ?
C00Y C017 H01J 109.5 . . ?
C00Y C017 H01K 109.5 . . ?
C00Y C017 H01L 109.5 . . ?
H01J C017 H01K 109.5 . . ?
H01J C017 H01L 109.5 . . ?
H01K C017 H01L 109.5 . . ?
C00O C018 H01M 109.5 . . ?
C00O C018 H01N 109.5 . . ?
C00O C018 H01O 109.5 . . ?
H01M C018 H01N 109.5 . . ?
H01M C018 H01O 109.5 . . ?
H01N C018 H01O 109.5 . . ?
C010 C019 H01P 109.5 . . ?
C010 C019 H01Q 109.5 . . ?
C010 C019 H01R 109.5 . . ?
H01P C019 H01Q 109.5 . . ?
H01P C019 H01R 109.5 . . ?
H01Q C019 H01R 109.5 . . ?
C00T C01A H01S 109.5 . . ?
C00T C01A H01T 109.5 . . ?
C00T C01A H01U 109.5 . . ?
H01S C01A H01T 109.5 . . ?
H01S C01A H01U 109.5 . . ?
H01T C01A H01U 109.5 . . ?
C00O C01B H01V 109.5 . . ?
C00O C01B H01W 109.5 . . ?
C00O C01B H01X 109.5 . . ?
H01V C01B H01W 109.5 . . ?
H01V C01B H01X 109.5 . . ?
H01W C01B H01X 109.5 . . ?
C00Y C01C H01Y 109.5 . . ?
C00Y C01C H 109.5 . . ?
C00Y C01C HA 109.5 . . ?
H01Y C01C H 109.5 . . ?
H01Y C01C HA 109.5 . . ?
H C01C HA 109.5 . . ?
C00O C01D H01Z 109.5 . . ?
C00O C01D HB 109.5 . . ?
C00O C01D HC 109.5 . . ?
H01Z C01D HB 109.5 . . ?
H01Z C01D HC 109.5 . . ?
HB C01D HC 109.5 . . ?
C015 C01E H01 109.5 . . ?
C015 C01E HD 109.5 . . ?
C015 C01E HE 109.5 . . ?
H01 C01E HD 109.5 . . ?
H01 C01E HE 109.5 . . ?
HD C01E HE 109.5 . . ?
C016 C01F H0AA 109.5 . . ?
C016 C01F HF 109.5 . . ?
C016 C01F HG 109.5 . . ?
H0AA C01F HF 109.5 . . ?
H0AA C01F HG 109.5 . . ?
HF C01F HG 109.5 . . ?
C5 C01G H2AA 125.2 . . ?
C5 C01G C7 109.7(16) . . ?
C7 C01G H2AA 125.2 . . ?
H3AA C01I HH 109.5 . . ?
H3AA C01I HI 109.5 . . ?
HH C01I HI 109.5 . . ?
C0AA C01I H3AA 109.5 . . ?
C0AA C01I HH 109.5 . . ?
C0AA C01I HI 109.5 . . ?
C01G C5 H5A 110.5 . . ?
C01G C5 H5B 110.5 . . ?
C01G C5 C0AA 106.2(13) . . ?
H5A C5 H5B 108.7 . . ?
C0AA C5 H5A 110.5 . . ?
C0AA C5 H5B 110.5 . . ?
C01G C7 H7A 109.5 . . ?
C01G C7 H7B 109.5 . . ?
C01G C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
H1A C1 H1B 103.5 . . ?
C3 C1 H1A 96.7 . . ?
C3 C1 H1B 96.7 . . ?
C3 C1 C4 158(3) . . ?
C4 C1 H1A 96.7 . . ?
C4 C1 H1B 96.7 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
C3 C2 H2C 109.5 . . ?
C1 C3 C2 164(3) . . ?
C1 C3 H3A 95.0 . . ?
C1 C3 H3B 95.0 . . ?
C2 C3 H3A 95.0 . . ?
C2 C3 H3B 95.0 . . ?
H3A C3 H3B 103.2 . . ?
C1 C4 H4A 103.2 . . ?
C1 C4 H4B 103.2 . . ?
H4A C4 H4B 105.1 . . ?
C1AA C4 C1 136(2) . . ?
C1AA C4 H4A 103.2 . . ?
C1AA C4 H4B 103.2 . . ?
C01I C0AA C5 108.3(12) . . ?
C01I C0AA H0AB 110.0 . . ?
C01I C0AA H0AC 110.0 . . ?
C5 C0AA H0AB 110.0 . . ?
C5 C0AA H0AC 110.0 . . ?
H0AB C0AA H0AC 108.4 . . ?
C4 C1AA H1AA 109.5 . . ?
C4 C1AA H1AB 109.5 . . ?
C4 C1AA H1AC 109.5 . . ?
H1AA C1AA H1AB 109.5 . . ?
H1AA C1AA H1AC 109.5 . . ?
H1AB C1AA H1AC 109.5 . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_final
_database_code_depnum_ccdc_archive 'CCDC 1907835'
loop_
_audit_author_name
_audit_author_address
'Kelly Aldrich'
;Michigan State University
United States of America
;
_audit_update_record             
;
2019-04-03 deposited with the CCDC.	2019-05-07 downloaded from the CCDC.
;
_audit_creation_date             2019-03-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_formula_moiety         'C40 H48 Br4 O4 Ti, 0.5(C8)'
_chemical_formula_sum            'C44 H48 Br4 O4 Ti'
_chemical_formula_weight         1008.35
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Br -0.28346 2.55990 17.17890 5.23580 5.63770 3.98510 2.17230 16.57960 0.26090
41.43280 2.95569992065
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Ti 0.29130 0.45317 9.75950 7.35580 1.69910 1.90210 7.85080 0.50000 35.63380
116.10500 1.28069996834
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -y+1/4,x+3/4,z+3/4
3 y+1/4,-x+1/4,z+1/4
4 -x,-y+1/2,z
5 -x,-y,-z
6 y-1/4,-x-3/4,-z-3/4
7 -y-1/4,x-1/4,-z-1/4
8 x,y-1/2,-z
9 x+1/2,y+1/2,z+1/2
10 -y+3/4,x+5/4,z+5/4
11 y+3/4,-x+3/4,z+3/4
12 -x+1/2,-y+1,z+1/2
13 -x+1/2,-y+1/2,-z+1/2
14 y+1/4,-x-1/4,-z-1/4
15 -y+1/4,x+1/4,-z+1/4
16 x+1/2,y,-z+1/2

_symmetry_Int_Tables_number      88
_cell_length_a                   22.370(3)
_cell_length_b                   22.370(3)
_cell_length_c                   9.5963(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4802.0(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4264
# end Validation Reply Form
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.76
_cell_measurement_theta_min      2.31
_exptl_absorpt_coefficient_mu    3.542
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4745
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1366 before and 0.0631 after correction. The Ratio of minimum to maximum transmission is 0.6367. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.3947
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2021.6064
_exptl_crystal_size_max          0.493
_exptl_crystal_size_mid          0.206
_exptl_crystal_size_min          0.163
_exptl_special_details           
;
Data was collected using a BRUKER CCD (charge coupled device) based
diffractometer equipped with an Oxford low-temperature apparatus operating at
173 K.  A suitable crystal was chosen and mounted on a nylon loop using 
Paratone oil.  Data  were measured using omega scans of 0.5° per frame 
for 30 s. The total number of images were based on 
results from the program COSMO where redundancy was expected to be 4 and 
completeness to 0.83Å to 100%. Cell parameters were
retrieved using APEX II software and refined using SAINT on all observed
reflections.Data reduction was performed using the SAINT software which 
corrects for Lp. Scaling and absorption corrections were applied using SADABS6 
multi-scan technique, supplied by George Sheldrick.  The structure was solved 
by the direct method using the SHELXT program and refined by least squares 
method on F2, SHELXL, incorporated in OLEX2. 
;
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            19286
_diffrn_reflns_theta_full        25.6731
_diffrn_reflns_theta_max         25.67
_diffrn_reflns_theta_min         1.82
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 8.36
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              27
_reflns_limit_h_min              0
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                1560
_reflns_number_total             2281
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.0492
_refine_diff_density_min         -0.5954
_refine_diff_density_rms         0.1415
_refine_ls_d_res_high            0.8203
_refine_ls_d_res_low             11.1849
_refine_ls_goodness_of_fit_ref   1.0431
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    18
_refine_ls_number_parameters     122
_refine_ls_number_reflns         2281
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0557
_refine_ls_restrained_S_all      1.0431
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1005P)²+9.6946P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1627
_refine_ls_wR_factor_ref         0.1847
_refine_special_details          
;
The structure was refined by Least Squares using version 2018/3 
of XL (Sheldrick, 2015) incorporated in Olex2 (Dolomanov et al., 2009). 
All non-hydrogen atoms were refined anisotropically. 
Hydrogen atom positions were calculated geometrically and refined using the 
riding model, except for the Hydrogen atom on the nitrogen atom which was found 
by difference Fourier methods and refined isotropically.
;
_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. Others
 Fixed Sof: C12(0.5) C11(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C2(H2)
3.b Idealised Me refined as rotating group:
 C10(H10a,H10b,H10c), C8(H8a,H8b,H8c), C9(H9a,H9b,H9c)
;
_atom_sites_solution_primary     dual
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Br1 Br 0.66157(4) 0.62132(4) -0.00668(7) 0.0781(4) Uani 1.000000 1 . . .
Ti1 Ti 0.5 0.75 0.625 0.0332(4) Uani 1.000000 4 S T P
O1 O 0.55873(15) 0.72277(18) 0.5182(4) 0.0501(10) Uani 1.000000 1 . . .
C6 C 0.6463(2) 0.6955(2) 0.3897(5) 0.0338(11) Uani 1.000000 1 . . .
C1 C 0.5837(2) 0.6992(2) 0.4009(5) 0.0371(11) Uani 1.000000 1 . . .
C5 C 0.6674(2) 0.6714(2) 0.2653(5) 0.0395(12) Uani 1.000000 1 . . .
H5 H 0.7094(2) 0.6678(2) 0.2520(5) 0.0474(14) Uiso 1.000000 1 R . .
C7 C 0.6888(2) 0.7178(3) 0.5039(5) 0.0424(13) Uani 1.000000 1 . . .
C3 C 0.5680(2) 0.6568(2) 0.1742(6) 0.0429(13) Uani 1.000000 1 . . .
H3 H 0.5421(2) 0.6440(2) 0.1016(6) 0.0515(15) Uiso 1.000000 1 R . .
C2 C 0.5455(2) 0.6801(2) 0.2964(6) 0.0417(12) Uani 1.000000 1 . . .
H2 H 0.5035(2) 0.6831(2) 0.3091(6) 0.0500(15) Uiso 1.000000 1 R . .
C4 C 0.6295(2) 0.6526(2) 0.1606(5) 0.0443(13) Uani 1.000000 1 . . .
C10 C 0.7547(2) 0.7070(3) 0.4655(6) 0.0571(16) Uani 1.000000 1 . . .
H10a H 0.7621(5) 0.6640(3) 0.458(4) 0.086(2) Uiso 1.000000 1 GR . .
H10b H 0.7636(5) 0.7264(15) 0.376(2) 0.086(2) Uiso 1.000000 1 GR . .
H10c H 0.7805(2) 0.7239(16) 0.538(2) 0.086(2) Uiso 1.000000 1 GR . .
C8 C 0.6797(3) 0.7854(3) 0.5249(7) 0.0591(16) Uani 1.000000 1 . . .
H8a H 0.6884(19) 0.8064(3) 0.4376(14) 0.089(2) Uiso 1.000000 1 GR . .
H8b H 0.6382(6) 0.7930(3) 0.552(4) 0.089(2) Uiso 1.000000 1 GR . .
H8c H 0.7066(14) 0.7997(5) 0.598(3) 0.089(2) Uiso 1.000000 1 GR . .
C9 C 0.6770(3) 0.6837(3) 0.6391(6) 0.0610(17) Uani 1.000000 1 . . .
H9a H 0.6359(7) 0.6910(16) 0.670(2) 0.092(3) Uiso 1.000000 1 GR . .
H9b H 0.6828(19) 0.6408(4) 0.6231(13) 0.092(3) Uiso 1.000000 1 GR . .
H9c H 0.7049(13) 0.6974(14) 0.7112(14) 0.092(3) Uiso 1.000000 1 GR . .
C12 C 0.7187(8) 0.5012(8) 0.456(2) 0.096(5) Uiso 0.500000 1 . . .
C11 C 0.7214(7) 0.5073(8) 0.2855(19) 0.091(5) Uiso 0.500000 1 . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C4 1.893(5) . ?
Ti1 O1 1.774(3) 4_665 ?
Ti1 O1 1.774(3) 15_656 ?
Ti1 O1 1.774(3) 6_577 ?
Ti1 O1 1.774(3) . ?
O1 C1 1.362(6) . ?
C6 C1 1.408(6) . ?
C6 C5 1.393(7) . ?
C6 C7 1.535(7) . ?
C1 C2 1.385(7) . ?
C5 H5 0.9500 . ?
C5 C4 1.381(7) . ?
C7 C10 1.539(7) . ?
C7 C8 1.538(8) . ?
C7 C9 1.528(8) . ?
C3 H3 0.9500 . ?
C3 C2 1.379(8) . ?
C3 C4 1.385(7) . ?
C2 H2 0.9500 . ?
C10 H10a 0.9800 . ?
C10 H10b 0.9800 . ?
C10 H10c 0.9800 . ?
C8 H8a 0.9800 . ?
C8 H8b 0.9800 . ?
C8 H8c 0.9800 . ?
C9 H9a 0.9800 . ?
C9 H9b 0.9800 . ?
C9 H9c 0.9800 . ?
C12 C11 1.31(2) 3_565 ?
C12 C11 1.64(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 O1 109.50(13) . 6_577 ?
O1 Ti1 O1 109.50(12) 4_665 6_577 ?
O1 Ti1 O1 109.4(2) 4_665 . ?
O1 Ti1 O1 109.50(13) 15_656 . ?
O1 Ti1 O1 109.4(2) 15_656 6_577 ?
O1 Ti1 O1 109.50(13) 4_665 15_656 ?
C1 O1 Ti1 156.0(3) . 15_656 ?
C5 C6 C1 115.2(4) . . ?
C7 C6 C1 122.9(4) . . ?
C7 C6 C5 121.9(4) . . ?
C6 C1 O1 119.6(4) . . ?
C2 C1 O1 117.7(4) . . ?
C2 C1 C6 122.7(5) . . ?
H5 C5 C6 118.9(3) . . ?
C4 C5 C6 122.2(5) . . ?
C4 C5 H5 118.9(3) . . ?
C10 C7 C6 111.8(4) . . ?
C8 C7 C6 109.3(4) . . ?
C8 C7 C10 108.3(5) . . ?
C9 C7 C6 109.7(4) . . ?
C9 C7 C10 106.9(5) . . ?
C9 C7 C8 110.9(5) . . ?
C2 C3 H3 121.0(3) . . ?
C4 C3 H3 121.0(3) . . ?
C4 C3 C2 117.9(5) . . ?
C3 C2 C1 120.5(5) . . ?
H2 C2 C1 119.8(3) . . ?
H2 C2 C3 119.8(3) . . ?
C5 C4 Br1 119.7(4) . . ?
C3 C4 Br1 118.8(4) . . ?
C3 C4 C5 121.5(5) . . ?
H10a C10 C7 109.5 . . ?
H10b C10 C7 109.5 . . ?
H10b C10 H10a 109.5 . . ?
H10c C10 C7 109.5 . . ?
H10c C10 H10a 109.5 . . ?
H10c C10 H10b 109.5 . . ?
H8a C8 C7 109.5 . . ?
H8b C8 C7 109.5 . . ?
H8b C8 H8a 109.5 . . ?
H8c C8 C7 109.5 . . ?
H8c C8 H8a 109.5 . . ?
H8c C8 H8b 109.5 . . ?
H9a C9 C7 109.5 . . ?
H9b C9 C7 109.5 . . ?
H9b C9 H9a 109.5 . . ?
H9c C9 C7 109.5 . . ?
H9c C9 H9a 109.5 . . ?
H9c C9 H9b 109.5 . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT315_final               
;
PROBLEM: Singly Bonded Carbon Detected (H-atoms Missing). C11 Check
RESPONSE: This is due to disordered solvent which appears as a fragment in the 
assymetric unit but grows to a repeating chain, due to the high symmetry of the 
crystal. The full solvent molecule could not be modeled. Based on conditions to
grow the crystal, we believe the solvent is n-hexane. 
;
####################################################################### 
# 
# 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_p21_n_a
_database_code_depnum_ccdc_archive 'CCDC 1905886'
loop_
_audit_author_name
_audit_author_address
'Kelly E Aldrich'
;Michigan State University
United States of America
;
_audit_update_record             
;
2019-03-27 deposited with the CCDC.	2019-05-07 downloaded from the CCDC.
;
_audit_creation_date             2019-03-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C19 H35 Cr N3 O'
_chemical_formula_sum            'C19 H35 Cr N3 O'
_chemical_formula_weight         373.50
_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 0.0181 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'
Cr Cr -0.1635 2.4439 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.1061(3)
_cell_length_b                   9.1819(2)
_cell_length_c                   25.8150(9)
_cell_angle_alpha                90
_cell_angle_beta                 93.065(2)
_cell_angle_gamma                90
_cell_volume                     2155.34(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5279
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.72
_cell_measurement_theta_min      3.43
_shelx_estimated_absorpt_T_max   0.547
_shelx_estimated_absorpt_T_min   0.397
_exptl_absorpt_coefficient_mu    4.427
_exptl_absorpt_correction_T_max  0.7535
_exptl_absorpt_correction_T_min  0.5502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0890 before and 0.0608 after correction. The Ratio of minimum to maximum transmission is 0.7302. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.155
_exptl_special_details           
;
Data was collected using a BRUKER CCD (charge coupled device) based
diffractometer equipped with an Oxford low-temperature apparatus operating at
173 K.  A suitable crystal was chosen and mounted on a nylon loop using 
Paratone oil.  Data  were measured using omega and phi scans of 1.0° per frame 
for 30 s. The total number of images were based on 
results from the program COSMO where redundancy was expected to be 4 and 
completeness to 0.83Å to 100%. Cell parameters were
retrieved using APEX II software and refined using SAINT on all observed
reflections.Data reduction was performed using the SAINT software which 
corrects for Lp. Scaling and absorption corrections were applied using SADABS6 
multi-scan technique, supplied by George Sheldrick.  The structures are solved 
by the direct method using the SHELXS-97 program and refined by least squares 
method on F2, SHELXL-97, incorporated in OLEX2. 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            16601
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.104
_diffrn_reflns_theta_min         3.429
_diffrn_ambient_temperature      173.01
_diffrn_detector_area_resol_mean 8.4
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3462
_reflns_number_total             4171
_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       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    
'SHELXS (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4171
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0557
_refine_ls_restrained_S_all      1.128
_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)+(0.0587P)²+2.4654P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1494
_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.a Ternary CH refined with riding coordinates:
 C007(H007), C008(H008), C009(H009), C00D(H00D)
2.b Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00B(H00B), C00C(H00C), C00H(H00K)
2.c Idealised Me refined as rotating group:
 C00F(H00E,H00F,H00G), C00G(H00H,H00I,H00J), C00I(H00L,H00M,H00N), C00J(H00O,
 H00P,H00Q), C00K(H00R,H00S,H00T), C00L(H00U,H00V,H00W), C00M(H00X,H00Y,H),
 C00N(H00Z,HA,HB), C00O(H00,HC,HD)
;
_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
Cr01 Cr 0.40397(6) 0.30092(5) 0.63792(2) 0.02357(16) Uani 1 1 d . . . . .
O002 O 0.2782(3) 0.4174(3) 0.59871(9) 0.0322(5) Uani 1 1 d . . . . .
N003 N 0.3446(3) 0.1139(3) 0.62647(10) 0.0257(5) Uani 1 1 d . . . . .
N004 N 0.3943(3) 0.3219(3) 0.69684(11) 0.0313(6) Uani 1 1 d . . . . .
N005 N 0.5898(3) 0.3578(3) 0.62536(10) 0.0265(6) Uani 1 1 d . . . . .
C006 C 0.1786(3) 0.5214(3) 0.60805(13) 0.0274(7) Uani 1 1 d . . . . .
C007 C 0.2948(4) 0.0050(4) 0.66407(13) 0.0340(8) Uani 1 1 d . . . . .
H007 H 0.2569 -0.0815 0.6440 0.041 Uiso 1 1 calc R . . . .
C008 C 0.6212(4) 0.3612(4) 0.56978(13) 0.0298(7) Uani 1 1 d . . . . .
H008 H 0.5337 0.3191 0.5501 0.036 Uiso 1 1 calc R . . . .
C009 C 0.3403(4) 0.0650(4) 0.57209(12) 0.0307(7) Uani 1 1 d . . . . .
H009 H 0.3865 0.1442 0.5519 0.037 Uiso 1 1 calc R . . . .
C00A C 0.0960(4) 0.5772(4) 0.56582(14) 0.0331(7) Uani 1 1 d . . . . .
H00A H 0.1102 0.5411 0.5320 0.040 Uiso 1 1 calc R . . . .
C00B C -0.0076(4) 0.6859(4) 0.57293(15) 0.0359(8) Uani 1 1 d . . . . .
H00B H -0.0629 0.7232 0.5436 0.043 Uiso 1 1 calc R . . . .
C00C C 0.1553(4) 0.5755(4) 0.65705(14) 0.0337(7) Uani 1 1 d . . . . .
H00C H 0.2112 0.5389 0.6863 0.040 Uiso 1 1 calc R . . . .
C00D C 0.7110(4) 0.4060(4) 0.66161(13) 0.0364(8) Uani 1 1 d . . . . .
H00D H 0.7954 0.4354 0.6406 0.044 Uiso 1 1 calc R . . . .
C00E C -0.0320(4) 0.7409(4) 0.62163(16) 0.0369(8) Uani 1 1 d . . . . .
C00F C 0.6368(4) 0.5194(4) 0.55153(15) 0.0384(8) Uani 1 1 d . . . . .
H00E H 0.5472 0.5736 0.5584 0.058 Uiso 1 1 calc GR . . . .
H00F H 0.6519 0.5207 0.5142 0.058 Uiso 1 1 calc GR . . . .
H00G H 0.7213 0.5648 0.5703 0.058 Uiso 1 1 calc GR . . . .
C00G C 0.7537(4) 0.2678(4) 0.55748(16) 0.0426(9) Uani 1 1 d . . . . .
H00H H 0.8423 0.3067 0.5758 0.064 Uiso 1 1 calc GR . . . .
