# Supplementary Information (SI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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. 
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data_vfr31_exfs_a
_database_code_depnum_ccdc_archive 'CCDC 2345354'
loop_
_audit_author_name
_audit_author_address
'Gino G. Lavoie'
;York University
Canada
;
_audit_update_record             
;
2024-04-02 deposited with the CCDC.	2024-08-06 downloaded from the CCDC.
;

_audit_creation_date             2023-07-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H40 Cl2 N6 O2 Ti, C7 H8'
_chemical_formula_sum            'C37 H48 Cl2 N6 O2 Ti'
_chemical_formula_weight         727.61
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.6343(7)
_cell_length_b                   30.9675(18)
_cell_length_c                   12.5823(8)
_cell_angle_alpha                90
_cell_angle_beta                 110.817(2)
_cell_angle_gamma                90
_cell_volume                     3873.1(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9707
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      33.04
_cell_measurement_theta_min      2.26
_shelx_estimated_absorpt_T_max   0.990
_shelx_estimated_absorpt_T_min   0.961
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rod
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.025
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            150839
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.152
_diffrn_ambient_temperature      173.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10282
_reflns_number_total             11792
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-1997  (Sheldrick, 2008)'
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         11792
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0600
_refine_ls_restrained_S_all      1.191
_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)+(0.0494P)²+2.5209P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1352
_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. Restrained distances
 C6S-C1S \\sim C9S-C8S
 with sigma of 0.02
 C6S-C5S \\sim C9S-C10S
 with sigma of 0.02
 C2S-C3S \\sim C13S-C12S
 with sigma of 0.02
 C1S-C7S \\sim C8S-C14S
 with sigma of 0.02
 C6S-C7S \\sim C9S-C14S
 with sigma of 0.04
 C1S-C5S \\sim C8S-C10S
 with sigma of 0.04
3. Others
 Sof(C10S)=Sof(H10S)=Sof(C9S)=Sof(H9S)=Sof(C8S)=Sof(C14S)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=Sof(C13S)=Sof(H13S)=Sof(C12S)=Sof(H12S)=Sof(C11S)=Sof(H11S)=1-FVAR(1)
 Sof(C6S)=Sof(H6S)=Sof(C2S)=Sof(H2S)=Sof(C1S)=Sof(C5S)=Sof(H5S)=Sof(C4S)=
 Sof(H4S)=Sof(C3S)=Sof(H3S)=Sof(C7S)=Sof(H7SA)=Sof(H7SB)=Sof(H7SC)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C4(H4), C7(H7), C19(H19), C22(H22)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C15(H15), C14(H14), C13(H13), C12(H12), C30(H30), C29(H29),
 C28(H28), C27(H27), C17(H17), C18(H18), C6S(H6S), C2S(H2S), C5S(H5S), C4S(H4S),
  C3S(H3S), C10S(H10S), C9S(H9S), C13S(H13S), C12S(H12S), C11S(H11S)
4.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C20(H20A,
 H20B,H20C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C),
 C7S(H7SA,H7SB,H7SC), C14S(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 0.80252(3) 0.63193(2) 0.62664(3) 0.02140(8) Uani 1 1 d . . . . .
Cl1 Cl 0.98574(5) 0.60531(2) 0.57929(5) 0.03454(12) Uani 1 1 d . . . . .
Cl2 Cl 0.85141(5) 0.70204(2) 0.57232(4) 0.03058(10) Uani 1 1 d . . . . .
O1 O 0.80916(14) 0.58128(4) 0.71508(11) 0.0286(3) Uani 1 1 d . . . . .
O2 O 0.62467(14) 0.64827(5) 0.61922(12) 0.0294(3) Uani 1 1 d . . . . .
N1 N 0.88978(16) 0.65442(5) 0.79125(13) 0.0242(3) Uani 1 1 d . . . . .
N2 N 0.84953(17) 0.72814(5) 0.83484(14) 0.0295(3) Uani 1 1 d . . . . .
N3 N 1.05511(16) 0.71148(5) 0.85542(14) 0.0291(3) Uani 1 1 d . . . . .
N4 N 0.67991(14) 0.60784(5) 0.47116(12) 0.0217(3) Uani 1 1 d . . . . .
N5 N 0.74831(16) 0.60135(5) 0.30835(13) 0.0275(3) Uani 1 1 d . . . . .
N6 N 0.73371(17) 0.54164(5) 0.39451(15) 0.0300(3) Uani 1 1 d . . . . .
C11 C 0.86139(18) 0.58232(6) 0.82859(15) 0.0240(3) Uani 1 1 d . . . . .
C10 C 0.90679(18) 0.62323(6) 0.87586(15) 0.0229(3) Uani 1 1 d . . . . .
C1 C 0.92944(19) 0.69581(6) 0.82633(15) 0.0245(3) Uani 1 1 d . . . . .
C4 C 0.7037(2) 0.72431(7) 0.8119(2) 0.0391(5) Uani 1 1 d . . . . .
H4 H 0.675539 0.694124 0.786019 0.047 Uiso 1 1 calc R U . . .
C6 C 0.6264(3) 0.75475(10) 0.7172(3) 0.0561(7) Uani 1 1 d . . . . .
H6A H 0.649489 0.784647 0.742111 0.084 Uiso 1 1 calc R U . . .
H6B H 0.529667 0.750278 0.698272 0.084 Uiso 1 1 calc R U . . .
H6C H 0.650053 0.749070 0.650032 0.084 Uiso 1 1 calc R U . . .
C5 C 0.6768(3) 0.73204(11) 0.9214(3) 0.0612(8) Uani 1 1 d . . . . .
H5A H 0.732667 0.712476 0.980642 0.092 Uiso 1 1 calc R U . . .
H5B H 0.581665 0.726608 0.908146 0.092 Uiso 1 1 calc R U . . .
H5C H 0.698900 0.762012 0.945967 0.092 Uiso 1 1 calc R U . . .
C2 C 0.9262(2) 0.76521(7) 0.8683(2) 0.0372(5) Uani 1 1 d . . . . .
H2 H 0.894491 0.792879 0.879688 0.045 Uiso 1 1 calc R U . . .
C3 C 1.0532(2) 0.75491(6) 0.8816(2) 0.0381(5) Uani 1 1 d . . . . .
H3 H 1.128249 0.773893 0.904767 0.046 Uiso 1 1 calc R U . . .
C7 C 1.1722(2) 0.68671(7) 0.8523(2) 0.0379(5) Uani 1 1 d . . . . .
H7 H 1.139752 0.657405 0.821199 0.045 Uiso 1 1 calc R U . . .
C9 C 1.2742(3) 0.68090(8) 0.9719(3) 0.0537(7) Uani 1 1 d . . . . .
H9A H 1.309375 0.709166 1.003772 0.080 Uiso 1 1 calc R U . . .
H9B H 1.348334 0.662685 0.969182 0.080 Uiso 1 1 calc R U . . .
H9C H 1.230571 0.667096 1.019857 0.080 Uiso 1 1 calc R U . . .
C8 C 1.2306(3) 0.70824(11) 0.7725(3) 0.0653(8) Uani 1 1 d . . . . .
H8A H 1.160135 0.711636 0.697489 0.098 Uiso 1 1 calc R U . . .
H8B H 1.303355 0.690350 0.765621 0.098 Uiso 1 1 calc R U . . .
H8C H 1.266180 0.736678 0.802553 0.098 Uiso 1 1 calc R U . . .
C15 C 0.9605(2) 0.62845(7) 0.99355(16) 0.0299(4) Uani 1 1 d . . . . .
H15 H 0.990194 0.655993 1.026004 0.036 Uiso 1 1 calc R U . . .
C14 C 0.9698(2) 0.59245(8) 1.06298(17) 0.0348(4) Uani 1 1 d . . . . .
H14 H 1.006880 0.595599 1.143279 0.042 Uiso 1 1 calc R U . . .
C13 C 0.9258(2) 0.55227(7) 1.01628(18) 0.0357(4) Uani 1 1 d . . . . .
H13 H 0.932941 0.528141 1.064711 0.043 Uiso 1 1 calc R U . . .
C12 C 0.8712(2) 0.54699(6) 0.89881(18) 0.0310(4) Uani 1 1 d . . . . .
H12 H 0.840867 0.519394 0.867008 0.037 Uiso 1 1 calc R U . . .
C26 C 0.51564(18) 0.63709(6) 0.53128(17) 0.0260(4) Uani 1 1 d . . . . .
C25 C 0.54143(17) 0.61456(6) 0.44407(16) 0.0244(3) Uani 1 1 d . . . . .
C30 C 0.4364(2) 0.60206(8) 0.3470(2) 0.0382(5) Uani 1 1 d . . . . .
H30 H 0.453453 0.587697 0.286757 0.046 Uiso 1 1 calc R U . . .
C29 C 0.3039(2) 0.61115(9) 0.3398(3) 0.0527(7) Uani 1 1 d . . . . .
H29 H 0.230698 0.602910 0.273708 0.063 Uiso 1 1 calc R U . . .
C28 C 0.2792(2) 0.63165(8) 0.4264(3) 0.0516(7) Uani 1 1 d . . . . .
H28 H 0.188900 0.636786 0.420538 0.062 Uiso 1 1 calc R U . . .
C27 C 0.3836(2) 0.64509(7) 0.5227(2) 0.0383(5) Uani 1 1 d . . . . .
H27 H 0.365385 0.659585 0.582215 0.046 Uiso 1 1 calc R U . . .
C16 C 0.71775(17) 0.58472(6) 0.39477(15) 0.0237(3) Uani 1 1 d . . . . .
C19 C 0.7447(2) 0.64795(7) 0.28247(17) 0.0324(4) Uani 1 1 d . . . . .
H19 H 0.721252 0.663483 0.342606 0.039 Uiso 1 1 calc R U . . .
C20 C 0.6344(4) 0.65756(11) 0.1695(3) 0.0714(10) Uani 1 1 d . . . . .
H20A H 0.655545 0.643486 0.108102 0.107 Uiso 1 1 calc R U . . .
H20B H 0.627838 0.688833 0.156718 0.107 Uiso 1 1 calc R U . . .
H20C H 0.548397 0.646573 0.170546 0.107 Uiso 1 1 calc R U . . .
C21 C 0.8821(3) 0.66344(9) 0.2898(3) 0.0586(8) Uani 1 1 d . . . . .
H21A H 0.948317 0.655886 0.364328 0.088 Uiso 1 1 calc R U . . .
H21B H 0.880358 0.694850 0.279900 0.088 Uiso 1 1 calc R U . . .
H21C H 0.906890 0.649638 0.229944 0.088 Uiso 1 1 calc R U . . .
C17 C 0.7853(2) 0.56797(7) 0.25270(19) 0.0369(5) Uani 1 1 d . . . . .
H17 H 0.812085 0.570606 0.188567 0.044 Uiso 1 1 calc R U . . .
C18 C 0.7764(2) 0.53106(7) 0.3059(2) 0.0394(5) Uani 1 1 d . . . . .
H18 H 0.795913 0.502868 0.286334 0.047 Uiso 1 1 calc R U . . .
C22 C 0.7119(2) 0.51159(7) 0.4778(2) 0.0361(5) Uani 1 1 d . . . . .
H22 H 0.682398 0.528986 0.531697 0.043 Uiso 1 1 calc R U . . .
C24 C 0.5989(3) 0.48048(9) 0.4158(3) 0.0547(7) Uani 1 1 d . . . . .
H24A H 0.517167 0.496864 0.374726 0.082 Uiso 1 1 calc R U . . .
H24B H 0.581600 0.461312 0.471084 0.082 Uiso 1 1 calc R U . . .
H24C H 0.625062 0.463228 0.361762 0.082 Uiso 1 1 calc R U . . .
C23 C 0.8423(3) 0.48919(9) 0.5459(3) 0.0567(7) Uani 1 1 d . . . . .
H23A H 0.871615 0.471053 0.495194 0.085 Uiso 1 1 calc R U . . .
H23B H 0.828257 0.471150 0.604660 0.085 Uiso 1 1 calc R U . . .
H23C H 0.911487 0.510888 0.581822 0.085 Uiso 1 1 calc R U . . .
C6S C 0.6928(5) 0.41559(14) 1.1806(4) 0.0359(9) Uani 0.720(5) 1 d D . P A 1
H6S H 0.723983 0.402534 1.253654 0.043 Uiso 0.720(5) 1 calc R U P A 1
C2S C 0.5120(10) 0.4382(5) 1.0148(10) 0.060(3) Uani 0.720(5) 1 d D . P A 1
H2S H 0.418630 0.440764 0.971899 0.072 Uiso 0.720(5) 1 calc R U P A 1
C1S C 0.5547(3) 0.41824(10) 1.1206(3) 0.0375(8) Uani 0.720(5) 1 d D . P A 1
C5S C 0.7837(4) 0.43118(13) 1.1372(4) 0.0538(11) Uani 0.720(5) 1 d D . P A 1
H5S H 0.877019 0.429088 1.180790 0.065 Uiso 0.720(5) 1 calc R U P A 1
C4S C 0.7438(6) 0.44969(16) 1.0328(6) 0.0699(16) Uani 0.720(5) 1 d . . P A 1
H4S H 0.808188 0.459214 1.001498 0.084 Uiso 0.720(5) 1 calc R U P A 1
C3S C 0.6059(8) 0.45448(16) 0.9721(4) 0.0798(19) Uani 0.720(5) 1 d D . P A 1
H3S H 0.576423 0.468996 0.900894 0.096 Uiso 0.720(5) 1 calc R U P A 1
C7S C 0.4580(5) 0.39884(19) 1.1682(5) 0.0666(14) Uani 0.720(5) 1 d D . P A 1
H7SA H 0.498287 0.373166 1.212781 0.100 Uiso 0.720(5) 1 calc R U P A 1
H7SB H 0.375450 0.390641 1.105812 0.100 Uiso 0.720(5) 1 calc R U P A 1
H7SC H 0.436387 0.419950 1.217153 0.100 Uiso 0.720(5) 1 calc R U P A 1
C10S C 0.4484(9) 0.4141(3) 1.0890(8) 0.044(2) Uani 0.280(5) 1 d D . P A 2
H10S H 0.353810 0.409890 1.063080 0.053 Uiso 0.280(5) 1 calc R U P A 2
C9S C 0.506(2) 0.4343(12) 1.022(3) 0.045(6) Uani 0.280(5) 1 d D . P A 2
H9S H 0.449229 0.447405 0.953205 0.054 Uiso 0.280(5) 1 calc R U P A 2
C8S C 0.6445(9) 0.4365(3) 1.0480(7) 0.038(2) Uani 0.280(5) 1 d D . P A 2
C14S C 0.6981(16) 0.4560(6) 0.9661(12) 0.073(4) Uani 0.280(5) 1 d D . P A 2
H14A H 0.734362 0.433296 0.930942 0.109 Uiso 0.280(5) 1 calc R U P A 2
H14B H 0.769763 0.476443 1.005748 0.109 Uiso 0.280(5) 1 calc R U P A 2
H14C H 0.625736 0.471272 0.907090 0.109 Uiso 0.280(5) 1 calc R U P A 2
C13S C 0.7230(11) 0.4218(4) 1.1548(10) 0.031(2) Uani 0.280(5) 1 d D . P A 2
H13S H 0.818211 0.423599 1.178434 0.037 Uiso 0.280(5) 1 calc R U P A 2
C12S C 0.6645(10) 0.4044(3) 1.2280(8) 0.038(2) Uani 0.280(5) 1 d D . P A 2
H12S H 0.719952 0.395434 1.302129 0.045 Uiso 0.280(5) 1 calc R U P A 2
C11S C 0.5280(10) 0.4000(3) 1.1943(8) 0.037(2) Uani 0.280(5) 1 d . . P A 2
H11S H 0.488676 0.387273 1.243752 0.045 Uiso 0.280(5) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 Cl1 2.3783(6) . ?
Ti1 Cl2 2.3883(6) . ?
Ti1 O1 1.9098(14) . ?
Ti1 O2 1.9277(14) . ?
Ti1 N1 2.0664(15) . ?
Ti1 N4 2.0666(14) . ?
O1 C11 1.336(2) . ?
O2 C26 1.333(2) . ?
N1 C10 1.401(2) . ?
N1 C1 1.372(2) . ?
N2 C1 1.342(2) . ?
N2 C4 1.478(3) . ?
N2 C2 1.384(3) . ?
N3 C1 1.345(2) . ?
N3 C3 1.387(2) . ?
N3 C7 1.474(3) . ?
N4 C25 1.404(2) . ?
N4 C16 1.369(2) . ?
N5 C16 1.343(2) . ?
N5 C19 1.477(3) . ?
N5 C17 1.382(3) . ?
N6 C16 1.345(2) . ?
N6 C18 1.384(3) . ?
N6 C22 1.480(3) . ?
C11 C10 1.410(2) . ?
C11 C12 1.387(3) . ?
C10 C15 1.394(3) . ?
C4 H4 1.0000 . ?
C4 C6 1.512(4) . ?
C4 C5 1.523(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C2 H2 0.9500 . ?
C2 C3 1.339(3) . ?
C3 H3 0.9500 . ?
C7 H7 1.0000 . ?
C7 C9 1.521(3) . ?
C7 C8 1.511(4) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C15 H15 0.9500 . ?
C15 C14 1.398(3) . ?
C14 H14 0.9500 . ?
C14 C13 1.385(3) . ?
C13 H13 0.9500 . ?
C13 C12 1.392(3) . ?
C12 H12 0.9500 . ?
C26 C25 1.407(3) . ?
C26 C27 1.391(3) . ?
C25 C30 1.385(3) . ?
C30 H30 0.9500 . ?
C30 C29 1.408(3) . ?
C29 H29 0.9500 . ?
C29 C28 1.365(4) . ?
C28 H28 0.9500 . ?
