# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 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. 
# 
#######################################################################

data_FIR-117
_database_code_depnum_ccdc_archive 'CCDC 2287493'
loop_
_audit_author_name
_audit_author_address
'Fei Wang'
;fujian institute
China
;
_audit_update_record             
;
2023-08-08 deposited with the CCDC.	2024-04-15 downloaded from the CCDC.
;
_audit_creation_date             2023-03-25
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H3 O9 Ti, C4 H12 N'
_chemical_formula_sum            'C16 H15 N O9 Ti'
_chemical_formula_weight         413.19
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ti C H O '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0137 0.0067 '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 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.3343 1.4243 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.1764(4)
_cell_length_b                   11.4887(4)
_cell_length_c                   13.5180(4)
_cell_angle_alpha                92.861(3)
_cell_angle_beta                 102.938(3)
_cell_angle_gamma                110.782(3)
_cell_volume                     1425.53(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    14236
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      60.4080
_cell_measurement_theta_min      2.9480
_shelx_estimated_absorpt_T_max   0.832
_shelx_estimated_absorpt_T_min   0.701
_exptl_absorpt_coefficient_mu    1.912
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.963
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.2
_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  0.0562
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29574
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.465
_diffrn_reflns_theta_min         3.614
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -112.00 -20.00   0.50    0.20    --  -75.07 125.00 120.00  184
  2  ω   -112.00 -20.00   0.50    0.20    --  -75.07 125.00-180.00  184
  3  ω     56.00 145.00   0.50    0.20    --   72.25  57.00-180.00  178
  4  ω     49.00 145.00   0.50    0.20    --   72.25  77.00   0.00  192
  5  ω     57.00 147.00   0.50    0.20    --   72.25  30.00 102.00  180
  6  ω   -112.00 -20.00   0.50    0.20    --  -75.07 125.00 150.00  184
  7  ω    -99.00  -2.00   0.50    0.20    --  -75.07  77.00  90.00  194
  8  ω    -99.00  -2.00   0.50    0.20    --  -75.07  77.00 120.00  194
  9  ω    -99.00  -2.00   0.50    0.20    --  -75.07  77.00 150.00  194
 10  ω    -69.00   0.00   0.50    0.20    --  -75.07  30.00 102.00  138
 11  ω    -71.00  -1.00   0.50    0.20    --  -75.07  38.00-150.00  140
 12  ω    -25.00  72.00   0.50    0.15    --   -1.41  77.00  90.00  194
 13  ω    -16.00  73.00   0.50    0.15    --   -1.41  30.00 102.00  178
 14  ω    -16.00  72.00   0.50    0.15    --   -1.41  38.00 -60.00  176
 15  ω    -25.00  72.00   0.50    0.15    --   -1.41  77.00-180.00  194
 16  ω     -1.00  89.00   0.50    0.20    --   72.25 -57.00 -30.00  180
 17  ω     -1.00  89.00   0.50    0.20    --   72.25 -57.00 -60.00  180
 18  ω     -2.00  69.00   0.50    0.20    --   72.25 -30.00 -58.00  142
 19  ω     20.00 111.00   0.50    0.20    --   72.25-125.00 -60.00  182
 20  ω     -1.00 106.00   0.50    0.20    --   72.25 -99.00 -60.00  214
 21  ω    -76.00  14.00   0.50    0.15    --   -1.41 -30.00 -58.00  180
 22  ω    -74.00  22.00   0.50    0.15    --   -1.41 -77.00   0.00  192
 23  ω    -75.00  13.00   0.50    0.15    --   -1.41 -38.00 120.00  176
 24  ω   -150.00 -60.00   0.50    0.20    --  -75.07 -30.00 -58.00  180
 25  ω   -148.00 -79.00   0.50    0.20    --  -75.07-125.00  90.00  138
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0252247000
_diffrn_orient_matrix_UB_12      0.1096809000
_diffrn_orient_matrix_UB_13      -0.0369221000
_diffrn_orient_matrix_UB_21      -0.1406542000
_diffrn_orient_matrix_UB_22      -0.0173346000
_diffrn_orient_matrix_UB_23      -0.0149513000
_diffrn_orient_matrix_UB_31      0.0285264000
_diffrn_orient_matrix_UB_32      0.0594470000
_diffrn_orient_matrix_UB_33      0.0946468000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ga k\a'
_diffrn_radiation_wavelength     1.3405
_diffrn_source                   'micro-focus metaljet'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4434
_reflns_number_total             6364
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         6364
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0741
_refine_ls_restrained_S_all      1.078
_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)+(0.1667P)²+0.1116P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2302
_refine_ls_wR_factor_ref         0.2479
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C14, N1, C13, C15, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C14 \\sim N1 \\sim C13 \\sim C15 \\sim C16: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 1.7A
Uanis(C16) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C13(H13A,H13B), C14(H14A,H14B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C8(H8), C11(H11)
4.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.73808(6) 0.84263(5) 0.69952(4) 0.0459(2) Uani 1 1 d . . . . .