H00I H 0.7664 0.2692 0.5200 0.064 Uiso 1 1 calc GR . . . .
H00J H 0.7375 0.1674 0.5687 0.064 Uiso 1 1 calc GR . . . .
C00H C 0.0508(4) 0.6831(4) 0.66353(15) 0.0375(8) Uani 1 1 d . . . . .
H00K H 0.0354 0.7182 0.6974 0.045 Uiso 1 1 calc R . . . .
C00I C 0.1686(4) 0.0656(4) 0.69436(15) 0.0436(9) Uani 1 1 d . . . . .
H00L H 0.2068 0.1388 0.7192 0.065 Uiso 1 1 calc GR . . . .
H00M H 0.1227 -0.0138 0.7131 0.065 Uiso 1 1 calc GR . . . .
H00N H 0.0953 0.1106 0.6702 0.065 Uiso 1 1 calc GR . . . .
C00J C 0.1821(5) 0.0507(4) 0.55016(15) 0.0428(9) Uani 1 1 d . . . . .
H00O H 0.1343 -0.0308 0.5671 0.064 Uiso 1 1 calc GR . . . .
H00P H 0.1817 0.0328 0.5127 0.064 Uiso 1 1 calc GR . . . .
H00Q H 0.1285 0.1410 0.5566 0.064 Uiso 1 1 calc GR . . . .
C00K C 0.4199(5) -0.0458(5) 0.70045(16) 0.0493(10) Uani 1 1 d . . . . .
H00R H 0.4962 -0.0908 0.6804 0.074 Uiso 1 1 calc GR . . . .
H00S H 0.3832 -0.1172 0.7248 0.074 Uiso 1 1 calc GR . . . .
H00T H 0.4616 0.0377 0.7198 0.074 Uiso 1 1 calc GR . . . .
C00L C 0.4307(5) -0.0717(4) 0.56420(16) 0.0469(10) Uani 1 1 d . . . . .
H00U H 0.5307 -0.0572 0.5793 0.070 Uiso 1 1 calc GR . . . .
H00V H 0.4345 -0.0916 0.5270 0.070 Uiso 1 1 calc GR . . . .
H00W H 0.3851 -0.1543 0.5812 0.070 Uiso 1 1 calc GR . . . .
C00M C -0.1457(5) 0.8586(4) 0.6292(2) 0.0525(11) Uani 1 1 d . . . . .
H00X H -0.1067 0.9528 0.6186 0.079 Uiso 1 1 calc GR . . . .
H00Y H -0.1683 0.8627 0.6659 0.079 Uiso 1 1 calc GR . . . .
H H -0.2354 0.8362 0.6081 0.079 Uiso 1 1 calc GR . . . .
C00N C 0.7622(5) 0.2820(6) 0.69688(18) 0.0605(13) Uani 1 1 d . . . . .
H00Z H 0.6828 0.2544 0.7191 0.091 Uiso 1 1 calc GR . . . .
HA H 0.8482 0.3132 0.7185 0.091 Uiso 1 1 calc GR . . . .
HB H 0.7887 0.1982 0.6758 0.091 Uiso 1 1 calc GR . . . .
C00O C 0.6661(5) 0.5377(5) 0.69288(18) 0.0578(12) Uani 1 1 d . . . . .
H00 H 0.6330 0.6158 0.6692 0.087 Uiso 1 1 calc GR . . . .
HC H 0.7505 0.5716 0.7148 0.087 Uiso 1 1 calc GR . . . .
HD H 0.5859 0.5104 0.7148 0.087 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
Cr01 O002 1.832(2) . ?
Cr01 N003 1.819(3) . ?
Cr01 N004 1.540(3) . ?
Cr01 N005 1.816(3) . ?
O002 C006 1.347(4) . ?
N003 C007 1.482(4) . ?
N003 C009 1.473(4) . ?
N005 C008 1.478(4) . ?
N005 C00D 1.477(4) . ?
C006 C00A 1.389(5) . ?
C006 C00C 1.386(5) . ?
C007 H007 1.0000 . ?
C007 C00I 1.530(5) . ?
C007 C00K 1.511(5) . ?
C008 H008 1.0000 . ?
C008 C00F 1.536(5) . ?
C008 C00G 1.528(5) . ?
C009 H009 1.0000 . ?
C009 C00J 1.525(5) . ?
C009 C00L 1.520(5) . ?
C00A H00A 0.9500 . ?
C00A C00B 1.392(5) . ?
C00B H00B 0.9500 . ?
C00B C00E 1.384(6) . ?
C00C H00C 0.9500 . ?
C00C C00H 1.388(5) . ?
C00D H00D 1.0000 . ?
C00D C00N 1.515(6) . ?
C00D C00O 1.522(5) . ?
C00E C00H 1.390(5) . ?
C00E C00M 1.516(5) . ?
C00F H00E 0.9800 . ?
C00F H00F 0.9800 . ?
C00F H00G 0.9800 . ?
C00G H00H 0.9800 . ?
C00G H00I 0.9800 . ?
C00G H00J 0.9800 . ?
C00H H00K 0.9500 . ?
C00I H00L 0.9800 . ?
C00I H00M 0.9800 . ?
C00I H00N 0.9800 . ?
C00J H00O 0.9800 . ?
C00J H00P 0.9800 . ?
C00J H00Q 0.9800 . ?
C00K H00R 0.9800 . ?
C00K H00S 0.9800 . ?
C00K H00T 0.9800 . ?
C00L H00U 0.9800 . ?
C00L H00V 0.9800 . ?
C00L H00W 0.9800 . ?
C00M H00X 0.9800 . ?
C00M H00Y 0.9800 . ?
C00M H 0.9800 . ?
C00N H00Z 0.9800 . ?
C00N HA 0.9800 . ?
C00N HB 0.9800 . ?
C00O H00 0.9800 . ?
C00O HC 0.9800 . ?
C00O HD 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N003 Cr01 O002 106.83(12) . . ?
N004 Cr01 O002 113.92(13) . . ?
N004 Cr01 N003 104.26(13) . . ?
N004 Cr01 N005 104.09(14) . . ?
N005 Cr01 O002 107.13(12) . . ?
N005 Cr01 N003 120.91(12) . . ?
C006 O002 Cr01 136.2(2) . . ?
C007 N003 Cr01 129.0(2) . . ?
C009 N003 Cr01 115.8(2) . . ?
C009 N003 C007 115.2(3) . . ?
C008 N005 Cr01 114.2(2) . . ?
C00D N005 Cr01 130.2(2) . . ?
C00D N005 C008 115.6(3) . . ?
O002 C006 C00A 117.5(3) . . ?
O002 C006 C00C 123.7(3) . . ?
C00C C006 C00A 118.7(3) . . ?
N003 C007 H007 107.8 . . ?
N003 C007 C00I 110.7(3) . . ?
N003 C007 C00K 111.6(3) . . ?
C00I C007 H007 107.8 . . ?
C00K C007 H007 107.8 . . ?
C00K C007 C00I 110.9(3) . . ?
N005 C008 H008 107.1 . . ?
N005 C008 C00F 110.1(3) . . ?
N005 C008 C00G 112.7(3) . . ?
C00F C008 H008 107.1 . . ?
C00G C008 H008 107.1 . . ?
C00G C008 C00F 112.4(3) . . ?
N003 C009 H009 106.5 . . ?
N003 C009 C00J 110.9(3) . . ?
N003 C009 C00L 113.1(3) . . ?
C00J C009 H009 106.5 . . ?
C00L C009 H009 106.5 . . ?
C00L C009 C00J 112.7(3) . . ?
C006 C00A H00A 119.9 . . ?
C006 C00A C00B 120.2(3) . . ?
C00B C00A H00A 119.9 . . ?
C00A C00B H00B 119.2 . . ?
C00E C00B C00A 121.6(3) . . ?
C00E C00B H00B 119.2 . . ?
C006 C00C H00C 119.8 . . ?
C006 C00C C00H 120.3(3) . . ?
C00H C00C H00C 119.8 . . ?
N005 C00D H00D 107.9 . . ?
N005 C00D C00N 110.6(3) . . ?
N005 C00D C00O 111.2(3) . . ?
C00N C00D H00D 107.9 . . ?
C00N C00D C00O 111.1(4) . . ?
C00O C00D H00D 107.9 . . ?
C00B C00E C00H 117.4(3) . . ?
C00B C00E C00M 121.5(4) . . ?
C00H C00E C00M 121.1(4) . . ?
C008 C00F H00E 109.5 . . ?
C008 C00F H00F 109.5 . . ?
C008 C00F H00G 109.5 . . ?
H00E C00F H00F 109.5 . . ?
H00E C00F H00G 109.5 . . ?
H00F C00F H00G 109.5 . . ?
C008 C00G H00H 109.5 . . ?
C008 C00G H00I 109.5 . . ?
C008 C00G H00J 109.5 . . ?
H00H C00G H00I 109.5 . . ?
H00H C00G H00J 109.5 . . ?
H00I C00G H00J 109.5 . . ?
C00C C00H C00E 121.6(3) . . ?
C00C C00H H00K 119.2 . . ?
C00E C00H H00K 119.2 . . ?
C007 C00I H00L 109.5 . . ?
C007 C00I H00M 109.5 . . ?
C007 C00I H00N 109.5 . . ?
H00L C00I H00M 109.5 . . ?
H00L C00I H00N 109.5 . . ?
H00M C00I H00N 109.5 . . ?
C009 C00J H00O 109.5 . . ?
C009 C00J H00P 109.5 . . ?
C009 C00J H00Q 109.5 . . ?
H00O C00J H00P 109.5 . . ?
H00O C00J H00Q 109.5 . . ?
H00P C00J H00Q 109.5 . . ?
C007 C00K H00R 109.5 . . ?
C007 C00K H00S 109.5 . . ?
C007 C00K H00T 109.5 . . ?
H00R C00K H00S 109.5 . . ?
H00R C00K H00T 109.5 . . ?
H00S C00K H00T 109.5 . . ?
C009 C00L H00U 109.5 . . ?
C009 C00L H00V 109.5 . . ?
C009 C00L H00W 109.5 . . ?
H00U C00L H00V 109.5 . . ?
H00U C00L H00W 109.5 . . ?
H00V C00L H00W 109.5 . . ?
C00E C00M H00X 109.5 . . ?
C00E C00M H00Y 109.5 . . ?
C00E C00M H 109.5 . . ?
H00X C00M H00Y 109.5 . . ?
H00X C00M H 109.5 . . ?
H00Y C00M H 109.5 . . ?
C00D C00N H00Z 109.5 . . ?
C00D C00N HA 109.5 . . ?
C00D C00N HB 109.5 . . ?
H00Z C00N HA 109.5 . . ?
H00Z C00N HB 109.5 . . ?
HA C00N HB 109.5 . . ?
C00D C00O H00 109.5 . . ?
C00D C00O HC 109.5 . . ?
C00D C00O HD 109.5 . . ?
H00 C00O HC 109.5 . . ?
H00 C00O HD 109.5 . . ?
HC C00O HD 109.5 . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_DK_III_13feb2018_1
_database_code_depnum_ccdc_archive 'CCDC 1907834'
loop_
_audit_author_name
_audit_author_address
'Kelly Aldrich'
;Michigan State University
United States of America
;
_audit_update_record             
;
2019-04-03 deposited with the CCDC.	2019-05-07 downloaded from the CCDC.
;
_audit_creation_date             2019-03-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_formula_moiety         'C44 H60 O4 Ti, 0.75(C6 H14)'
_chemical_formula_sum            'C48.5 H70.5 O4 Ti'
_chemical_formula_weight         765.46
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Ti 0.29130 0.45317 9.75950 7.35580 1.69910 1.90210 7.85080 0.50000 35.63380
116.10500 1.28069996834
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y,-z+1/2
3 -x,-y,-z
4 x,-y,z-1/2
5 x+1/2,y+1/2,z
6 -x+1/2,y+1/2,-z+1/2
7 -x+1/2,-y+1/2,-z
8 x+1/2,-y+1/2,z-1/2

_symmetry_Int_Tables_number      15
_cell_length_a                   22.452(2)
_cell_length_b                   9.4744(8)
_cell_length_c                   22.253(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.7100(10)
_cell_angle_gamma                90
_cell_volume                     4733.3(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6652
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.33
_exptl_absorpt_coefficient_mu    0.219
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0715 before and 0.0478 after correction. The Ratio of minimum to maximum transmission is 0.9168. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear orangish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.0741
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1663.8352
_exptl_crystal_size_max          0.432
_exptl_crystal_size_mid          0.402
_exptl_crystal_size_min          0.21
_exptl_special_details           
;
Data was collected using a BRUKER CCD (charge coupled device) based
diffractometer equipped with an Oxford low-temperature apparatus operating at
173 K.  A suitable crystal was chosen and mounted on a nylon loop using 
Paratone oil.  Data  were measured using omega scans of 0.5° per frame 
for 30 s. The total number of images were based on 
results from the program COSMO where redundancy was expected to be 4 and 
completeness to 0.83Å to 100%. Cell parameters were
retrieved using APEX II software and refined using SAINT on all observed
reflections.Data reduction was performed using the SAINT software which 
corrects for Lp. Scaling and absorption corrections were applied using SADABS6 
multi-scan technique, supplied by George Sheldrick.  The structure was solved 
by the direct method using the SHELXT program and refined by least squares 
method on F2, SHELXL, incorporated in OLEX2. 
;
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18717
_diffrn_reflns_theta_full        25.4042
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_min         1.81
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 8.36
_diffrn_measured_fraction_theta_full 0.9989
_diffrn_measured_fraction_theta_max 0.9989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              26
_reflns_limit_h_min              -26
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                3350
_reflns_number_total             4367
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.6453
_refine_diff_density_min         -0.3466
_refine_diff_density_rms         0.0673
_refine_ls_d_res_high            0.8284
_refine_ls_d_res_low             11.2249
_refine_ls_goodness_of_fit_ref   1.0323
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    54
_refine_ls_number_parameters     242
_refine_ls_number_reflns         4367
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0601
_refine_ls_restrained_S_all      1.0322
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1292P)²+1.8643P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1751
_refine_ls_wR_factor_ref         0.1958
_refine_special_details          
;
The structure was refined by Least Squares using version 2018/3 
of XL (Sheldrick, 2015) incorporated in Olex2 (Dolomanov et al., 2009). 
All non-hydrogen atoms were refined anisotropically. 
Hydrogen atom positions were calculated geometrically and refined using the 
riding model, except for the Hydrogen atom on the nitrogen atom which was found 
by difference Fourier methods and refined isotropically.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C24-C25
 1.55 with sigma of 0.02
3. Others
 Fixed Sof: C24(0.75) H24a(0.75) H24b(0.75) C23(0.75) H23b(0.75) H23a(0.75)
 C25(0.75) H25a(0.75) H25b(0.75) H25c(0.75)
4.a Riding coordinates:
 C25(H25a,H25b,H25c)
4.b Secondary CH2 refined with riding coordinates:
 C24(H24a,H24b), C23(H23a,H23b)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C16(H16), C3(H3), C13(H13), C14(H14), C5(H5)
4.d Idealised Me refined as rotating group:
 C21(H21a,H21b,H21c), C10(H10a,H10b,H10c), C9(H9a,H9b,H9c), C20(H20a,H20b,
 H20c), C11(H11a,H11b,H11c), C22(H22a,H22b,H22c), C18(H18a,H18b,H18c), C7(H7a,
 H7b,H7c)
;
_atom_sites_solution_primary     dual
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ti1 Ti 0.5 0.37451(6) 0.75 0.0379(2) Uani 1.000000 2 S T P
O1 O 0.52709(9) 0.26660(18) 0.69091(8) 0.0504(5) Uani 1.000000 1 . . .
O2 O 0.55819(8) 0.48367(19) 0.77880(9) 0.0534(5) Uani 1.000000 1 . . .
C1 C 0.55228(10) 0.1509(2) 0.66444(10) 0.0387(5) Uani 1.000000 1 . . .
C6 C 0.55708(11) 0.1437(2) 0.60193(10) 0.0388(5) Uani 1.000000 1 . . .
C12 C 0.58289(11) 0.6048(2) 0.80133(11) 0.0389(5) Uani 1.000000 1 . . .
C17 C 0.64472(10) 0.6207(2) 0.80468(11) 0.0379(5) Uani 1.000000 1 . . .
C19 C 0.68733(11) 0.5045(3) 0.78423(12) 0.0452(6) Uani 1.000000 1 . . .
C2 C 0.57143(11) 0.0422(3) 0.70158(11) 0.0447(6) Uani 1.000000 1 . . .
H2 H 0.56699(11) 0.0503(3) 0.74384(11) 0.0537(7) Uiso 1.000000 1 R . .
C16 C 0.66477(11) 0.7492(2) 0.82747(12) 0.0447(6) Uani 1.000000 1 . . .
H16 H 0.70655(11) 0.7635(2) 0.83095(12) 0.0536(7) Uiso 1.000000 1 R . .
C8 C 0.53416(12) 0.2615(3) 0.56059(11) 0.0461(6) Uani 1.000000 1 . . .
C3 C 0.59671(11) -0.0770(3) 0.67802(12) 0.0474(6) Uani 1.000000 1 . . .
H3 H 0.60956(11) -0.1511(3) 0.70383(12) 0.0569(8) Uiso 1.000000 1 R . .
C15 C 0.62748(12) 0.8578(3) 0.84543(12) 0.0467(6) Uani 1.000000 1 . . .
C13 C 0.54441(11) 0.7104(3) 0.81977(11) 0.0439(6) Uani 1.000000 1 . . .
H13 H 0.50258(11) 0.6959(3) 0.81726(11) 0.0527(7) Uiso 1.000000 1 R . .
C14 C 0.56665(12) 0.8367(3) 0.84179(11) 0.0451(6) Uani 1.000000 1 . . .
H14 H 0.54014(12) 0.9087(3) 0.85438(11) 0.0541(7) Uiso 1.000000 1 R . .
C5 C 0.58342(12) 0.0210(3) 0.58014(11) 0.0474(6) Uani 1.000000 1 . . .
H5 H 0.58800(12) 0.0118(3) 0.53794(11) 0.0569(7) Uiso 1.000000 1 R . .
C4 C 0.60341(12) -0.0888(3) 0.61682(13) 0.0519(7) Uani 1.000000 1 . . .
C21 C 0.67666(14) 0.3699(3) 0.82078(15) 0.0598(8) Uani 1.000000 1 . . .
H21a H 0.6793(9) 0.3918(5) 0.86377(15) 0.0897(12) Uiso 1.000000 1 GR . .
H21b H 0.6370(4) 0.3324(13) 0.8112(7) 0.0897(12) Uiso 1.000000 1 GR . .
H21c H 0.7069(6) 0.2993(8) 0.8108(7) 0.0897(12) Uiso 1.000000 1 GR . .
C10 C 0.56579(16) 0.4005(3) 0.57526(13) 0.0625(8) Uani 1.000000 1 . . .
H10a H 0.5533(8) 0.4341(12) 0.6148(5) 0.0938(12) Uiso 1.000000 1 GR . .
H10b H 0.60898(16) 0.3854(6) 0.5757(10) 0.0938(12) Uiso 1.000000 1 GR . .
H10c H 0.5554(8) 0.4710(7) 0.5447(6) 0.0938(12) Uiso 1.000000 1 GR . .
C9 C 0.46677(14) 0.2785(3) 0.56764(13) 0.0627(8) Uani 1.000000 1 . . .
H9a H 0.44697(16) 0.1888(8) 0.5585(10) 0.0941(12) Uiso 1.000000 1 GR . .
H9b H 0.45806(16) 0.306(2) 0.6090(3) 0.0941(12) Uiso 1.000000 1 GR . .
H9c H 0.4522(2) 0.3515(17) 0.5399(7) 0.0941(12) Uiso 1.000000 1 GR . .
C20 C 0.67760(14) 0.4754(3) 0.71695(14) 0.0636(8) Uani 1.000000 1 . . .
H20a H 0.6367(4) 0.443(2) 0.7099(2) 0.0955(12) Uiso 1.000000 1 GR . .
H20b H 0.6844(10) 0.5623(7) 0.69414(17) 0.0955(12) Uiso 1.000000 1 GR . .
H20c H 0.7055(7) 0.4025(18) 0.7038(3) 0.0955(12) Uiso 1.000000 1 GR . .
C11 C 0.54592(16) 0.2275(3) 0.49398(12) 0.0631(8) Uani 1.000000 1 . . .
H11a H 0.58895(16) 0.222(2) 0.4875(2) 0.0947(12) Uiso 1.000000 1 GR . .
H11b H 0.5275(8) 0.1369(12) 0.4836(3) 0.0947(12) Uiso 1.000000 1 GR . .
H11c H 0.5288(9) 0.3020(13) 0.46858(13) 0.0947(12) Uiso 1.000000 1 GR . .
C22 C 0.75261(12) 0.5460(3) 0.79311(17) 0.0669(9) Uani 1.000000 1 . . .
H22a H 0.7609(3) 0.6316(14) 0.7700(8) 0.1004(13) Uiso 1.000000 1 GR . .
H22b H 0.7606(3) 0.564(2) 0.8358(2) 0.1004(13) Uiso 1.000000 1 GR . .
H22c H 0.77821(12) 0.4691(11) 0.7792(10) 0.1004(13) Uiso 1.000000 1 GR . .
C18 C 0.65277(17) 0.9957(3) 0.86795(17) 0.0705(9) Uani 1.000000 1 . . .
H18a H 0.6401(9) 1.0116(12) 0.9094(4) 0.1058(14) Uiso 1.000000 1 GR . .
H18b H 0.69636(17) 0.9922(10) 0.8667(10) 0.1058(14) Uiso 1.000000 1 GR . .
H18c H 0.6383(8) 1.0729(4) 0.8424(6) 0.1058(14) Uiso 1.000000 1 GR . .
C7 C 0.63199(19) -0.2185(3) 0.58921(17) 0.0838(11) Uani 1.000000 1 . . .
H7a H 0.6750(3) -0.2171(15) 0.5974(11) 0.1257(17) Uiso 1.000000 1 GR . .
H7b H 0.6146(9) -0.3037(3) 0.6067(9) 0.1257(17) Uiso 1.000000 1 GR . .
H7c H 0.6248(11) -0.2183(15) 0.5457(2) 0.1257(17) Uiso 1.000000 1 GR . .
C24 C 0.7289(4) 0.4379(9) 0.4850(4) 0.131(2) Uiso 0.750000 1 D . .
H24a H 0.7450(4) 0.4415(9) 0.4438(4) 0.157(3) Uiso 0.750000 1 R . .