C28 C27 1.385(4) . ?
C27 H27 0.9500 . ?
C19 H19 1.0000 . ?
C19 C20 1.517(3) . ?
C19 C21 1.509(3) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C17 H17 0.9500 . ?
C17 C18 1.345(3) . ?
C18 H18 0.9500 . ?
C22 H22 1.0000 . ?
C22 C24 1.521(3) . ?
C22 C23 1.515(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C6S H6S 0.9500 . ?
C6S C1S 1.394(5) . ?
C6S C5S 1.357(6) . ?
C2S H2S 0.9500 . ?
C2S C1S 1.390(12) . ?
C2S C3S 1.386(10) . ?
C1S C7S 1.488(6) . ?
C5S H5S 0.9500 . ?
C5S C4S 1.356(9) . ?
C4S H4S 0.9500 . ?
C4S C3S 1.400(9) . ?
C3S H3S 0.9500 . ?
C7S H7SA 0.9800 . ?
C7S H7SB 0.9800 . ?
C7S H7SC 0.9800 . ?
C10S H10S 0.9500 . ?
C10S C9S 1.364(18) . ?
C10S C11S 1.365(13) . ?
C9S H9S 0.9500 . ?
C9S C8S 1.389(18) . ?
C8S C14S 1.473(13) . ?
C8S C13S 1.383(15) . ?
C14S H14A 0.9800 . ?
C14S H14B 0.9800 . ?
C14S H14C 0.9800 . ?
C13S H13S 0.9500 . ?
C13S C12S 1.391(11) . ?
C12S H12S 0.9500 . ?
C12S C11S 1.368(15) . ?
C11S H11S 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Ti1 Cl2 87.84(2) . . ?
O1 Ti1 Cl1 89.85(5) . . ?
O1 Ti1 Cl2 161.19(4) . . ?
O1 Ti1 O2 94.38(6) . . ?
O1 Ti1 N1 77.43(6) . . ?
O1 Ti1 N4 97.78(6) . . ?
O2 Ti1 Cl1 162.91(5) . . ?
O2 Ti1 Cl2 93.27(5) . . ?
O2 Ti1 N1 92.49(6) . . ?
O2 Ti1 N4 76.75(6) . . ?
N1 Ti1 Cl1 104.59(5) . . ?
N1 Ti1 Cl2 85.10(4) . . ?
N1 Ti1 N4 167.97(6) . . ?
N4 Ti1 Cl1 86.28(4) . . ?
N4 Ti1 Cl2 100.69(5) . . ?
C11 O1 Ti1 121.21(11) . . ?
C26 O2 Ti1 121.41(12) . . ?
C10 N1 Ti1 114.84(11) . . ?
C1 N1 Ti1 127.91(12) . . ?
C1 N1 C10 117.24(15) . . ?
C1 N2 C4 125.08(16) . . ?
C1 N2 C2 108.79(17) . . ?
C2 N2 C4 126.14(17) . . ?
C1 N3 C3 108.52(17) . . ?
C1 N3 C7 124.87(16) . . ?
C3 N3 C7 126.50(17) . . ?
C25 N4 Ti1 115.51(11) . . ?
C16 N4 Ti1 127.56(11) . . ?
C16 N4 C25 116.86(15) . . ?
C16 N5 C19 123.93(16) . . ?
C16 N5 C17 108.53(17) . . ?
C17 N5 C19 127.52(17) . . ?
C16 N6 C18 108.33(17) . . ?
C16 N6 C22 124.77(16) . . ?
C18 N6 C22 126.88(17) . . ?
O1 C11 C10 114.99(16) . . ?
O1 C11 C12 124.79(17) . . ?
C12 C11 C10 120.22(17) . . ?
N1 C10 C11 111.51(15) . . ?
C15 C10 N1 128.38(16) . . ?
C15 C10 C11 120.11(17) . . ?
N2 C1 N1 126.27(17) . . ?
N2 C1 N3 107.76(15) . . ?
N3 C1 N1 125.94(17) . . ?
N2 C4 H4 108.1 . . ?
N2 C4 C6 110.0(2) . . ?
N2 C4 C5 109.4(2) . . ?
C6 C4 H4 108.1 . . ?
C6 C4 C5 113.0(2) . . ?
C5 C4 H4 108.1 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C2 H2 126.3 . . ?
C3 C2 N2 107.41(18) . . ?
C3 C2 H2 126.3 . . ?
N3 C3 H3 126.2 . . ?
C2 C3 N3 107.50(18) . . ?
C2 C3 H3 126.2 . . ?
N3 C7 H7 107.8 . . ?
N3 C7 C9 110.3(2) . . ?
N3 C7 C8 109.8(2) . . ?
C9 C7 H7 107.8 . . ?
C8 C7 H7 107.8 . . ?
C8 C7 C9 113.1(2) . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 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 . . ?
C10 C15 H15 120.6 . . ?
C10 C15 C14 118.87(19) . . ?
C14 C15 H15 120.6 . . ?
C15 C14 H14 119.6 . . ?
C13 C14 C15 120.88(19) . . ?
C13 C14 H14 119.6 . . ?
C14 C13 H13 119.8 . . ?
C14 C13 C12 120.44(19) . . ?
C12 C13 H13 119.8 . . ?
C11 C12 C13 119.48(19) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
O2 C26 C25 115.02(16) . . ?
O2 C26 C27 125.02(19) . . ?
C27 C26 C25 119.93(19) . . ?
N4 C25 C26 111.25(16) . . ?
C30 C25 N4 128.29(19) . . ?
C30 C25 C26 120.45(18) . . ?
C25 C30 H30 120.8 . . ?
C25 C30 C29 118.4(2) . . ?
C29 C30 H30 120.8 . . ?
C30 C29 H29 119.5 . . ?
C28 C29 C30 120.9(2) . . ?
C28 C29 H29 119.5 . . ?
C29 C28 H28 119.5 . . ?
C29 C28 C27 121.1(2) . . ?
C27 C28 H28 119.5 . . ?
C26 C27 H27 120.4 . . ?
C28 C27 C26 119.2(2) . . ?
C28 C27 H27 120.4 . . ?
N5 C16 N4 125.74(17) . . ?
N5 C16 N6 108.13(16) . . ?
N6 C16 N4 126.12(17) . . ?
N5 C19 H19 107.3 . . ?
N5 C19 C20 110.44(19) . . ?
N5 C19 C21 110.38(19) . . ?
C20 C19 H19 107.3 . . ?
C21 C19 H19 107.3 . . ?
C21 C19 C20 113.9(2) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N5 C17 H17 126.3 . . ?
C18 C17 N5 107.47(18) . . ?
C18 C17 H17 126.3 . . ?
N6 C18 H18 126.2 . . ?
C17 C18 N6 107.53(18) . . ?
C17 C18 H18 126.2 . . ?
N6 C22 H22 107.9 . . ?
N6 C22 C24 109.2(2) . . ?
N6 C22 C23 110.23(19) . . ?
C24 C22 H22 107.9 . . ?
C23 C22 H22 107.9 . . ?
C23 C22 C24 113.4(2) . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C1S C6S H6S 119.1 . . ?
C5S C6S H6S 119.1 . . ?
C5S C6S C1S 121.7(4) . . ?
C1S C2S H2S 120.1 . . ?
C3S C2S H2S 120.1 . . ?
C3S C2S C1S 119.9(8) . . ?
C6S C1S C7S 120.3(4) . . ?
C2S C1S C6S 117.9(5) . . ?
C2S C1S C7S 121.8(5) . . ?
C6S C5S H5S 119.4 . . ?
C4S C5S C6S 121.2(4) . . ?
C4S C5S H5S 119.4 . . ?
C5S C4S H4S 120.6 . . ?
C5S C4S C3S 118.7(5) . . ?
C3S C4S H4S 120.6 . . ?
C2S C3S C4S 120.6(7) . . ?
C2S C3S H3S 119.7 . . ?
C4S C3S H3S 119.7 . . ?
C1S C7S H7SA 109.5 . . ?
C1S C7S H7SB 109.5 . . ?
C1S C7S H7SC 109.5 . . ?
H7SA C7S H7SB 109.5 . . ?
H7SA C7S H7SC 109.5 . . ?
H7SB C7S H7SC 109.5 . . ?
C9S C10S H10S 120.4 . . ?
C9S C10S C11S 119.3(14) . . ?
C11S C10S H10S 120.4 . . ?
C10S C9S H9S 118.4 . . ?
C10S C9S C8S 123(2) . . ?
C8S C9S H9S 118.4 . . ?
C9S C8S C14S 119.5(13) . . ?
C13S C8S C9S 116.0(13) . . ?
C13S C8S C14S 124.4(10) . . ?
C8S C14S H14A 109.5 . . ?
C8S C14S H14B 109.5 . . ?
C8S C14S H14C 109.5 . . ?
H14A C14S H14B 109.5 . . ?
H14A C14S H14C 109.5 . . ?
H14B C14S H14C 109.5 . . ?
C8S C13S H13S 119.6 . . ?
C8S C13S C12S 120.9(9) . . ?
C12S C13S H13S 119.6 . . ?
C13S C12S H12S 119.7 . . ?
C11S C12S C13S 120.5(9) . . ?
C11S C12S H12S 119.7 . . ?
C10S C11S C12S 119.6(10) . . ?
C10S C11S H11S 120.2 . . ?
C12S C11S H11S 120.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ti1 O1 C11 C10 1.5(2) . . . . ?
Ti1 O1 C11 C12 -179.32(15) . . . . ?
Ti1 O2 C26 C25 -2.7(2) . . . . ?
Ti1 O2 C26 C27 175.58(14) . . . . ?
Ti1 N1 C10 C11 0.94(19) . . . . ?
Ti1 N1 C10 C15 -179.12(16) . . . . ?
Ti1 N1 C1 N2 80.6(2) . . . . ?
Ti1 N1 C1 N3 -97.4(2) . . . . ?
Ti1 N4 C25 C26 0.25(18) . . . . ?
Ti1 N4 C25 C30 -179.84(17) . . . . ?
Ti1 N4 C16 N5 -91.7(2) . . . . ?
Ti1 N4 C16 N6 86.7(2) . . . . ?
O1 C11 C10 N1 -1.5(2) . . . . ?
O1 C11 C10 C15 178.57(17) . . . . ?
O1 C11 C12 C13 -178.99(18) . . . . ?
O2 C26 C25 N4 1.4(2) . . . . ?
O2 C26 C25 C30 -178.51(17) . . . . ?
O2 C26 C27 C28 -179.91(19) . . . . ?
N1 C10 C15 C14 -179.12(19) . . . . ?
N2 C2 C3 N3 0.5(3) . . . . ?
N4 C25 C30 C29 178.0(2) . . . . ?
N5 C17 C18 N6 0.1(3) . . . . ?
C11 C10 C15 C14 0.8(3) . . . . ?
C10 N1 C1 N2 -97.8(2) . . . . ?
C10 N1 C1 N3 84.1(2) . . . . ?
C10 C11 C12 C13 0.2(3) . . . . ?
C10 C15 C14 C13 -0.5(3) . . . . ?
C1 N1 C10 C11 179.61(16) . . . . ?
C1 N1 C10 C15 -0.5(3) . . . . ?
C1 N2 C4 C6 -120.3(2) . . . . ?
C1 N2 C4 C5 115.0(2) . . . . ?
C1 N2 C2 C3 -0.9(3) . . . . ?
C1 N3 C3 C2 0.1(3) . . . . ?
C1 N3 C7 C9 -114.4(2) . . . . ?
C1 N3 C7 C8 120.2(2) . . . . ?
C4 N2 C1 N1 2.6(3) . . . . ?
C4 N2 C1 N3 -179.07(19) . . . . ?
C4 N2 C2 C3 179.1(2) . . . . ?
C2 N2 C1 N1 -177.39(18) . . . . ?
C2 N2 C1 N3 1.0(2) . . . . ?
C2 N2 C4 C6 59.6(3) . . . . ?
C2 N2 C4 C5 -65.0(3) . . . . ?
C3 N3 C1 N1 177.72(19) . . . . ?
C3 N3 C1 N2 -0.7(2) . . . . ?
C3 N3 C7 C9 69.7(3) . . . . ?
C3 N3 C7 C8 -55.6(3) . . . . ?
C7 N3 C1 N1 1.2(3) . . . . ?
C7 N3 C1 N2 -177.14(19) . . . . ?
C7 N3 C3 C2 176.5(2) . . . . ?
C15 C14 C13 C12 0.0(3) . . . . ?
C14 C13 C12 C11 0.2(3) . . . . ?
C12 C11 C10 N1 179.26(17) . . . . ?
C12 C11 C10 C15 -0.7(3) . . . . ?
C26 C25 C30 C29 -2.1(3) . . . . ?
C25 N4 C16 N5 91.4(2) . . . . ?
C25 N4 C16 N6 -90.2(2) . . . . ?
C25 C26 C27 C28 -1.7(3) . . . . ?
C25 C30 C29 C28 -0.2(4) . . . . ?
C30 C29 C28 C27 1.6(4) . . . . ?
C29 C28 C27 C26 -0.6(3) . . . . ?
C27 C26 C25 N4 -176.95(16) . . . . ?
C27 C26 C25 C30 3.1(3) . . . . ?
C16 N4 C25 C26 177.53(15) . . . . ?
C16 N4 C25 C30 -2.6(3) . . . . ?
C16 N5 C19 C20 -113.5(2) . . . . ?
C16 N5 C19 C21 119.7(2) . . . . ?
C16 N5 C17 C18 0.2(2) . . . . ?
C16 N6 C18 C17 -0.3(3) . . . . ?
C16 N6 C22 C24 118.0(2) . . . . ?
C16 N6 C22 C23 -116.7(2) . . . . ?
C19 N5 C16 N4 -0.3(3) . . . . ?
C19 N5 C16 N6 -179.00(17) . . . . ?
C19 N5 C17 C18 178.7(2) . . . . ?
C17 N5 C16 N4 178.26(18) . . . . ?
C17 N5 C16 N6 -0.4(2) . . . . ?
C17 N5 C19 C20 68.2(3) . . . . ?
C17 N5 C19 C21 -58.6(3) . . . . ?
C18 N6 C16 N4 -178.21(18) . . . . ?
C18 N6 C16 N5 0.5(2) . . . . ?
C18 N6 C22 C24 -63.7(3) . . . . ?
C18 N6 C22 C23 61.6(3) . . . . ?
C22 N6 C16 N4 0.4(3) . . . . ?
C22 N6 C16 N5 179.03(18) . . . . ?
C22 N6 C18 C17 -178.9(2) . . . . ?
C6S C5S C4S C3S 3.2(6) . . . . ?
C1S C6S C5S C4S -0.7(6) . . . . ?
C1S C2S C3S C4S 2.1(17) . . . . ?
C5S C6S C1S C2S -1.2(10) . . . . ?
C5S C6S C1S C7S 176.9(4) . . . . ?
C5S C4S C3S C2S -3.9(11) . . . . ?
C3S C2S C1S C6S 0.4(17) . . . . ?
C3S C2S C1S C7S -177.6(9) . . . . ?
C10S C9S C8S C14S 175(2) . . . . ?
C10S C9S C8S C13S -8(4) . . . . ?
C9S C10S C11S C12S -3(2) . . . . ?
C9S C8S C13S C12S 2(2) . . . . ?
C8S C13S C12S C11S 2.3(16) . . . . ?
C14S C8S C13S C12S 178.9(12) . . . . ?
C13S C12S C11S C10S -2.0(14) . . . . ?
C11S C10S C9S C8S 9(4) . . . . ?

_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_vfr29_a
_database_code_depnum_ccdc_archive 'CCDC 2345356'
loop_
_audit_author_name
_audit_author_address
'Gino G. Lavoie'
;York University
Canada
;
_audit_update_record             
;
2024-04-02 deposited with the CCDC.	2024-08-06 downloaded from the CCDC.
;
_audit_creation_date             2023-02-25
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H46 N6 O4 Ti'
_chemical_formula_sum            'C30 H46 N6 O4 Ti'
_chemical_formula_weight         602.63
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y, z'

_cell_length_a                   14.5172(8)
_cell_length_b                   11.5840(6)
_cell_length_c                   19.1268(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3216.5(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8914
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      2.49
_shelx_estimated_absorpt_T_max   0.970
_shelx_estimated_absorpt_T_min   0.941
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6433
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1604 before and 0.0680 after correction.
The Ratio of minimum to maximum transmission is 0.8628.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0835
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39189
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.553
_diffrn_reflns_theta_min         2.249
_diffrn_ambient_temperature      173.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_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_Friedel_coverage         0.928
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                5138
_reflns_number_total             7358
_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 V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-1997  (Sheldrick, 2008)'
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 
;
 Flack x determined using 1998 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         7358
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0481
_refine_ls_restrained_S_all      1.053
_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)+(0.0556P)²+0.8133P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1296
_refine_special_details          ?
_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 Ternary CH refined with riding coordinates:
 C25(H25), C28(H28)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B)
2.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C11(H11), C10(H10), C9(H9), C24(H24), C23(H23), C22(H22), C21(H21)
2.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C6(H6A,H6B,H6C), C5(H5A,H5B,H5C),
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 0.54278(5) 0.26028(6) 0.45015(5) 0.03171(19) Uani 1 1 d . . . . .
O3 O 0.4342(2) 0.2615(3) 0.40371(17) 0.0382(8) Uani 1 1 d . . . . .
O1 O 0.4981(2) 0.1438(3) 0.51456(17) 0.0372(7) Uani 1 1 d . . . . .
O4 O 0.6080(2) 0.1799(3) 0.38283(17) 0.0423(8) Uani 1 1 d . . . . .
O2 O 0.5914(2) 0.4075(3) 0.41941(18) 0.0378(7) Uani 1 1 d . . . . .