O3 O 0.7293(2) 0.69625(19) 0.62721(16) 0.0464(5) Uani 1 1 d . . . . .
O6 O 0.8308(2) 0.82486(19) 0.83151(16) 0.0471(5) Uani 1 1 d . . . . .
O4 O 0.7137(3) 0.9887(2) 0.77048(16) 0.0521(6) Uani 1 1 d . . . . .
O1 O 0.5365(2) 0.7401(2) 0.70727(16) 0.0488(5) Uani 1 1 d . . . . .
O9 O 0.9171(2) 0.9417(2) 0.67740(16) 0.0477(5) Uani 1 1 d . . . . .
O7 O 0.6467(2) 0.8906(2) 0.56817(17) 0.0539(6) Uani 1 1 d . . . . .
O5 O 0.7743(3) 1.1641(2) 0.87413(18) 0.0685(8) Uani 1 1 d . . . . .
O2 O 0.3246(3) 0.5867(3) 0.6824(2) 0.0741(8) Uani 1 1 d . . . . .
C2 C 0.4744(3) 0.5655(3) 0.5787(2) 0.0420(7) Uani 1 1 d . . . . .
C3 C 0.6146(3) 0.6011(3) 0.5652(2) 0.0398(6) Uani 1 1 d . . . . .
C4 C 0.6391(3) 0.5361(3) 0.4858(2) 0.0419(7) Uani 1 1 d . . . . .
H4 H 0.734046 0.561271 0.475491 0.050 Uiso 1 1 calc R U . . .
C7 C 0.9130(3) 0.9122(3) 0.9124(2) 0.0399(6) Uani 1 1 d . . . . .
N1 N 0.3309(4) 0.7736(3) 0.3181(3) 0.0704(9) Uani 1 1 d . U . . .
H1A H 0.314567 0.801231 0.256334 0.084 Uiso 1 1 calc R U . . .
H1B H 0.417855 0.829362 0.357317 0.084 Uiso 1 1 calc R U . . .
C5 C 0.7889(4) 1.0628(3) 0.8549(2) 0.0494(8) Uani 1 1 d . . . . .
C1 C 0.4404(4) 0.6327(3) 0.6605(2) 0.0486(7) Uani 1 1 d . . . . .
C9 C 0.9552(3) 0.9700(3) 0.5902(2) 0.0477(7) Uani 1 1 d . . . . .
O8 O 0.6102(3) 0.9196(4) 0.4068(2) 0.1062(13) Uani 1 1 d . . . . .
C6 C 0.8976(3) 1.0288(3) 0.9277(2) 0.0405(6) Uani 1 1 d . . . . .
C8 C 1.0137(3) 0.8857(3) 0.9857(2) 0.0439(7) Uani 1 1 d . . . . .
H8 H 1.022307 0.806428 0.976499 0.053 Uiso 1 1 calc R U . . .
C11 C 0.8990(4) 0.9877(3) 0.4098(2) 0.0514(8) Uani 1 1 d . . . . .
H11 H 0.829185 0.978914 0.347198 0.062 Uiso 1 1 calc R U . . .
C10 C 0.8504(4) 0.9577(3) 0.4965(2) 0.0528(8) Uani 1 1 d . . . . .