H24b H 0.6859(4) 0.4185(9) 0.4794(4) 0.157(3) Uiso 0.750000 1 R . .
C23 C 0.7507(5) 0.3096(9) 0.5066(5) 0.161(3) Uiso 0.750000 1 . . .
H23b H 0.7939(5) 0.3281(9) 0.5106(5) 0.194(4) Uiso 0.750000 1 R . .
H23a H 0.7360(5) 0.3082(9) 0.5484(5) 0.194(4) Uiso 0.750000 1 R . .
C25 C 0.7293(7) 0.5615(15) 0.4999(8) 0.281(7) Uiso 0.750000 1 D . .
H25a H 0.7699(7) 0.5910(15) 0.5106(8) 0.422(10) Uiso 0.750000 1 R . .
H25b H 0.7148(7) 0.6177(15) 0.4658(8) 0.422(10) Uiso 0.750000 1 R . .
H25c H 0.7032(7) 0.5759(15) 0.5344(8) 0.422(10) Uiso 0.750000 1 R . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O1 1.7788(17) 2_656 ?
Ti1 O1 1.7788(17) . ?
Ti1 O2 1.7794(18) . ?
Ti1 O2 1.7794(18) 2_656 ?
O1 C1 1.370(3) . ?
O2 C12 1.367(3) . ?
C1 C6 1.398(3) . ?
C1 C2 1.386(3) . ?
C6 C8 1.531(3) . ?
C6 C5 1.394(3) . ?
C12 C17 1.397(3) . ?
C12 C13 1.387(3) . ?
C17 C19 1.531(3) . ?
C17 C16 1.392(3) . ?
C19 C21 1.533(4) . ?
C19 C20 1.535(4) . ?
C19 C22 1.528(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.371(4) . ?
C16 H16 0.9500 . ?
C16 C15 1.389(4) . ?
C8 C10 1.529(4) . ?
C8 C9 1.532(4) . ?
C8 C11 1.543(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.377(4) . ?
C15 C14 1.382(4) . ?
C15 C18 1.508(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.384(4) . ?
C14 H14 0.9500 . ?
C5 H5 0.9500 . ?
C5 C4 1.393(4) . ?
C4 C7 1.519(4) . ?
C21 H21a 0.9800 . ?
C21 H21b 0.9800 . ?
C21 H21c 0.9800 . ?
C10 H10a 0.9800 . ?
C10 H10b 0.9800 . ?
C10 H10c 0.9800 . ?
C9 H9a 0.9800 . ?
C9 H9b 0.9800 . ?
C9 H9c 0.9800 . ?
C20 H20a 0.9800 . ?
C20 H20b 0.9800 . ?
C20 H20c 0.9800 . ?
C11 H11a 0.9800 . ?
C11 H11b 0.9800 . ?
C11 H11c 0.9800 . ?
C22 H22a 0.9800 . ?
C22 H22b 0.9800 . ?
C22 H22c 0.9800 . ?
C18 H18a 0.9800 . ?
C18 H18b 0.9800 . ?
C18 H18c 0.9800 . ?
C7 H7a 0.9800 . ?
C7 H7b 0.9800 . ?
C7 H7c 0.9800 . ?
C24 H24a 0.9900 . ?
C24 H24b 0.9900 . ?
C24 C23 1.394(10) . ?
C24 C25 1.217(13) . ?
C23 C23 1.167(16) 7_656 ?
C23 H23b 0.9900 . ?
C23 H23a 0.9900 . ?
C25 H25a 0.9800 . ?
C25 H25b 0.9799 . ?
C25 H25c 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 O1 109.84(12) . 2_656 ?
O2 Ti1 O1 110.12(9) 2_656 2_656 ?
O2 Ti1 O1 108.91(9) 2_656 . ?
O2 Ti1 O1 108.91(9) . 2_656 ?
O2 Ti1 O1 110.12(9) . . ?
O2 Ti1 O2 108.92(12) . 2_656 ?
C1 O1 Ti1 157.59(16) . 2_656 ?
C12 O2 Ti1 155.88(17) . 2_656 ?
C6 C1 O1 120.3(2) . . ?
C2 C1 O1 117.7(2) . . ?
C2 C1 C6 122.0(2) . . ?
C8 C6 C1 122.2(2) . . ?
C5 C6 C1 115.2(2) . . ?
C5 C6 C8 122.7(2) . . ?
C17 C12 O2 120.6(2) . . ?
C13 C12 O2 117.5(2) . . ?
C13 C12 C17 121.9(2) . . ?
C19 C17 C12 122.0(2) . . ?
C16 C17 C12 115.5(2) . . ?
C16 C17 C19 122.5(2) . . ?
C21 C19 C17 109.8(2) . . ?
C20 C19 C17 109.7(2) . . ?
C20 C19 C21 110.3(2) . . ?
C22 C19 C17 112.2(2) . . ?
C22 C19 C21 107.5(2) . . ?
C22 C19 C20 107.3(2) . . ?
H2 C2 C1 119.64(15) . . ?
C3 C2 C1 120.7(2) . . ?
C3 C2 H2 119.64(14) . . ?
H16 C16 C17 117.97(14) . . ?
C15 C16 C17 124.1(2) . . ?
C15 C16 H16 117.97(15) . . ?
C10 C8 C6 110.3(2) . . ?
C9 C8 C6 109.9(2) . . ?
C9 C8 C10 110.1(2) . . ?
C11 C8 C6 111.4(2) . . ?
C11 C8 C10 107.5(2) . . ?
C11 C8 C9 107.5(2) . . ?
H3 C3 C2 120.12(14) . . ?
C4 C3 C2 119.8(2) . . ?
C4 C3 H3 120.12(15) . . ?
C14 C15 C16 118.4(2) . . ?
C18 C15 C16 120.8(3) . . ?
C18 C15 C14 120.8(3) . . ?
H13 C13 C12 119.83(14) . . ?
C14 C13 C12 120.3(2) . . ?
C14 C13 H13 119.83(15) . . ?
C13 C14 C15 119.9(2) . . ?
H14 C14 C15 120.07(15) . . ?
H14 C14 C13 120.07(15) . . ?
H5 C5 C6 118.18(14) . . ?
C4 C5 C6 123.6(2) . . ?
C4 C5 H5 118.18(16) . . ?
C5 C4 C3 118.7(2) . . ?
C7 C4 C3 121.2(3) . . ?
C7 C4 C5 120.1(3) . . ?
H21a C21 C19 109.5 . . ?
H21b C21 C19 109.5 . . ?
H21b C21 H21a 109.5 . . ?
H21c C21 C19 109.5 . . ?
H21c C21 H21a 109.5 . . ?
H21c C21 H21b 109.5 . . ?
H10a C10 C8 109.5 . . ?
H10b C10 C8 109.5 . . ?
H10b C10 H10a 109.5 . . ?
H10c C10 C8 109.5 . . ?
H10c C10 H10a 109.5 . . ?
H10c C10 H10b 109.5 . . ?
H9a C9 C8 109.5 . . ?
H9b C9 C8 109.5 . . ?
H9b C9 H9a 109.5 . . ?
H9c C9 C8 109.5 . . ?
H9c C9 H9a 109.5 . . ?
H9c C9 H9b 109.5 . . ?
H20a C20 C19 109.5 . . ?
H20b C20 C19 109.5 . . ?
H20b C20 H20a 109.5 . . ?
H20c C20 C19 109.5 . . ?
H20c C20 H20a 109.5 . . ?
H20c C20 H20b 109.5 . . ?
H11a C11 C8 109.5 . . ?
H11b C11 C8 109.5 . . ?
H11b C11 H11a 109.5 . . ?
H11c C11 C8 109.5 . . ?
H11c C11 H11a 109.5 . . ?
H11c C11 H11b 109.5 . . ?
H22a C22 C19 109.5 . . ?
H22b C22 C19 109.5 . . ?
H22b C22 H22a 109.5 . . ?
H22c C22 C19 109.5 . . ?
H22c C22 H22a 109.5 . . ?
H22c C22 H22b 109.5 . . ?
H18a C18 C15 109.5 . . ?
H18b C18 C15 109.5 . . ?
H18b C18 H18a 109.5 . . ?
H18c C18 C15 109.5 . . ?
H18c C18 H18a 109.5 . . ?
H18c C18 H18b 109.5 . . ?
H7a C7 C4 109.5 . . ?
H7b C7 C4 109.5 . . ?
H7b C7 H7a 109.5 . . ?
H7c C7 C4 109.5 . . ?
H7c C7 H7a 109.5 . . ?
H7c C7 H7b 109.5 . . ?
H24b C24 H24a 105.0 . . ?
C23 C24 H24a 102.6(6) . . ?
C23 C24 H24b 102.6(6) . . ?
C25 C24 H24a 102.6(10) . . ?
C25 C24 H24b 102.6(10) . . ?
C25 C24 C23 138.0(12) . . ?
C23 C23 C24 138.5(14) 7_656 . ?
H23b C23 C24 102.5(6) . . ?
H23a C23 C24 102.5(6) . . ?
H23a C23 H23b 104.9 . . ?
H25a C25 C24 110.2 . . ?
H25b C25 C24 108.1 . . ?
H25b C25 H25a 109.5 . . ?
H25c C25 C24 110.1 . . ?
H25c C25 H25a 109.5 . . ?
H25c C25 H25b 109.5 . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_restr_distance_atom_site_label_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
_restr_distance_diff
C24 C25 1 1.5500 0.0200 0.3330

####################################################################### 
# 
# 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_rjs
_database_code_depnum_ccdc_archive 'CCDC 1905884'
loop_
_audit_author_name
_audit_author_address
'Kelly E Aldrich'
;Michigan State University
United States of America
;
_audit_update_record             
;
2019-03-27 deposited with the CCDC.	2019-05-07 downloaded from the CCDC.
;
_audit_creation_date             2019-03-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C29 H44 O4 Ti, C H Cl3'
_chemical_formula_sum            'C30 H45 Cl3 O4 Ti'
_chemical_formula_weight         623.91
_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 0.0181 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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.57250(10)
_cell_length_b                   12.38990(10)
_cell_length_c                   13.0612(2)
_cell_angle_alpha                67.6580(10)
_cell_angle_beta                 80.5460(10)
_cell_angle_gamma                66.6990(10)
_cell_volume                     1590.67(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5635
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.02
_cell_measurement_theta_min      3.66
_shelx_estimated_absorpt_T_max   0.625
_shelx_estimated_absorpt_T_min   0.429
_exptl_absorpt_coefficient_mu    4.849
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0790 before and 0.0592 after correction. The Ratio of minimum to maximum transmission is 0.7854. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.107
_exptl_special_details           
;
Data was collected using a BRUKER CCD (charge coupled device) based
diffractometer equipped with an Oxford low-temperature apparatus operating at
173 K.  A suitable crystal was chosen and mounted on a nylon loop using 
Paratone oil.  Data  were measured using omega and phi scans of 1.0° per frame 
for 30 s. The total number of images were based on 
results from the program COSMO where redundancy was expected to be 4 and 
completeness to 0.83Å to 100%. Cell parameters were
retrieved using APEX II software and refined using SAINT on all observed
reflections.Data reduction was performed using the SAINT software which 
corrects for Lp. Scaling and absorption corrections were applied using SADABS6 
multi-scan technique, supplied by George Sheldrick.  The structure was solved 
by the direct method using the SHELXT program and refined by least squares 
method on F2, SHELXL, incorporated in OLEX2. 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            20754
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.176
_diffrn_reflns_theta_min         3.659
_diffrn_ambient_temperature      173.01
_diffrn_detector_area_resol_mean 8.36
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4246
_reflns_number_total             5629
_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       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         5629
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0509
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0844P)²+0.1693P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1479
_refine_special_details          
;
The structure was refined by Least Squares using version 2018/3 
of XL (Sheldrick, 2015) incorporated in Olex2 (Dolomanov et al., 2009). 
All non-hydrogen atoms were refined anisotropically. 
Hydrogen atom positions were calculated geometrically and refined using the 
riding model, except for the hydrogen atom(s) on the non-carbon atom(s) 
which was found by difference Fourier methods and refined isotropically.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1-C2 \\sim C011-C010 \\sim C1-C0 \\sim C012-C011
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C012) = Uanis(C0)
Uanis(C010) = Uanis(C2)
Uanis(C011) = Uanis(C1)
4. Others
 Sof(C1)=Sof(H1)=Sof(C0)=Sof(H0A)=Sof(H0B)=Sof(H0C)=Sof(C2)=Sof(H2A)=Sof(H2B)=
 Sof(H2C)=1-FVAR(1)
 Sof(C010)=Sof(H01A)=Sof(H01B)=Sof(H01C)=Sof(C011)=Sof(H011)=Sof(C012)=
 Sof(H01D)=Sof(H01E)=Sof(H01F)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C00O(H00O), C00Z(H2AA), C011(H011), C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C00J(H00A,H00C)
5.c Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00E(H00E), C00G(H00G), C00N(H00N)
5.d Idealised Me refined as rotating group:
 C00P(H00D,H00F,H00H), C00Q(H00I,H00J,H00K), C00R(H00L,H00M,H00P), C00S(H00Q,
 H00R,H00S), C00T(H00T,H00U,H00V), C00U(H00W,H00X,H00Y), C00V(H00Z,H,HA),
 C00W(H00,HB,HC), C00X(H0AA,HD,HE), C00Y(H1AA,HF,HG), C010(H01A,H01B,H01C),
 C012(H01D,H01E,H01F), C0(H0A,H0B,H0C), C2(H2A,H2B,H2C)
;
_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
Ti01 Ti 0.48603(5) 0.52752(5) 0.36858(4) 0.02139(16) Uani 1 1 d . . . . .
Cl02 Cl 0.75666(11) 0.88916(12) 0.34815(9) 0.0608(3) Uani 1 1 d . . . . .
Cl03 Cl 0.85929(14) 0.97491(12) 0.47651(11) 0.0732(4) Uani 1 1 d . . . . .
Cl04 Cl 0.87203(12) 0.72048(12) 0.55727(13) 0.0832(5) Uani 1 1 d . . . . .
O005 O 0.38920(18) 0.53055(18) 0.51227(16) 0.0234(4) Uani 1 1 d . . . . .
O006 O 0.34229(19) 0.64371(19) 0.29085(17) 0.0262(5) Uani 1 1 d . . . . .
O007 O 0.5850(2) 0.59799(19) 0.25954(17) 0.0274(5) Uani 1 1 d . . . . .
O008 O 0.5020(2) 0.38784(19) 0.35257(19) 0.0316(5) Uani 1 1 d . . . . .
C009 C 0.2639(3) 0.7649(3) 0.2650(2) 0.0232(6) Uani 1 1 d . . . . .
C00A C 0.5286(3) 0.8136(3) 0.2342(2) 0.0245(6) Uani 1 1 d . . . . .
C00B C 0.6803(3) 0.8406(3) 0.0460(3) 0.0271(7) Uani 1 1 d . . . . .
H00B H 0.7297 0.8515 -0.0202 0.033 Uiso 1 1 calc R . . . .
C00C C 0.1472(3) 0.8047(3) 0.2155(2) 0.0253(6) Uani 1 1 d . . . . .
C00D C 0.6287(3) 0.9386(3) 0.0860(3) 0.0276(7) Uani 1 1 d . . . . .
C00E C 0.5492(3) 0.9247(3) 0.1784(2) 0.0260(6) Uani 1 1 d . . . . .
H00E H 0.5079 0.9932 0.2039 0.031 Uiso 1 1 calc R . . . .
C00F C 0.3005(3) 0.8485(3) 0.2882(2) 0.0246(6) Uani 1 1 d . . . . .
C00G C 0.2154(3) 0.9716(3) 0.2687(3) 0.0282(7) Uani 1 1 d . . . . .
H00G H 0.2394 1.0286 0.2844 0.034 Uiso 1 1 calc R . . . .
C00H C 0.1138(3) 0.7190(3) 0.1760(3) 0.0296(7) Uani 1 1 d . . . . .
C00I C 0.5911(3) 0.7117(3) 0.1975(2) 0.0251(6) Uani 1 1 d . . . . .
C00J C 0.4324(3) 0.8097(3) 0.3281(2) 0.0258(6) Uani 1 1 d . . . . .
H00A H 0.4314 0.8664 0.3653 0.031 Uiso 1 1 calc R . . . .
H00C H 0.4575 0.7236 0.3832 0.031 Uiso 1 1 calc R . . . .
C00K C 0.6633(3) 0.7265(3) 0.0980(3) 0.0265(7) Uani 1 1 d . . . . .
C00L C 0.7145(3) 0.6242(3) 0.0445(3) 0.0317(7) Uani 1 1 d . . . . .
C00M C 0.0969(3) 1.0123(3) 0.2270(3) 0.0306(7) Uani 1 1 d . . . . .
C00N C 0.0664(3) 0.9293(3) 0.1987(3) 0.0299(7) Uani 1 1 d . . . . .
H00N H -0.0131 0.9583 0.1665 0.036 Uiso 1 1 calc R . . . .
C00O C 0.2524(3) 0.5759(3) 0.5232(3) 0.0292(7) Uani 1 1 d . . . . .
H00O H 0.2184 0.6168 0.4465 0.035 Uiso 1 1 calc R . . . .
C00P C 0.2070(3) 0.4677(3) 0.5816(3) 0.0377(8) Uani 1 1 d . . . . .
H00D H 0.2532 0.3999 0.5524 0.057 Uiso 1 1 calc GR . . . .
H00F H 0.1168 0.4964 0.5691 0.057 Uiso 1 1 calc GR . . . .
H00H H 0.2216 0.4370 0.6612 0.057 Uiso 1 1 calc GR . . . .
C00Q C 0.6570(3) 1.0567(3) 0.0300(3) 0.0343(8) Uani 1 1 d . . . . .
H00I H 0.6844 1.0770 0.0852 0.052 Uiso 1 1 calc GR . . . .
H00J H 0.5810 1.1258 -0.0059 0.052 Uiso 1 1 calc GR . . . .
H00K H 0.7239 1.0441 -0.0258 0.052 Uiso 1 1 calc GR . . . .
C00R C 0.2081(3) 0.6766(3) 0.5745(3) 0.0376(8) Uani 1 1 d . . . . .
H00L H 0.2445 0.6415 0.6481 0.056 Uiso 1 1 calc GR . . . .
H00M H 0.1161 0.7075 0.5813 0.056 Uiso 1 1 calc GR . . . .
H00P H 0.2351 0.7459 0.5275 0.056 Uiso 1 1 calc GR . . . .
C00S C 0.2128(3) 0.6786(3) 0.0914(3) 0.0373(8) Uani 1 1 d . . . . .
H00Q H 0.2149 0.7529 0.0284 0.056 Uiso 1 1 calc GR . . . .
H00R H 0.1913 0.6244 0.0654 0.056 Uiso 1 1 calc GR . . . .
H00S H 0.2955 0.6326 0.1259 0.056 Uiso 1 1 calc GR . . . .
C00T C -0.0139(3) 0.7863(4) 0.1182(3) 0.0440(9) Uani 1 1 d . . . . .
H00T H -0.0806 0.8109 0.1708 0.066 Uiso 1 1 calc GR . . . .
H00U H -0.0300 0.7298 0.0913 0.066 Uiso 1 1 calc GR . . . .
H00V H -0.0126 0.8612 0.0555 0.066 Uiso 1 1 calc GR . . . .
C00U C 0.0038(3) 1.1443(3) 0.2097(3) 0.0426(9) Uani 1 1 d . . . . .
H00W H 0.0334 1.1836 0.2472 0.064 Uiso 1 1 calc GR . . . .
H00X H -0.0785 1.1415 0.2405 0.064 Uiso 1 1 calc GR . . . .
H00Y H -0.0036 1.1932 0.1303 0.064 Uiso 1 1 calc GR . . . .
C00V C 0.8185(4) 0.5084(3) 0.1154(3) 0.0449(9) Uani 1 1 d . . . . .
H00Z H 0.8899 0.5310 0.1180 0.067 Uiso 1 1 calc GR . . . .
H H 0.8463 0.4427 0.0828 0.067 Uiso 1 1 calc GR . . . .
HA H 0.7859 0.4776 0.1906 0.067 Uiso 1 1 calc GR . . . .
C00W C 0.1061(4) 0.6020(3) 0.2728(3) 0.0418(9) Uani 1 1 d . . . . .
H00 H 0.1889 0.5513 0.3067 0.063 Uiso 1 1 calc GR . . . .
HB H 0.0797 0.5522 0.2450 0.063 Uiso 1 1 calc GR . . . .
HC H 0.0448 0.6281 0.3283 0.063 Uiso 1 1 calc GR . . . .
C00X C 0.6047(4) 0.5901(4) 0.0307(3) 0.0418(9) Uani 1 1 d . . . . .
H0AA H 0.5656 0.5608 0.1031 0.063 Uiso 1 1 calc GR . . . .
HD H 0.6368 0.5236 -0.0013 0.063 Uiso 1 1 calc GR . . . .
HE H 0.5421 0.6643 -0.0186 0.063 Uiso 1 1 calc GR . . . .
C00Y C 0.7713(4) 0.6696(4) -0.0713(3) 0.0533(11) Uani 1 1 d . . . . .
H1AA H 0.7066 0.7426 -0.1195 0.080 Uiso 1 1 calc GR . . . .
HF H 0.8022 0.6022 -0.1022 0.080 Uiso 1 1 calc GR . . . .
HG H 0.8412 0.6929 -0.0661 0.080 Uiso 1 1 calc GR . . . .
C00Z C 0.8735(4) 0.8505(4) 0.4395(3) 0.0459(9) Uani 1 1 d . . . . .
H2AA H 0.9568 0.8258 0.4010 0.055 Uiso 1 1 calc R . . . .