N1 N 0.6683(2) 0.2162(3) 0.5167(2) 0.0345(9) Uani 1 1 d . . . . .
N2 N 0.7846(3) 0.0870(3) 0.4781(2) 0.0417(10) Uani 1 1 d . . . . .
N3 N 0.8008(2) 0.2813(3) 0.4594(3) 0.0399(10) Uani 1 1 d . . . . .
N4 N 0.5032(3) 0.3872(3) 0.5358(2) 0.0348(9) Uani 1 1 d . . . . .
N5 N 0.3937(3) 0.3094(4) 0.6104(2) 0.0413(10) Uani 1 1 d . . . . .
C25 C 0.3599(4) 0.3083(5) 0.3675(3) 0.0498(14) Uani 1 1 d . . . . .
H25 H 0.311177 0.328319 0.402475 0.060 Uiso 1 1 calc R U . . .
C27 C 0.3868(6) 0.4159(6) 0.3311(4) 0.085(2) Uani 1 1 d . . . . .
H27A H 0.407777 0.472801 0.365490 0.128 Uiso 1 1 calc R U . . .
H27B H 0.333611 0.446707 0.305639 0.128 Uiso 1 1 calc R U . . .
H27C H 0.436678 0.399294 0.298129 0.128 Uiso 1 1 calc R U . . .
C26 C 0.3202(5) 0.2206(6) 0.3182(4) 0.072(2) Uani 1 1 d . . . . .
H26A H 0.358651 0.216001 0.276207 0.108 Uiso 1 1 calc R U . . .
H26B H 0.257554 0.243486 0.305114 0.108 Uiso 1 1 calc R U . . .
H26C H 0.318503 0.144971 0.341180 0.108 Uiso 1 1 calc R U . . .
C7 C 0.6419(3) 0.1397(4) 0.5711(3) 0.0377(11) Uani 1 1 d . . . . .
C12 C 0.6969(4) 0.1014(5) 0.6251(3) 0.0488(13) Uani 1 1 d . . . . .
H12 H 0.758529 0.128406 0.629018 0.059 Uiso 1 1 calc R U . . .
C11 C 0.6625(4) 0.0233(5) 0.6742(3) 0.0568(15) Uani 1 1 d . . . . .
H11 H 0.701026 -0.003839 0.710799 0.068 Uiso 1 1 calc R U . . .
C10 C 0.5724(4) -0.0145(5) 0.6695(3) 0.0546(14) Uani 1 1 d . . . . .
H10 H 0.549322 -0.068057 0.702738 0.066 Uiso 1 1 calc R U . . .
C9 C 0.5157(4) 0.0252(4) 0.6165(3) 0.0447(12) Uani 1 1 d . . . . .
H9 H 0.453832 -0.001181 0.613456 0.054 Uiso 1 1 calc R U . . .
C8 C 0.5490(3) 0.1034(4) 0.5679(2) 0.0348(10) Uani 1 1 d . . . . .
C1 C 0.7493(3) 0.1945(4) 0.4853(3) 0.0357(10) Uani 1 1 d . . . . .
C2 C 0.8796(3) 0.0765(4) 0.4524(3) 0.0507(13) Uani 1 1 d . . . . .
H2A H 0.894830 -0.005671 0.444057 0.061 Uiso 1 1 calc R U . . .
H2B H 0.923174 0.107535 0.487520 0.061 Uiso 1 1 calc R U . . .
C3 C 0.8869(4) 0.1434(5) 0.3858(3) 0.0551(15) Uani 1 1 d . . . . .
H3A H 0.949717 0.135949 0.366186 0.066 Uiso 1 1 calc R U . . .
H3B H 0.842425 0.113217 0.351045 0.066 Uiso 1 1 calc R U . . .
C4 C 0.8664(3) 0.2668(4) 0.4015(3) 0.0462(12) Uani 1 1 d . . . . .
H4A H 0.924551 0.306885 0.413368 0.055 Uiso 1 1 calc R U . . .
H4B H 0.840822 0.303856 0.359030 0.055 Uiso 1 1 calc R U . . .
C6 C 0.7874(3) 0.3999(4) 0.4822(3) 0.0486(13) Uani 1 1 d . . . . .
H6A H 0.759962 0.444841 0.444104 0.073 Uiso 1 1 calc R U . . .
H6B H 0.846930 0.433570 0.495064 0.073 Uiso 1 1 calc R U . . .
H6C H 0.746188 0.401157 0.522790 0.073 Uiso 1 1 calc R U . . .
C5 C 0.7249(4) -0.0143(4) 0.4741(3) 0.0497(14) Uani 1 1 d . . . . .
H5A H 0.720074 -0.049887 0.520446 0.075 Uiso 1 1 calc R U . . .
H5B H 0.751157 -0.070105 0.441111 0.075 Uiso 1 1 calc R U . . .
H5C H 0.663599 0.009019 0.458073 0.075 Uiso 1 1 calc R U . . .
C28 C 0.5938(4) 0.1652(6) 0.3108(3) 0.0590(16) Uani 1 1 d . . . . .
H28 H 0.526669 0.173983 0.300454 0.071 Uiso 1 1 calc R U . . .
C29 C 0.6465(6) 0.2551(7) 0.2708(4) 0.091(3) Uani 1 1 d . . . . .
H29A H 0.631685 0.331850 0.289213 0.136 Uiso 1 1 calc R U . . .
H29B H 0.629522 0.251354 0.221233 0.136 Uiso 1 1 calc R U . . .
H29C H 0.712748 0.240912 0.275734 0.136 Uiso 1 1 calc R U . . .
C30 C 0.6238(5) 0.0424(7) 0.2919(4) 0.074(2) Uani 1 1 d . . . . .
H30A H 0.686934 0.029426 0.308144 0.111 Uiso 1 1 calc R U . . .
H30B H 0.621100 0.032391 0.241058 0.111 Uiso 1 1 calc R U . . .
H30C H 0.582401 -0.013215 0.314371 0.111 Uiso 1 1 calc R U . . .
C20 C 0.5808(3) 0.5051(4) 0.4550(3) 0.0373(10) Uani 1 1 d . . . . .
C19 C 0.5373(3) 0.4990(4) 0.5205(3) 0.0380(11) Uani 1 1 d . . . . .
C24 C 0.5268(4) 0.6001(5) 0.5599(3) 0.0524(14) Uani 1 1 d . . . . .
H24 H 0.497751 0.597453 0.604311 0.063 Uiso 1 1 calc R U . . .
C23 C 0.5595(4) 0.7049(4) 0.5334(4) 0.0585(18) Uani 1 1 d . . . . .
H23 H 0.552821 0.773331 0.560279 0.070 Uiso 1 1 calc R U . . .
C22 C 0.6013(4) 0.7102(5) 0.4687(4) 0.0602(19) Uani 1 1 d . . . . .
H22 H 0.623005 0.781931 0.451162 0.072 Uiso 1 1 calc R U . . .
C21 C 0.6114(3) 0.6121(4) 0.4299(3) 0.0496(15) Uani 1 1 d . . . . .
H21 H 0.639512 0.616376 0.385091 0.060 Uiso 1 1 calc R U . . .
C13 C 0.4752(3) 0.3631(4) 0.6007(3) 0.0380(11) Uani 1 1 d . . . . .
N6 N 0.5247(3) 0.3891(4) 0.6584(2) 0.0485(11) Uani 1 1 d . . . . .
C17 C 0.6240(4) 0.4090(5) 0.6546(3) 0.0545(15) Uani 1 1 d . . . . .
H17A H 0.646361 0.387942 0.607937 0.082 Uiso 1 1 calc R U . . .
H17B H 0.655149 0.361622 0.689803 0.082 Uiso 1 1 calc R U . . .
H17C H 0.636942 0.490710 0.663395 0.082 Uiso 1 1 calc R U . . .
C14 C 0.4827(5) 0.3740(6) 0.7271(3) 0.0632(17) Uani 1 1 d . . . . .
H14A H 0.435216 0.433918 0.734850 0.076 Uiso 1 1 calc R U . . .
H14B H 0.530159 0.381676 0.764003 0.076 Uiso 1 1 calc R U . . .
C15 C 0.4400(5) 0.2570(5) 0.7304(3) 0.0619(17) Uani 1 1 d . . . . .
H15A H 0.411974 0.244465 0.776981 0.074 Uiso 1 1 calc R U . . .
H15B H 0.487519 0.196963 0.722851 0.074 Uiso 1 1 calc R U . . .
C16 C 0.3675(4) 0.2489(5) 0.6747(3) 0.0565(15) Uani 1 1 d . . . . .
H16A H 0.356143 0.166561 0.663821 0.068 Uiso 1 1 calc R U . . .
H16B H 0.309360 0.282153 0.692752 0.068 Uiso 1 1 calc R U . . .
C18 C 0.3269(4) 0.3007(5) 0.5537(3) 0.0468(13) Uani 1 1 d . . . . .
H18A H 0.340170 0.359658 0.518411 0.070 Uiso 1 1 calc R U . . .
H18B H 0.264700 0.312594 0.572326 0.070 Uiso 1 1 calc R U . . .
H18C H 0.330878 0.223947 0.532385 0.070 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O3 1.809(3) . ?
Ti1 O1 1.939(3) . ?
Ti1 O4 1.850(3) . ?
Ti1 O2 1.937(3) . ?
Ti1 N1 2.281(4) . ?
Ti1 N4 2.275(4) . ?
O3 C25 1.392(6) . ?
O1 C8 1.344(6) . ?
O4 C28 1.403(7) . ?
O2 C20 1.329(6) . ?
N1 C7 1.419(6) . ?
N1 C1 1.343(6) . ?
N2 C1 1.354(6) . ?
N2 C2 1.469(6) . ?
N2 C5 1.460(6) . ?
N3 C1 1.348(6) . ?
N3 C4 1.471(7) . ?
N3 C6 1.454(6) . ?
N4 C19 1.417(6) . ?
N4 C13 1.335(6) . ?
N5 C13 1.350(6) . ?
N5 C16 1.466(7) . ?
N5 C18 1.458(6) . ?
C25 H25 1.0000 . ?
C25 C27 1.480(9) . ?
C25 C26 1.501(9) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C7 C12 1.380(7) . ?
C7 C8 1.414(7) . ?
C12 H12 0.9500 . ?
C12 C11 1.395(8) . ?
C11 H11 0.9500 . ?
C11 C10 1.382(8) . ?
C10 H10 0.9500 . ?
C10 C9 1.385(8) . ?
C9 H9 0.9500 . ?
C9 C8 1.384(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.496(8) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.491(7) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C28 H28 1.0000 . ?
C28 C29 1.503(10) . ?
C28 C30 1.530(9) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C20 C19 1.404(7) . ?
C20 C21 1.402(6) . ?
C19 C24 1.400(7) . ?
C24 H24 0.9500 . ?
C24 C23 1.398(8) . ?
C23 H23 0.9500 . ?
C23 C22 1.380(9) . ?
C22 H22 0.9500 . ?
C22 C21 1.365(8) . ?
C21 H21 0.9500 . ?
C13 N6 1.350(6) . ?
N6 C17 1.461(7) . ?
N6 C14 1.460(7) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.492(9) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.500(8) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 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 O1 91.48(14) . . ?
O3 Ti1 O4 96.19(15) . . ?
O3 Ti1 O2 99.31(15) . . ?
O3 Ti1 N1 166.37(15) . . ?
O3 Ti1 N4 97.40(15) . . ?
O1 Ti1 N1 75.94(14) . . ?
O1 Ti1 N4 84.69(14) . . ?
O4 Ti1 O1 105.26(15) . . ?
O4 Ti1 O2 92.61(15) . . ?
O4 Ti1 N1 82.35(15) . . ?
O4 Ti1 N4 162.92(14) . . ?
O2 Ti1 O1 158.03(15) . . ?
O2 Ti1 N1 94.30(13) . . ?
O2 Ti1 N4 75.02(14) . . ?
N4 Ti1 N1 86.81(14) . . ?
C25 O3 Ti1 157.3(3) . . ?
C8 O1 Ti1 122.8(3) . . ?
C28 O4 Ti1 132.0(3) . . ?
C20 O2 Ti1 123.4(3) . . ?
C7 N1 Ti1 109.4(3) . . ?
C1 N1 Ti1 119.4(3) . . ?
C1 N1 C7 116.5(4) . . ?
C1 N2 C2 117.8(4) . . ?
C1 N2 C5 121.3(4) . . ?
C5 N2 C2 118.2(4) . . ?
C1 N3 C4 123.4(4) . . ?
C1 N3 C6 121.4(4) . . ?
C6 N3 C4 114.9(4) . . ?
C19 N4 Ti1 110.7(3) . . ?
C13 N4 Ti1 127.7(3) . . ?
C13 N4 C19 119.3(4) . . ?
C13 N5 C16 124.3(4) . . ?
C13 N5 C18 120.8(4) . . ?
C18 N5 C16 114.7(4) . . ?
O3 C25 H25 107.8 . . ?
O3 C25 C27 110.9(5) . . ?
O3 C25 C26 110.2(5) . . ?
C27 C25 H25 107.8 . . ?
C27 C25 C26 112.1(6) . . ?
C26 C25 H25 107.8 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C12 C7 N1 126.4(5) . . ?
C12 C7 C8 119.2(5) . . ?
C8 C7 N1 114.4(4) . . ?
C7 C12 H12 119.9 . . ?
C7 C12 C11 120.3(5) . . ?
C11 C12 H12 119.9 . . ?
C12 C11 H11 120.0 . . ?
C10 C11 C12 120.0(5) . . ?
C10 C11 H11 120.0 . . ?
C11 C10 H10 119.8 . . ?
C11 C10 C9 120.4(5) . . ?
C9 C10 H10 119.8 . . ?
C10 C9 H9 120.0 . . ?
C8 C9 C10 120.0(5) . . ?
C8 C9 H9 120.0 . . ?
O1 C8 C7 116.9(4) . . ?
O1 C8 C9 123.0(4) . . ?
C9 C8 C7 120.0(5) . . ?
N1 C1 N2 123.3(4) . . ?
N1 C1 N3 120.6(4) . . ?
N3 C1 N2 116.0(4) . . ?
N2 C2 H2A 110.1 . . ?
N2 C2 H2B 110.1 . . ?
N2 C2 C3 108.0(4) . . ?
H2A C2 H2B 108.4 . . ?
C3 C2 H2A 110.1 . . ?
C3 C2 H2B 110.1 . . ?
C2 C3 H3A 110.1 . . ?
C2 C3 H3B 110.1 . . ?
H3A C3 H3B 108.4 . . ?
C4 C3 C2 108.1(5) . . ?
C4 C3 H3A 110.1 . . ?
C4 C3 H3B 110.1 . . ?
N3 C4 C3 113.0(4) . . ?
N3 C4 H4A 109.0 . . ?
N3 C4 H4B 109.0 . . ?
C3 C4 H4A 109.0 . . ?
C3 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O4 C28 H28 109.0 . . ?
O4 C28 C29 110.0(5) . . ?
O4 C28 C30 107.6(5) . . ?
C29 C28 H28 109.0 . . ?
C29 C28 C30 112.3(6) . . ?
C30 C28 H28 109.0 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O2 C20 C19 117.8(4) . . ?
O2 C20 C21 122.6(5) . . ?
C21 C20 C19 119.6(5) . . ?
C20 C19 N4 112.8(4) . . ?
C24 C19 N4 128.0(5) . . ?
C24 C19 C20 119.1(5) . . ?
C19 C24 H24 120.2 . . ?
C23 C24 C19 119.7(6) . . ?
C23 C24 H24 120.2 . . ?
C24 C23 H23 119.6 . . ?
C22 C23 C24 120.8(6) . . ?
C22 C23 H23 119.6 . . ?
C23 C22 H22 120.1 . . ?
C21 C22 C23 119.9(5) . . ?
C21 C22 H22 120.1 . . ?
C20 C21 H21 119.5 . . ?
C22 C21 C20 121.0(6) . . ?
C22 C21 H21 119.5 . . ?
N4 C13 N5 119.5(4) . . ?
N4 C13 N6 123.4(4) . . ?
N5 C13 N6 117.2(4) . . ?
C13 N6 C17 121.3(4) . . ?
C13 N6 C14 119.2(4) . . ?
C14 N6 C17 118.4(4) . . ?
N6 C17 H17A 109.5 . . ?
N6 C17 H17B 109.5 . . ?
N6 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N6 C14 H14A 109.9 . . ?
N6 C14 H14B 109.9 . . ?
N6 C14 C15 108.7(5) . . ?
H14A C14 H14B 108.3 . . ?
C15 C14 H14A 109.9 . . ?
C15 C14 H14B 109.9 . . ?
C14 C15 H15A 110.0 . . ?
C14 C15 H15B 110.0 . . ?
C14 C15 C16 108.6(5) . . ?
H15A C15 H15B 108.4 . . ?
C16 C15 H15A 110.0 . . ?
C16 C15 H15B 110.0 . . ?
N5 C16 C15 112.6(5) . . ?
N5 C16 H16A 109.1 . . ?
N5 C16 H16B 109.1 . . ?
C15 C16 H16A 109.1 . . ?
C15 C16 H16B 109.1 . . ?
H16A C16 H16B 107.8 . . ?
N5 C18 H18A 109.5 . . ?
N5 C18 H18B 109.5 . . ?
N5 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ti1 O3 C25 C27 26.7(12) . . . . ?
Ti1 O3 C25 C26 151.5(7) . . . . ?
Ti1 O1 C8 C7 -7.0(5) . . . . ?
Ti1 O1 C8 C9 176.1(4) . . . . ?
Ti1 O4 C28 C29 93.1(6) . . . . ?
Ti1 O4 C28 C30 -144.3(4) . . . . ?
Ti1 O2 C20 C19 4.4(5) . . . . ?
Ti1 O2 C20 C21 -175.8(3) . . . . ?