C12 C 0.6926(4) 0.9188(4) 0.4897(3) 0.0644(10) Uani 1 1 d . . . . .
C13 C 0.2139(6) 0.7780(5) 0.3684(5) 0.0882(14) Uani 1 1 d . U . . .
H13A H 0.209189 0.862619 0.368527 0.106 Uiso 1 1 calc R U . . .
H13B H 0.118516 0.716060 0.328145 0.106 Uiso 1 1 calc R U . . .
C15 C 0.2405(7) 0.7521(6) 0.4672(5) 0.1049(17) Uani 1 1 d . U . . .
H15A H 0.203515 0.660813 0.466849 0.157 Uiso 1 1 calc R U . . .
H15B H 0.191461 0.789367 0.506385 0.157 Uiso 1 1 calc R U . . .
H15C H 0.345514 0.787620 0.498934 0.157 Uiso 1 1 calc R U . . .
C14 C 0.3452(9) 0.6548(6) 0.3014(5) 0.122(2) Uani 1 1 d . U . . .
H14A H 0.380438 0.631638 0.368956 0.147 Uiso 1 1 calc R U . . .
H14B H 0.247246 0.590502 0.269116 0.147 Uiso 1 1 calc R U . . .
C16 C 0.4371(12) 0.6491(10) 0.2411(6) 0.174(4) Uani 1 1 d . U . . .
H16A H 0.379059 0.604929 0.172509 0.261 Uiso 1 1 calc R U . . .
H16B H 0.497423 0.603745 0.272450 0.261 Uiso 1 1 calc R U . . .
H16C H 0.499844 0.734556 0.235613 0.261 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 1.866(2) . ?
Ti1 O6 1.880(2) . ?
Ti1 O4 2.010(2) . ?
Ti1 O1 2.000(2) . ?
Ti1 O9 1.874(2) . ?
Ti1 O7 2.011(2) . ?
O3 C3 1.351(3) . ?
O6 C7 1.337(3) . ?
O4 C5 1.290(3) . ?
O1 C1 1.292(4) . ?
O9 C9 1.341(4) . ?
O7 C12 1.264(5) . ?
O5 C5 1.247(4) . ?
O2 C1 1.218(4) . ?
C2 C3 1.395(4) . ?
C2 C4 1.396(4) 2_666 ?
C2 C1 1.489(4) . ?
C3 C4 1.394(4) . ?
C4 H4 0.9500 . ?
C7 C6 1.413(4) . ?
C7 C8 1.387(4) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 C13 1.511(6) . ?
N1 C14 1.434(6) . ?
C5 C6 1.483(4) . ?
C9 C11 1.387(5) 2_776 ?
C9 C10 1.426(4) . ?
O8 C12 1.243(4) . ?
C6 C8 1.390(4) 2_777 ?
C8 H8 0.9500 . ?
C11 H11 0.9500 . ?
C11 C10 1.385(5) . ?
C10 C12 1.485(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C15 1.371(8) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C16 1.387(9) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 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 O6 98.97(9) . . ?
O3 Ti1 O4 171.10(9) . . ?
O3 Ti1 O1 85.31(9) . . ?
O3 Ti1 O9 93.92(10) . . ?
O3 Ti1 O7 90.09(10) . . ?
O6 Ti1 O4 85.27(8) . . ?
O6 Ti1 O1 95.48(10) . . ?
O6 Ti1 O7 170.69(9) . . ?
O1 Ti1 O4 86.50(10) . . ?
O1 Ti1 O7 87.38(10) . . ?
O9 Ti1 O6 91.06(10) . . ?
O9 Ti1 O4 93.82(10) . . ?
O9 Ti1 O1 173.45(9) . . ?
O9 Ti1 O7 86.12(10) . . ?
O7 Ti1 O4 86.06(9) . . ?
C3 O3 Ti1 130.46(19) . . ?
C7 O6 Ti1 130.01(18) . . ?
C5 O4 Ti1 131.4(2) . . ?
C1 O1 Ti1 133.9(2) . . ?
C9 O9 Ti1 130.77(19) . . ?
C12 O7 Ti1 131.0(2) . . ?
C3 C2 C4 119.8(3) . 2_666 ?