C010 C 0.6087(16) 0.2714(13) 0.2354(10) 0.059(3) Uani 0.771(7) 1 d D . P A 1
H01A H 0.6180 0.3472 0.1795 0.088 Uiso 0.771(7) 1 calc GR . P A 1
H01B H 0.6039 0.2175 0.1987 0.088 Uiso 0.771(7) 1 calc GR . P A 1
H01C H 0.6813 0.2261 0.2843 0.088 Uiso 0.771(7) 1 calc GR . P A 1
C011 C 0.4891(5) 0.3076(5) 0.3031(4) 0.0483(14) Uani 0.771(7) 1 d D . P A 1
H011 H 0.4138 0.3526 0.2546 0.058 Uiso 0.771(7) 1 calc R . P A 1
C012 C 0.4746(8) 0.1924(6) 0.3994(7) 0.066(2) Uani 0.771(7) 1 d D . P A 1
H01D H 0.5523 0.1450 0.4420 0.098 Uiso 0.771(7) 1 calc GR . P A 1
H01E H 0.4579 0.1387 0.3693 0.098 Uiso 0.771(7) 1 calc GR . P A 1
H01F H 0.4043 0.2209 0.4479 0.098 Uiso 0.771(7) 1 calc GR . P A 1
C1 C 0.5507(17) 0.2648(17) 0.3479(17) 0.0483(14) Uani 0.229(7) 1 d D . P A 2
H1 H 0.6094 0.2017 0.4095 0.058 Uiso 0.229(7) 1 calc R . P A 2
C0 C 0.432(2) 0.237(3) 0.349(3) 0.066(2) Uani 0.229(7) 1 d D . P A 2
H0A H 0.4304 0.1662 0.4165 0.098 Uiso 0.229(7) 1 calc GR . P A 2
H0B H 0.4323 0.2165 0.2840 0.098 Uiso 0.229(7) 1 calc GR . P A 2
H0C H 0.3569 0.3112 0.3490 0.098 Uiso 0.229(7) 1 calc GR . P A 2
C2 C 0.597(6) 0.251(5) 0.235(3) 0.059(3) Uani 0.229(7) 1 d D . P A 2
H2A H 0.5259 0.2683 0.1930 0.088 Uiso 0.229(7) 1 calc GR . P A 2
H2B H 0.6574 0.1658 0.2463 0.088 Uiso 0.229(7) 1 calc GR . P A 2
H2C H 0.6389 0.3111 0.1948 0.088 Uiso 0.229(7) 1 calc GR . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti01 Ti01 3.2811(10) 2_666 ?
Ti01 O005 2.022(2) 2_666 ?
Ti01 O005 2.027(2) . ?
Ti01 O006 1.849(2) . ?
Ti01 O007 1.847(2) . ?
Ti01 O008 1.756(2) . ?
Cl02 C00Z 1.750(4) . ?
Cl03 C00Z 1.726(4) . ?
Cl04 C00Z 1.758(4) . ?
O005 Ti01 2.022(2) 2_666 ?
O005 C00O 1.458(4) . ?
O006 C009 1.352(3) . ?
O007 C00I 1.355(4) . ?
O008 C011 1.438(5) . ?
O008 C1 1.423(17) . ?
C009 C00C 1.414(4) . ?
C009 C00F 1.405(4) . ?
C00A C00E 1.387(4) . ?
C00A C00I 1.404(4) . ?
C00A C00J 1.514(4) . ?
C00B C00D 1.382(4) . ?
C00B C00K 1.394(5) . ?
C00C C00H 1.533(4) . ?
C00C C00N 1.405(4) . ?
C00D C00E 1.390(4) . ?
C00D C00Q 1.507(4) . ?
C00F C00G 1.400(4) . ?
C00F C00J 1.524(4) . ?
C00G C00M 1.386(5) . ?
C00H C00S 1.528(5) . ?
C00H C00T 1.538(5) . ?
C00H C00W 1.543(5) . ?
C00I C00K 1.416(4) . ?
C00K C00L 1.546(4) . ?
C00L C00V 1.534(5) . ?
C00L C00X 1.543(5) . ?
C00L C00Y 1.535(5) . ?
C00M C00N 1.392(5) . ?
C00M C00U 1.514(4) . ?
C00O C00P 1.517(5) . ?
C00O C00R 1.512(4) . ?
C010 C011 1.518(11) . ?
C011 C012 1.550(8) . ?
C1 C0 1.540(16) . ?
C1 C2 1.528(17) . ?

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
O005 Ti01 Ti01 35.92(6) 2_666 2_666 ?
O005 Ti01 Ti01 35.83(6) . 2_666 ?
O005 Ti01 O005 71.75(9) 2_666 . ?
O006 Ti01 Ti01 122.08(7) . 2_666 ?
O006 Ti01 O005 150.63(9) . 2_666 ?
O006 Ti01 O005 89.44(9) . . ?
O007 Ti01 Ti01 122.23(8) . 2_666 ?
O007 Ti01 O005 145.23(9) . . ?
O007 Ti01 O005 92.41(9) . 2_666 ?
O007 Ti01 O006 90.73(10) . . ?
O008 Ti01 Ti01 108.84(8) . 2_666 ?
O008 Ti01 O005 106.94(10) . . ?
O008 Ti01 O005 103.41(10) . 2_666 ?
O008 Ti01 O006 103.59(10) . . ?
O008 Ti01 O007 106.79(10) . . ?
Ti01 O005 Ti01 108.25(9) 2_666 . ?
C00O O005 Ti01 124.62(18) . . ?
C00O O005 Ti01 127.00(18) . 2_666 ?
C009 O006 Ti01 142.7(2) . . ?
C00I O007 Ti01 140.27(19) . . ?
C011 O008 Ti01 158.5(3) . . ?
C1 O008 Ti01 163.7(8) . . ?
O006 C009 C00C 119.6(3) . . ?
O006 C009 C00F 118.9(3) . . ?
C00F C009 C00C 121.4(3) . . ?
C00E C00A C00I 119.1(3) . . ?
C00E C00A C00J 118.5(3) . . ?
C00I C00A C00J 122.3(3) . . ?
C00D C00B C00K 123.2(3) . . ?
C009 C00C C00H 121.8(3) . . ?
C00N C00C C009 116.5(3) . . ?
C00N C00C C00H 121.6(3) . . ?
C00B C00D C00E 117.7(3) . . ?
C00B C00D C00Q 120.7(3) . . ?
C00E C00D C00Q 121.6(3) . . ?
C00A C00E C00D 121.9(3) . . ?
C009 C00F C00J 121.3(3) . . ?
C00G C00F C009 118.8(3) . . ?
C00G C00F C00J 119.8(3) . . ?
C00M C00G C00F 121.5(3) . . ?
C00C C00H C00T 112.0(3) . . ?
C00C C00H C00W 111.9(3) . . ?
C00S C00H C00C 109.3(3) . . ?
C00S C00H C00T 107.0(3) . . ?
C00S C00H C00W 109.6(3) . . ?
C00T C00H C00W 107.0(3) . . ?
O007 C00I C00A 119.7(3) . . ?
O007 C00I C00K 120.1(3) . . ?
C00A C00I C00K 120.2(3) . . ?
C00A C00J C00F 112.3(2) . . ?
C00B C00K C00I 117.4(3) . . ?
C00B C00K C00L 120.8(3) . . ?
C00I C00K C00L 121.7(3) . . ?
C00V C00L C00K 110.5(3) . . ?
C00V C00L C00X 111.1(3) . . ?
C00V C00L C00Y 107.2(3) . . ?
C00X C00L C00K 109.0(3) . . ?
C00Y C00L C00K 112.1(3) . . ?
C00Y C00L C00X 106.9(3) . . ?
C00G C00M C00N 118.2(3) . . ?
C00G C00M C00U 121.2(3) . . ?
C00N C00M C00U 120.6(3) . . ?
C00M C00N C00C 123.2(3) . . ?
O005 C00O C00P 110.9(3) . . ?
O005 C00O C00R 109.5(3) . . ?
C00R C00O C00P 115.3(3) . . ?
Cl02 C00Z Cl04 110.0(2) . . ?
Cl03 C00Z Cl02 112.5(2) . . ?
Cl03 C00Z Cl04 110.8(2) . . ?
O008 C011 C010 106.3(5) . . ?
O008 C011 C012 106.8(4) . . ?
C010 C011 C012 112.0(7) . . ?
O008 C1 C0 103.5(15) . . ?
O008 C1 C2 117(2) . . ?
C2 C1 C0 94(3) . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_dk_methoxy
_database_code_depnum_ccdc_archive 'CCDC 1907833'
loop_
_audit_author_name
_audit_author_address
'Kelly Aldrich'
;Michigan State University
United States of America
;
_audit_update_record             
;
2019-04-03 deposited with the CCDC.	2019-05-07 downloaded from the CCDC.
;
_audit_creation_date             2019-04-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C44 H60 O8 Ti'
_chemical_formula_sum            'C44 H60 O8 Ti'
_chemical_formula_weight         764.82
_chemical_absolute_configuration ad
_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 0.0181 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'
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      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   10.0587(2)
_cell_length_b                   14.8851(4)
_cell_length_c                   14.1568(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.284(2)
_cell_angle_gamma                90
_cell_volume                     2119.60(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      72.009
_cell_measurement_theta_min      3.122
_shelx_estimated_absorpt_T_max   0.828
_shelx_estimated_absorpt_T_min   0.667
_exptl_absorpt_coefficient_mu    2.107
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.093
_exptl_special_details           
;
Data was collected using a BRUKER CCD (charge coupled device) based
diffractometer equipped with an Oxford low-temperature apparatus operating at
173 K.  A suitable crystal was chosen and mounted on a nylon loop using 
Paratone oil.  Data  were measured using omega and phi scans of 1.0° per frame 
for 30 s. The total number of images were based on 
results from the program COSMO where redundancy was expected to be 4 and 
completeness to 0.83Å to 100%. Cell parameters were
retrieved using APEX II software and refined using SAINT on all observed
reflections.Data reduction was performed using the SAINT software which 
corrects for Lp. Scaling and absorption corrections were applied using SADABS6 
multi-scan technique, supplied by George Sheldrick.  The structure was solved 
by the direct method using the SHELXT program and refined by least squares 
method on F2, SHELXL, incorporated in OLEX2. 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1277
_diffrn_reflns_av_unetI/netI     0.1044
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29340
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.445
_diffrn_reflns_theta_min         2.969
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.36
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω and φ'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.913
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                6317
_reflns_number_total             8185
_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       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 
;
 Flack x determined using 2147 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.004(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         8185
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0545
_refine_ls_restrained_S_all      0.987
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0287P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1122
_refine_special_details          
;
The structure was refined by Least Squares using version 2014/6 
of XL (Sheldrick, 2008) incorporated in Olex2 (Dolomanov et al., 2009). 
All non-hydrogen atoms were refined anisotropically. 
Hydrogen atom positions were calculated geometrically and refined using the 
riding model, except for the hydrogen atom(s) on the non-carbon atom(s) 
which was found by difference Fourier methods and refined isotropically.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.6195(19)
 0.3805(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C27(H27), C17(H17), C39(H39), C36(H36), C25(H25), C38(H38), C14(H14), C3(H3),
 C5(H5), C16(H16), C28(H28), C6(H6)
3.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C19(H19A,H19B,H19C), C9(H9A,H9B,H9C), C44(H44A,H44B,
 H44C), C42(H42A,H42B,H42C), C41(H41A,H41B,H41C), C22(H22A,H22B,H22C), C30(H30A,
 H30B,H30C), C32(H32A,H32B,H32C), C43(H43A,H43B,H43C), C20(H20A,H20B,H20C),
 C21(H21A,H21B,H21C), C11(H11A,H11B,H11C), C31(H31A,H31B,H31C), C8(H8A,H8B,H8C),
  C33(H33A,H33B,H33C)
;
_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
Ti1 Ti 0.26905(12) 0.50167(8) 0.76949(11) 0.0279(2) Uani 1 1 d . . . . .
O5 O 0.8207(5) 0.7793(4) 0.6421(4) 0.0389(14) Uani 1 1 d . . . . .
O3 O 0.1701(5) 0.5105(4) 0.8736(4) 0.0404(13) Uani 1 1 d . . . . .
O2 O 0.3452(5) 0.3930(3) 0.7656(5) 0.0424(15) Uani 1 1 d . . . . .
O8 O -0.2744(6) 0.3953(4) 0.4695(4) 0.0496(15) Uani 1 1 d . . . . .
O1 O 0.3928(5) 0.5882(3) 0.7748(4) 0.0333(12) Uani 1 1 d . . . . .
O7 O -0.3181(5) 0.5359(4) 1.0431(5) 0.0482(16) Uani 1 1 d . . . . .
C4 C 0.7161(7) 0.7263(5) 0.6715(5) 0.0286(16) Uani 1 1 d . . . . .
O6 O 0.7819(6) 0.1772(4) 0.8279(5) 0.0631(19) Uani 1 1 d . . . . .
O4 O 0.1673(5) 0.5132(4) 0.6659(4) 0.0405(14) Uani 1 1 d . . . . .
C27 C -0.1705(9) 0.5823(5) 0.9181(6) 0.040(2) Uani 1 1 d . . . . .
H27 H -0.2357 0.6209 0.8914 0.048 Uiso 1 1 calc R . . . .
C35 C 0.0529(7) 0.4914(5) 0.5163(6) 0.0319(17) Uani 1 1 d . . . . .
C13 C 0.4542(7) 0.2495(4) 0.7462(6) 0.0320(19) Uani 1 1 d . . . . .
C1 C 0.4967(6) 0.6367(4) 0.7396(6) 0.0278(15) Uani 1 1 d . . . . .
C23 C 0.0496(7) 0.5164(5) 0.9186(6) 0.0326(18) Uani 1 1 d . . . . .
C40 C 0.1651(8) 0.5318(5) 0.4571(7) 0.041(2) Uani 1 1 d . . . . .
C17 C 0.5591(8) 0.3722(5) 0.8338(6) 0.0339(18) Uani 1 1 d . . . . .
H17 H 0.5529 0.4316 0.8580 0.041 Uiso 1 1 calc R . . . .
C39 C -0.0413(8) 0.4393(5) 0.6650(6) 0.0351(19) Uani 1 1 d . . . . .
H39 H -0.0317 0.4314 0.7312 0.042 Uiso 1 1 calc R . . . .
C12 C 0.4525(7) 0.3382(4) 0.7808(7) 0.0365(19) Uani 1 1 d . . . . .
C10 C 0.4023(7) 0.8875(4) 0.7746(7) 0.044(2) Uani 1 1 d . . . . .
H10A H 0.4130 0.9025 0.7077 0.066 Uiso 1 1 calc GR . . . .
H10B H 0.4821 0.9056 0.8097 0.066 Uiso 1 1 calc GR . . . .
H10C H 0.3248 0.9191 0.7998 0.066 Uiso 1 1 calc GR . . . .
C18 C 0.3367(8) 0.2079(5) 0.6926(6) 0.038(2) Uani 1 1 d . . . . .
C36 C -0.0641(8) 0.4616(5) 0.4732(6) 0.0348(18) Uani 1 1 d . . . . .
H36 H -0.0741 0.4696 0.4070 0.042 Uiso 1 1 calc R . . . .
C7 C 0.3818(7) 0.7851(5) 0.7850(6) 0.0337(18) Uani 1 1 d . . . . .
C25 C -0.1026(7) 0.4777(4) 1.0376(6) 0.0335(19) Uani 1 1 d . . . . .
H25 H -0.1250 0.4446 1.0926 0.040 Uiso 1 1 calc R . . . .
C24 C 0.0245(7) 0.4677(5) 0.9997(5) 0.0281(16) Uani 1 1 d . . . . .
C38 C -0.1554(7) 0.4086(5) 0.6208(6) 0.0325(18) Uani 1 1 d . . . . .
H38 H -0.2240 0.3802 0.6557 0.039 Uiso 1 1 calc R . . . .
C19 C 0.2127(8) 0.2061(6) 0.7558(8) 0.061(3) Uani 1 1 d . . . . .
H19A H 0.2324 0.1721 0.8135 0.091 Uiso 1 1 calc GR . . . .
H19B H 0.1391 0.1774 0.7218 0.091 Uiso 1 1 calc GR . . . .
H19C H 0.1878 0.2677 0.7725 0.091 Uiso 1 1 calc GR . . . .
C9 C 0.2512(7) 0.7638(5) 0.7342(6) 0.0389(18) Uani 1 1 d . . . . .
H9A H 0.1845 0.8090 0.7508 0.058 Uiso 1 1 calc GR . . . .
H9B H 0.2199 0.7043 0.7534 0.058 Uiso 1 1 calc GR . . . .
H9C H 0.2654 0.7646 0.6658 0.058 Uiso 1 1 calc GR . . . .
C2 C 0.4971(7) 0.7310(5) 0.7444(5) 0.0272(16) Uani 1 1 d . . . . .
C14 C 0.5686(8) 0.2011(4) 0.7668(7) 0.0383(18) Uani 1 1 d . . . . .
H14 H 0.5735 0.1408 0.7451 0.046 Uiso 1 1 calc R . . . .
C3 C 0.6102(7) 0.7734(4) 0.7094(5) 0.0266(16) Uani 1 1 d . . . . .
H3 H 0.6148 0.8371 0.7117 0.032 Uiso 1 1 calc R . . . .
C37 C -0.1668(8) 0.4208(5) 0.5228(6) 0.0358(18) Uani 1 1 d . . . . .
C5 C 0.7133(7) 0.6344(5) 0.6635(6) 0.0314(17) Uani 1 1 d . . . . .
H5 H 0.7844 0.6022 0.6354 0.038 Uiso 1 1 calc R . . . .
C34 C 0.0601(7) 0.4814(4) 0.6152(6) 0.0301(17) Uani 1 1 d . . . . .
C26 C -0.1975(7) 0.5343(5) 0.9977(6) 0.0338(18) Uani 1 1 d . . . . .
C16 C 0.6732(8) 0.3231(5) 0.8526(6) 0.0362(18) Uani 1 1 d . . . . .
H16 H 0.7451 0.3478 0.8877 0.043 Uiso 1 1 calc R . . . .
C44 C -0.3858(8) 0.3579(6) 0.5144(7) 0.048(2) Uani 1 1 d . . . . .
H44A H -0.3622 0.2990 0.5406 0.072 Uiso 1 1 calc GR . . . .
H44B H -0.4582 0.3507 0.4684 0.072 Uiso 1 1 calc GR . . . .
H44C H -0.4147 0.3977 0.5655 0.072 Uiso 1 1 calc GR . . . .
C42 C 0.2951(8) 0.4777(5) 0.4735(7) 0.045(2) Uani 1 1 d . . . . .
H42A H 0.2768 0.4134 0.4664 0.067 Uiso 1 1 calc GR . . . .
H42B H 0.3290 0.4895 0.5373 0.067 Uiso 1 1 calc GR . . . .
H42C H 0.3617 0.4961 0.4270 0.067 Uiso 1 1 calc GR . . . .
C41 C 0.1904(10) 0.6312(5) 0.4836(8) 0.059(3) Uani 1 1 d . . . . .
H41A H 0.1131 0.6675 0.4653 0.088 Uiso 1 1 calc GR . . . .
H41B H 0.2692 0.6531 0.4504 0.088 Uiso 1 1 calc GR . . . .
H41C H 0.2048 0.6361 0.5519 0.088 Uiso 1 1 calc GR . . . .
C28 C -0.0452(9) 0.5739(5) 0.8762(7) 0.041(2) Uani 1 1 d . . . . .
H28 H -0.0244 0.6063 0.8204 0.049 Uiso 1 1 calc R . . . .
C22 C 0.8929(9) 0.2107(7) 0.8835(8) 0.067(3) Uani 1 1 d . . . . .
H22A H 0.9093 0.2738 0.8674 0.100 Uiso 1 1 calc GR . . . .
H22B H 0.9725 0.1752 0.8697 0.100 Uiso 1 1 calc GR . . . .
H22C H 0.8720 0.2059 0.9508 0.100 Uiso 1 1 calc GR . . . .
C29 C 0.1296(8) 0.4083(5) 1.0499(6) 0.0372(19) Uani 1 1 d . . . . .
C15 C 0.6774(8) 0.2354(5) 0.8174(6) 0.039(2) Uani 1 1 d . . . . .
C30 C 0.1808(9) 0.3347(5) 0.9800(8) 0.053(3) Uani 1 1 d . . . . .
H30A H 0.1048 0.3022 0.9531 0.079 Uiso 1 1 calc GR . . . .
H30B H 0.2385 0.2925 1.0140 0.079 Uiso 1 1 calc GR . . . .
H30C H 0.2311 0.3633 0.9291 0.079 Uiso 1 1 calc GR . . . .
C32 C 0.0741(9) 0.3590(7) 1.1328(6) 0.053(2) Uani 1 1 d . . . . .
H32A H 0.0420 0.4022 1.1796 0.080 Uiso 1 1 calc GR . . . .
H32B H 0.1437 0.3215 1.1612 0.080 Uiso 1 1 calc GR . . . .
H32C H 0.0002 0.3208 1.1119 0.080 Uiso 1 1 calc GR . . . .
C43 C 0.1352(9) 0.5287(6) 0.3537(6) 0.055(3) Uani 1 1 d . . . . .
H43A H 0.1212 0.4662 0.3342 0.082 Uiso 1 1 calc GR . . . .
H43B H 0.2100 0.5541 0.3186 0.082 Uiso 1 1 calc GR . . . .
H43C H 0.0547 0.5637 0.3405 0.082 Uiso 1 1 calc GR . . . .
C20 C 0.3054(10) 0.2617(6) 0.6045(7) 0.058(3) Uani 1 1 d . . . . .
H20A H 0.2903 0.3247 0.6217 0.088 Uiso 1 1 calc GR . . . .
H20B H 0.2254 0.2375 0.5741 0.088 Uiso 1 1 calc GR . . . .
H20C H 0.3804 0.2579 0.5607 0.088 Uiso 1 1 calc GR . . . .
C21 C 0.3667(11) 0.1120(6) 0.6586(9) 0.077(4) Uani 1 1 d . . . . .
H21A H 0.4476 0.1124 0.6203 0.116 Uiso 1 1 calc GR . . . .
H21B H 0.2921 0.0899 0.6204 0.116 Uiso 1 1 calc GR . . . .
H21C H 0.3797 0.0726 0.7133 0.116 Uiso 1 1 calc GR . . . .
C11 C 0.9356(8) 0.7324(6) 0.6083(7) 0.048(2) Uani 1 1 d . . . . .
H11A H 0.9077 0.6841 0.5656 0.072 Uiso 1 1 calc GR . . . .
H11B H 0.9844 0.7068 0.6620 0.072 Uiso 1 1 calc GR . . . .
H11C H 0.9933 0.7744 0.5743 0.072 Uiso 1 1 calc GR . . . .
C31 C 0.2452(9) 0.4672(6) 1.0806(8) 0.063(3) Uani 1 1 d . . . . .
H31A H 0.2730 0.5050 1.0277 0.094 Uiso 1 1 calc GR . . . .
H31B H 0.3197 0.4291 1.1007 0.094 Uiso 1 1 calc GR . . . .
H31C H 0.2176 0.5053 1.1334 0.094 Uiso 1 1 calc GR . . . .
C6 C 0.6021(8) 0.5909(5) 0.6983(6) 0.0353(19) Uani 1 1 d . . . . .
H6 H 0.5976 0.5273 0.6938 0.042 Uiso 1 1 calc R . . . .
C8 C 0.3694(9) 0.7643(6) 0.8917(6) 0.049(2) Uani 1 1 d . . . . .