Ti1 N1 C7 C12 -174.2(4) . . . . ?
Ti1 N1 C7 C8 4.4(5) . . . . ?
Ti1 N1 C1 N2 -104.5(5) . . . . ?
Ti1 N1 C1 N3 76.2(5) . . . . ?
Ti1 N4 C19 C20 4.0(4) . . . . ?
Ti1 N4 C19 C24 179.5(4) . . . . ?
Ti1 N4 C13 N5 -66.2(6) . . . . ?
Ti1 N4 C13 N6 113.3(5) . . . . ?
O3 Ti1 O4 C28 22.8(5) . . . . ?
O1 Ti1 O3 C25 141.9(9) . . . . ?
O1 Ti1 O4 C28 116.0(5) . . . . ?
O4 Ti1 O3 C25 -112.6(9) . . . . ?
O2 Ti1 O3 C25 -18.9(9) . . . . ?
O2 Ti1 O4 C28 -76.9(5) . . . . ?
O2 C20 C19 N4 -5.4(6) . . . . ?
O2 C20 C19 C24 178.7(4) . . . . ?
O2 C20 C21 C22 -178.3(4) . . . . ?
N1 Ti1 O3 C25 164.3(8) . . . . ?
N1 Ti1 O4 C28 -170.9(5) . . . . ?
N1 C7 C12 C11 -178.2(5) . . . . ?
N1 C7 C8 O1 0.7(6) . . . . ?
N1 C7 C8 C9 177.6(4) . . . . ?
N2 C2 C3 C4 61.6(6) . . . . ?
N4 Ti1 O3 C25 57.1(9) . . . . ?
N4 Ti1 O4 C28 -119.8(6) . . . . ?
N4 C19 C24 C23 -175.0(5) . . . . ?
N4 C13 N6 C17 -21.2(8) . . . . ?
N4 C13 N6 C14 171.5(5) . . . . ?
N5 C13 N6 C17 158.4(5) . . . . ?
N5 C13 N6 C14 -8.9(7) . . . . ?
C7 N1 C1 N2 30.6(7) . . . . ?
C7 N1 C1 N3 -148.7(4) . . . . ?
C7 C12 C11 C10 -1.2(9) . . . . ?
C12 C7 C8 O1 179.4(4) . . . . ?
C12 C7 C8 C9 -3.6(7) . . . . ?
C12 C11 C10 C9 -0.4(9) . . . . ?
C11 C10 C9 C8 -0.1(8) . . . . ?
C10 C9 C8 O1 178.8(5) . . . . ?
C10 C9 C8 C7 2.1(7) . . . . ?
C8 C7 C12 C11 3.2(8) . . . . ?
C1 N1 C7 C12 46.5(7) . . . . ?
C1 N1 C7 C8 -134.9(4) . . . . ?
C1 N2 C2 C3 -53.0(6) . . . . ?
C1 N3 C4 C3 -13.8(7) . . . . ?
C2 N2 C1 N1 -170.9(5) . . . . ?
C2 N2 C1 N3 8.5(7) . . . . ?
C2 C3 C4 N3 -30.9(6) . . . . ?
C4 N3 C1 N1 -153.7(5) . . . . ?
C4 N3 C1 N2 26.9(7) . . . . ?
C6 N3 C1 N1 19.3(7) . . . . ?
C6 N3 C1 N2 -160.2(5) . . . . ?
C6 N3 C4 C3 172.8(5) . . . . ?
C5 N2 C1 N1 28.0(8) . . . . ?
C5 N2 C1 N3 -152.6(5) . . . . ?
C5 N2 C2 C3 108.7(5) . . . . ?
C20 C19 C24 C23 0.2(7) . . . . ?
C19 N4 C13 N5 132.7(5) . . . . ?
C19 N4 C13 N6 -47.7(7) . . . . ?
C19 C20 C21 C22 1.4(7) . . . . ?
C19 C24 C23 C22 0.5(8) . . . . ?
C24 C23 C22 C21 -0.2(8) . . . . ?
C23 C22 C21 C20 -0.8(8) . . . . ?
C21 C20 C19 N4 174.8(4) . . . . ?
C21 C20 C19 C24 -1.1(7) . . . . ?
C13 N4 C19 C20 168.1(4) . . . . ?
C13 N4 C19 C24 -16.5(7) . . . . ?
C13 N5 C16 C15 2.4(8) . . . . ?
C13 N6 C14 C15 48.7(7) . . . . ?
N6 C14 C15 C16 -60.5(7) . . . . ?
C17 N6 C14 C15 -118.9(6) . . . . ?
C14 C15 C16 N5 36.9(7) . . . . ?
C16 N5 C13 N4 161.3(5) . . . . ?
C16 N5 C13 N6 -18.2(7) . . . . ?
C18 N5 C13 N4 -14.0(7) . . . . ?
C18 N5 C13 N6 166.4(5) . . . . ?
C18 N5 C16 C15 177.9(5) . . . . ?

_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_vfr027_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2345357'
loop_
_audit_author_name
_audit_author_address
'Gino G. Lavoie'
;York University
Canada
;
_audit_update_record             
;
2024-04-02 deposited with the CCDC.	2024-08-06 downloaded from the CCDC.
;
_audit_creation_date             2023-02-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H42 N6 O4 Zr'
_chemical_formula_sum            'C28 H42 N6 O4 Zr'
_chemical_formula_weight         617.89
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 '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                   9.6548(4)
_cell_length_b                   15.7838(6)
_cell_length_c                   19.7193(7)
_cell_angle_alpha                90
_cell_angle_beta                 90.246(2)
_cell_angle_gamma                90
_cell_volume                     3005.0(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.34
_cell_measurement_theta_min      2.34
_shelx_estimated_absorpt_T_max   0.960
_shelx_estimated_absorpt_T_min   0.854
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0775 before and 0.0690 after correction.
The Ratio of minimum to maximum transmission is 0.9303.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       shard
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1255
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            94441
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.567
_diffrn_reflns_theta_min         2.109
_diffrn_ambient_temperature      173.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4861
_reflns_number_total             6938
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-1997  (Sheldrick, 2008)'
_refine_diff_density_max         1.101
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6938
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0580
_refine_ls_restrained_S_all      1.049
_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)+(0.0122P)²+8.2958P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1126
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.9958(5)
 0.0042(5)
2. 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
3.a Ternary CH refined with riding coordinates:
 C23(H23), C26(H26)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C13(H13A,H13B), C14(H14A,H14B)
3.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C18(H18), C19(H19), C20(H20), C21(H21)
3.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C27(H27A,H27B,
 H27C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
Zr1 Zr 0.35595(4) 0.44014(2) 0.75657(2) 0.03032(10) Uani 1 1 d . . . . .
O1 O 0.2904(3) 0.56096(17) 0.73305(12) 0.0342(6) Uani 1 1 d . . . . .
O2 O 0.4123(3) 0.31983(17) 0.72799(13) 0.0370(6) Uani 1 1 d . . . . .
O3 O 0.2067(3) 0.40318(19) 0.81772(13) 0.0446(7) Uani 1 1 d . . . . .
N1 N 0.2183(3) 0.43221(19) 0.65600(14) 0.0285(7) Uani 1 1 d . . . . .
N2 N 0.1881(3) 0.28956(19) 0.62559(15) 0.0328(7) Uani 1 1 d . . . . .
N3 N 0.2630(3) 0.37487(19) 0.54491(15) 0.0335(7) Uani 1 1 d . . . . .
N4 N 0.5537(3) 0.4504(2) 0.67908(16) 0.0343(7) Uani 1 1 d . . . . .
O4 O 0.4881(3) 0.4710(2) 0.82696(14) 0.0519(8) Uani 1 1 d . . . . .
C11 C 0.2137(4) 0.5807(2) 0.67826(19) 0.0302(8) Uani 1 1 d . . . . .
C6 C 0.1756(4) 0.5143(2) 0.63434(19) 0.0313(8) Uani 1 1 d . . . . .
C1 C 0.2223(4) 0.3699(2) 0.61084(18) 0.0280(8) Uani 1 1 d . . . . .
C2 C 0.1944(5) 0.2359(2) 0.5656(2) 0.0410(10) Uani 1 1 d . . . . .
H2A H 0.100469 0.223337 0.547897 0.049 Uiso 1 1 calc R U . . .
H2B H 0.242674 0.181931 0.575510 0.049 Uiso 1 1 calc R U . . .
C3 C 0.2758(5) 0.2894(2) 0.5161(2) 0.0401(10) Uani 1 1 d . . . . .
H3A H 0.373841 0.271223 0.514222 0.048 Uiso 1 1 calc R U . . .
H3B H 0.235106 0.286561 0.469993 0.048 Uiso 1 1 calc R U . . .
C5 C 0.3565(5) 0.4396(3) 0.5200(2) 0.0443(10) Uani 1 1 d . . . . .
H5A H 0.363567 0.485363 0.553383 0.066 Uiso 1 1 calc R U . . .
H5B H 0.320925 0.462269 0.477079 0.066 Uiso 1 1 calc R U . . .
H5C H 0.448306 0.414745 0.512697 0.066 Uiso 1 1 calc R U . . .
C4 C 0.1125(4) 0.2615(3) 0.6844(2) 0.0404(10) Uani 1 1 d . . . . .
H4A H 0.117737 0.304886 0.719853 0.061 Uiso 1 1 calc R U . . .
H4B H 0.153066 0.208578 0.701367 0.061 Uiso 1 1 calc R U . . .
H4C H 0.015385 0.251797 0.672000 0.061 Uiso 1 1 calc R U . . .
C7 C 0.0908(5) 0.5319(3) 0.5797(2) 0.0495(12) Uani 1 1 d . . . . .
H7 H 0.059680 0.487007 0.551392 0.059 Uiso 1 1 calc R U . . .
C8 C 0.0502(5) 0.6148(3) 0.5654(3) 0.0590(14) Uani 1 1 d . . . . .
H8 H -0.005290 0.626525 0.526622 0.071 Uiso 1 1 calc R U . . .
C9 C 0.0911(5) 0.6797(3) 0.6080(2) 0.0489(12) Uani 1 1 d . . . . .
H9 H 0.063647 0.736276 0.598529 0.059 Uiso 1 1 calc R U . . .
C10 C 0.1713(4) 0.6626(2) 0.6641(2) 0.0365(9) Uani 1 1 d . . . . .
H10 H 0.198018 0.707471 0.693422 0.044 Uiso 1 1 calc R U . . .
C12 C 0.6598(4) 0.5008(3) 0.6937(2) 0.0422(10) Uani 1 1 d . . . . .
N5 N 0.7904(4) 0.4796(3) 0.7111(2) 0.0648(12) Uani 1 1 d . . . . .
C15 C 0.8288(6) 0.3974(4) 0.7378(3) 0.089(2) Uani 1 1 d . . . . .
H15A H 0.752980 0.375117 0.765418 0.134 Uiso 1 1 calc R U . . .
H15B H 0.912323 0.403048 0.765854 0.134 Uiso 1 1 calc R U . . .
H15C H 0.847162 0.358482 0.700174 0.134 Uiso 1 1 calc R U . . .
C13 C 0.8643(6) 0.5566(5) 0.7341(3) 0.088(2) Uani 1 1 d . . . . .
H13A H 0.956105 0.560924 0.712246 0.105 Uiso 1 1 calc R U . . .
H13B H 0.877363 0.555841 0.783943 0.105 Uiso 1 1 calc R U . . .
C14 C 0.7740(6) 0.6283(4) 0.7135(3) 0.083(2) Uani 1 1 d . . . . .
H14A H 0.761474 0.668925 0.751213 0.099 Uiso 1 1 calc R U . . .
H14B H 0.812788 0.658620 0.673915 0.099 Uiso 1 1 calc R U . . .
N6 N 0.6444(4) 0.5868(2) 0.6961(2) 0.0531(10) Uani 1 1 d . . . . .
C16 C 0.5412(5) 0.6333(3) 0.6604(2) 0.0511(12) Uani 1 1 d . . . . .
H16A H 0.585552 0.669674 0.626547 0.077 Uiso 1 1 calc R U . . .
H16B H 0.489127 0.668405 0.692348 0.077 Uiso 1 1 calc R U . . .
H16C H 0.477944 0.593851 0.637596 0.077 Uiso 1 1 calc R U . . .
C17 C 0.5808(4) 0.3686(3) 0.6517(2) 0.0363(9) Uani 1 1 d . . . . .
C18 C 0.6731(5) 0.3518(3) 0.5988(2) 0.0490(11) Uani 1 1 d . . . . .
H18 H 0.726584 0.396369 0.579888 0.059 Uiso 1 1 calc R U . . .
C19 C 0.6864(5) 0.2696(3) 0.5739(3) 0.0597(14) Uani 1 1 d . . . . .
H19 H 0.749891 0.258230 0.538406 0.072 Uiso 1 1 calc R U . . .
C20 C 0.6081(6) 0.2048(3) 0.6005(3) 0.0603(14) Uani 1 1 d . . . . .
H20 H 0.618528 0.148973 0.583309 0.072 Uiso 1 1 calc R U . . .
C21 C 0.5142(5) 0.2202(3) 0.6520(2) 0.0480(11) Uani 1 1 d . . . . .
H21 H 0.459643 0.175290 0.669630 0.058 Uiso 1 1 calc R U . . .
C22 C 0.5006(4) 0.3022(3) 0.6777(2) 0.0373(9) Uani 1 1 d . . . . .
C23 C 0.5953(5) 0.4832(3) 0.8726(2) 0.0539(12) Uani 1 1 d . . . . .
H23 H 0.679584 0.494420 0.844751 0.065 Uiso 1 1 calc R U . . .
C24 C 0.6259(6) 0.4035(3) 0.9123(3) 0.0717(16) Uani 1 1 d . . . . .
H24A H 0.546203 0.389529 0.940834 0.108 Uiso 1 1 calc R U . . .
H24B H 0.707608 0.412610 0.941037 0.108 Uiso 1 1 calc R U . . .
H24C H 0.643622 0.356773 0.880841 0.108 Uiso 1 1 calc R U . . .
C25 C 0.5736(6) 0.5595(4) 0.9136(3) 0.0725(16) Uani 1 1 d . . . . .
H25A H 0.578467 0.609702 0.884401 0.109 Uiso 1 1 calc R U . . .
H25B H 0.645548 0.563075 0.948688 0.109 Uiso 1 1 calc R U . . .
H25C H 0.482346 0.556896 0.935041 0.109 Uiso 1 1 calc R U . . .
C26 C 0.1718(5) 0.4054(3) 0.8869(2) 0.0527(12) Uani 1 1 d . . . . .
H26 H 0.258437 0.393385 0.913089 0.063 Uiso 1 1 calc R U . . .
C28 C 0.1258(7) 0.4924(3) 0.9061(3) 0.086(2) Uani 1 1 d . . . . .
H28A H 0.195512 0.533744 0.891706 0.129 Uiso 1 1 calc R U . . .
H28B H 0.114560 0.495573 0.955425 0.129 Uiso 1 1 calc R U . . .
H28C H 0.037257 0.505078 0.883877 0.129 Uiso 1 1 calc R U . . .
C27 C 0.0722(6) 0.3386(3) 0.9039(3) 0.0721(17) Uani 1 1 d . . . . .
H27A H -0.012945 0.346746 0.877457 0.108 Uiso 1 1 calc R U . . .
H27B H 0.050843 0.341257 0.952368 0.108 Uiso 1 1 calc R U . . .
H27C H 0.112274 0.283177 0.893164 0.108 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O1 2.061(3) . ?
Zr1 O2 2.055(3) . ?
Zr1 O3 1.971(3) . ?
Zr1 N1 2.386(3) . ?
Zr1 N4 2.456(3) . ?
Zr1 O4 1.944(3) . ?
O1 C11 1.344(4) . ?
O2 C22 1.340(5) . ?
O3 C26 1.407(5) . ?
N1 C6 1.425(5) . ?
N1 C1 1.328(4) . ?
N2 C1 1.342(5) . ?
N2 C2 1.457(5) . ?
N2 C4 1.443(5) . ?
N3 C1 1.362(5) . ?
N3 C3 1.470(5) . ?
N3 C5 1.450(5) . ?
N4 C12 1.328(5) . ?
N4 C17 1.424(5) . ?
O4 C23 1.382(5) . ?
C11 C6 1.406(5) . ?
C11 C10 1.384(5) . ?
C6 C7 1.379(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.513(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C7 H7 0.9500 . ?
C7 C8 1.393(6) . ?
C8 H8 0.9500 . ?
C8 C9 1.382(6) . ?
C9 H9 0.9500 . ?
C9 C10 1.374(6) . ?
C10 H10 0.9500 . ?
C12 N5 1.348(6) . ?
C12 N6 1.365(6) . ?
N5 C15 1.447(7) . ?
N5 C13 1.480(7) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.484(9) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 N6 1.452(6) . ?
N6 C16 1.422(6) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.400(6) . ?
C17 C22 1.402(6) . ?
C18 H18 0.9500 . ?
C18 C19 1.392(7) . ?
C19 H19 0.9500 . ?
C19 C20 1.377(7) . ?
C20 H20 0.9500 . ?
C20 C21 1.385(7) . ?
C21 H21 0.9500 . ?
C21 C22 1.396(6) . ?
C23 H23 1.0000 . ?
C23 C24 1.509(6) . ?
C23 C25 1.467(7) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26 1.0000 . ?
C26 C28 1.492(7) . ?
C26 C27 1.467(6) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 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 Zr1 N1 72.08(10) . . ?
O1 Zr1 N4 92.17(10) . . ?
O2 Zr1 O1 151.00(10) . . ?
O2 Zr1 N1 82.57(10) . . ?
O2 Zr1 N4 71.49(11) . . ?
O3 Zr1 O1 100.78(11) . . ?
O3 Zr1 O2 95.13(12) . . ?