C3 C2 C1 122.1(3) . . ?
C4 C2 C1 118.0(3) 2_666 . ?
O3 C3 C2 122.3(3) . . ?
O3 C3 C4 118.2(3) . . ?
C4 C3 C2 119.5(3) . . ?
C2 C4 H4 119.7 2_666 . ?
C3 C4 C2 120.7(3) . 2_666 ?
C3 C4 H4 119.7 . . ?
O6 C7 C6 122.5(3) . . ?
O6 C7 C8 118.7(2) . . ?
C8 C7 C6 118.7(2) . . ?
H1A N1 H1B 107.2 . . ?
C13 N1 H1A 107.9 . . ?
C13 N1 H1B 107.9 . . ?
C14 N1 H1A 107.9 . . ?
C14 N1 H1B 107.9 . . ?
C14 N1 C13 117.8(4) . . ?
O4 C5 C6 119.4(3) . . ?
O5 C5 O4 120.5(3) . . ?
O5 C5 C6 120.0(3) . . ?
O1 C1 C2 118.2(3) . . ?
O2 C1 O1 121.4(3) . . ?
O2 C1 C2 120.4(3) . . ?
O9 C9 C11 119.5(3) . 2_776 ?
O9 C9 C10 122.1(3) . . ?
C11 C9 C10 118.4(3) 2_776 . ?
C7 C6 C5 122.2(2) . . ?
C8 C6 C7 119.0(3) 2_777 . ?
C8 C6 C5 118.8(3) 2_777 . ?
C7 C8 C6 122.2(3) . 2_777 ?
C7 C8 H8 118.9 . . ?
C6 C8 H8 118.9 2_777 . ?
C9 C11 H11 118.4 2_776 . ?
C10 C11 C9 123.2(3) . 2_776 ?
C10 C11 H11 118.4 . . ?
C9 C10 C12 122.5(3) . . ?
C11 C10 C9 118.3(3) . . ?
C11 C10 C12 119.2(3) . . ?
O7 C12 C10 119.8(3) . . ?
O8 C12 O7 122.0(4) . . ?
O8 C12 C10 118.2(4) . . ?
N1 C13 H13A 109.3 . . ?
N1 C13 H13B 109.3 . . ?
H13A C13 H13B 108.0 . . ?
C15 C13 N1 111.6(5) . . ?
C15 C13 H13A 109.3 . . ?
C15 C13 H13B 109.3 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C14 H14A 108.2 . . ?
N1 C14 H14B 108.2 . . ?
H14A C14 H14B 107.3 . . ?
C16 C14 N1 116.4(7) . . ?
C16 C14 H14A 108.2 . . ?
C16 C14 H14B 108.2 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 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 C3 C2 -30.3(4) . . . . ?
Ti1 O3 C3 C4 150.4(2) . . . . ?
Ti1 O6 C7 C6 27.3(4) . . . . ?
Ti1 O6 C7 C8 -155.0(2) . . . . ?
Ti1 O4 C5 O5 164.1(3) . . . . ?
Ti1 O4 C5 C6 -13.6(5) . . . . ?
Ti1 O1 C1 O2 176.8(2) . . . . ?
Ti1 O1 C1 C2 -3.0(5) . . . . ?
Ti1 O9 C9 C11 -160.3(2) . . . 2_776 ?
Ti1 O9 C9 C10 19.5(4) . . . . ?
Ti1 O7 C12 O8 164.0(3) . . . . ?
Ti1 O7 C12 C10 -18.7(5) . . . . ?
O3 Ti1 O6 C7 154.6(3) . . . . ?
O3 Ti1 O9 C9 61.5(3) . . . . ?
O3 C3 C4 C2 178.0(3) . . . 2_666 ?
O6 Ti1 O3 C3 125.3(3) . . . . ?
O6 Ti1 O9 C9 160.6(3) . . . . ?
O6 C7 C6 C5 -0.1(5) . . . . ?
O6 C7 C6 C8 179.4(3) . . . 2_777 ?
O6 C7 C8 C6 -179.5(3) . . . 2_777 ?
O4 Ti1 O6 C7 -33.3(3) . . . . ?