H8A H 0.4539 0.7776 0.9235 0.074 Uiso 1 1 calc GR . . . .
H8B H 0.3476 0.7007 0.9003 0.074 Uiso 1 1 calc GR . . . .
H8C H 0.2989 0.8014 0.9190 0.074 Uiso 1 1 calc GR . . . .
C33 C -0.4172(8) 0.5972(6) 1.0101(7) 0.045(2) Uani 1 1 d . . . . .
H33A H -0.4270 0.5912 0.9415 0.067 Uiso 1 1 calc GR . . . .
H33B H -0.3903 0.6588 1.0257 0.067 Uiso 1 1 calc GR . . . .
H33C H -0.5021 0.5837 1.0406 0.067 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
Ti1 O3 1.788(5) . ?
Ti1 O2 1.792(5) . ?
Ti1 O1 1.792(5) . ?
Ti1 O4 1.792(5) . ?
O5 C4 1.381(8) . ?
O5 C11 1.434(9) . ?
O3 C23 1.375(9) . ?
O2 C12 1.368(9) . ?
O8 C37 1.371(9) . ?
O8 C44 1.407(9) . ?
O1 C1 1.368(8) . ?
O7 C26 1.376(9) . ?
O7 C33 1.428(9) . ?
C4 C3 1.386(10) . ?
C4 C5 1.373(9) . ?
O6 C22 1.452(11) . ?
O6 C15 1.369(9) . ?
O4 C34 1.377(9) . ?
C27 H27 0.9500 . ?
C27 C26 1.363(11) . ?
C27 C28 1.400(11) . ?
C35 C40 1.532(10) . ?
C35 C36 1.395(10) . ?
C35 C34 1.410(10) . ?
C13 C12 1.408(9) . ?
C13 C18 1.532(11) . ?
C13 C14 1.387(10) . ?
C1 C2 1.405(9) . ?
C1 C6 1.391(10) . ?
C23 C24 1.383(10) . ?
C23 C28 1.413(12) . ?
C40 C42 1.552(10) . ?
C40 C41 1.547(11) . ?
C40 C43 1.494(12) . ?
C17 H17 0.9500 . ?
C17 C12 1.401(11) . ?
C17 C16 1.385(11) . ?
C39 H39 0.9500 . ?
C39 C38 1.382(11) . ?
C39 C34 1.391(11) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 C7 1.545(10) . ?
C18 C19 1.539(12) . ?
C18 C20 1.514(12) . ?
C18 C21 1.536(11) . ?
C36 H36 0.9500 . ?
C36 C37 1.391(11) . ?
C7 C9 1.528(10) . ?
C7 C2 1.526(10) . ?
C7 C8 1.548(11) . ?
C25 H25 0.9500 . ?
C25 C24 1.397(10) . ?
C25 C26 1.391(10) . ?
C24 C29 1.547(10) . ?
C38 H38 0.9500 . ?
C38 C37 1.404(11) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C2 C3 1.394(10) . ?
C14 H14 0.9500 . ?
C14 C15 1.402(11) . ?
C3 H3 0.9500 . ?
C5 H5 0.9500 . ?
C5 C6 1.386(10) . ?
C16 H16 0.9500 . ?
C16 C15 1.398(10) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C28 H28 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C29 C30 1.566(12) . ?
C29 C32 1.495(12) . ?
C29 C31 1.518(11) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C6 H6 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ti1 O2 109.4(3) . . ?
O3 Ti1 O1 107.6(3) . . ?
O3 Ti1 O4 110.4(2) . . ?
O2 Ti1 O1 110.7(2) . . ?
O2 Ti1 O4 107.7(3) . . ?
O1 Ti1 O4 111.1(3) . . ?
C4 O5 C11 116.1(6) . . ?
C23 O3 Ti1 151.9(5) . . ?
C12 O2 Ti1 150.5(5) . . ?
C37 O8 C44 119.3(7) . . ?
C1 O1 Ti1 153.7(5) . . ?
C26 O7 C33 118.3(7) . . ?
O5 C4 C3 114.6(6) . . ?
C5 C4 O5 124.0(7) . . ?
C5 C4 C3 121.4(7) . . ?
C15 O6 C22 115.4(7) . . ?
C34 O4 Ti1 146.8(5) . . ?
C26 C27 H27 120.4 . . ?
C26 C27 C28 119.2(8) . . ?
C28 C27 H27 120.4 . . ?
C36 C35 C40 120.5(7) . . ?
C36 C35 C34 116.0(7) . . ?
C34 C35 C40 123.4(7) . . ?
C12 C13 C18 122.8(7) . . ?
C14 C13 C12 115.1(7) . . ?
C14 C13 C18 122.1(6) . . ?
O1 C1 C2 120.8(7) . . ?
O1 C1 C6 118.7(6) . . ?
C6 C1 C2 120.5(7) . . ?
O3 C23 C24 121.0(7) . . ?
O3 C23 C28 115.9(7) . . ?
C24 C23 C28 123.0(7) . . ?
C35 C40 C42 109.7(7) . . ?
C35 C40 C41 111.3(7) . . ?
C41 C40 C42 108.8(7) . . ?
C43 C40 C35 112.2(7) . . ?
C43 C40 C42 107.2(7) . . ?
C43 C40 C41 107.4(8) . . ?
C12 C17 H17 118.5 . . ?
C16 C17 H17 118.5 . . ?
C16 C17 C12 122.9(7) . . ?
C38 C39 H39 119.0 . . ?
C38 C39 C34 121.9(8) . . ?
C34 C39 H39 119.0 . . ?
O2 C12 C13 121.0(7) . . ?
O2 C12 C17 118.0(6) . . ?
C17 C12 C13 121.0(7) . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
C13 C18 C19 110.1(7) . . ?
C13 C18 C21 112.2(7) . . ?
C20 C18 C13 110.5(6) . . ?
C20 C18 C19 108.8(8) . . ?
C20 C18 C21 105.9(8) . . ?
C21 C18 C19 109.1(7) . . ?
C35 C36 H36 118.5 . . ?
C37 C36 C35 123.0(7) . . ?
C37 C36 H36 118.5 . . ?
C10 C7 C8 107.5(7) . . ?
C9 C7 C10 105.9(6) . . ?
C9 C7 C8 110.2(7) . . ?
C2 C7 C10 112.5(6) . . ?
C2 C7 C9 111.5(6) . . ?
C2 C7 C8 109.1(7) . . ?
C24 C25 H25 118.8 . . ?
C26 C25 H25 118.8 . . ?
C26 C25 C24 122.5(7) . . ?
C23 C24 C25 115.7(7) . . ?
C23 C24 C29 123.7(7) . . ?
C25 C24 C29 120.6(7) . . ?
C39 C38 H38 121.1 . . ?
C39 C38 C37 117.9(7) . . ?
C37 C38 H38 121.1 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C1 C2 C7 122.9(7) . . ?
C3 C2 C1 116.0(6) . . ?
C3 C2 C7 121.1(6) . . ?
C13 C14 H14 117.8 . . ?
C13 C14 C15 124.3(7) . . ?
C15 C14 H14 117.8 . . ?
C4 C3 C2 122.6(6) . . ?
C4 C3 H3 118.7 . . ?
C2 C3 H3 118.7 . . ?
O8 C37 C36 115.4(7) . . ?
O8 C37 C38 124.7(7) . . ?
C36 C37 C38 119.9(7) . . ?
C4 C5 H5 121.6 . . ?
C4 C5 C6 116.9(7) . . ?
C6 C5 H5 121.6 . . ?
O4 C34 C35 121.2(7) . . ?
O4 C34 C39 117.7(7) . . ?
C39 C34 C35 121.1(7) . . ?
O7 C26 C25 115.2(7) . . ?
C27 C26 O7 123.8(7) . . ?
C27 C26 C25 120.9(7) . . ?
C17 C16 H16 121.6 . . ?
C17 C16 C15 116.8(8) . . ?
C15 C16 H16 121.6 . . ?
O8 C44 H44A 109.5 . . ?
O8 C44 H44B 109.5 . . ?
O8 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C27 C28 C23 118.7(8) . . ?
C27 C28 H28 120.6 . . ?
C23 C28 H28 120.6 . . ?
O6 C22 H22A 109.5 . . ?
O6 C22 H22B 109.5 . . ?
O6 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C29 C30 109.6(7) . . ?
C32 C29 C24 112.6(7) . . ?
C32 C29 C30 106.1(7) . . ?
C32 C29 C31 110.3(8) . . ?
C31 C29 C24 108.8(7) . . ?
C31 C29 C30 109.3(8) . . ?
O6 C15 C14 115.0(7) . . ?
O6 C15 C16 125.2(8) . . ?
C16 C15 C14 119.8(7) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O5 C11 H11A 109.5 . . ?
O5 C11 H11B 109.5 . . ?
O5 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C1 C6 H6 118.7 . . ?
C5 C6 C1 122.6(7) . . ?
C5 C6 H6 118.7 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O7 C33 H33A 109.5 . . ?
O7 C33 H33B 109.5 . . ?
O7 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.6195(19)
2 0.3805(19)

####################################################################### 
# 
# 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_dk_4august_final
_database_code_depnum_ccdc_archive 'CCDC 1907836'
loop_
_audit_author_name
_audit_author_address
'Kelly Aldrich'
;Michigan State University
United States of America
;
_audit_update_record             
;
2019-04-03 deposited with the CCDC.	2019-05-07 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_dk_4august_final    
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.949 Why?
RESPONSE: This is low due to the three circle geometry combined with the requested and integrated data out to 0.81 Angstroms using Copper radiation. Although this is typically calculated in the programs fine based on the initial unit cell determination, changes to the best calculated unit cell upon collection of more data and the orientation of the mounted cystal can result in a lower than expected value.
;
# Added during the CSD deposition process: Wednesday 03 April 2019 07:53 PM
# end Validation Reply Form

_audit_creation_date             2019-04-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C44 H48 F12 O4 Ti'
_chemical_formula_sum            'C44 H48 F12 O4 Ti'
_chemical_formula_weight         916.72
_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 0.0181 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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   22.0590(7)
_cell_length_b                   9.8711(3)
_cell_length_c                   22.6307(6)
_cell_angle_alpha                90
_cell_angle_beta                 110.609(2)
_cell_angle_gamma                90
_cell_volume                     4612.4(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4843
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.62
_cell_measurement_theta_min      4.17
_shelx_estimated_absorpt_T_max   0.822
_shelx_estimated_absorpt_T_min   0.332
_exptl_absorpt_coefficient_mu    2.348
_exptl_absorpt_correction_T_max  0.7535
_exptl_absorpt_correction_T_min  0.5798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1313 before and 0.0626 after correction. The Ratio of minimum to maximum transmission is 0.7695. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.603
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.087
_exptl_special_details           
;
Data was collected using a BRUKER CCD (charge coupled device) based
diffractometer equipped with an Oxford low-temperature apparatus operating at
173 K.  A suitable crystal was chosen and mounted on a nylon loop using 
Paratone oil.  Data  were measured using omega and phi scans of 1.0° per frame 
for 30 s. The total number of images were based on 
results from the program COSMO where redundancy was expected to be 4 and 
completeness to 0.83Å to 100%. Cell parameters were
retrieved using APEX II software and refined using SAINT on all observed
reflections.Data reduction was performed using the SAINT software which 
corrects for Lp. Scaling and absorption corrections were applied using SADABS6 
multi-scan technique, supplied by George Sheldrick.  The structures are solved 
by the direct method using the SHELXS-97 program and refined by least squares 
method on F2, SHELXL-97, incorporated in OLEX2. 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 0.949
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            14837
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.047
_diffrn_reflns_theta_min         4.174
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.4
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω and φ'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3234
_reflns_number_total             4284
_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       'APEX2 (BRUKER, V2012.10-0, 2012)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.174
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4284
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0885
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1677P)²+12.3775P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2590
_refine_ls_wR_factor_ref         0.2860
_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. Uiso/Uaniso restraints and constraints
Uanis(F6B) = Uanis(F6A) = Uanis(F4B) = Uanis(F4A) = Uanis(F5B) = Uanis(F5A) =
Uanis(F3A) = Uanis(F3B) = Uanis(F1A) = Uanis(F1B) = Uanis(F2A) = Uanis(F2B)
3. Others
 Fixed Sof: F2A(0.5) F1A(0.5) F3A(0.5) F4B(0.5) F5B(0.5) F6B(0.5) F1B(0.5)
 F3B(0.5) F2B(0.5) F4A(0.5) F6A(0.5) F5A(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C3(H3), C16(H16), C17(H17), C14(H14)
4.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C21(H21A,H21B,H21C),
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C)
;
_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
Ti1 Ti 0.5000 0.46162(11) 0.7500 0.0323(3) Uani 1 2 d S T P . .
F2A F 0.5563(5) 1.0782(8) 0.5589(5) 0.0785(8) Uani 0.5 1 d . . . A 2
F1A F 0.6232(5) 1.1385(7) 0.6488(4) 0.0785(8) Uani 0.5 1 d . . . A 2
F3A F 0.6546(5) 1.0178(8) 0.5878(5) 0.0785(8) Uani 0.5 1 d . . . A 2
F4B F 0.3297(5) -0.1661(8) 0.5379(5) 0.0785(8) Uani 0.5 1 d . . . B 1
F5B F 0.2566(5) -0.1144(8) 0.5734(4) 0.0785(8) Uani 0.5 1 d . . . B 1
F6B F 0.3433(6) -0.2322(10) 0.6317(5) 0.0785(8) Uani 0.5 1 d . . . B 1
O1 O 0.54655(15) 0.5665(4) 0.71801(18) 0.0476(9) Uani 1 1 d . . . . .
O2 O 0.44669(17) 0.3563(3) 0.68989(16) 0.0460(8) Uani 1 1 d . . . . .
C11 C 0.6014(3) 1.0362(5) 0.6079(3) 0.0502(12) Uani 1 1 d . . . . .
C4 C 0.5880(2) 0.9116(5) 0.6378(2) 0.0407(10) Uani 1 1 d . . . . .
C5 C 0.5279(2) 0.8961(5) 0.6432(3) 0.0488(12) Uani 1 1 d . . . . .
H5 H 0.4958 0.9645 0.6283 0.059 Uiso 1 1 calc R . . . .
C6 C 0.5155(2) 0.7803(5) 0.6702(3) 0.0480(12) Uani 1 1 d . . . . .
H6 H 0.4744 0.7682 0.6741 0.058 Uiso 1 1 calc R . . . .
C1 C 0.56273(19) 0.6797(5) 0.6921(2) 0.0358(9) Uani 1 1 d . . . . .
C2 C 0.62433(18) 0.6928(4) 0.68781(19) 0.0308(8) Uani 1 1 d . . . . .
C3 C 0.63514(19) 0.8122(4) 0.6605(2) 0.0338(9) Uani 1 1 d . . . . .
H3 H 0.6764 0.8264 0.6572 0.041 Uiso 1 1 calc R . . . .
C7 C 0.67598(19) 0.5808(5) 0.7109(2) 0.0362(9) Uani 1 1 d . . . . .
C10 C 0.7391(2) 0.6223(6) 0.7013(3) 0.0491(12) Uani 1 1 d . . . . .
H10A H 0.7304 0.6380 0.6563 0.074 Uiso 1 1 calc GR . . . .
H10B H 0.7711 0.5497 0.7165 0.074 Uiso 1 1 calc GR . . . .
H10C H 0.7559 0.7055 0.7250 0.074 Uiso 1 1 calc GR . . . .
C8 C 0.6916(3) 0.5534(6) 0.7814(2) 0.0541(13) Uani 1 1 d . . . . .
H8A H 0.7091 0.6357 0.8055 0.081 Uiso 1 1 calc GR . . . .
H8B H 0.7236 0.4804 0.7951 0.081 Uiso 1 1 calc GR . . . .
H8C H 0.6519 0.5264 0.7885 0.081 Uiso 1 1 calc GR . . . .
C9 C 0.6514(3) 0.4516(5) 0.6726(3) 0.0494(12) Uani 1 1 d . . . . .
H9A H 0.6119 0.4208 0.6788 0.074 Uiso 1 1 calc GR . . . .
H9B H 0.6846 0.3809 0.6868 0.074 Uiso 1 1 calc GR . . . .
H9C H 0.6421 0.4702 0.6277 0.074 Uiso 1 1 calc GR . . . .
C22 C 0.3189(3) -0.1262(5) 0.5887(3) 0.0533(13) Uani 1 1 d . . . . .
C15 C 0.3541(2) 0.0018(5) 0.6152(2) 0.0406(10) Uani 1 1 d . . . . .
C16 C 0.38319(19) 0.0155(5) 0.6799(2) 0.0382(10) Uani 1 1 d . . . . .
H16 H 0.3821 -0.0564 0.7074 0.046 Uiso 1 1 calc R . . . .
C17 C 0.4138(2) 0.1356(5) 0.7035(2) 0.0371(9) Uani 1 1 d . . . . .
H17 H 0.4343 0.1462 0.7478 0.045 Uiso 1 1 calc R . . . .
C12 C 0.41536(19) 0.2417(5) 0.6636(2) 0.0351(9) Uani 1 1 d . . . . .
C13 C 0.3857(2) 0.2298(5) 0.5976(2) 0.0377(9) Uani 1 1 d . . . . .
C14 C 0.3552(2) 0.1076(5) 0.5749(2) 0.0415(10) Uani 1 1 d . . . . .
H14 H 0.3345 0.0959 0.5307 0.050 Uiso 1 1 calc R . . . .
C18 C 0.3856(3) 0.3477(5) 0.5526(2) 0.0512(13) Uani 1 1 d . . . . .
C21 C 0.4565(4) 0.3825(8) 0.5590(4) 0.081(2) Uani 1 1 d . . . . .
H21A H 0.4806 0.4130 0.6021 0.121 Uiso 1 1 calc GR . . . .
H21B H 0.4562 0.4547 0.5292 0.121 Uiso 1 1 calc GR . . . .
H21C H 0.4774 0.3018 0.5497 0.121 Uiso 1 1 calc GR . . . .
C20 C 0.3517(4) 0.4707(6) 0.5676(3) 0.076(2) Uani 1 1 d . . . . .
H20A H 0.3072 0.4464 0.5631 0.113 Uiso 1 1 calc GR . . . .
H20B H 0.3509 0.5444 0.5384 0.113 Uiso 1 1 calc GR . . . .
H20C H 0.3751 0.5004 0.6110 0.113 Uiso 1 1 calc GR . . . .
C19 C 0.3472(5) 0.3081(7) 0.4842(3) 0.088(3) Uani 1 1 d . . . . .
H19A H 0.3664 0.2270 0.4731 0.132 Uiso 1 1 calc GR . . . .
H19B H 0.3484 0.3827 0.4561 0.132 Uiso 1 1 calc GR . . . .
H19C H 0.3022 0.2894 0.4797 0.132 Uiso 1 1 calc GR . . . .
F1B F 0.5786(5) 1.1497(7) 0.6275(4) 0.0785(8) Uani 0.5 1 d . . . A 1
F3B F 0.6611(5) 1.0545(8) 0.6123(5) 0.0785(8) Uani 0.5 1 d . . . A 1
F2B F 0.5684(5) 1.0329(8) 0.5443(5) 0.0785(8) Uani 0.5 1 d . . . A 1
F4A F 0.2978(5) -0.1331(8) 0.5237(5) 0.0785(8) Uani 0.5 1 d . . . B 2
F6A F 0.3462(6) -0.2349(10) 0.6123(5) 0.0785(8) Uani 0.5 1 d . . . B 2
F5A F 0.2610(5) -0.1390(8) 0.5990(4) 0.0785(8) Uani 0.5 1 d . . . B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O1 1.781(3) 2_656 ?
Ti1 O1 1.781(3) . ?
Ti1 O2 1.786(3) 2_656 ?
Ti1 O2 1.786(3) . ?
F2A C11 1.272(11) . ?
F1A C11 1.339(10) . ?
F3A C11 1.411(12) . ?
F4B C22 1.313(11) . ?
F5B C22 1.298(11) . ?
F6B C22 1.400(12) . ?
O1 C1 1.366(5) . ?
O2 C12 1.349(6) . ?
C11 C4 1.483(7) . ?
C11 F1B 1.364(10) . ?
C11 F3B 1.298(11) . ?
C11 F2B 1.366(11) . ?
C4 C5 1.382(7) . ?
C4 C3 1.390(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.369(8) . ?
C6 H6 0.9500 . ?
C6 C1 1.398(6) . ?
C1 C2 1.402(5) . ?
C2 C3 1.390(6) . ?
C2 C7 1.540(5) . ?
C3 H3 0.9500 . ?
C7 C10 1.537(6) . ?
C7 C8 1.533(7) . ?
C7 C9 1.530(7) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C22 C15 1.494(7) . ?
C22 F4A 1.381(11) . ?
C22 F6A 1.254(13) . ?
C22 F5A 1.383(11) . ?
C15 C16 1.382(7) . ?
C15 C14 1.393(7) . ?
C16 H16 0.9500 . ?
C16 C17 1.376(7) . ?
C17 H17 0.9500 . ?
C17 C12 1.392(6) . ?
C12 C13 1.407(6) . ?
C13 C14 1.389(7) . ?
C13 C18 1.546(6) . ?
C14 H14 0.9500 . ?
C18 C21 1.558(10) . ?
C18 C20 1.526(8) . ?
C18 C19 1.531(8) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 O1 108.9(2) 2_656 . ?
O1 Ti1 O2 109.19(16) . 2_656 ?
O1 Ti1 O2 110.36(16) 2_656 2_656 ?
O1 Ti1 O2 109.19(16) 2_656 . ?
O1 Ti1 O2 110.37(16) . . ?
O2 Ti1 O2 108.8(2) . 2_656 ?
C1 O1 Ti1 157.6(3) . . ?
C12 O2 Ti1 157.2(3) . . ?
F2A C11 F1A 109.7(7) . . ?
F2A C11 F3A 104.2(7) . . ?
F2A C11 C4 116.6(6) . . ?
F1A C11 F3A 100.5(6) . . ?
F1A C11 C4 113.0(6) . . ?
F3A C11 C4 111.2(5) . . ?
F1B C11 C4 112.2(6) . . ?
F1B C11 F2B 103.9(6) . . ?
F3B C11 C4 116.1(6) . . ?
F3B C11 F1B 110.0(6) . . ?
F3B C11 F2B 103.6(7) . . ?
F2B C11 C4 110.0(5) . . ?
C5 C4 C11 118.9(4) . . ?
C5 C4 C3 120.4(4) . . ?
C3 C4 C11 120.7(4) . . ?
C4 C5 H5 120.7 . . ?