O3 Zr1 N1 95.00(11) . . ?
O3 Zr1 N4 166.49(12) . . ?
N1 Zr1 N4 85.29(10) . . ?
O4 Zr1 O1 97.40(12) . . ?
O4 Zr1 O2 104.69(12) . . ?
O4 Zr1 O3 96.70(12) . . ?
O4 Zr1 N1 165.58(12) . . ?
O4 Zr1 N4 85.29(12) . . ?
C11 O1 Zr1 124.2(2) . . ?
C22 O2 Zr1 124.4(2) . . ?
C26 O3 Zr1 139.9(3) . . ?
C6 N1 Zr1 111.1(2) . . ?
C1 N1 Zr1 125.4(2) . . ?
C1 N1 C6 118.8(3) . . ?
C1 N2 C2 111.2(3) . . ?
C1 N2 C4 126.2(3) . . ?
C4 N2 C2 119.8(3) . . ?
C1 N3 C3 109.9(3) . . ?
C1 N3 C5 123.1(3) . . ?
C5 N3 C3 117.5(3) . . ?
C12 N4 Zr1 120.3(3) . . ?
C12 N4 C17 118.9(3) . . ?
C17 N4 Zr1 108.7(2) . . ?
C23 O4 Zr1 171.0(3) . . ?
O1 C11 C6 117.7(3) . . ?
O1 C11 C10 122.7(3) . . ?
C10 C11 C6 119.6(4) . . ?
C11 C6 N1 114.7(3) . . ?
C7 C6 N1 126.0(3) . . ?
C7 C6 C11 119.0(3) . . ?
N1 C1 N2 123.1(3) . . ?
N1 C1 N3 127.3(3) . . ?
N2 C1 N3 109.5(3) . . ?
N2 C2 H2A 111.2 . . ?
N2 C2 H2B 111.2 . . ?
N2 C2 C3 102.9(3) . . ?
H2A C2 H2B 109.1 . . ?
C3 C2 H2A 111.2 . . ?
C3 C2 H2B 111.2 . . ?
N3 C3 C2 102.6(3) . . ?
N3 C3 H3A 111.2 . . ?
N3 C3 H3B 111.2 . . ?
C2 C3 H3A 111.2 . . ?
C2 C3 H3B 111.2 . . ?
H3A C3 H3B 109.2 . . ?
N3 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
N3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C7 H7 119.6 . . ?
C6 C7 C8 120.8(4) . . ?
C8 C7 H7 119.6 . . ?
C7 C8 H8 120.2 . . ?
C9 C8 C7 119.6(4) . . ?
C9 C8 H8 120.2 . . ?
C8 C9 H9 119.9 . . ?
C10 C9 C8 120.1(4) . . ?
C10 C9 H9 119.9 . . ?
C11 C10 H10 119.6 . . ?
C9 C10 C11 120.8(4) . . ?
C9 C10 H10 119.6 . . ?
N4 C12 N5 128.7(5) . . ?
N4 C12 N6 121.3(4) . . ?
N5 C12 N6 109.9(4) . . ?
C12 N5 C15 123.6(5) . . ?
C12 N5 C13 108.8(5) . . ?
C15 N5 C13 120.1(5) . . ?
N5 C15 H15A 109.5 . . ?
N5 C15 H15B 109.5 . . ?
N5 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N5 C13 H13A 110.7 . . ?
N5 C13 H13B 110.7 . . ?
N5 C13 C14 105.1(4) . . ?
H13A C13 H13B 108.8 . . ?
C14 C13 H13A 110.7 . . ?
C14 C13 H13B 110.7 . . ?
C13 C14 H14A 111.2 . . ?
C13 C14 H14B 111.2 . . ?
H14A C14 H14B 109.1 . . ?
N6 C14 C13 103.0(5) . . ?
N6 C14 H14A 111.2 . . ?
N6 C14 H14B 111.2 . . ?
C12 N6 C14 111.3(5) . . ?
C12 N6 C16 124.9(4) . . ?
C16 N6 C14 119.0(4) . . ?
N6 C16 H16A 109.5 . . ?
N6 C16 H16B 109.5 . . ?
N6 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 N4 124.9(4) . . ?
C18 C17 C22 119.0(4) . . ?
C22 C17 N4 115.9(3) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 C17 119.9(5) . . ?
C19 C18 H18 120.0 . . ?
C18 C19 H19 119.8 . . ?
C20 C19 C18 120.4(5) . . ?
C20 C19 H19 119.8 . . ?
C19 C20 H20 119.6 . . ?
C19 C20 C21 120.7(5) . . ?
C21 C20 H20 119.6 . . ?
C20 C21 H21 120.3 . . ?
C20 C21 C22 119.4(5) . . ?
C22 C21 H21 120.3 . . ?
O2 C22 C17 118.0(4) . . ?
O2 C22 C21 121.5(4) . . ?
C21 C22 C17 120.5(4) . . ?
O4 C23 H23 106.0 . . ?
O4 C23 C24 111.5(4) . . ?
O4 C23 C25 111.4(4) . . ?
C24 C23 H23 106.0 . . ?
C25 C23 H23 106.0 . . ?
C25 C23 C24 115.3(4) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O3 C26 H26 107.0 . . ?
O3 C26 C28 110.0(4) . . ?
O3 C26 C27 111.3(4) . . ?
C28 C26 H26 107.0 . . ?
C27 C26 H26 107.0 . . ?
C27 C26 C28 114.1(4) . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zr1 O1 C11 C6 0.1(5) . . . . ?
Zr1 O1 C11 C10 179.9(3) . . . . ?
Zr1 O2 C22 C17 13.4(5) . . . . ?
Zr1 O2 C22 C21 -167.3(3) . . . . ?
Zr1 O3 C26 C28 74.7(6) . . . . ?
Zr1 O3 C26 C27 -157.9(4) . . . . ?
Zr1 N1 C6 C11 -4.4(4) . . . . ?
Zr1 N1 C6 C7 -177.3(4) . . . . ?
Zr1 N1 C1 N2 63.0(5) . . . . ?
Zr1 N1 C1 N3 -115.4(4) . . . . ?
Zr1 N4 C12 N5 110.8(4) . . . . ?
Zr1 N4 C12 N6 -65.7(5) . . . . ?
Zr1 N4 C17 C18 170.7(3) . . . . ?
Zr1 N4 C17 C22 -4.8(4) . . . . ?
O1 C11 C6 N1 3.2(5) . . . . ?
O1 C11 C6 C7 176.6(4) . . . . ?
O1 C11 C10 C9 -179.0(4) . . . . ?
N1 C6 C7 C8 176.6(4) . . . . ?
N2 C2 C3 N3 -18.8(4) . . . . ?
N4 C12 N5 C15 -20.6(7) . . . . ?
N4 C12 N5 C13 -170.2(4) . . . . ?
N4 C12 N6 C14 179.7(4) . . . . ?
N4 C12 N6 C16 -25.5(7) . . . . ?
N4 C17 C18 C19 -177.0(4) . . . . ?
N4 C17 C22 O2 -3.7(5) . . . . ?
N4 C17 C22 C21 176.9(4) . . . . ?
C11 C6 C7 C8 4.0(7) . . . . ?
C6 N1 C1 N2 -143.4(4) . . . . ?
C6 N1 C1 N3 38.2(6) . . . . ?
C6 C11 C10 C9 0.8(6) . . . . ?
C6 C7 C8 C9 -2.5(8) . . . . ?
C1 N1 C6 C11 -161.5(3) . . . . ?
C1 N1 C6 C7 25.6(6) . . . . ?
C1 N2 C2 C3 15.3(4) . . . . ?
C1 N3 C3 C2 17.5(4) . . . . ?
C2 N2 C1 N1 176.7(3) . . . . ?
C2 N2 C1 N3 -4.7(4) . . . . ?
C3 N3 C1 N1 169.9(4) . . . . ?
C3 N3 C1 N2 -8.7(4) . . . . ?
C5 N3 C1 N1 24.5(6) . . . . ?
C5 N3 C1 N2 -154.1(4) . . . . ?
C5 N3 C3 C2 165.1(3) . . . . ?
C4 N2 C1 N1 15.7(6) . . . . ?
C4 N2 C1 N3 -165.6(4) . . . . ?
C4 N2 C2 C3 177.6(3) . . . . ?
C7 C8 C9 C10 0.0(8) . . . . ?
C8 C9 C10 C11 0.8(7) . . . . ?
C10 C11 C6 N1 -176.6(3) . . . . ?
C10 C11 C6 C7 -3.2(6) . . . . ?
C12 N4 C17 C18 -46.5(6) . . . . ?
C12 N4 C17 C22 137.9(4) . . . . ?
C12 N5 C13 C14 -12.8(6) . . . . ?
N5 C12 N6 C14 2.6(6) . . . . ?
N5 C12 N6 C16 157.4(4) . . . . ?
N5 C13 C14 N6 13.4(6) . . . . ?
C15 N5 C13 C14 -163.7(5) . . . . ?
C13 C14 N6 C12 -10.3(6) . . . . ?
C13 C14 N6 C16 -166.8(4) . . . . ?
N6 C12 N5 C15 156.2(5) . . . . ?
N6 C12 N5 C13 6.6(5) . . . . ?
C17 N4 C12 N5 -27.6(6) . . . . ?
C17 N4 C12 N6 155.9(4) . . . . ?
C17 C18 C19 C20 0.8(7) . . . . ?
C18 C17 C22 O2 -179.6(4) . . . . ?
C18 C17 C22 C21 1.1(6) . . . . ?
C18 C19 C20 C21 0.4(8) . . . . ?
C19 C20 C21 C22 -0.8(7) . . . . ?
C20 C21 C22 O2 -179.2(4) . . . . ?
C20 C21 C22 C17 0.1(6) . . . . ?
C22 C17 C18 C19 -1.5(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.9958(5)
2 0.0042(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_zn001_0m
_database_code_depnum_ccdc_archive 'CCDC 2345355'
loop_
_audit_author_name
_audit_author_address
'Gino G. Lavoie'
;York University
Canada
;
_audit_update_record             
;
2024-04-02 deposited with the CCDC.	2024-08-06 downloaded from the CCDC.
;
_audit_creation_date             2022-02-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H42 N6 O4 Ti'
_chemical_formula_sum            'C28 H42 N6 O4 Ti'
_chemical_formula_weight         574.57
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   23.2014(7)
_cell_length_b                   10.7004(3)
_cell_length_c                   24.3975(7)
_cell_angle_alpha                90
_cell_angle_beta                 95.7949(12)
_cell_angle_gamma                90
_cell_volume                     6026.1(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.60
_shelx_estimated_absorpt_T_max   0.968
_shelx_estimated_absorpt_T_min   0.968
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2448
_exptl_crystal_recrystallization_method 
'evaporation from saturated pentane solution'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0771
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            157194
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.033
_diffrn_reflns_theta_min         2.538
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                15053
_reflns_number_total             17589
_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 V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     779
_refine_ls_number_reflns         17589
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0532
_refine_ls_restrained_S_all      1.131
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0497P)²+3.7815P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1316
_refine_special_details          ?
_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
 Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25A)=
 Sof(H25A)=Sof(H25B)=Sof(H25C)=1-FVAR(1)
 Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31A)=
 Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(1)
 Sof(C26B)=Sof(H26B)=Sof(C27B)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C28B)=
 Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(2)
 Sof(C29B)=Sof(H29B)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C31B)=
 Sof(H31D)=Sof(H31E)=Sof(H31F)=FVAR(2)
3.a Ternary CH refined with riding coordinates:
 C26A(H26A), C29A(H29A), C23A(H23A), C23B(H23B), C29B(H29B), C26B(H26B)
3.b Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C3A(H3AA,H3AB), C13A(H13A,H13B), C14A(H14A,H14B), C2B(H2BB,
 H2BA), C3B(H3BA,H3BB), C13B(H13C,H13D), C14B(H14C,H14D)
3.c Aromatic/amide H refined with riding coordinates:
 C8A(H8A), C9A(H9A), C10A(H10A), C11A(H11A), C19A(H19A), C20A(H20A),
 C21A(H21A), C22A(H22A), C8B(H8B), C9B(H9B), C10B(H10B), C11B(H11B), C19B(H19B),
  C20B(H20B), C21B(H21B), C22B(H22B)
3.d Idealised Me refined as rotating group:
 C4A(H4AA,H4AC,H4AB), C5A(H5AA,H5AC,H5AB), C15A(H15B,H15C,H15A), C16A(H16A,
 H16B,H16C), C27A(H27A,H27B,H27C), C28A(H28C,H28A,H28B), C30A(H30A,H30B,H30C),
 C31A(H31A,H31B,H31C), C24A(H24A,H24B,H24C), C25A(H25A,H25B,H25C), C4B(H4BB,
 H4BC,H4BA), C5B(H5BA,H5BB,H5BC), C15B(H15E,H15F,H15D), C16B(H16D,H16E,H16F),
 C24B(H24D,H24E,H24F), C25B(H25D,H25E,H25F), C30B(H30D,H30E,H30F), C31B(H31D,
 H31E,H31F), C27B(H27D,H27E,H27F), C28B(H28D,H28E,H28F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
Ti1A Ti 0.17038(2) 0.23239(3) 0.51635(2) 0.02579(7) Uani 1 1 d . . . . .
O1A O 0.18744(5) 0.38530(11) 0.48025(5) 0.0247(2) Uani 1 1 d . . . . .
O2A O 0.17429(7) 0.10651(13) 0.57294(6) 0.0427(3) Uani 1 1 d . . . . .
O3A O 0.09303(6) 0.25982(14) 0.51128(6) 0.0416(3) Uani 1 1 d . . . . .
O4A O 0.17131(6) 0.11619(12) 0.46049(5) 0.0329(3) Uani 1 1 d . . . . .
N1A N 0.27233(6) 0.23232(13) 0.51380(6) 0.0244(3) Uani 1 1 d . . . . .
N2A N 0.32264(7) 0.11846(15) 0.44760(6) 0.0320(3) Uani 1 1 d . . . . .
N3A N 0.30564(7) 0.02619(15) 0.52583(7) 0.0355(3) Uani 1 1 d . . . . .
N4A N 0.18979(6) 0.33968(14) 0.59654(5) 0.0254(3) Uani 1 1 d . . . . .
N5A N 0.26732(7) 0.48210(18) 0.62735(6) 0.0373(4) Uani 1 1 d . . . . .
N6A N 0.18992(7) 0.55314(15) 0.57620(7) 0.0347(3) Uani 1 1 d . . . . .
C1A C 0.29886(7) 0.13275(16) 0.49628(7) 0.0268(3) Uani 1 1 d . . . . .
C2A C 0.33914(10) -0.0128(2) 0.44078(9) 0.0426(5) Uani 1 1 d . . . . .
H2AA H 0.377980 -0.019315 0.427529 0.051 Uiso 1 1 calc R U . . .
H2AB H 0.310632 -0.056561 0.414569 0.051 Uiso 1 1 calc R U . . .
C3A C 0.33924(11) -0.0659(2) 0.49846(10) 0.0456(5) Uani 1 1 d . . . . .
H3AA H 0.320557 -0.149148 0.497788 0.055 Uiso 1 1 calc R U . . .
H3AB H 0.379149 -0.072859 0.516835 0.055 Uiso 1 1 calc R U . . .
C4A C 0.30116(10) 0.1847(2) 0.39757(8) 0.0410(5) Uani 1 1 d . . . . .
H4AA H 0.304243 0.274987 0.403966 0.061 Uiso 1 1 calc R U . . .
H4AC H 0.260519 0.162410 0.387383 0.061 Uiso 1 1 calc R U . . .
H4AB H 0.324247 0.161344 0.367675 0.061 Uiso 1 1 calc R U . . .
C5A C 0.30181(11) 0.0169(2) 0.58435(9) 0.0474(5) Uani 1 1 d . . . . .
H5AA H 0.291546 0.098604 0.598699 0.071 Uiso 1 1 calc R U . . .
H5AC H 0.339266 -0.009882 0.602768 0.071 Uiso 1 1 calc R U . . .
H5AB H 0.272006 -0.044347 0.591345 0.071 Uiso 1 1 calc R U . . .
C6A C 0.28773(7) 0.35046(15) 0.49376(6) 0.0239(3) Uani 1 1 d . . . . .
C7A C 0.24085(7) 0.42959(15) 0.47708(6) 0.0235(3) Uani 1 1 d . . . . .
C8A C 0.25092(8) 0.54854(17) 0.45664(7) 0.0309(3) Uani 1 1 d . . . . .
H8A H 0.219308 0.602073 0.445215 0.037 Uiso 1 1 calc R U . . .
C9A C 0.30763(9) 0.58841(18) 0.45307(8) 0.0367(4) Uani 1 1 d . . . . .
H9A H 0.314495 0.668458 0.438188 0.044 Uiso 1 1 calc R U . . .
C10A C 0.35396(9) 0.51256(19) 0.47098(8) 0.0363(4) Uani 1 1 d . . . . .
H10A H 0.392467 0.541325 0.469222 0.044 Uiso 1 1 calc R U . . .
C11A C 0.34415(8) 0.39388(18) 0.49160(7) 0.0314(4) Uani 1 1 d . . . . .
H11A H 0.376049 0.342241 0.504271 0.038 Uiso 1 1 calc R U . . .
C12A C 0.21435(7) 0.45128(18) 0.60046(7) 0.0282(3) Uani 1 1 d . . . . .
C13A C 0.28338(10) 0.6060(2) 0.60865(9) 0.0478(6) Uani 1 1 d . . . . .
H13A H 0.309204 0.599862 0.578841 0.057 Uiso 1 1 calc R U . . .
H13B H 0.302939 0.655552 0.639380 0.057 Uiso 1 1 calc R U . . .
C14A C 0.22583(11) 0.6631(2) 0.58784(10) 0.0483(5) Uani 1 1 d . . . . .