O4 Ti1 O9 C9 -114.1(2) . . . . ?
O4 C5 C6 C7 -5.8(5) . . . . ?
O4 C5 C6 C8 174.7(3) . . . 2_777 ?
O1 Ti1 O3 C3 30.5(3) . . . . ?
O1 Ti1 O6 C7 -119.3(3) . . . . ?
O9 Ti1 O3 C3 -143.0(3) . . . . ?
O9 Ti1 O6 C7 60.4(3) . . . . ?
O9 C9 C10 C11 -179.3(3) . . . . ?
O9 C9 C10 C12 3.0(5) . . . . ?
O7 Ti1 O3 C3 -56.8(3) . . . . ?
O7 Ti1 O9 C9 -28.3(3) . . . . ?
O5 C5 C6 C7 176.5(3) . . . . ?
O5 C5 C6 C8 -3.0(5) . . . 2_777 ?
C2 C3 C4 C2 -1.3(5) . . . 2_666 ?
C3 C2 C1 O1 13.1(5) . . . . ?
C3 C2 C1 O2 -166.7(3) . . . . ?
C4 C2 C3 O3 -177.9(3) 2_666 . . . ?
C4 C2 C3 C4 1.3(5) 2_666 . . . ?
C4 C2 C1 O1 -166.9(3) 2_666 . . . ?
C4 C2 C1 O2 13.3(5) 2_666 . . . ?
C1 C2 C3 O3 2.1(5) . . . . ?
C1 C2 C3 C4 -178.7(3) . . . . ?
C9 C11 C10 C9 -0.5(5) 2_776 . . . ?
C9 C11 C10 C12 177.3(3) 2_776 . . . ?
C9 C10 C12 O7 -2.7(5) . . . . ?
C9 C10 C12 O8 174.7(4) . . . . ?
C6 C7 C8 C6 -1.7(5) . . . 2_777 ?
C8 C7 C6 C5 -177.8(3) . . . . ?
C8 C7 C6 C8 1.7(5) . . . 2_777 ?
C11 C9 C10 C11 0.5(5) 2_776 . . . ?
C11 C9 C10 C12 -177.2(3) 2_776 . . . ?
C11 C10 C12 O7 179.7(3) . . . . ?
C11 C10 C12 O8 -3.0(6) . . . . ?
C13 N1 C14 C16 170.2(7) . . . . ?
C14 N1 C13 C15 65.0(6) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.131 -0.319 -0.586 710.7 165.7 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.549
_oxdiff_exptl_absorpt_empirical_full_min 0.680
####################################################################### 
# 
# 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_FIR-119
_database_code_depnum_ccdc_archive 'CCDC 2287495'
loop_
_audit_author_name
_audit_author_address
'Fei Wang'
;fujian institute
China
;
_audit_update_record             
;
2023-08-08 deposited with the CCDC.	2024-04-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT026_FIR-119             
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        28% Check
RESPONSE: weak diffraction at high 2theta angle
;
_vrf_PLAT029_FIR-119             
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.938 Why?
RESPONSE: weak diffraction at high 2theta angle
;
# Added during the CSD deposition process: Tuesday 08 August 2023 09:53 AM
# end Validation Reply Form

_audit_creation_date             2023-03-29
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H3 O9 Ti1'
_chemical_formula_sum            'C12 H3 O9 Ti'
_chemical_formula_weight         339.04
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ti C H O '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0147 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.3614 1.4656 '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      cubic
_space_group_IT_number           220
_space_group_name_H-M_alt        'I -4 3 d'
_space_group_name_Hall           'I -4bd 2c 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+1/4, x+1/4, z+1/4'
'-y+1/4, -x+3/4, z+3/4'
'y+3/4, -x+1/4, -z+3/4'
'-y+3/4, x+3/4, -z+1/4'
'x+1/4, z+1/4, y+1/4'
'-x+3/4, z+3/4, -y+1/4'
'-x+1/4, -z+3/4, y+3/4'
'x+3/4, -z+1/4, -y+3/4'
'z+1/4, y+1/4, x+1/4'
'z+3/4, -y+1/4, -x+3/4'
'-z+3/4, y+3/4, -x+1/4'
'-z+1/4, -y+3/4, x+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'y+3/4, x+3/4, z+3/4'
'-y+3/4, -x+5/4, z+5/4'
'y+5/4, -x+3/4, -z+5/4'
'-y+5/4, x+5/4, -z+3/4'
'x+3/4, z+3/4, y+3/4'
'-x+5/4, z+5/4, -y+3/4'
'-x+3/4, -z+5/4, y+5/4'
'x+5/4, -z+3/4, -y+5/4'
'z+3/4, y+3/4, x+3/4'
'z+5/4, -y+3/4, -x+5/4'
'-z+5/4, y+5/4, -x+3/4'
'-z+3/4, -y+5/4, x+5/4'

_cell_length_a                   21.8295(8)
_cell_length_b                   21.8295(8)
_cell_length_c                   21.8295(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10402.3(11)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    1175
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      36.9720
_cell_measurement_theta_min      4.3120
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.941
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.866
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2704
_exptl_crystal_preparation       ?