C6 C5 C4 118.7(4) . . ?
C6 C5 H5 120.7 . . ?
C5 C6 H6 119.6 . . ?
C5 C6 C1 120.7(4) . . ?
C1 C6 H6 119.6 . . ?
O1 C1 C6 117.3(4) . . ?
O1 C1 C2 120.7(4) . . ?
C6 C1 C2 122.0(4) . . ?
C1 C2 C7 122.0(4) . . ?
C3 C2 C1 115.5(4) . . ?
C3 C2 C7 122.5(4) . . ?
C4 C3 H3 118.7 . . ?
C2 C3 C4 122.7(4) . . ?
C2 C3 H3 118.7 . . ?
C10 C7 C2 111.1(4) . . ?
C8 C7 C2 110.3(4) . . ?
C8 C7 C10 108.1(4) . . ?
C9 C7 C2 109.5(4) . . ?
C9 C7 C10 107.4(4) . . ?
C9 C7 C8 110.3(4) . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
F4B C22 F6B 103.9(7) . . ?
F4B C22 C15 112.1(6) . . ?
F5B C22 F4B 107.1(7) . . ?
F5B C22 F6B 111.4(7) . . ?
F5B C22 C15 112.5(5) . . ?
F6B C22 C15 109.6(6) . . ?
F4A C22 C15 113.7(5) . . ?
F4A C22 F5A 101.0(7) . . ?
F6A C22 C15 116.7(7) . . ?
F6A C22 F4A 110.1(7) . . ?
F6A C22 F5A 100.6(7) . . ?
F5A C22 C15 112.9(5) . . ?
C16 C15 C22 119.4(5) . . ?
C16 C15 C14 120.7(4) . . ?
C14 C15 C22 119.9(5) . . ?
C15 C16 H16 120.7 . . ?
C17 C16 C15 118.5(4) . . ?
C17 C16 H16 120.7 . . ?
C16 C17 H17 119.4 . . ?
C16 C17 C12 121.1(4) . . ?
C12 C17 H17 119.4 . . ?
O2 C12 C17 118.0(4) . . ?
O2 C12 C13 120.9(4) . . ?
C17 C12 C13 121.1(4) . . ?
C12 C13 C18 121.9(4) . . ?
C14 C13 C12 116.7(4) . . ?
C14 C13 C18 121.4(4) . . ?
C15 C14 H14 119.1 . . ?
C13 C14 C15 121.8(4) . . ?
C13 C14 H14 119.1 . . ?
C13 C18 C21 109.7(5) . . ?
C20 C18 C13 109.8(5) . . ?
C20 C18 C21 111.0(6) . . ?
C20 C18 C19 106.7(5) . . ?
C19 C18 C13 110.2(5) . . ?
C19 C18 C21 109.3(6) . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'



####################################################################### 
# 
# 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_c2c_early_a
_database_code_depnum_ccdc_archive 'CCDC 1905880'
loop_
_audit_author_name
_audit_author_address
'Kelly E Aldrich'
;Michigan State University
United States of America
;
_audit_update_record             
;
2019-03-27 deposited with the CCDC.	2019-05-07 downloaded from the CCDC.
;
_audit_creation_date             2019-03-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C62 H81 N3 O4 Ti2, 0.5(C6 H14)'
_chemical_formula_sum            'C65 H88 N3 O4 Ti2'
_chemical_formula_weight         1071.18
_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 0.0181 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'
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'
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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   34.0256(18)
_cell_length_b                   17.3283(7)
_cell_length_c                   25.5196(12)
_cell_angle_alpha                90
_cell_angle_beta                 121.054(2)
_cell_angle_gamma                90
_cell_volume                     12890.1(11)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9449
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.21
_cell_measurement_theta_min      2.97
_shelx_estimated_absorpt_T_max   0.695
_shelx_estimated_absorpt_T_min   0.611
_exptl_absorpt_coefficient_mu    2.448
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 172391 reflections, Rint = 0.1500
 (19148 with I > 3sig(I), Rint = 0.0549)
;
_exptl_crystal_colour            'orangish brown'
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4600
_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.16
_exptl_special_details           
;
Data was collected using a BRUKER CCD (charge coupled device) based
diffractometer equipped with an Oxford low-temperature apparatus operating at
173 K.  A suitable crystal was chosen and mounted on a nylon loop using 
Paratone oil.  Data  were measured using omega and phi scans of 1.0° per frame 
for 30 s. The total number of images were based on 
results from the program COSMO where redundancy was expected to be 4 and 
completeness to 0.83Å to 100%. Cell parameters were
retrieved using APEX II software and refined using SAINT on all observed
reflections.Data reduction was performed using the SAINT software which 
corrects for Lp. Scaling and absorption corrections were applied using SADABS6 
multi-scan technique, supplied by George Sheldrick.  The structure was solved 
by the direct method using the SHELXT program and refined by least squares 
method on F2, SHELXL, incorporated in OLEX2. 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1037
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            83762
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.244
_diffrn_reflns_theta_min         2.967
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'ω and φ'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8329
_reflns_number_total             11768
_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       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.910
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         11768
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0593
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0983P)²+14.4446P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1602
_refine_ls_wR_factor_ref         0.1812
_refine_special_details          
;
The structure was refined by Least Squares using version 2018/3 
of XL (Sheldrick, 2015) incorporated in Olex2 (Dolomanov et al., 2009). 
All non-hydrogen atoms were refined anisotropically. 
Hydrogen atom positions were calculated geometrically and refined using the 
riding model, except for the hydrogen atom(s) on the non-carbon atom(s) 
which was found by difference Fourier methods and refined isotropically.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1S-C3S = C2S-C4S = C3S-C5S = C4S-C6S
 2.2 with sigma of 0.002
 C1S-C2S \\sim C3S-C2S \\sim C3S-C4S \\sim C5S-C4S \\sim C6S-C5S
 with sigma of 0.02
3. Others
 Fixed Sof: C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) C2S(0.5) H2SA(0.5)
 H2SB(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) C5S(0.5)
 H5SA(0.5) H5SB(0.5) C6S(0.5) H6SA(0.5) H6SB(0.5) H6SC(0.5)
4.a Ternary CH refined with riding coordinates:
 N007(H007)
4.b Secondary CH2 refined with riding coordinates:
 C00M(H00A,H00B), C00N(H00C,H00D), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,
 H4SB), C5S(H5SA,H5SB)
4.c Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00K(H00K), C00L(H00L), C00Q(H00Q), C00S(H00S), C00T(H00T),
 C01B(H01B), C01E(H01H), C01G(H01L), C01P(H01), C012(H012), C013(H013),
 C014(H014), C016(H016), C018(H018), C019(H019)
4.d Idealised Me refined as rotating group:
 C00V(H00F,H00G,H00H), C01C(H01A,H01C,H01D), C01D(H01E,H01F,H01G), C01F(H01I,
 H01J,H01K), C01H(H01M,H01N,H01O), C01I(H01P,H01Q,H01R), C01J(H01S,H01T,H01U),
 C01K(H01V,H01W,H01X), C01M(H01Y,H,HA), C01O(H01Z,HB,HC), C01Q(H0AA,HD,HE),
 C01R(H1AA,HF,HG), C01S(H2AA,HH,HI), C01T(H3AA,HJ,HK), C01U(H4AA,HL,HM),
 C01V(H5AA,HN,HO), C01W(H6AA,HP,HQ), C01X(H7AA,HR,HS), C01Y(H8AA,HT,HU),
 C01Z(H9AA,HV,HW), C1S(H1SA,H1SB,H1SC), C6S(H6SA,H6SB,H6SC)
;
_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
Ti01 Ti 0.24459(2) 0.22034(3) 0.25688(2) 0.02836(15) Uani 1 1 d . . . . .
Ti02 Ti 0.32824(2) 0.29580(3) 0.34817(2) 0.02950(16) Uani 1 1 d . . . . .
O003 O 0.20574(7) 0.17385(13) 0.27707(10) 0.0351(5) Uani 1 1 d . . . . .
O004 O 0.36283(8) 0.37241(14) 0.34082(10) 0.0409(6) Uani 1 1 d . . . . .
O005 O 0.36130(8) 0.27399(13) 0.42966(9) 0.0369(5) Uani 1 1 d . . . . .
O006 O 0.21400(7) 0.26746(13) 0.18288(9) 0.0339(5) Uani 1 1 d . . . . .
N00G N 0.31165(9) 0.20752(15) 0.29677(12) 0.0325(6) Uani 1 1 d . . . . .
N007 N 0.24578(10) 0.10335(16) 0.21521(12) 0.0392(7) Uani 1 1 d . . . . .
H007 H 0.2749 0.0785 0.2473 0.047 Uiso 1 1 calc R . . . .
N008 N 0.26577(9) 0.31288(15) 0.31470(11) 0.0299(6) Uani 1 1 d . . . . .
C00A C 0.13129(11) 0.22827(19) 0.21502(14) 0.0338(7) Uani 1 1 d . . . . .
C00B C 0.41238(13) 0.0348(2) 0.34712(18) 0.0518(10) Uani 1 1 d . . . . .
C00C C 0.38581(10) 0.30248(19) 0.48760(14) 0.0316(7) Uani 1 1 d . . . . .
C00D C 0.18018(12) 0.3520(2) 0.09528(15) 0.0372(8) Uani 1 1 d . . . . .
C00E C 0.37779(13) 0.0267(2) 0.36005(16) 0.0469(9) Uani 1 1 d . . . . .
H00E H 0.3770 -0.0181 0.3809 0.056 Uiso 1 1 calc R . . . .
C00F C 0.23769(10) 0.35957(17) 0.32674(14) 0.0293(7) Uani 1 1 d . . . . .
C00H C 0.45378(11) 0.5520(2) 0.43527(17) 0.0413(8) Uani 1 1 d . . . . .
C00I C 0.09595(12) 0.3552(2) 0.03216(16) 0.0460(9) Uani 1 1 d . . . . .
C00J C 0.43214(12) 0.3620(2) 0.60589(15) 0.0410(8) Uani 1 1 d . . . . .
C00K C 0.43440(11) 0.2840(2) 0.59487(15) 0.0367(8) Uani 1 1 d . . . . .
H00K H 0.4524 0.2511 0.6288 0.044 Uiso 1 1 calc R . . . .
C00L C 0.09463(12) 0.2683(2) 0.21097(16) 0.0470(9) Uani 1 1 d . . . . .
H00L H 0.0700 0.2834 0.1719 0.056 Uiso 1 1 calc R . . . .
C00M C 0.36151(11) 0.43794(19) 0.44317(15) 0.0357(7) Uani 1 1 d . . . . .
H00A H 0.3506 0.4831 0.4558 0.043 Uiso 1 1 calc R . . . .
H00B H 0.3344 0.4124 0.4089 0.043 Uiso 1 1 calc R . . . .
C00N C 0.12969(12) 0.2052(2) 0.15687(14) 0.0365(7) Uani 1 1 d . . . . .
H00C H 0.1551 0.1685 0.1678 0.044 Uiso 1 1 calc R . . . .
H00D H 0.1006 0.1770 0.1307 0.044 Uiso 1 1 calc R . . . .
C00O C 0.38486(11) 0.38197(19) 0.49642(15) 0.0340(7) Uani 1 1 d . . . . .
C00P C 0.19543(10) 0.17201(19) 0.38671(14) 0.0327(7) Uani 1 1 d . . . . .
C00Q C 0.42301(11) 0.52622(19) 0.45151(16) 0.0389(8) Uani 1 1 d . . . . .
H00Q H 0.4225 0.5505 0.4845 0.047 Uiso 1 1 calc R . . . .
C00R C 0.41169(11) 0.2518(2) 0.53680(14) 0.0343(7) Uani 1 1 d . . . . .
C00S C 0.19787(11) 0.3942(2) 0.27968(15) 0.0365(7) Uani 1 1 d . . . . .
H00S H 0.1893 0.3865 0.2383 0.044 Uiso 1 1 calc R . . . .
C00T C 0.45410(12) 0.5149(2) 0.38744(17) 0.0436(9) Uani 1 1 d . . . . .
H00T H 0.4752 0.5320 0.3762 0.052 Uiso 1 1 calc R . . . .
C00U C 0.13303(11) 0.26940(19) 0.11933(14) 0.0345(7) Uani 1 1 d . . . . .
C00V C 0.24653(11) 0.1684(2) 0.40721(16) 0.0405(8) Uani 1 1 d . . . . .
H00F H 0.2504 0.1367 0.3784 0.061 Uiso 1 1 calc GR . . . .
H00G H 0.2639 0.1456 0.4481 0.061 Uiso 1 1 calc GR . . . .
H00H H 0.2579 0.2207 0.4082 0.061 Uiso 1 1 calc GR . . . .
C00W C 0.22686(13) 0.3822(2) 0.10842(17) 0.0457(9) Uani 1 1 d . . . . .
C00X C 0.39289(11) 0.46579(18) 0.42092(15) 0.0350(7) Uani 1 1 d . . . . .
C00Y C 0.17607(10) 0.29681(18) 0.13287(14) 0.0311(7) Uani 1 1 d . . . . .
C00Z C 0.41573(11) 0.1657(2) 0.52681(15) 0.0374(8) Uani 1 1 d . . . . .
C01A C 0.34391(11) 0.14817(19) 0.31119(15) 0.0337(7) Uani 1 1 d . . . . .
C01B C 0.37746(12) 0.1548(2) 0.29586(18) 0.0442(8) Uani 1 1 d . . . . .
H01B H 0.3771 0.1976 0.2723 0.053 Uiso 1 1 calc R . . . .
C01C C 0.36851(12) 0.1268(2) 0.49540(17) 0.0444(9) Uani 1 1 d . . . . .
H01A H 0.3552 0.1319 0.5213 0.067 Uiso 1 1 calc GR . . . .
H01C H 0.3718 0.0720 0.4890 0.067 Uiso 1 1 calc GR . . . .
H01D H 0.3483 0.1517 0.4558 0.067 Uiso 1 1 calc GR . . . .
C01D C 0.17707(13) 0.0889(2) 0.37698(19) 0.0507(9) Uani 1 1 d . . . . .
H01E H 0.1805 0.0641 0.3450 0.076 Uiso 1 1 calc GR . . . .
H01F H 0.1446 0.0899 0.3645 0.076 Uiso 1 1 calc GR . . . .
H01G H 0.1945 0.0599 0.4152 0.076 Uiso 1 1 calc GR . . . .
C01E C 0.41159(13) 0.0993(2) 0.3148(2) 0.0529(10) Uani 1 1 d . . . . .
H01H H 0.4350 0.1058 0.3054 0.063 Uiso 1 1 calc R . . . .
C01F C 0.22150(15) 0.4375(3) 0.0583(2) 0.0662(12) Uani 1 1 d . . . . .
H01I H 0.2067 0.4105 0.0190 0.099 Uiso 1 1 calc GR . . . .
H01J H 0.2518 0.4558 0.0681 0.099 Uiso 1 1 calc GR . . . .
H01K H 0.2026 0.4817 0.0559 0.099 Uiso 1 1 calc GR . . . .
C01G C 0.12747(13) 0.2578(2) 0.31867(17) 0.0478(9) Uani 1 1 d . . . . .
H01L H 0.1255 0.2677 0.3539 0.057 Uiso 1 1 calc R . . . .
C01H C 0.25007(13) 0.4259(2) 0.16990(19) 0.0534(10) Uani 1 1 d . . . . .
H01M H 0.2298 0.4673 0.1681 0.080 Uiso 1 1 calc GR . . . .
H01N H 0.2791 0.4481 0.1777 0.080 Uiso 1 1 calc GR . . . .
H01O H 0.2561 0.3900 0.2029 0.080 Uiso 1 1 calc GR . . . .
C01I C 0.25766(14) 0.3162(3) 0.1115(2) 0.0560(10) Uani 1 1 d . . . . .
H01P H 0.2634 0.2812 0.1450 0.084 Uiso 1 1 calc GR . . . .
H01Q H 0.2869 0.3371 0.1189 0.084 Uiso 1 1 calc GR . . . .
H01R H 0.2425 0.2878 0.0728 0.084 Uiso 1 1 calc GR . . . .
C01J C 0.19243(13) 0.2076(2) 0.43903(16) 0.0458(9) Uani 1 1 d . . . . .
H01S H 0.2139 0.1813 0.4773 0.069 Uiso 1 1 calc GR . . . .
H01T H 0.1611 0.2020 0.4310 0.069 Uiso 1 1 calc GR . . . .
H01U H 0.2003 0.2625 0.4425 0.069 Uiso 1 1 calc GR . . . .
C01K C 0.43886(13) 0.1560(2) 0.48887(17) 0.0487(9) Uani 1 1 d . . . . .
H01V H 0.4200 0.1808 0.4489 0.073 Uiso 1 1 calc GR . . . .
H01W H 0.4420 0.1009 0.4830 0.073 Uiso 1 1 calc GR . . . .
H01X H 0.4693 0.1800 0.5105 0.073 Uiso 1 1 calc GR . . . .
C01L C 0.42916(14) 0.4093(3) 0.30582(19) 0.0558(11) Uani 1 1 d . . . . .
C01M C 0.48688(12) 0.6172(2) 0.46959(19) 0.0522(10) Uani 1 1 d . . . . .
H01Y H 0.4916 0.6479 0.4411 0.078 Uiso 1 1 calc GR . . . .
H H 0.5163 0.5957 0.5014 0.078 Uiso 1 1 calc GR . . . .
HA H 0.4742 0.6501 0.4885 0.078 Uiso 1 1 calc GR . . . .
C01N C 0.09322(14) 0.2868(3) 0.26272(19) 0.0580(11) Uani 1 1 d . . . . .
C01O C 0.05286(14) 0.3887(3) -0.0214(2) 0.0674(13) Uani 1 1 d . . . . .
H01Z H 0.0291 0.3488 -0.0395 0.101 Uiso 1 1 calc GR . . . .
HB H 0.0596 0.4075 -0.0521 0.101 Uiso 1 1 calc GR . . . .
HC H 0.0420 0.4316 -0.0071 0.101 Uiso 1 1 calc GR . . . .
C01P C 0.34450(12) 0.08259(19) 0.34317(15) 0.0384(8) Uani 1 1 d . . . . .
H01 H 0.3216 0.0762 0.3535 0.046 Uiso 1 1 calc R . . . .
C01Q C 0.44524(15) 0.1229(2) 0.58776(17) 0.0562(11) Uani 1 1 d . . . . .
H0AA H 0.4764 0.1441 0.6090 0.084 Uiso 1 1 calc GR . . . .
HD H 0.4463 0.0678 0.5797 0.084 Uiso 1 1 calc GR . . . .
HE H 0.4318 0.1294 0.6134 0.084 Uiso 1 1 calc GR . . . .
C01R C 0.45557(15) 0.3921(3) 0.67068(17) 0.0547(10) Uani 1 1 d . . . . .
H1AA H 0.4434 0.3653 0.6932 0.082 Uiso 1 1 calc GR . . . .
HF H 0.4498 0.4476 0.6701 0.082 Uiso 1 1 calc GR . . . .
HG H 0.4887 0.3829 0.6908 0.082 Uiso 1 1 calc GR . . . .
C01S C 0.20992(14) 0.0451(2) 0.2014(2) 0.0581(11) Uani 1 1 d . . . . .
H2AA H 0.2030 0.0448 0.2342 0.087 Uiso 1 1 calc GR . . . .
HH H 0.2209 -0.0060 0.1983 0.087 Uiso 1 1 calc GR . . . .
HI H 0.1821 0.0580 0.1625 0.087 Uiso 1 1 calc GR . . . .
C01T C 0.44640(16) 0.3280(3) 0.3291(2) 0.0663(12) Uani 1 1 d . . . . .
H3AA H 0.4771 0.3308 0.3658 0.099 Uiso 1 1 calc GR . . . .
HJ H 0.4478 0.2984 0.2974 0.099 Uiso 1 1 calc GR . . . .
HK H 0.4254 0.3025 0.3392 0.099 Uiso 1 1 calc GR . . . .
C01U C 0.25200(19) 0.1130(3) 0.1630(2) 0.0696(13) Uani 1 1 d . . . . .
H4AA H 0.2252 0.1393 0.1298 0.104 Uiso 1 1 calc GR . . . .
HL H 0.2554 0.0623 0.1489 0.104 Uiso 1 1 calc GR . . . .
HM H 0.2795 0.1440 0.1754 0.104 Uiso 1 1 calc GR . . . .
C01V C 0.46421(18) 0.4471(4) 0.2924(2) 0.0823(16) Uani 1 1 d . . . . .
H5AA H 0.4558 0.5012 0.2808 0.123 Uiso 1 1 calc GR . . . .
HN H 0.4642 0.4195 0.2589 0.123 Uiso 1 1 calc GR . . . .
HO H 0.4949 0.4445 0.3291 0.123 Uiso 1 1 calc GR . . . .
C01W C 0.38316(17) 0.4063(3) 0.2445(2) 0.0763(15) Uani 1 1 d . . . . .
H6AA H 0.3609 0.3763 0.2495 0.114 Uiso 1 1 calc GR . . . .
HP H 0.3878 0.3818 0.2134 0.114 Uiso 1 1 calc GR . . . .
HQ H 0.3716 0.4589 0.2315 0.114 Uiso 1 1 calc GR . . . .
C01X C 0.45015(16) -0.0248(3) 0.3685(3) 0.0857(18) Uani 1 1 d . . . . .
H7AA H 0.4368 -0.0767 0.3609 0.129 Uiso 1 1 calc GR . . . .
HR H 0.4719 -0.0182 0.4124 0.129 Uiso 1 1 calc GR . . . .
HS H 0.4662 -0.0182 0.3461 0.129 Uiso 1 1 calc GR . . . .
C01Y C 0.15255(19) 0.5045(4) 0.3672(2) 0.0892(18) Uani 1 1 d . . . . .
H8AA H 0.1449 0.4767 0.3942 0.134 Uiso 1 1 calc GR . . . .
HT H 0.1243 0.5180 0.3291 0.134 Uiso 1 1 calc GR . . . .
HU H 0.1694 0.5517 0.3876 0.134 Uiso 1 1 calc GR . . . .
C01Z C 0.0549(2) 0.3348(5) 0.2586(2) 0.117(3) Uani 1 1 d . . . . .
H9AA H 0.0664 0.3866 0.2746 0.175 Uiso 1 1 calc GR . . . .
HV H 0.0433 0.3106 0.2827 0.175 Uiso 1 1 calc GR . . . .
HW H 0.0301 0.3386 0.2158 0.175 Uiso 1 1 calc GR . . . .
C009 C 0.16756(10) 0.20586(18) 0.27327(14) 0.0302(7) Uani 1 1 d . . . . .