H14A H 0.210563 0.716370 0.616253 0.058 Uiso 1 1 calc R U . . .
H14B H 0.228851 0.713317 0.554159 0.058 Uiso 1 1 calc R U . . .
C15A C 0.31355(8) 0.3900(3) 0.63801(8) 0.0472(6) Uani 1 1 d . . . . .
H15B H 0.302869 0.313021 0.617707 0.071 Uiso 1 1 calc R U . . .
H15C H 0.319293 0.371851 0.677553 0.071 Uiso 1 1 calc R U . . .
H15A H 0.349524 0.423320 0.625913 0.071 Uiso 1 1 calc R U . . .
C16A C 0.12943(9) 0.5644(2) 0.55592(10) 0.0439(5) Uani 1 1 d . . . . .
H16A H 0.109661 0.617014 0.581044 0.066 Uiso 1 1 calc R U . . .
H16B H 0.111590 0.481268 0.553757 0.066 Uiso 1 1 calc R U . . .
H16C H 0.126029 0.602428 0.519197 0.066 Uiso 1 1 calc R U . . .
C17A C 0.19534(7) 0.25695(19) 0.64160(7) 0.0324(4) Uani 1 1 d . . . . .
C18A C 0.18450(9) 0.1325(2) 0.62688(9) 0.0403(5) Uani 1 1 d . . . . .
C19A C 0.18513(11) 0.0413(3) 0.66789(11) 0.0593(7) Uani 1 1 d . . . . .
H19A H 0.177715 -0.043640 0.658356 0.071 Uiso 1 1 calc R U . . .
C20A C 0.19675(11) 0.0763(3) 0.72314(11) 0.0698(10) Uani 1 1 d . . . . .
H20A H 0.197826 0.014358 0.751135 0.084 Uiso 1 1 calc R U . . .
C21A C 0.20664(10) 0.1991(3) 0.73732(9) 0.0605(8) Uani 1 1 d . . . . .
H21A H 0.214052 0.221442 0.775056 0.073 Uiso 1 1 calc R U . . .
C22A C 0.20592(8) 0.2908(3) 0.69727(8) 0.0444(5) Uani 1 1 d . . . . .
H22A H 0.212517 0.375774 0.707346 0.053 Uiso 1 1 calc R U . . .
C26A C 0.13336(9) 0.01264(18) 0.44969(9) 0.0384(4) Uani 1 1 d . . . . .
H26A H 0.102574 0.015542 0.475536 0.046 Uiso 1 1 calc R U . . .
C27A C 0.16747(14) -0.1062(2) 0.45922(13) 0.0640(8) Uani 1 1 d . . . . .
H27A H 0.186166 -0.107503 0.497079 0.096 Uiso 1 1 calc R U . . .
H27B H 0.197106 -0.110635 0.433372 0.096 Uiso 1 1 calc R U . . .
H27C H 0.141364 -0.178087 0.453438 0.096 Uiso 1 1 calc R U . . .
C28A C 0.10528(13) 0.0217(2) 0.39109(11) 0.0586(7) Uani 1 1 d . . . . .
H28C H 0.135189 0.017476 0.365515 0.088 Uiso 1 1 calc R U . . .
H28A H 0.084433 0.101221 0.386088 0.088 Uiso 1 1 calc R U . . .
H28B H 0.078013 -0.047641 0.383705 0.088 Uiso 1 1 calc R U . . .
C29A C 0.0522(2) 0.2539(6) 0.5546(3) 0.0470(14) Uani 0.429(5) 1 d . . P A 1
H29A H 0.069037 0.299606 0.588187 0.056 Uiso 0.429(5) 1 calc R U P A 1
C30A C 0.0010(3) 0.3276(12) 0.5263(5) 0.096(4) Uani 0.429(5) 1 d . . P A 1
H30A H -0.013667 0.285552 0.492040 0.145 Uiso 0.429(5) 1 calc R U P A 1
H30B H 0.013633 0.412282 0.518030 0.145 Uiso 0.429(5) 1 calc R U P A 1
H30C H -0.029916 0.332193 0.550877 0.145 Uiso 0.429(5) 1 calc R U P A 1
C31A C 0.0372(3) 0.1214(7) 0.5697(3) 0.072(2) Uani 0.429(5) 1 d . . P A 1
H31A H 0.071680 0.080494 0.588159 0.108 Uiso 0.429(5) 1 calc R U P A 1
H31B H 0.023690 0.074959 0.536273 0.108 Uiso 0.429(5) 1 calc R U P A 1
H31C H 0.006585 0.123076 0.594592 0.108 Uiso 0.429(5) 1 calc R U P A 1
C23A C 0.03841(17) 0.2225(4) 0.5247(2) 0.0442(11) Uani 0.571(5) 1 d . . P A 2
H23A H 0.043715 0.143444 0.546461 0.053 Uiso 0.571(5) 1 calc R U P A 2
C24A C 0.0138(3) 0.3176(7) 0.5605(3) 0.076(2) Uani 0.571(5) 1 d . . P A 2
H24A H 0.005981 0.394960 0.539572 0.114 Uiso 0.571(5) 1 calc R U P A 2
H24B H 0.041637 0.334406 0.592586 0.114 Uiso 0.571(5) 1 calc R U P A 2
H24C H -0.022331 0.285815 0.572820 0.114 Uiso 0.571(5) 1 calc R U P A 2
C25A C -0.00455(17) 0.1954(5) 0.4746(2) 0.0645(15) Uani 0.571(5) 1 d . . P A 2
H25A H 0.011289 0.130584 0.452045 0.097 Uiso 0.571(5) 1 calc R U P A 2
H25B H -0.011348 0.271790 0.452780 0.097 Uiso 0.571(5) 1 calc R U P A 2
H25C H -0.041201 0.166357 0.486881 0.097 Uiso 0.571(5) 1 calc R U P A 2
Ti1B Ti 0.46736(2) 0.05222(3) 0.31622(2) 0.01962(6) Uani 1 1 d . . . . .
O1B O 0.54570(5) 0.03333(12) 0.29883(5) 0.0286(2) Uani 1 1 d . . . . .
O2B O 0.38359(4) 0.04287(10) 0.30722(4) 0.0207(2) Uani 1 1 d . . . . .
O3B O 0.48136(5) 0.19902(12) 0.35375(5) 0.0295(3) Uani 1 1 d . . . . .
O4B O 0.47277(5) -0.05478(12) 0.37525(5) 0.0278(2) Uani 1 1 d . . . . .
N1B N 0.46322(5) -0.10036(12) 0.25158(5) 0.0213(2) Uani 1 1 d . . . . .
N2B N 0.37072(6) -0.19081(13) 0.24459(6) 0.0244(3) Uani 1 1 d . . . . .
N3B N 0.40420(6) -0.14010(14) 0.16578(6) 0.0285(3) Uani 1 1 d . . . . .
N4B N 0.44019(6) 0.18374(12) 0.24294(5) 0.0222(3) Uani 1 1 d . . . . .
N5B N 0.43261(7) 0.40514(14) 0.25679(7) 0.0349(3) Uani 1 1 d . . . . .
N6B N 0.51561(7) 0.32644(14) 0.23567(7) 0.0336(3) Uani 1 1 d . . . . .
C1B C 0.41569(7) -0.14151(14) 0.22165(6) 0.0217(3) Uani 1 1 d . . . . .
C2B C 0.32527(8) -0.23256(18) 0.20297(8) 0.0323(4) Uani 1 1 d . . . . .
H2BB H 0.286640 -0.203809 0.211570 0.039 Uiso 1 1 calc R U . . .
H2BA H 0.324962 -0.324744 0.199479 0.039 Uiso 1 1 calc R U . . .
C3B C 0.34274(8) -0.17042(19) 0.15097(7) 0.0332(4) Uani 1 1 d . . . . .
H3BA H 0.337878 -0.228251 0.119166 0.040 Uiso 1 1 calc R U . . .
H3BB H 0.319663 -0.093964 0.142018 0.040 Uiso 1 1 calc R U . . .
C4B C 0.37183(8) -0.23019(16) 0.30132(7) 0.0293(3) Uani 1 1 d . . . . .
H4BB H 0.371603 -0.321686 0.303067 0.044 Uiso 1 1 calc R U . . .
H4BC H 0.337659 -0.197338 0.317039 0.044 Uiso 1 1 calc R U . . .
H4BA H 0.406974 -0.198263 0.322353 0.044 Uiso 1 1 calc R U . . .
C5B C 0.43124(9) -0.05260(19) 0.13053(8) 0.0367(4) Uani 1 1 d . . . . .
H5BA H 0.409004 0.025407 0.127758 0.055 Uiso 1 1 calc R U . . .
H5BB H 0.431973 -0.089031 0.093753 0.055 Uiso 1 1 calc R U . . .
H5BC H 0.470951 -0.035256 0.146346 0.055 Uiso 1 1 calc R U . . .
C6B C 0.51831(7) -0.12308(16) 0.23415(7) 0.0252(3) Uani 1 1 d . . . . .
C7B C 0.56223(7) -0.05158(17) 0.26318(7) 0.0289(3) Uani 1 1 d . . . . .
C8B C 0.62004(8) -0.0718(2) 0.25490(9) 0.0420(5) Uani 1 1 d . . . . .
H8B H 0.649742 -0.023709 0.274510 0.050 Uiso 1 1 calc R U . . .
C9B C 0.63404(9) -0.1630(3) 0.21772(10) 0.0515(6) Uani 1 1 d . . . . .
H9B H 0.673461 -0.177139 0.212202 0.062 Uiso 1 1 calc R U . . .
C10B C 0.59121(10) -0.2328(2) 0.18883(10) 0.0466(5) Uani 1 1 d . . . . .
H10B H 0.601275 -0.294426 0.163417 0.056 Uiso 1 1 calc R U . . .
C11B C 0.53308(8) -0.21352(18) 0.19677(8) 0.0344(4) Uani 1 1 d . . . . .
H11B H 0.503691 -0.261796 0.176791 0.041 Uiso 1 1 calc R U . . .
C12B C 0.46119(7) 0.29891(15) 0.24487(7) 0.0256(3) Uani 1 1 d . . . . .
C13B C 0.47197(10) 0.51149(19) 0.26020(11) 0.0490(5) Uani 1 1 d . . . . .
H13C H 0.479294 0.541974 0.298579 0.059 Uiso 1 1 calc R U . . .
H13D H 0.456087 0.580854 0.236419 0.059 Uiso 1 1 calc R U . . .
C14B C 0.52702(10) 0.45967(19) 0.23994(11) 0.0484(5) Uani 1 1 d . . . . .
H14C H 0.533648 0.495541 0.203698 0.058 Uiso 1 1 calc R U . . .
H14D H 0.561147 0.477129 0.266565 0.058 Uiso 1 1 calc R U . . .
C15B C 0.38392(9) 0.40475(19) 0.28993(10) 0.0415(5) Uani 1 1 d . . . . .
H15E H 0.348273 0.424896 0.266555 0.062 Uiso 1 1 calc R U . . .
H15F H 0.390415 0.467252 0.319261 0.062 Uiso 1 1 calc R U . . .
H15D H 0.380258 0.321856 0.306294 0.062 Uiso 1 1 calc R U . . .
C16B C 0.55518(9) 0.2419(2) 0.21238(10) 0.0430(5) Uani 1 1 d . . . . .
H16D H 0.586408 0.219012 0.240676 0.065 Uiso 1 1 calc R U . . .
H16E H 0.571674 0.282923 0.181619 0.065 Uiso 1 1 calc R U . . .
H16F H 0.534290 0.166460 0.199067 0.065 Uiso 1 1 calc R U . . .
C17B C 0.38014(7) 0.16822(15) 0.22838(7) 0.0230(3) Uani 1 1 d . . . . .
C18B C 0.35221(6) 0.08785(14) 0.26260(6) 0.0205(3) Uani 1 1 d . . . . .
C19B C 0.29364(7) 0.05907(16) 0.24967(7) 0.0275(3) Uani 1 1 d . . . . .
H19B H 0.274624 0.003896 0.272479 0.033 Uiso 1 1 calc R U . . .
C20B C 0.26338(7) 0.11177(19) 0.20318(8) 0.0347(4) Uani 1 1 d . . . . .
H20B H 0.223748 0.091212 0.193975 0.042 Uiso 1 1 calc R U . . .
C21B C 0.29043(8) 0.19368(19) 0.17033(8) 0.0362(4) Uani 1 1 d . . . . .
H21B H 0.268961 0.231219 0.139414 0.043 Uiso 1 1 calc R U . . .
C22B C 0.34891(8) 0.22158(18) 0.18220(7) 0.0320(4) Uani 1 1 d . . . . .
H22B H 0.367550 0.276631 0.159041 0.038 Uiso 1 1 calc R U . . .
C23B C 0.51506(8) 0.23977(18) 0.40156(8) 0.0342(4) Uani 1 1 d . . . . .
H23B H 0.518360 0.169862 0.428901 0.041 Uiso 1 1 calc R U . . .
C24B C 0.57496(10) 0.2748(3) 0.38820(12) 0.0607(7) Uani 1 1 d . . . . .
H24D H 0.592304 0.204052 0.370321 0.091 Uiso 1 1 calc R U . . .
H24E H 0.599016 0.296154 0.422254 0.091 Uiso 1 1 calc R U . . .
H24F H 0.572540 0.346933 0.363329 0.091 Uiso 1 1 calc R U . . .
C25B C 0.48473(13) 0.3479(3) 0.42581(11) 0.0617(7) Uani 1 1 d . . . . .
H25D H 0.481303 0.417225 0.399420 0.093 Uiso 1 1 calc R U . . .
H25E H 0.507152 0.375213 0.459910 0.093 Uiso 1 1 calc R U . . .
H25F H 0.446006 0.321741 0.433894 0.093 Uiso 1 1 calc R U . . .
C29B C 0.5026(2) -0.1712(5) 0.3872(2) 0.0386(11) Uani 0.479(5) 1 d . . P B 3
H29B H 0.503758 -0.219257 0.352218 0.046 Uiso 0.479(5) 1 calc R U P B 3
C30B C 0.4700(2) -0.2475(5) 0.4268(2) 0.0544(15) Uani 0.479(5) 1 d . . P B 3
H30D H 0.466178 -0.198522 0.460183 0.082 Uiso 0.479(5) 1 calc R U P B 3
H30E H 0.491503 -0.324490 0.436612 0.082 Uiso 0.479(5) 1 calc R U P B 3
H30F H 0.431459 -0.268539 0.409094 0.082 Uiso 0.479(5) 1 calc R U P B 3
C31B C 0.5628(2) -0.1430(8) 0.4105(3) 0.082(3) Uani 0.479(5) 1 d . . P B 3
H31D H 0.581792 -0.091875 0.384257 0.123 Uiso 0.479(5) 1 calc R U P B 3
H31E H 0.584216 -0.221275 0.417298 0.123 Uiso 0.479(5) 1 calc R U P B 3
H31F H 0.561996 -0.097227 0.445175 0.123 Uiso 0.479(5) 1 calc R U P B 3
C26B C 0.52023(17) -0.1142(5) 0.40614(16) 0.0358(9) Uani 0.521(5) 1 d . . P B 4
H26B H 0.555644 -0.063993 0.401004 0.043 Uiso 0.521(5) 1 calc R U P B 4
C27B C 0.5122(2) -0.1111(6) 0.46600(17) 0.0590(14) Uani 0.521(5) 1 d . . P B 4
H27D H 0.506507 -0.024584 0.477440 0.088 Uiso 0.521(5) 1 calc R U P B 4
H27E H 0.546674 -0.145736 0.487217 0.088 Uiso 0.521(5) 1 calc R U P B 4
H27F H 0.478221 -0.161051 0.472701 0.088 Uiso 0.521(5) 1 calc R U P B 4
C28B C 0.5290(3) -0.2411(5) 0.3829(2) 0.0692(19) Uani 0.521(5) 1 d . . P B 4
H28D H 0.495922 -0.294528 0.389091 0.104 Uiso 0.521(5) 1 calc R U P B 4
H28E H 0.564587 -0.277853 0.401041 0.104 Uiso 0.521(5) 1 calc R U P B 4
H28F H 0.532078 -0.234269 0.343227 0.104 Uiso 0.521(5) 1 calc R U P B 4


_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
Ti1A O1A 1.9182(12) . ?
Ti1A O2A 1.9245(14) . ?
Ti1A O3A 1.8103(14) . ?
Ti1A O4A 1.8466(13) . ?
Ti1A N1A 2.3724(14) . ?
Ti1A N4A 2.2738(14) . ?
O1A C7A 1.3364(19) . ?
O2A C18A 1.342(3) . ?
O3A C29A 1.489(6) . ?
O3A C23A 1.399(4) . ?
O4A C26A 1.423(2) . ?
N1A C1A 1.323(2) . ?
N1A C6A 1.414(2) . ?
N2A C1A 1.368(2) . ?
N2A C2A 1.470(2) . ?
N2A C4A 1.455(2) . ?
N3A C1A 1.350(2) . ?
N3A C3A 1.459(2) . ?
N3A C5A 1.443(3) . ?
N4A C12A 1.322(2) . ?
N4A C17A 1.407(2) . ?
N5A C12A 1.374(2) . ?
N5A C13A 1.463(3) . ?
N5A C15A 1.461(3) . ?
N6A C12A 1.339(3) . ?
N6A C14A 1.453(3) . ?
N6A C16A 1.445(3) . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C2A C3A 1.517(3) . ?
C3A H3AA 0.9900 . ?
C3A H3AB 0.9900 . ?
C4A H4AA 0.9800 . ?
C4A H4AC 0.9800 . ?
C4A H4AB 0.9800 . ?
C5A H5AA 0.9800 . ?
C5A H5AC 0.9800 . ?
C5A H5AB 0.9800 . ?