C010 C 0.16449(10) 0.21498(19) 0.32560(14) 0.0328(7) Uani 1 1 d . . . . .
C011 C 0.42491(12) 0.4535(2) 0.35489(16) 0.0414(8) Uani 1 1 d . . . . .
C012 C 0.09379(12) 0.2994(2) 0.06940(15) 0.0406(8) Uani 1 1 d . . . . .
H012 H 0.0646 0.2812 0.0605 0.049 Uiso 1 1 calc R . . . .
C013 C 0.22204(12) 0.4205(2) 0.39944(16) 0.0400(8) Uani 1 1 d . . . . .
H013 H 0.2308 0.4296 0.4408 0.048 Uiso 1 1 calc R . . . .
C014 C 0.13918(12) 0.3792(2) 0.04539(16) 0.0427(8) Uani 1 1 d . . . . .
H014 H 0.1409 0.4160 0.0191 0.051 Uiso 1 1 calc R . . . .
C015 C 0.18208(13) 0.4537(2) 0.35290(18) 0.0484(9) Uani 1 1 d . . . . .
C016 C 0.24913(11) 0.37482(19) 0.38704(14) 0.0326(7) Uani 1 1 d . . . . .
H016 H 0.2763 0.3530 0.4200 0.039 Uiso 1 1 calc R . . . .
C017 C 0.39317(11) 0.43059(19) 0.37200(15) 0.0356(7) Uani 1 1 d . . . . .
C018 C 0.40767(11) 0.4100(2) 0.55597(15) 0.0374(8) Uani 1 1 d . . . . .
H018 H 0.4064 0.4637 0.5626 0.045 Uiso 1 1 calc R . . . .
C019 C 0.17096(12) 0.4395(2) 0.29345(17) 0.0479(9) Uani 1 1 d . . . . .
H019 H 0.1438 0.4618 0.2608 0.057 Uiso 1 1 calc R . . . .
C1S C 0.3204(4) 0.6122(8) 0.5169(6) 0.107(4) Uiso 0.5 1 d D . P . .
H1SA H 0.3088 0.5707 0.4865 0.161 Uiso 0.5 1 calc GR . P . .
H1SB H 0.2949 0.6450 0.5106 0.161 Uiso 0.5 1 calc GR . P . .
H1SC H 0.3354 0.5899 0.5581 0.161 Uiso 0.5 1 calc GR . P . .
C2S C 0.3499(4) 0.6536(7) 0.5111(5) 0.098(4) Uiso 0.5 1 d D . P . .
H2SA H 0.3572 0.6260 0.4831 0.118 Uiso 0.5 1 calc R . P . .
H2SB H 0.3349 0.7028 0.4911 0.118 Uiso 0.5 1 calc R . P . .
C3S C 0.3878(4) 0.6693(10) 0.5603(8) 0.175(8) Uiso 0.5 1 d D . P . .
H3SA H 0.4110 0.6808 0.5490 0.210 Uiso 0.5 1 calc R . P . .
H3SB H 0.3981 0.6223 0.5860 0.210 Uiso 0.5 1 calc R . P . .
C4S C 0.3880(5) 0.7254(8) 0.5935(6) 0.133(5) Uiso 0.5 1 d D . P . .
H4SA H 0.3722 0.7695 0.5660 0.159 Uiso 0.5 1 calc R . P . .
H4SB H 0.3692 0.7094 0.6110 0.159 Uiso 0.5 1 calc R . P . .
C5S C 0.4259(5) 0.7498(9) 0.6371(7) 0.156(7) Uiso 0.5 1 d D . P . .
H5SA H 0.4473 0.7545 0.6219 0.188 Uiso 0.5 1 calc R . P . .
H5SB H 0.4385 0.7099 0.6695 0.188 Uiso 0.5 1 calc R . P . .
C6S C 0.4261(7) 0.8153(10) 0.6623(8) 0.198(10) Uiso 0.5 1 d D . P . .
H6SA H 0.4143 0.8075 0.6898 0.297 Uiso 0.5 1 calc GR . P . .
H6SB H 0.4065 0.8525 0.6304 0.297 Uiso 0.5 1 calc GR . P . .
H6SC H 0.4575 0.8353 0.6857 0.297 Uiso 0.5 1 calc GR . P . .


_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
Ti01 Ti02 2.8978(8) . ?
Ti01 O003 1.834(2) . ?
Ti01 O006 1.813(2) . ?
Ti01 N00G 1.974(3) . ?
Ti01 N007 2.299(3) . ?
Ti01 N008 2.042(3) . ?
Ti02 O004 1.847(2) . ?
Ti02 O005 1.822(2) . ?
Ti02 N00G 1.901(3) . ?
Ti02 N008 1.860(3) . ?
O003 C009 1.369(4) . ?
O004 C017 1.367(4) . ?
O005 C00C 1.361(4) . ?
O006 C00Y 1.362(4) . ?
N00G C01A 1.408(4) . ?
N007 H007 1.0000 . ?
N007 C01S 1.479(5) . ?
N007 C01U 1.462(5) . ?
N008 C00F 1.402(4) . ?
C00A C00L 1.384(5) . ?
C00A C00N 1.511(5) . ?
C00A C009 1.411(4) . ?
C00B C00E 1.383(6) . ?
C00B C01E 1.380(6) . ?
C00B C01X 1.515(5) . ?
C00C C00O 1.399(5) . ?
C00C C00R 1.408(5) . ?
C00D C00W 1.536(5) . ?
C00D C00Y 1.412(5) . ?
C00D C014 1.399(5) . ?
C00E H00E 0.9500 . ?
C00E C01P 1.379(5) . ?
C00F C00S 1.400(4) . ?
C00F C016 1.404(4) . ?
C00H C00Q 1.384(5) . ?
C00H C00T 1.385(5) . ?
C00H C01M 1.514(5) . ?
C00I C01O 1.512(5) . ?
C00I C012 1.383(5) . ?
C00I C014 1.392(5) . ?
C00J C00K 1.392(5) . ?
C00J C01R 1.510(5) . ?
C00J C018 1.383(5) . ?
C00K H00K 0.9500 . ?
C00K C00R 1.386(5) . ?
C00L H00L 0.9500 . ?
C00L C01N 1.383(5) . ?
C00M H00A 0.9900 . ?
C00M H00B 0.9900 . ?
C00M C00O 1.518(5) . ?
C00M C00X 1.523(5) . ?
C00N H00C 0.9900 . ?
C00N H00D 0.9900 . ?
C00N C00U 1.511(5) . ?
C00O C018 1.390(5) . ?
C00P C00V 1.537(4) . ?
C00P C01D 1.538(5) . ?
C00P C01J 1.521(5) . ?
C00P C010 1.549(4) . ?
C00Q H00Q 0.9500 . ?
C00Q C00X 1.390(5) . ?
C00R C00Z 1.532(5) . ?
C00S H00S 0.9500 . ?
C00S C019 1.382(5) . ?
C00T H00T 0.9500 . ?
C00T C011 1.399(5) . ?
C00U C00Y 1.403(5) . ?
C00U C012 1.386(5) . ?
C00V H00F 0.9800 . ?
C00V H00G 0.9800 . ?
C00V H00H 0.9800 . ?
C00W C01F 1.531(5) . ?
C00W C01H 1.542(5) . ?
C00W C01I 1.526(6) . ?
C00X C017 1.394(5) . ?
C00Z C01C 1.533(5) . ?
C00Z C01K 1.540(5) . ?
C00Z C01Q 1.539(5) . ?
C01A C01B 1.389(5) . ?
C01A C01P 1.393(5) . ?
C01B H01B 0.9500 . ?
C01B C01E 1.389(5) . ?
C01C H01A 0.9800 . ?
C01C H01C 0.9800 . ?
C01C H01D 0.9800 . ?
C01D H01E 0.9800 . ?
C01D H01F 0.9800 . ?
C01D H01G 0.9800 . ?
C01E H01H 0.9500 . ?
C01F H01I 0.9800 . ?
C01F H01J 0.9800 . ?
C01F H01K 0.9800 . ?
C01G H01L 0.9500 . ?
C01G C01N 1.390(5) . ?
C01G C010 1.392(5) . ?
C01H H01M 0.9800 . ?
C01H H01N 0.9800 . ?
C01H H01O 0.9800 . ?
C01I H01P 0.9800 . ?
C01I H01Q 0.9800 . ?
C01I H01R 0.9800 . ?
C01J H01S 0.9800 . ?
C01J H01T 0.9800 . ?
C01J H01U 0.9800 . ?
C01K H01V 0.9800 . ?
C01K H01W 0.9800 . ?
C01K H01X 0.9800 . ?
C01L C01T 1.524(7) . ?
C01L C01V 1.546(6) . ?
C01L C01W 1.541(6) . ?
C01L C011 1.537(6) . ?
C01M H01Y 0.9800 . ?
C01M H 0.9800 . ?
C01M HA 0.9800 . ?
C01N C01Z 1.505(6) . ?
C01O H01Z 0.9800 . ?
C01O HB 0.9800 . ?
C01O HC 0.9800 . ?
C01P H01 0.9500 . ?
C01Q H0AA 0.9800 . ?
C01Q HD 0.9800 . ?
C01Q HE 0.9800 . ?
C01R H1AA 0.9800 . ?
C01R HF 0.9800 . ?
C01R HG 0.9800 . ?
C01S H2AA 0.9800 . ?
C01S HH 0.9800 . ?
C01S HI 0.9800 . ?
C01T H3AA 0.9800 . ?
C01T HJ 0.9800 . ?
C01T HK 0.9800 . ?
C01U H4AA 0.9800 . ?
C01U HL 0.9800 . ?
C01U HM 0.9800 . ?
C01V H5AA 0.9800 . ?
C01V HN 0.9800 . ?
C01V HO 0.9800 . ?
C01W H6AA 0.9800 . ?
C01W HP 0.9800 . ?
C01W HQ 0.9800 . ?
C01X H7AA 0.9800 . ?
C01X HR 0.9800 . ?
C01X HS 0.9800 . ?
C01Y H8AA 0.9800 . ?
C01Y HT 0.9800 . ?
C01Y HU 0.9800 . ?
C01Y C015 1.516(6) . ?
C01Z H9AA 0.9800 . ?
C01Z HV 0.9800 . ?
C01Z HW 0.9800 . ?
C009 C010 1.401(5) . ?
C011 C017 1.414(5) . ?
C012 H012 0.9500 . ?
C013 H013 0.9500 . ?
C013 C015 1.387(5) . ?
C013 C016 1.370(5) . ?
C014 H014 0.9500 . ?
C015 C019 1.383(5) . ?
C016 H016 0.9500 . ?
C018 H018 0.9500 . ?
C019 H019 0.9500 . ?
C1S H1SA 0.9800 . ?
C1S H1SB 0.9800 . ?
C1S H1SC 0.9800 . ?
C1S C2S 1.302(11) . ?
C2S H2SA 0.9900 . ?
C2S H2SB 0.9900 . ?
C2S C3S 1.282(11) . ?
C3S H3SA 0.9900 . ?
C3S H3SB 0.9900 . ?
C3S C4S 1.286(13) . ?
C4S H4SA 0.9900 . ?
C4S H4SB 0.9900 . ?
C4S C5S 1.263(13) . ?
C5S H5SA 0.9900 . ?
C5S H5SB 0.9900 . ?
C5S C6S 1.304(13) . ?
C6S H6SA 0.9800 . ?
C6S H6SB 0.9800 . ?
C6S H6SC 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O003 Ti01 Ti02 121.58(7) . . ?
O003 Ti01 N00G 127.92(10) . . ?
O003 Ti01 N007 85.98(10) . . ?
O003 Ti01 N008 100.31(10) . . ?
O006 Ti01 Ti02 115.60(7) . . ?
O006 Ti01 O003 112.38(10) . . ?
O006 Ti01 N00G 118.52(11) . . ?
O006 Ti01 N007 93.03(10) . . ?
O006 Ti01 N008 101.42(10) . . ?
N00G Ti01 Ti02 40.66(8) . . ?
N00G Ti01 N007 81.24(11) . . ?
N00G Ti01 N008 80.36(11) . . ?
N007 Ti01 Ti02 121.69(7) . . ?
N008 Ti01 Ti02 39.70(7) . . ?
N008 Ti01 N007 160.49(10) . . ?
O004 Ti02 Ti01 130.98(8) . . ?
O004 Ti02 N00G 119.08(11) . . ?
O004 Ti02 N008 118.42(11) . . ?
O005 Ti02 Ti01 126.60(8) . . ?
O005 Ti02 O004 102.38(10) . . ?
O005 Ti02 N00G 114.16(11) . . ?
O005 Ti02 N008 116.33(11) . . ?
N00G Ti02 Ti01 42.57(8) . . ?
N008 Ti02 Ti01 44.52(8) . . ?
N008 Ti02 N00G 87.08(11) . . ?
C009 O003 Ti01 126.66(19) . . ?
C017 O004 Ti02 143.2(2) . . ?
C00C O005 Ti02 146.7(2) . . ?
C00Y O006 Ti01 154.4(2) . . ?
Ti02 N00G Ti01 96.77(12) . . ?
C01A N00G Ti01 139.0(2) . . ?
C01A N00G Ti02 119.6(2) . . ?
Ti01 N007 H007 104.3 . . ?
C01S N007 Ti01 120.2(2) . . ?
C01S N007 H007 104.3 . . ?
C01U N007 Ti01 111.4(2) . . ?
C01U N007 H007 104.3 . . ?
C01U N007 C01S 110.5(3) . . ?
Ti02 N008 Ti01 95.78(11) . . ?
C00F N008 Ti01 125.8(2) . . ?
C00F N008 Ti02 137.5(2) . . ?
C00L C00A C00N 119.0(3) . . ?
C00L C00A C009 118.8(3) . . ?
C009 C00A C00N 122.0(3) . . ?
C00E C00B C01X 120.8(4) . . ?
C01E C00B C00E 117.9(3) . . ?
C01E C00B C01X 121.3(4) . . ?
O005 C00C C00O 118.7(3) . . ?
O005 C00C C00R 119.6(3) . . ?
C00O C00C C00R 121.8(3) . . ?
C00Y C00D C00W 122.4(3) . . ?
C014 C00D C00W 121.2(3) . . ?
C014 C00D C00Y 116.4(3) . . ?
C00B C00E H00E 119.4 . . ?
C01P C00E C00B 121.1(4) . . ?
C01P C00E H00E 119.4 . . ?
N008 C00F C016 120.9(3) . . ?
C00S C00F N008 121.8(3) . . ?
C00S C00F C016 117.3(3) . . ?
C00Q C00H C00T 117.7(3) . . ?
C00Q C00H C01M 121.3(4) . . ?
C00T C00H C01M 121.0(3) . . ?
C012 C00I C01O 121.2(3) . . ?
C012 C00I C014 117.8(3) . . ?
C014 C00I C01O 121.0(3) . . ?
C00K C00J C01R 120.3(3) . . ?
C018 C00J C00K 117.9(3) . . ?
C018 C00J C01R 121.8(3) . . ?
C00J C00K H00K 118.4 . . ?
C00R C00K C00J 123.2(3) . . ?
C00R C00K H00K 118.4 . . ?
C00A C00L H00L 119.4 . . ?
C01N C00L C00A 121.2(3) . . ?
C01N C00L H00L 119.4 . . ?
H00A C00M H00B 107.8 . . ?
C00O C00M H00A 109.0 . . ?
C00O C00M H00B 109.0 . . ?
C00O C00M C00X 113.1(3) . . ?
C00X C00M H00A 109.0 . . ?
C00X C00M H00B 109.0 . . ?
C00A C00N H00C 108.1 . . ?
C00A C00N H00D 108.1 . . ?
H00C C00N H00D 107.3 . . ?
C00U C00N C00A 116.8(3) . . ?
C00U C00N H00C 108.1 . . ?
C00U C00N H00D 108.1 . . ?
C00C C00O C00M 122.0(3) . . ?
C018 C00O C00C 118.3(3) . . ?
C018 C00O C00M 119.7(3) . . ?
C00V C00P C01D 108.1(3) . . ?
C00V C00P C010 115.1(3) . . ?
C01D C00P C010 106.2(3) . . ?
C01J C00P C00V 107.1(3) . . ?
C01J C00P C01D 108.4(3) . . ?
C01J C00P C010 111.7(3) . . ?
C00H C00Q H00Q 119.1 . . ?
C00H C00Q C00X 121.8(4) . . ?
C00X C00Q H00Q 119.1 . . ?
C00C C00R C00Z 121.8(3) . . ?
C00K C00R C00C 116.8(3) . . ?
C00K C00R C00Z 121.4(3) . . ?
C00F C00S H00S 120.0 . . ?
C019 C00S C00F 120.0(3) . . ?
C019 C00S H00S 120.0 . . ?
C00H C00T H00T 118.3 . . ?
C00H C00T C011 123.4(3) . . ?
C011 C00T H00T 118.3 . . ?
C00Y C00U C00N 120.3(3) . . ?
C012 C00U C00N 120.5(3) . . ?
C012 C00U C00Y 119.2(3) . . ?
C00P C00V H00F 109.5 . . ?
C00P C00V H00G 109.5 . . ?
C00P C00V H00H 109.5 . . ?
H00F C00V H00G 109.5 . . ?
H00F C00V H00H 109.5 . . ?
H00G C00V H00H 109.5 . . ?
C00D C00W C01H 108.6(3) . . ?
C01F C00W C00D 111.5(3) . . ?
C01F C00W C01H 108.7(3) . . ?
C01I C00W C00D 111.1(3) . . ?
C01I C00W C01F 107.2(3) . . ?
C01I C00W C01H 109.7(3) . . ?
C00Q C00X C00M 119.0(3) . . ?
C00Q C00X C017 119.3(3) . . ?
C017 C00X C00M 121.7(3) . . ?
O006 C00Y C00D 120.8(3) . . ?
O006 C00Y C00U 118.0(3) . . ?
C00U C00Y C00D 121.3(3) . . ?
C00R C00Z C01C 110.8(3) . . ?
C00R C00Z C01K 109.3(3) . . ?
C00R C00Z C01Q 111.7(3) . . ?
C01C C00Z C01K 111.1(3) . . ?
C01C C00Z C01Q 106.1(3) . . ?
C01Q C00Z C01K 107.7(3) . . ?
C01B C01A N00G 120.6(3) . . ?
C01B C01A C01P 117.8(3) . . ?
C01P C01A N00G 121.5(3) . . ?
C01A C01B H01B 119.8 . . ?
C01E C01B C01A 120.3(4) . . ?
C01E C01B H01B 119.8 . . ?
C00Z C01C H01A 109.5 . . ?
C00Z C01C H01C 109.5 . . ?
C00Z C01C H01D 109.5 . . ?
H01A C01C H01C 109.5 . . ?
H01A C01C H01D 109.5 . . ?
H01C C01C H01D 109.5 . . ?
C00P C01D H01E 109.5 . . ?
C00P C01D H01F 109.5 . . ?
C00P C01D H01G 109.5 . . ?
H01E C01D H01F 109.5 . . ?
H01E C01D H01G 109.5 . . ?
H01F C01D H01G 109.5 . . ?
C00B C01E C01B 121.6(4) . . ?
C00B C01E H01H 119.2 . . ?
C01B C01E H01H 119.2 . . ?
C00W C01F H01I 109.5 . . ?
C00W C01F H01J 109.5 . . ?
C00W C01F H01K 109.5 . . ?
H01I C01F H01J 109.5 . . ?
H01I C01F H01K 109.5 . . ?
H01J C01F H01K 109.5 . . ?
C01N C01G H01L 118.4 . . ?
C01N C01G C010 123.2(3) . . ?
C010 C01G H01L 118.4 . . ?
C00W C01H H01M 109.5 . . ?
C00W C01H H01N 109.5 . . ?
C00W C01H H01O 109.5 . . ?
H01M C01H H01N 109.5 . . ?
H01M C01H H01O 109.5 . . ?
H01N C01H H01O 109.5 . . ?
C00W C01I H01P 109.5 . . ?
C00W C01I H01Q 109.5 . . ?
C00W C01I H01R 109.5 . . ?
H01P C01I H01Q 109.5 . . ?
H01P C01I H01R 109.5 . . ?
H01Q C01I H01R 109.5 . . ?
C00P C01J H01S 109.5 . . ?
C00P C01J H01T 109.5 . . ?
C00P C01J H01U 109.5 . . ?
H01S C01J H01T 109.5 . . ?
H01S C01J H01U 109.5 . . ?
H01T C01J H01U 109.5 . . ?
C00Z C01K H01V 109.5 . . ?
C00Z C01K H01W 109.5 . . ?
C00Z C01K H01X 109.5 . . ?
H01V C01K H01W 109.5 . . ?
H01V C01K H01X 109.5 . . ?
H01W C01K H01X 109.5 . . ?
C01T C01L C01V 107.0(4) . . ?
C01T C01L C01W 110.5(4) . . ?
C01T C01L C011 108.7(3) . . ?
C01W C01L C01V 106.6(4) . . ?
C011 C01L C01V 112.1(4) . . ?
C011 C01L C01W 111.8(4) . . ?
C00H C01M H01Y 109.5 . . ?
C00H C01M H 109.5 . . ?
C00H C01M HA 109.5 . . ?
H01Y C01M H 109.5 . . ?
H01Y C01M HA 109.5 . . ?
H C01M HA 109.5 . . ?
C00L C01N C01G 118.3(3) . . ?
C00L C01N C01Z 121.1(4) . . ?
C01G C01N C01Z 120.6(4) . . ?
C00I C01O H01Z 109.5 . . ?
C00I C01O HB 109.5 . . ?
C00I C01O HC 109.5 . . ?
H01Z C01O HB 109.5 . . ?
H01Z C01O HC 109.5 . . ?
HB C01O HC 109.5 . . ?
C00E C01P C01A 121.1(3) . . ?
C00E C01P H01 119.4 . . ?
C01A C01P H01 119.4 . . ?
C00Z C01Q H0AA 109.5 . . ?
C00Z C01Q HD 109.5 . . ?
C00Z C01Q HE 109.5 . . ?
H0AA C01Q HD 109.5 . . ?
H0AA C01Q HE 109.5 . . ?
HD C01Q HE 109.5 . . ?
C00J C01R H1AA 109.5 . . ?
C00J C01R HF 109.5 . . ?
C00J C01R HG 109.5 . . ?
H1AA C01R HF 109.5 . . ?
H1AA C01R HG 109.5 . . ?
HF C01R HG 109.5 . . ?
N007 C01S H2AA 109.5 . . ?
N007 C01S HH 109.5 . . ?
N007 C01S HI 109.5 . . ?