C6A C7A 1.406(2) . ?
C6A C11A 1.395(2) . ?
C7A C8A 1.395(2) . ?
C8A H8A 0.9500 . ?
C8A C9A 1.394(3) . ?
C9A H9A 0.9500 . ?
C9A C10A 1.382(3) . ?
C10A H10A 0.9500 . ?
C10A C11A 1.393(3) . ?
C11A H11A 0.9500 . ?
C13A H13A 0.9900 . ?
C13A H13B 0.9900 . ?
C13A C14A 1.509(4) . ?
C14A H14A 0.9900 . ?
C14A H14B 0.9900 . ?
C15A H15B 0.9800 . ?
C15A H15C 0.9800 . ?
C15A H15A 0.9800 . ?
C16A H16A 0.9800 . ?
C16A H16B 0.9800 . ?
C16A H16C 0.9800 . ?
C17A C18A 1.396(3) . ?
C17A C22A 1.403(3) . ?
C18A C19A 1.396(3) . ?
C19A H19A 0.9500 . ?
C19A C20A 1.398(4) . ?
C20A H20A 0.9500 . ?
C20A C21A 1.373(5) . ?
C21A H21A 0.9500 . ?
C21A C22A 1.384(3) . ?
C22A H22A 0.9500 . ?
C26A H26A 1.0000 . ?
C26A C27A 1.504(3) . ?
C26A C28A 1.513(3) . ?
C27A H27A 0.9800 . ?
C27A H27B 0.9800 . ?
C27A H27C 0.9800 . ?
C28A H28C 0.9800 . ?
C28A H28A 0.9800 . ?
C28A H28B 0.9800 . ?
C29A H29A 1.0000 . ?
C29A C30A 1.532(11) . ?
C29A C31A 1.514(9) . ?
C30A H30A 0.9800 . ?
C30A H30B 0.9800 . ?
C30A H30C 0.9800 . ?
C31A H31A 0.9800 . ?
C31A H31B 0.9800 . ?
C31A H31C 0.9800 . ?
C23A H23A 1.0000 . ?
C23A C24A 1.491(8) . ?
C23A C25A 1.524(7) . ?
C24A H24A 0.9800 . ?
C24A H24B 0.9800 . ?
C24A H24C 0.9800 . ?
C25A H25A 0.9800 . ?
C25A H25B 0.9800 . ?
C25A H25C 0.9800 . ?
Ti1B O1B 1.9184(12) . ?
Ti1B O2B 1.9364(10) . ?
Ti1B O3B 1.8306(12) . ?
Ti1B O4B 1.8343(12) . ?
Ti1B N1B 2.2652(13) . ?
Ti1B N4B 2.3123(13) . ?
O1B C7B 1.340(2) . ?
O2B C18B 1.3366(18) . ?
O3B C23B 1.406(2) . ?
O4B C29B 1.441(4) . ?
O4B C26B 1.420(3) . ?
N1B C1B 1.334(2) . ?
N1B C6B 1.4084(19) . ?
N2B C1B 1.3408(19) . ?
N2B C2B 1.458(2) . ?
N2B C4B 1.445(2) . ?
N3B C1B 1.362(2) . ?
N3B C3B 1.471(2) . ?
N3B C5B 1.456(2) . ?
N4B C12B 1.324(2) . ?
N4B C17B 1.4125(19) . ?
N5B C12B 1.362(2) . ?
N5B C13B 1.456(2) . ?
N5B C15B 1.454(2) . ?
N6B C12B 1.337(2) . ?
N6B C14B 1.452(2) . ?
N6B C16B 1.445(3) . ?
C2B H2BB 0.9900 . ?
C2B H2BA 0.9900 . ?
C2B C3B 1.523(3) . ?
C3B H3BA 0.9900 . ?
C3B H3BB 0.9900 . ?
C4B H4BB 0.9800 . ?
C4B H4BC 0.9800 . ?
C4B H4BA 0.9800 . ?
C5B H5BA 0.9800 . ?
C5B H5BB 0.9800 . ?
C5B H5BC 0.9800 . ?
C6B C7B 1.407(2) . ?
C6B C11B 1.396(2) . ?
C7B C8B 1.393(2) . ?
C8B H8B 0.9500 . ?
C8B C9B 1.392(3) . ?
C9B H9B 0.9500 . ?
C9B C10B 1.379(4) . ?
C10B H10B 0.9500 . ?
C10B C11B 1.397(3) . ?
C11B H11B 0.9500 . ?
C13B H13C 0.9900 . ?
C13B H13D 0.9900 . ?
C13B C14B 1.520(3) . ?
C14B H14C 0.9900 . ?
C14B H14D 0.9900 . ?
C15B H15E 0.9800 . ?
C15B H15F 0.9800 . ?
C15B H15D 0.9800 . ?
C16B H16D 0.9800 . ?
C16B H16E 0.9800 . ?
C16B H16F 0.9800 . ?
C17B C18B 1.402(2) . ?
C17B C22B 1.398(2) . ?
C18B C19B 1.398(2) . ?
C19B H19B 0.9500 . ?
C19B C20B 1.392(3) . ?
C20B H20B 0.9500 . ?
C20B C21B 1.381(3) . ?
C21B H21B 0.9500 . ?
C21B C22B 1.391(3) . ?
C22B H22B 0.9500 . ?
C23B H23B 1.0000 . ?
C23B C24B 1.507(3) . ?
C23B C25B 1.506(3) . ?
C24B H24D 0.9800 . ?
C24B H24E 0.9800 . ?
C24B H24F 0.9800 . ?
C25B H25D 0.9800 . ?
C25B H25E 0.9800 . ?
C25B H25F 0.9800 . ?
C29B H29B 1.0000 . ?
C29B C30B 1.521(6) . ?
C29B C31B 1.484(8) . ?
C30B H30D 0.9800 . ?
C30B H30E 0.9800 . ?
C30B H30F 0.9800 . ?
C31B H31D 0.9800 . ?
C31B H31E 0.9800 . ?
C31B H31F 0.9800 . ?
C26B H26B 1.0000 . ?
C26B C27B 1.491(6) . ?
C26B C28B 1.494(7) . ?
C27B H27D 0.9800 . ?
C27B H27E 0.9800 . ?
C27B H27F 0.9800 . ?
C28B H28D 0.9800 . ?
C28B H28E 0.9800 . ?
C28B H28F 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
O1A Ti1A O2A 158.35(6) . . ?
O1A Ti1A N1A 74.68(5) . . ?
O1A Ti1A N4A 86.12(5) . . ?
O2A Ti1A N1A 92.51(6) . . ?
O2A Ti1A N4A 75.24(6) . . ?
O3A Ti1A O1A 94.55(6) . . ?
O3A Ti1A O2A 97.88(7) . . ?
O3A Ti1A O4A 98.28(6) . . ?
O3A Ti1A N1A 169.23(6) . . ?
O3A Ti1A N4A 94.92(6) . . ?
O4A Ti1A O1A 102.54(5) . . ?
O4A Ti1A O2A 93.15(6) . . ?
O4A Ti1A N1A 83.95(5) . . ?
O4A Ti1A N4A 163.52(6) . . ?
N4A Ti1A N1A 84.91(5) . . ?
C7A O1A Ti1A 124.37(10) . . ?
C18A O2A Ti1A 123.32(13) . . ?
C29A O3A Ti1A 129.9(3) . . ?
C23A O3A Ti1A 148.6(2) . . ?
C26A O4A Ti1A 127.44(12) . . ?
C1A N1A Ti1A 120.42(11) . . ?
C1A N1A C6A 117.78(13) . . ?
C6A N1A Ti1A 107.22(10) . . ?
C1A N2A C2A 109.74(15) . . ?
C1A N2A C4A 122.68(15) . . ?
C4A N2A C2A 116.21(16) . . ?
C1A N3A C3A 111.39(15) . . ?
C1A N3A C5A 124.84(16) . . ?
C5A N3A C3A 119.70(16) . . ?
C12A N4A Ti1A 124.38(11) . . ?
C12A N4A C17A 120.45(15) . . ?
C17A N4A Ti1A 110.44(12) . . ?
C12A N5A C13A 108.21(17) . . ?
C12A N5A C15A 121.92(18) . . ?
C15A N5A C13A 117.49(17) . . ?
C12A N6A C14A 111.36(17) . . ?
C12A N6A C16A 124.91(17) . . ?
C16A N6A C14A 121.15(18) . . ?
N1A C1A N2A 127.76(16) . . ?
N1A C1A N3A 122.72(15) . . ?
N3A C1A N2A 109.51(15) . . ?
N2A C2A H2AA 111.1 . . ?
N2A C2A H2AB 111.1 . . ?
N2A C2A C3A 103.23(15) . . ?
H2AA C2A H2AB 109.1 . . ?
C3A C2A H2AA 111.1 . . ?
C3A C2A H2AB 111.1 . . ?
N3A C3A C2A 102.75(16) . . ?
N3A C3A H3AA 111.2 . . ?
N3A C3A H3AB 111.2 . . ?
C2A C3A H3AA 111.2 . . ?
C2A C3A H3AB 111.2 . . ?
H3AA C3A H3AB 109.1 . . ?
N2A C4A H4AA 109.5 . . ?
N2A C4A H4AC 109.5 . . ?
N2A C4A H4AB 109.5 . . ?
H4AA C4A H4AC 109.5 . . ?
H4AA C4A H4AB 109.5 . . ?
H4AC C4A H4AB 109.5 . . ?
N3A C5A H5AA 109.5 . . ?
N3A C5A H5AC 109.5 . . ?
N3A C5A H5AB 109.5 . . ?
H5AA C5A H5AC 109.5 . . ?
H5AA C5A H5AB 109.5 . . ?
H5AC C5A H5AB 109.5 . . ?
C7A C6A N1A 115.06(14) . . ?
C11A C6A N1A 125.55(16) . . ?
C11A C6A C7A 119.34(16) . . ?
O1A C7A C6A 117.68(14) . . ?
O1A C7A C8A 122.27(15) . . ?
C8A C7A C6A 120.02(16) . . ?
C7A C8A H8A 120.2 . . ?
C9A C8A C7A 119.64(17) . . ?
C9A C8A H8A 120.2 . . ?
C8A C9A H9A 119.7 . . ?
C10A C9A C8A 120.62(17) . . ?
C10A C9A H9A 119.7 . . ?
C9A C10A H10A 120.0 . . ?
C9A C10A C11A 119.95(17) . . ?
C11A C10A H10A 120.0 . . ?
C6A C11A H11A 119.8 . . ?
C10A C11A C6A 120.36(17) . . ?
C10A C11A H11A 119.8 . . ?
N4A C12A N5A 127.55(18) . . ?
N4A C12A N6A 122.90(16) . . ?
N6A C12A N5A 109.52(17) . . ?
N5A C13A H13A 111.1 . . ?
N5A C13A H13B 111.1 . . ?
N5A C13A C14A 103.14(16) . . ?
H13A C13A H13B 109.1 . . ?
C14A C13A H13A 111.1 . . ?
C14A C13A H13B 111.1 . . ?
N6A C14A C13A 102.02(18) . . ?
N6A C14A H14A 111.4 . . ?
N6A C14A H14B 111.4 . . ?
C13A C14A H14A 111.4 . . ?
C13A C14A H14B 111.4 . . ?
H14A C14A H14B 109.2 . . ?
N5A C15A H15B 109.5 . . ?
N5A C15A H15C 109.5 . . ?
N5A C15A H15A 109.5 . . ?
H15B C15A H15C 109.5 . . ?
H15B C15A H15A 109.5 . . ?
H15C C15A H15A 109.5 . . ?
N6A C16A H16A 109.5 . . ?
N6A C16A H16B 109.5 . . ?
N6A C16A H16C 109.5 . . ?
H16A C16A H16B 109.5 . . ?
H16A C16A H16C 109.5 . . ?
H16B C16A H16C 109.5 . . ?
C18A C17A N4A 113.54(16) . . ?
C18A C17A C22A 120.33(19) . . ?
C22A C17A N4A 125.9(2) . . ?
O2A C18A C17A 117.33(16) . . ?
O2A C18A C19A 123.1(2) . . ?
C17A C18A C19A 119.6(2) . . ?
C18A C19A H19A 120.3 . . ?
C18A C19A C20A 119.4(3) . . ?
C20A C19A H19A 120.3 . . ?
C19A C20A H20A 119.7 . . ?
C21A C20A C19A 120.6(2) . . ?
C21A C20A H20A 119.7 . . ?
C20A C21A H21A 119.6 . . ?
C20A C21A C22A 120.8(2) . . ?
C22A C21A H21A 119.6 . . ?
C17A C22A H22A 120.4 . . ?
C21A C22A C17A 119.3(3) . . ?
C21A C22A H22A 120.4 . . ?
O4A C26A H26A 109.1 . . ?
O4A C26A C27A 108.90(19) . . ?
O4A C26A C28A 108.92(17) . . ?
C27A C26A H26A 109.1 . . ?
C27A C26A C28A 111.7(2) . . ?
C28A C26A H26A 109.1 . . ?
C26A C27A H27A 109.5 . . ?
C26A C27A H27B 109.5 . . ?
C26A C27A H27C 109.5 . . ?
H27A C27A H27B 109.5 . . ?
H27A C27A H27C 109.5 . . ?
H27B C27A H27C 109.5 . . ?
C26A C28A H28C 109.5 . . ?
C26A C28A H28A 109.5 . . ?
C26A C28A H28B 109.5 . . ?
H28C C28A H28A 109.5 . . ?
H28C C28A H28B 109.5 . . ?
H28A C28A H28B 109.5 . . ?
O3A C29A H29A 109.7 . . ?
O3A C29A C30A 100.4(6) . . ?
O3A C29A C31A 113.1(5) . . ?
C30A C29A H29A 109.7 . . ?
C31A C29A H29A 109.7 . . ?
C31A C29A C30A 113.9(7) . . ?
C29A C30A H30A 109.5 . . ?
C29A C30A H30B 109.5 . . ?
C29A C30A H30C 109.5 . . ?
H30A C30A H30B 109.5 . . ?
H30A C30A H30C 109.5 . . ?
H30B C30A H30C 109.5 . . ?
C29A C31A H31A 109.5 . . ?
C29A C31A H31B 109.5 . . ?
C29A C31A H31C 109.5 . . ?
H31A C31A H31B 109.5 . . ?
H31A C31A H31C 109.5 . . ?
H31B C31A H31C 109.5 . . ?
O3A C23A H23A 107.5 . . ?
O3A C23A C24A 110.6(5) . . ?
O3A C23A C25A 113.7(4) . . ?
C24A C23A H23A 107.5 . . ?
C24A C23A C25A 110.0(5) . . ?
C25A C23A H23A 107.5 . . ?
C23A C24A H24A 109.5 . . ?
C23A C24A H24B 109.5 . . ?
C23A C24A H24C 109.5 . . ?
H24A C24A H24B 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C23A C25A H25A 109.5 . . ?
C23A C25A H25B 109.5 . . ?
C23A C25A H25C 109.5 . . ?
H25A C25A H25B 109.5 . . ?
H25A C25A H25C 109.5 . . ?
H25B C25A H25C 109.5 . . ?
O1B Ti1B O2B 158.75(5) . . ?
O1B Ti1B N1B 75.21(5) . . ?
O1B Ti1B N4B 94.80(5) . . ?
O2B Ti1B N1B 84.96(5) . . ?
O2B Ti1B N4B 75.62(5) . . ?
O3B Ti1B O1B 94.40(6) . . ?
O3B Ti1B O2B 103.09(5) . . ?
O3B Ti1B O4B 98.52(6) . . ?
O3B Ti1B N1B 163.66(5) . . ?
O3B Ti1B N4B 83.41(5) . . ?
O4B Ti1B O1B 96.69(5) . . ?
O4B Ti1B O2B 92.58(5) . . ?
O4B Ti1B N1B 95.25(5) . . ?
O4B Ti1B N4B 168.16(5) . . ?
N1B Ti1B N4B 84.91(5) . . ?
C7B O1B Ti1B 123.67(11) . . ?
C18B O2B Ti1B 122.12(9) . . ?
C23B O3B Ti1B 137.44(12) . . ?
C29B O4B Ti1B 133.8(2) . . ?
C26B O4B Ti1B 133.15(19) . . ?
C1B N1B Ti1B 126.40(10) . . ?
C1B N1B C6B 120.19(14) . . ?
C6B N1B Ti1B 111.02(10) . . ?
C1B N2B C2B 111.61(14) . . ?
C1B N2B C4B 125.12(14) . . ?
C4B N2B C2B 121.30(14) . . ?
C1B N3B C3B 109.27(13) . . ?
C1B N3B C5B 123.08(15) . . ?
C5B N3B C3B 117.49(15) . . ?
C12B N4B Ti1B 117.92(11) . . ?
C12B N4B C17B 117.94(13) . . ?
C17B N4B Ti1B 107.93(9) . . ?
C12B N5B C13B 110.39(16) . . ?
C12B N5B C15B 122.59(15) . . ?
C15B N5B C13B 119.23(17) . . ?
C12B N6B C14B 111.87(16) . . ?
C12B N6B C16B 125.17(16) . . ?
C16B N6B C14B 121.63(16) . . ?
N1B C1B N2B 122.43(14) . . ?
N1B C1B N3B 127.68(14) . . ?
N2B C1B N3B 109.88(14) . . ?
N2B C2B H2BB 111.3 . . ?
N2B C2B H2BA 111.3 . . ?
N2B C2B C3B 102.23(14) . . ?
H2BB C2B H2BA 109.2 . . ?
C3B C2B H2BB 111.3 . . ?
C3B C2B H2BA 111.3 . . ?
N3B C3B C2B 102.98(14) . . ?
N3B C3B H3BA 111.2 . . ?
N3B C3B H3BB 111.2 . . ?
C2B C3B H3BA 111.2 . . ?
C2B C3B H3BB 111.2 . . ?
H3BA C3B H3BB 109.1 . . ?
N2B C4B H4BB 109.5 . . ?
N2B C4B H4BC 109.5 . . ?
N2B C4B H4BA 109.5 . . ?
H4BB C4B H4BC 109.5 . . ?
H4BB C4B H4BA 109.5 . . ?
H4BC C4B H4BA 109.5 . . ?
N3B C5B H5BA 109.5 . . ?
N3B C5B H5BB 109.5 . . ?
N3B C5B H5BC 109.5 . . ?
H5BA C5B H5BB 109.5 . . ?
H5BA C5B H5BC 109.5 . . ?
H5BB C5B H5BC 109.5 . . ?
C7B C6B N1B 112.79(14) . . ?
C11B C6B N1B 127.39(16) . . ?
C11B C6B C7B 119.51(15) . . ?
O1B C7B C6B 117.08(14) . . ?
O1B C7B C8B 122.83(18) . . ?
C8B C7B C6B 120.08(18) . . ?
C7B C8B H8B 120.2 . . ?
C9B C8B C7B 119.6(2) . . ?
C9B C8B H8B 120.2 . . ?
C8B C9B H9B 119.7 . . ?
C10B C9B C8B 120.61(18) . . ?
C10B C9B H9B 119.7 . . ?
C9B C10B H10B 119.8 . . ?
C9B C10B C11B 120.3(2) . . ?
C11B C10B H10B 119.8 . . ?
C6B C11B C10B 119.8(2) . . ?
C6B C11B H11B 120.1 . . ?
C10B C11B H11B 120.1 . . ?
N4B C12B N5B 126.79(15) . . ?
N4B C12B N6B 123.31(16) . . ?
N6B C12B N5B 109.89(15) . . ?
N5B C13B H13C 111.0 . . ?
N5B C13B H13D 111.0 . . ?
N5B C13B C14B 103.83(17) . . ?
H13C C13B H13D 109.0 . . ?
C14B C13B H13C 111.0 . . ?
C14B C13B H13D 111.0 . . ?
N6B C14B C13B 103.21(16) . . ?
N6B C14B H14C 111.1 . . ?
N6B C14B H14D 111.1 . . ?
C13B C14B H14C 111.1 . . ?
C13B C14B H14D 111.1 . . ?
H14C C14B H14D 109.1 . . ?
N5B C15B H15E 109.5 . . ?
N5B C15B H15F 109.5 . . ?
N5B C15B H15D 109.5 . . ?
H15E C15B H15F 109.5 . . ?
H15E C15B H15D 109.5 . . ?
H15F C15B H15D 109.5 . . ?
N6B C16B H16D 109.5 . . ?
N6B C16B H16E 109.5 . . ?
N6B C16B H16F 109.5 . . ?
H16D C16B H16E 109.5 . . ?
H16D C16B H16F 109.5 . . ?
H16E C16B H16F 109.5 . . ?
C18B C17B N4B 115.21(13) . . ?
C22B C17B N4B 124.90(15) . . ?
C22B C17B C18B 119.82(15) . . ?
O2B C18B C17B 117.35(13) . . ?
O2B C18B C19B 122.78(14) . . ?
C19B C18B C17B 119.86(15) . . ?
C18B C19B H19B 120.2 . . ?
C20B C19B C18B 119.58(16) . . ?
C20B C19B H19B 120.2 . . ?
C19B C20B H20B 119.7 . . ?
C21B C20B C19B 120.58(16) . . ?
C21B C20B H20B 119.7 . . ?
C20B C21B H21B 119.8 . . ?
C20B C21B C22B 120.43(17) . . ?
C22B C21B H21B 119.8 . . ?
C17B C22B H22B 120.2 . . ?
C21B C22B C17B 119.68(17) . . ?
C21B C22B H22B 120.2 . . ?
O3B C23B H23B 108.7 . . ?
O3B C23B C24B 110.20(17) . . ?
O3B C23B C25B 108.75(17) . . ?
C24B C23B H23B 108.7 . . ?
C24B C23B C25B 111.8(2) . . ?
C25B C23B H23B 108.7 . . ?
C23B C24B H24D 109.5 . . ?
C23B C24B H24E 109.5 . . ?
C23B C24B H24F 109.5 . . ?
H24D C24B H24E 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
C23B C25B H25D 109.5 . . ?
C23B C25B H25E 109.5 . . ?
C23B C25B H25F 109.5 . . ?
H25D C25B H25E 109.5 . . ?
H25D C25B H25F 109.5 . . ?
H25E C25B H25F 109.5 . . ?
O4B C29B H29B 109.0 . . ?
O4B C29B C30B 109.5(4) . . ?
O4B C29B C31B 108.4(5) . . ?
C30B C29B H29B 109.0 . . ?
C31B C29B H29B 109.0 . . ?
C31B C29B C30B 112.0(4) . . ?
C29B C30B H30D 109.5 . . ?
C29B C30B H30E 109.5 . . ?
C29B C30B H30F 109.5 . . ?
H30D C30B H30E 109.5 . . ?
H30D C30B H30F 109.5 . . ?
H30E C30B H30F 109.5 . . ?
C29B C31B H31D 109.5 . . ?
C29B C31B H31E 109.5 . . ?
C29B C31B H31F 109.5 . . ?
H31D C31B H31E 109.5 . . ?
H31D C31B H31F 109.5 . . ?
H31E C31B H31F 109.5 . . ?
O4B C26B H26B 107.2 . . ?
O4B C26B C27B 110.1(3) . . ?
O4B C26B C28B 109.4(4) . . ?
C27B C26B H26B 107.2 . . ?
C27B C26B C28B 115.3(4) . . ?
C28B C26B H26B 107.2 . . ?
C26B C27B H27D 109.5 . . ?
C26B C27B H27E 109.5 . . ?
C26B C27B H27F 109.5 . . ?
H27D C27B H27E 109.5 . . ?
H27D C27B H27F 109.5 . . ?
H27E C27B H27F 109.5 . . ?
C26B C28B H28D 109.5 . . ?
C26B C28B H28E 109.5 . . ?
C26B C28B H28F 109.5 . . ?
H28D C28B H28E 109.5 . . ?
H28D C28B H28F 109.5 . . ?
H28E C28B H28F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ti1A O1A C7A C6A 10.14(19) . . . . ?
Ti1A O1A C7A C8A -171.64(12) . . . . ?
Ti1A O2A C18A C17A -3.0(2) . . . . ?
Ti1A O2A C18A C19A 177.50(16) . . . . ?
Ti1A O3A C29A C30A 162.2(6) . . . . ?
Ti1A O3A C29A C31A -76.2(6) . . . . ?
Ti1A O3A C23A C24A 114.9(5) . . . . ?
Ti1A O3A C23A C25A -120.8(4) . . . . ?
Ti1A O4A C26A C27A -113.84(19) . . . . ?
Ti1A O4A C26A C28A 124.08(18) . . . . ?
Ti1A N1A C1A N2A 107.35(18) . . . . ?
Ti1A N1A C1A N3A -71.9(2) . . . . ?
Ti1A N1A C6A C7A -4.78(15) . . . . ?
Ti1A N1A C6A C11A 172.56(13) . . . . ?
Ti1A N4A C12A N5A -115.13(17) . . . . ?
Ti1A N4A C12A N6A 63.0(2) . . . . ?
Ti1A N4A C17A C18A -3.45(17) . . . . ?
Ti1A N4A C17A C22A -178.41(14) . . . . ?
O1A Ti1A O3A C29A -129.5(3) . . . . ?
O1A Ti1A O3A C23A -173.7(5) . . . . ?
O1A Ti1A O4A C26A -140.66(15) . . . . ?
O1A C7A C8A C9A -178.41(15) . . . . ?
O2A Ti1A O3A C29A 32.7(4) . . . . ?
O2A Ti1A O3A C23A -11.5(5) . . . . ?
O2A Ti1A O4A C26A 54.35(16) . . . . ?
O2A C18A C19A C20A 179.3(2) . . . . ?
O3A Ti1A O4A C26A -44.09(16) . . . . ?
O4A Ti1A O3A C29A 127.1(3) . . . . ?
O4A Ti1A O3A C23A 82.9(5) . . . . ?
N1A Ti1A O3A C29A -131.7(4) . . . . ?
N1A Ti1A O3A C23A -175.9(5) . . . . ?
N1A Ti1A O4A C26A 146.54(16) . . . . ?
N1A C6A C7A O1A -1.8(2) . . . . ?
N1A C6A C7A C8A 179.94(14) . . . . ?
N1A C6A C11A C10A -179.90(16) . . . . ?
N2A C2A C3A N3A 17.6(2) . . . . ?
N4A Ti1A O3A C29A -43.0(3) . . . . ?
N4A Ti1A O3A C23A -87.2(5) . . . . ?
N4A Ti1A O4A C26A 98.8(2) . . . . ?
N4A C17A C18A O2A 4.2(2) . . . . ?
N4A C17A C18A C19A -176.24(18) . . . . ?
N4A C17A C22A C21A 175.92(17) . . . . ?
N5A C13A C14A N6A -22.56(19) . . . . ?
C1A N1A C6A C7A 134.91(16) . . . . ?
C1A N1A C6A C11A -47.8(2) . . . . ?
C1A N2A C2A C3A -16.7(2) . . . . ?
C1A N3A C3A C2A -13.9(2) . . . . ?
C2A N2A C1A N1A -170.79(18) . . . . ?
C2A N2A C1A N3A 8.6(2) . . . . ?
C3A N3A C1A N1A -176.69(18) . . . . ?
C3A N3A C1A N2A 3.9(2) . . . . ?
C4A N2A C1A N1A -28.8(3) . . . . ?
C4A N2A C1A N3A 150.54(19) . . . . ?
C4A N2A C2A C3A -161.34(18) . . . . ?
C5A N3A C1A N1A -19.6(3) . . . . ?
C5A N3A C1A N2A 160.97(19) . . . . ?
C5A N3A C3A C2A -172.3(2) . . . . ?
C6A N1A C1A N2A -26.9(3) . . . . ?
C6A N1A C1A N3A 153.83(17) . . . . ?
C6A C7A C8A C9A -0.2(2) . . . . ?
C7A C6A C11A C10A -2.7(2) . . . . ?
C7A C8A C9A C10A -1.8(3) . . . . ?
C8A C9A C10A C11A 1.5(3) . . . . ?
C9A C10A C11A C6A 0.7(3) . . . . ?
C11A C6A C7A O1A -179.31(14) . . . . ?
C11A C6A C7A C8A 2.4(2) . . . . ?
C12A N4A C17A C18A -160.08(16) . . . . ?
C12A N4A C17A C22A 25.0(2) . . . . ?
C12A N5A C13A C14A 22.73(19) . . . . ?
C12A N6A C14A C13A 16.1(2) . . . . ?
C13A N5A C12A N4A 164.89(16) . . . . ?
C13A N5A C12A N6A -13.47(19) . . . . ?
C14A N6A C12A N4A 179.26(16) . . . . ?
C14A N6A C12A N5A -2.3(2) . . . . ?
C15A N5A C12A N4A 23.9(3) . . . . ?
C15A N5A C12A N6A -154.49(17) . . . . ?
C15A N5A C13A C14A 165.73(16) . . . . ?
C16A N6A C12A N4A 17.4(3) . . . . ?
C16A N6A C12A N5A -164.12(17) . . . . ?
C16A N6A C14A C13A 178.76(18) . . . . ?
C17A N4A C12A N5A 38.1(2) . . . . ?
C17A N4A C12A N6A -143.74(16) . . . . ?
C17A C18A C19A C20A -0.2(3) . . . . ?
C18A C17A C22A C21A 1.3(3) . . . . ?
C18A C19A C20A C21A 1.0(4) . . . . ?
C19A C20A C21A C22A -0.7(4) . . . . ?
C20A C21A C22A C17A -0.4(3) . . . . ?
C22A C17A C18A O2A 179.51(16) . . . . ?
C22A C17A C18A C19A -1.0(3) . . . . ?
Ti1B O1B C7B C6B 5.2(2) . . . . ?
Ti1B O1B C7B C8B -173.84(14) . . . . ?
Ti1B O2B C18B C17B -14.80(18) . . . . ?
Ti1B O2B C18B C19B 165.96(12) . . . . ?
Ti1B O3B C23B C24B 87.5(2) . . . . ?
Ti1B O3B C23B C25B -149.65(17) . . . . ?
Ti1B O4B C29B C30B -152.4(3) . . . . ?
Ti1B O4B C29B C31B 85.1(5) . . . . ?
Ti1B O4B C26B C27B 138.8(3) . . . . ?
Ti1B O4B C26B C28B -93.6(5) . . . . ?
Ti1B N1B C1B N2B -59.47(19) . . . . ?
Ti1B N1B C1B N3B 119.75(16) . . . . ?
Ti1B N1B C6B C7B 3.52(16) . . . . ?
Ti1B N1B C6B C11B 177.02(15) . . . . ?
Ti1B N4B C12B N5B -103.32(18) . . . . ?
Ti1B N4B C12B N6B 75.77(19) . . . . ?
Ti1B N4B C17B C18B 4.21(16) . . . . ?
Ti1B N4B C17B C22B -172.70(14) . . . . ?
O1B Ti1B O3B C23B -63.56(17) . . . . ?
O1B Ti1B O4B C29B -36.9(3) . . . . ?
O1B Ti1B O4B C26B 11.2(3) . . . . ?
O1B C7B C8B C9B 179.08(19) . . . . ?
O2B Ti1B O3B C23B 128.58(17) . . . . ?
O2B Ti1B O4B C29B 124.0(3) . . . . ?
O2B Ti1B O4B C26B 172.0(3) . . . . ?
O2B C18B C19B C20B 178.48(15) . . . . ?
O3B Ti1B O4B C29B -132.4(3) . . . . ?
O3B Ti1B O4B C26B -84.3(3) . . . . ?
O4B Ti1B O3B C23B 33.90(18) . . . . ?
N1B Ti1B O3B C23B -113.2(2) . . . . ?
N1B Ti1B O4B C29B 38.8(3) . . . . ?
N1B Ti1B O4B C26B 86.9(3) . . . . ?
N1B C6B C7B O1B -5.5(2) . . . . ?
N1B C6B C7B C8B 173.57(16) . . . . ?
N1B C6B C11B C10B -172.64(18) . . . . ?
N2B C2B C3B N3B 18.95(18) . . . . ?
N4B Ti1B O3B C23B -157.89(17) . . . . ?
N4B Ti1B O4B C29B 129.0(4) . . . . ?
N4B Ti1B O4B C26B 177.1(3) . . . . ?
N4B C17B C18B O2B 5.2(2) . . . . ?
N4B C17B C18B C19B -175.55(14) . . . . ?
N4B C17B C22B C21B 176.27(16) . . . . ?
N5B C13B C14B N6B -8.6(3) . . . . ?
C1B N1B C6B C7B 167.05(14) . . . . ?
C1B N1B C6B C11B -19.4(2) . . . . ?
C1B N2B C2B C3B -14.14(19) . . . . ?
C1B N3B C3B C2B -18.81(19) . . . . ?
C2B N2B C1B N1B -177.93(15) . . . . ?
C2B N2B C1B N3B 2.73(19) . . . . ?
C3B N3B C1B N1B -168.55(16) . . . . ?
C3B N3B C1B N2B 10.74(19) . . . . ?
C4B N2B C1B N1B -13.8(2) . . . . ?
C4B N2B C1B N3B 166.85(15) . . . . ?
C4B N2B C2B C3B -178.95(15) . . . . ?
C5B N3B C1B N1B -24.3(3) . . . . ?
C5B N3B C1B N2B 154.97(16) . . . . ?
C5B N3B C3B C2B -165.29(15) . . . . ?
C6B N1B C1B N2B 139.73(15) . . . . ?
C6B N1B C1B N3B -41.1(2) . . . . ?
C6B C7B C8B C9B 0.1(3) . . . . ?
C7B C6B C11B C10B 0.5(3) . . . . ?
C7B C8B C9B C10B 0.3(4) . . . . ?
C8B C9B C10B C11B -0.4(4) . . . . ?
C9B C10B C11B C6B 0.0(3) . . . . ?
C11B C6B C7B O1B -179.54(15) . . . . ?
C11B C6B C7B C8B -0.5(3) . . . . ?
C12B N4B C17B C18B -132.56(15) . . . . ?
C12B N4B C17B C22B 50.5(2) . . . . ?
C12B N5B C13B C14B 8.5(3) . . . . ?
C12B N6B C14B C13B 6.4(3) . . . . ?
C13B N5B C12B N4B 174.34(19) . . . . ?
C13B N5B C12B N6B -4.8(2) . . . . ?
C14B N6B C12B N4B 179.52(18) . . . . ?
C14B N6B C12B N5B -1.3(2) . . . . ?
C15B N5B C12B N4B 25.5(3) . . . . ?
C15B N5B C12B N6B -153.72(19) . . . . ?
C15B N5B C13B C14B 158.5(2) . . . . ?
C16B N6B C12B N4B 12.6(3) . . . . ?
C16B N6B C12B N5B -168.20(19) . . . . ?
C16B N6B C14B C13B 173.8(2) . . . . ?
C17B N4B C12B N5B 29.2(3) . . . . ?
C17B N4B C12B N6B -151.76(16) . . . . ?
C17B C18B C19B C20B -0.7(2) . . . . ?
C18B C17B C22B C21B -0.5(3) . . . . ?
C18B C19B C20B C21B -1.1(3) . . . . ?
C19B C20B C21B C22B 2.1(3) . . . . ?
C20B C21B C22B C17B -1.3(3) . . . . ?
C22B C17B C18B O2B -177.74(15) . . . . ?
C22B C17B C18B C19B 1.5(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