H2AA C01S HH 109.5 . . ?
H2AA C01S HI 109.5 . . ?
HH C01S HI 109.5 . . ?
C01L C01T H3AA 109.5 . . ?
C01L C01T HJ 109.5 . . ?
C01L C01T HK 109.5 . . ?
H3AA C01T HJ 109.5 . . ?
H3AA C01T HK 109.5 . . ?
HJ C01T HK 109.5 . . ?
N007 C01U H4AA 109.5 . . ?
N007 C01U HL 109.5 . . ?
N007 C01U HM 109.5 . . ?
H4AA C01U HL 109.5 . . ?
H4AA C01U HM 109.5 . . ?
HL C01U HM 109.5 . . ?
C01L C01V H5AA 109.5 . . ?
C01L C01V HN 109.5 . . ?
C01L C01V HO 109.5 . . ?
H5AA C01V HN 109.5 . . ?
H5AA C01V HO 109.5 . . ?
HN C01V HO 109.5 . . ?
C01L C01W H6AA 109.5 . . ?
C01L C01W HP 109.5 . . ?
C01L C01W HQ 109.5 . . ?
H6AA C01W HP 109.5 . . ?
H6AA C01W HQ 109.5 . . ?
HP C01W HQ 109.5 . . ?
C00B C01X H7AA 109.5 . . ?
C00B C01X HR 109.5 . . ?
C00B C01X HS 109.5 . . ?
H7AA C01X HR 109.5 . . ?
H7AA C01X HS 109.5 . . ?
HR C01X HS 109.5 . . ?
H8AA C01Y HT 109.5 . . ?
H8AA C01Y HU 109.5 . . ?
HT C01Y HU 109.5 . . ?
C015 C01Y H8AA 109.5 . . ?
C015 C01Y HT 109.5 . . ?
C015 C01Y HU 109.5 . . ?
C01N C01Z H9AA 109.5 . . ?
C01N C01Z HV 109.5 . . ?
C01N C01Z HW 109.5 . . ?
H9AA C01Z HV 109.5 . . ?
H9AA C01Z HW 109.5 . . ?
HV C01Z HW 109.5 . . ?
O003 C009 C00A 117.9(3) . . ?
O003 C009 C010 120.8(3) . . ?
C010 C009 C00A 121.2(3) . . ?
C01G C010 C00P 119.0(3) . . ?
C01G C010 C009 116.5(3) . . ?
C009 C010 C00P 124.0(3) . . ?
C00T C011 C01L 121.8(3) . . ?
C00T C011 C017 116.8(3) . . ?
C017 C011 C01L 121.3(3) . . ?
C00I C012 C00U 121.7(3) . . ?
C00I C012 H012 119.1 . . ?
C00U C012 H012 119.1 . . ?
C015 C013 H013 119.3 . . ?
C016 C013 H013 119.3 . . ?
C016 C013 C015 121.4(3) . . ?
C00D C014 H014 118.2 . . ?
C00I C014 C00D 123.6(3) . . ?
C00I C014 H014 118.2 . . ?
C013 C015 C01Y 120.9(4) . . ?
C019 C015 C01Y 121.8(4) . . ?
C019 C015 C013 117.3(3) . . ?
C00F C016 H016 119.2 . . ?
C013 C016 C00F 121.5(3) . . ?
C013 C016 H016 119.2 . . ?
O004 C017 C00X 119.5(3) . . ?
O004 C017 C011 119.6(3) . . ?
C00X C017 C011 120.9(3) . . ?
C00J C018 C00O 121.9(3) . . ?
C00J C018 H018 119.1 . . ?
C00O C018 H018 119.1 . . ?
C00S C019 C015 122.5(3) . . ?
C00S C019 H019 118.7 . . ?
C015 C019 H019 118.7 . . ?
H1SA C1S H1SB 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?
C2S C1S H1SA 109.5 . . ?
C2S C1S H1SB 109.5 . . ?
C2S C1S H1SC 109.5 . . ?
C1S C2S H2SA 108.1 . . ?
C1S C2S H2SB 108.1 . . ?
H2SA C2S H2SB 107.3 . . ?
C3S C2S C1S 116.7(11) . . ?
C3S C2S H2SA 108.1 . . ?
C3S C2S H2SB 108.1 . . ?
C2S C3S H3SA 107.8 . . ?
C2S C3S H3SB 107.8 . . ?
C2S C3S C4S 117.9(13) . . ?
H3SA C3S H3SB 107.2 . . ?
C4S C3S H3SA 107.8 . . ?
C4S C3S H3SB 107.8 . . ?
C3S C4S H4SA 107.5 . . ?
C3S C4S H4SB 107.5 . . ?
H4SA C4S H4SB 107.0 . . ?
C5S C4S C3S 119.3(14) . . ?
C5S C4S H4SA 107.5 . . ?
C5S C4S H4SB 107.5 . . ?
C4S C5S H5SA 107.8 . . ?
C4S C5S H5SB 107.8 . . ?
C4S C5S C6S 117.9(15) . . ?
H5SA C5S H5SB 107.2 . . ?
C6S C5S H5SA 107.8 . . ?
C6S C5S H5SB 107.8 . . ?
C5S C6S H6SA 109.5 . . ?
C5S C6S H6SB 109.5 . . ?
C5S C6S H6SC 109.5 . . ?
H6SA C6S H6SB 109.5 . . ?
H6SA C6S H6SC 109.5 . . ?
H6SB C6S H6SC 109.5 . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_early_a
_database_code_depnum_ccdc_archive 'CCDC 1905885'
loop_
_audit_author_name
_audit_author_address
'Kelly E Aldrich'
;Michigan State University
United States of America
;
_audit_update_record             
;
2019-03-27 deposited with the CCDC.	2019-05-07 downloaded from the CCDC.
;
_audit_creation_date             2019-03-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C23 H30 I2 O2 Ti'
_chemical_formula_sum            'C23 H30 I2 O2 Ti'
_chemical_formula_weight         640.17
_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 0.0181 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'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6900(10)
_cell_length_b                   9.8844(13)
_cell_length_c                   13.151(2)
_cell_angle_alpha                90.518(7)
_cell_angle_beta                 92.411(5)
_cell_angle_gamma                95.161(4)
_cell_volume                     1253.3(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    720
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.07
_cell_measurement_theta_min      25.12
_shelx_estimated_absorpt_T_max   0.329
_shelx_estimated_absorpt_T_min   0.123
_exptl_absorpt_coefficient_mu    22.340
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.4177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1246 before and 0.0743 after correction. The Ratio of minimum to maximum transmission is 0.5547. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.064
_exptl_special_details           
;
Data was collected using a BRUKER CCD (charge coupled device) based
diffractometer equipped with an Oxford low-temperature apparatus operating at
173 K.  A suitable crystal was chosen and mounted on a nylon loop using 
Paratone oil.  Data  were measured using omega and phi scans of 1.0° per frame 
for 30 s. The total number of images were based on 
results from the program COSMO where redundancy was expected to be 4 and 
completeness to 0.83Å to 100%. Cell parameters were
retrieved using APEX II software and refined using SAINT on all observed
reflections.Data reduction was performed using the SAINT software which 
corrects for Lp. Scaling and absorption corrections were applied using SADABS6 
multi-scan technique, supplied by George Sheldrick.  The structure was solved 
by the direct method using the SHELXT program and refined by least squares 
method on F2, SHELXL, incorporated in OLEX2. 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1065
_diffrn_reflns_av_unetI/netI     0.0869
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15520
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.154
_diffrn_reflns_theta_min         4.492
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean 8.36
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3281
_reflns_number_total             4410
_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       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.185
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         4410
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0521
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0596P)²+0.9570P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1365
_refine_special_details          
;
The structure was refined by Least Squares using version 2018/3 
of XL (Sheldrick, 2015) incorporated in Olex2 (Dolomanov et al., 2009). 
All non-hydrogen atoms were refined anisotropically. 
Hydrogen atom positions were calculated geometrically and refined using the 
riding model, except for the hydrogen atom(s) on the non-carbon atom(s) 
which was found by difference Fourier methods and refined isotropically.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00G(H00E,H00G)
2.b Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00F(H00F), C00O(H00T), C00Q(H00X)
2.c Idealised Me refined as rotating group:
 C00E(H00B,H00C,H00D), C00I(H00H,H00I,H00J), C00L(H00K,H00L,H00M), C00M(H00N,
 H00O,H00P), C00N(H00Q,H00R,H00S), C00P(H00U,H00V,H00W), C00R(H00Y,H,HA),
 C00S(H00Z,HB,HC)
;
_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
I001 I 0.06336(6) 0.32430(7) 0.09509(4) 0.04569(19) Uani 1 1 d . . . . .
I002 I 0.04048(6) 0.57809(6) 0.35070(4) 0.04517(19) Uani 1 1 d . . . . .
Ti03 Ti 0.20781(12) 0.48357(13) 0.22516(9) 0.0241(3) Uani 1 1 d . . . . .
O004 O 0.3079(5) 0.6145(5) 0.1633(4) 0.0282(11) Uani 1 1 d . . . . .
O005 O 0.3251(5) 0.3909(5) 0.2942(3) 0.0244(10) Uani 1 1 d . . . . .
C006 C 0.7137(7) 0.7906(8) 0.1556(5) 0.0264(15) Uani 1 1 d . . . . .
C007 C 0.4498(7) 0.3399(7) 0.3160(5) 0.0249(15) Uani 1 1 d . . . . .
C008 C 0.4415(6) 0.6743(7) 0.1553(5) 0.0206(14) Uani 1 1 d . . . . .
C009 C 0.5517(7) 0.3622(7) 0.2443(5) 0.0249(15) Uani 1 1 d . . . . .
C00A C 0.6805(7) 0.3115(8) 0.2644(6) 0.0280(15) Uani 1 1 d . . . . .
H00A H 0.7512 0.3258 0.2167 0.034 Uiso 1 1 calc R . . . .
C00B C 0.4720(7) 0.2729(7) 0.4078(5) 0.0226(14) Uani 1 1 d . . . . .
C00C C 0.7063(8) 0.2407(8) 0.3528(6) 0.0337(17) Uani 1 1 d . . . . .
C00D C 0.3611(7) 0.2561(8) 0.4898(5) 0.0256(15) Uani 1 1 d . . . . .
C00E C 0.3315(8) 0.3946(8) 0.5295(6) 0.0342(18) Uani 1 1 d . . . . .
H00B H 0.4176 0.4427 0.5578 0.051 Uiso 1 1 calc GR . . . .
H00C H 0.2638 0.3834 0.5827 0.051 Uiso 1 1 calc GR . . . .
H00D H 0.2940 0.4472 0.4736 0.051 Uiso 1 1 calc GR . . . .
C00F C 0.6862(7) 0.6524(8) 0.1528(5) 0.0286(16) Uani 1 1 d . . . . .
H00F H 0.7613 0.5971 0.1511 0.034 Uiso 1 1 calc R . . . .
C00G C 0.5248(7) 0.4363(7) 0.1456(5) 0.0264(15) Uani 1 1 d . . . . .
H00E H 0.5851 0.4034 0.0936 0.032 Uiso 1 1 calc R . . . .
H00G H 0.4274 0.4117 0.1218 0.032 Uiso 1 1 calc R . . . .
C00H C 0.3448(8) 0.9106(8) 0.1449(6) 0.0301(16) Uani 1 1 d . . . . .
C00I C 0.2277(8) 0.1772(9) 0.4458(6) 0.0367(19) Uani 1 1 d . . . . .
H00H H 0.1928 0.2246 0.3862 0.055 Uiso 1 1 calc GR . . . .
H00I H 0.1576 0.1710 0.4975 0.055 Uiso 1 1 calc GR . . . .
H00J H 0.2478 0.0856 0.4255 0.055 Uiso 1 1 calc GR . . . .
C00J C 0.4632(7) 0.8158(8) 0.1508(5) 0.0247(15) Uani 1 1 d . . . . .
C00K C 0.5492(7) 0.5895(8) 0.1524(5) 0.0254(15) Uani 1 1 d . . . . .
C00L C 0.8434(9) 0.1846(10) 0.3738(8) 0.050(2) Uani 1 1 d . . . . .
H00K H 0.9042 0.2066 0.3174 0.075 Uiso 1 1 calc GR . . . .
H00L H 0.8290 0.0857 0.3806 0.075 Uiso 1 1 calc GR . . . .
H00M H 0.8866 0.2247 0.4371 0.075 Uiso 1 1 calc GR . . . .
C00M C 0.8599(8) 0.8548(9) 0.1617(7) 0.0395(19) Uani 1 1 d . . . . .
H00N H 0.8828 0.8899 0.2309 0.059 Uiso 1 1 calc GR . . . .
H00O H 0.8694 0.9296 0.1134 0.059 Uiso 1 1 calc GR . . . .
H00P H 0.9233 0.7868 0.1449 0.059 Uiso 1 1 calc GR . . . .
C00N C 0.2443(8) 0.8673(8) 0.0538(6) 0.0357(18) Uani 1 1 d . . . . .
H00Q H 0.2948 0.8728 -0.0092 0.054 Uiso 1 1 calc GR . . . .
H00R H 0.1696 0.9280 0.0498 0.054 Uiso 1 1 calc GR . . . .
H00S H 0.2046 0.7738 0.0631 0.054 Uiso 1 1 calc GR . . . .
C00O C 0.6023(8) 0.2252(8) 0.4228(6) 0.0304(16) Uani 1 1 d . . . . .
H00T H 0.6213 0.1795 0.4844 0.036 Uiso 1 1 calc R . . . .
C00P C 0.2661(9) 0.9020(9) 0.2446(7) 0.0402(19) Uani 1 1 d . . . . .
H00U H 0.2237 0.8091 0.2528 0.060 Uiso 1 1 calc GR . . . .
H00V H 0.1937 0.9651 0.2419 0.060 Uiso 1 1 calc GR . . . .
H00W H 0.3311 0.9262 0.3023 0.060 Uiso 1 1 calc GR . . . .
C00Q C 0.6021(8) 0.8685(8) 0.1521(5) 0.0276(15) Uani 1 1 d . . . . .
H00X H 0.6211 0.9644 0.1505 0.033 Uiso 1 1 calc R . . . .
C00R C 0.4104(10) 0.1746(10) 0.5810(7) 0.044(2) Uani 1 1 d . . . . .
H00Y H 0.4283 0.0835 0.5579 0.067 Uiso 1 1 calc GR . . . .
H H 0.3386 0.1673 0.6314 0.067 Uiso 1 1 calc GR . . . .
HA H 0.4959 0.2210 0.6118 0.067 Uiso 1 1 calc GR . . . .
C00S C 0.3961(9) 1.0578(9) 0.1299(7) 0.041(2) Uani 1 1 d . . . . .
H00Z H 0.4554 1.0906 0.1889 0.061 Uiso 1 1 calc GR . . . .
HB H 0.3167 1.1123 0.1229 0.061 Uiso 1 1 calc GR . . . .
HC H 0.4495 1.0659 0.0683 0.061 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
I001 Ti03 2.5917(14) . ?
I002 Ti03 2.5880(13) . ?
Ti03 O004 1.771(5) . ?
Ti03 O005 1.753(5) . ?
O004 C008 1.383(8) . ?
O005 C007 1.371(9) . ?
C006 C00F 1.368(11) . ?
C006 C00M 1.498(10) . ?
C006 C00Q 1.382(11) . ?
C007 C009 1.399(10) . ?
C007 C00B 1.401(10) . ?
C008 C00J 1.398(11) . ?
C008 C00K 1.397(10) . ?
C009 C00A 1.402(10) . ?
C009 C00G 1.520(10) . ?
C00A H00A 0.9500 . ?
C00A C00C 1.388(11) . ?
C00B C00D 1.554(9) . ?
C00B C00O 1.394(10) . ?
C00C C00L 1.502(11) . ?
C00C C00O 1.392(11) . ?
C00D C00E 1.516(11) . ?
C00D C00I 1.537(10) . ?
C00D C00R 1.534(11) . ?
C00E H00B 0.9800 . ?
C00E H00C 0.9800 . ?
C00E H00D 0.9800 . ?
C00F H00F 0.9500 . ?
C00F C00K 1.414(10) . ?
C00G H00E 0.9900 . ?
C00G H00G 0.9900 . ?
C00G C00K 1.513(11) . ?
C00H C00J 1.545(10) . ?
C00H C00N 1.544(10) . ?
C00H C00P 1.543(11) . ?
C00H C00S 1.512(12) . ?
C00I H00H 0.9800 . ?
C00I H00I 0.9800 . ?
C00I H00J 0.9800 . ?
C00J C00Q 1.398(10) . ?
C00L H00K 0.9800 . ?
C00L H00L 0.9800 . ?
C00L H00M 0.9800 . ?
C00M H00N 0.9800 . ?
C00M H00O 0.9800 . ?
C00M H00P 0.9800 . ?
C00N H00Q 0.9800 . ?
C00N H00R 0.9800 . ?
C00N H00S 0.9800 . ?
C00O H00T 0.9500 . ?
C00P H00U 0.9800 . ?
C00P H00V 0.9800 . ?
C00P H00W 0.9800 . ?
C00Q H00X 0.9500 . ?
C00R H00Y 0.9800 . ?
C00R H 0.9800 . ?
C00R HA 0.9800 . ?
C00S H00Z 0.9800 . ?
C00S HB 0.9800 . ?
C00S HC 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I002 Ti03 I001 108.41(5) . . ?
O004 Ti03 I001 111.37(17) . . ?
O004 Ti03 I002 112.25(17) . . ?
O005 Ti03 I001 109.58(17) . . ?
O005 Ti03 I002 108.50(16) . . ?
O005 Ti03 O004 106.7(2) . . ?
C008 O004 Ti03 143.1(5) . . ?
C007 O005 Ti03 155.9(5) . . ?
C00F C006 C00M 120.9(7) . . ?
C00F C006 C00Q 117.7(7) . . ?
C00Q C006 C00M 121.4(7) . . ?
O005 C007 C009 116.8(6) . . ?
O005 C007 C00B 120.1(6) . . ?
C009 C007 C00B 123.0(7) . . ?
O004 C008 C00J 119.0(6) . . ?
O004 C008 C00K 118.0(6) . . ?
C00K C008 C00J 123.0(6) . . ?
C007 C009 C00A 118.2(7) . . ?
C007 C009 C00G 121.8(6) . . ?
C00A C009 C00G 120.0(6) . . ?
C009 C00A H00A 119.5 . . ?
C00C C00A C009 121.0(7) . . ?
C00C C00A H00A 119.5 . . ?
C007 C00B C00D 122.6(6) . . ?
C00O C00B C007 115.7(6) . . ?
C00O C00B C00D 121.7(6) . . ?
C00A C00C C00L 121.1(8) . . ?
C00A C00C C00O 118.2(7) . . ?
C00O C00C C00L 120.7(8) . . ?
C00E C00D C00B 109.8(6) . . ?
C00E C00D C00I 110.9(6) . . ?
C00E C00D C00R 107.5(6) . . ?
C00I C00D C00B 110.6(6) . . ?
C00R C00D C00B 111.8(6) . . ?
C00R C00D C00I 106.3(7) . . ?
C00D C00E H00B 109.5 . . ?
C00D C00E H00C 109.5 . . ?
C00D C00E H00D 109.5 . . ?
H00B C00E H00C 109.5 . . ?
H00B C00E H00D 109.5 . . ?
H00C C00E H00D 109.5 . . ?
C006 C00F H00F 119.0 . . ?
C006 C00F C00K 121.9(7) . . ?
C00K C00F H00F 119.0 . . ?
C009 C00G H00E 108.4 . . ?
C009 C00G H00G 108.4 . . ?
H00E C00G H00G 107.5 . . ?
C00K C00G C009 115.3(6) . . ?
C00K C00G H00E 108.4 . . ?
C00K C00G H00G 108.4 . . ?
C00N C00H C00J 109.5(6) . . ?
C00P C00H C00J 109.6(6) . . ?
C00P C00H C00N 109.8(7) . . ?
C00S C00H C00J 113.0(6) . . ?
C00S C00H C00N 107.2(7) . . ?
C00S C00H C00P 107.7(7) . . ?
C00D C00I H00H 109.5 . . ?
C00D C00I H00I 109.5 . . ?
C00D C00I H00J 109.5 . . ?
H00H C00I H00I 109.5 . . ?
H00H C00I H00J 109.5 . . ?
H00I C00I H00J 109.5 . . ?
C008 C00J C00H 123.8(6) . . ?
C008 C00J C00Q 115.2(6) . . ?
C00Q C00J C00H 121.0(7) . . ?
C008 C00K C00F 117.3(7) . . ?
C008 C00K C00G 123.1(6) . . ?
C00F C00K C00G 119.6(7) . . ?
C00C C00L H00K 109.5 . . ?
C00C C00L H00L 109.5 . . ?
C00C C00L H00M 109.5 . . ?
H00K C00L H00L 109.5 . . ?
H00K C00L H00M 109.5 . . ?
H00L C00L H00M 109.5 . . ?
C006 C00M H00N 109.5 . . ?
C006 C00M H00O 109.5 . . ?
C006 C00M H00P 109.5 . . ?
H00N C00M H00O 109.5 . . ?
H00N C00M H00P 109.5 . . ?
H00O C00M H00P 109.5 . . ?
C00H C00N H00Q 109.5 . . ?
C00H C00N H00R 109.5 . . ?
C00H C00N H00S 109.5 . . ?
H00Q C00N H00R 109.5 . . ?
H00Q C00N H00S 109.5 . . ?
H00R C00N H00S 109.5 . . ?
C00B C00O H00T 118.1 . . ?
C00C C00O C00B 123.8(7) . . ?
C00C C00O H00T 118.1 . . ?
C00H C00P H00U 109.5 . . ?
C00H C00P H00V 109.5 . . ?
C00H C00P H00W 109.5 . . ?
H00U C00P H00V 109.5 . . ?
H00U C00P H00W 109.5 . . ?
H00V C00P H00W 109.5 . . ?
C006 C00Q C00J 124.5(7) . . ?
C006 C00Q H00X 117.7 . . ?
C00J C00Q H00X 117.7 . . ?
C00D C00R H00Y 109.5 . . ?
C00D C00R H 109.5 . . ?
C00D C00R HA 109.5 . . ?
H00Y C00R H 109.5 . . ?
H00Y C00R HA 109.5 . . ?
H C00R HA 109.5 . . ?
C00H C00S H00Z 109.5 . . ?
C00H C00S HB 109.5 . . ?
C00H C00S HC 109.5 . . ?
H00Z C00S HB 109.5 . . ?
H00Z C00S HC 109.5 . . ?
HB C00S HC 109.5 . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