_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  0.0277
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.938
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5268
_diffrn_reflns_point_group_measured_fraction_full 0.874
_diffrn_reflns_point_group_measured_fraction_max 0.833
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         58.430
_diffrn_reflns_theta_min         4.982
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    104.00 132.00   0.50   12.45    --   63.90 109.00 -90.00   56
  2  ω   -116.00 -82.00   0.50   12.45    --  -66.71 -84.00 -55.00   68
  3  ω    -26.00   8.00   0.50    3.11    --   -1.41  84.00  63.00   68
  4  ω   -132.00-100.00   0.50   12.45    --  -66.71 -99.00-150.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0050510000
_diffrn_orient_matrix_UB_12      -0.0538969000
_diffrn_orient_matrix_UB_13      0.0288810000
_diffrn_orient_matrix_UB_21      0.0611084000
_diffrn_orient_matrix_UB_22      -0.0037152000
_diffrn_orient_matrix_UB_23      0.0036968000
_diffrn_orient_matrix_UB_31      -0.0016591000
_diffrn_orient_matrix_UB_32      0.0290649000
_diffrn_orient_matrix_UB_33      0.0540028000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_source                   'micro-focus metaljet'
_reflns_Friedel_coverage         0.677
_reflns_Friedel_fraction_full    0.797
_reflns_Friedel_fraction_max     0.731
_reflns_number_gt                440
_reflns_number_total             1560
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.160
_refine_diff_density_min         -0.124
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         1560
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1609
_refine_ls_R_factor_gt           0.0798
_refine_ls_restrained_S_all      0.982
_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)+(0.1385P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2334
_refine_ls_wR_factor_ref         0.2863
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.68147(10) 0.68147(10) 0.68147(10) 0.2128(19) Uani 1 3 d S T P . .
O1 O 0.7682(3) 0.7058(5) 0.6710(5) 0.238(4) Uani 1 1 d . . . . .
O3 O 0.6725(4) 0.6956(3) 0.5968(5) 0.223(3) Uani 1 1 d . . . . .
O2 O 0.8569(6) 0.7155(5) 0.6249(4) 0.276(5) Uani 1 1 d . . . . .
C3 C 0.6868(5) 0.7009(4) 0.4941(7) 0.185(3) Uani 1 1 d . . . . .
H3 H 0.643740 0.703537 0.488560 0.222 Uiso 1 1 calc R U . . .
C2 C 0.7086(6) 0.6994(5) 0.5519(8) 0.199(4) Uani 1 1 d . . . . .
C1 C 0.7747(5) 0.6985(5) 0.5602(8) 0.214(4) Uani 1 1 d . . . . .
C4 C 0.8022(8) 0.7087(7) 0.6168(8) 0.234(6) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O1 1.980(8) 9 ?
Ti1 O1 1.980(8) 5 ?
Ti1 O1 1.980(9) . ?
Ti1 O3 1.884(10) 9 ?
Ti1 O3 1.884(10) . ?
Ti1 O3 1.884(10) 5 ?
O1 C4 1.398(14) . ?
O3 C2 1.261(12) . ?
O2 C4 1.216(15) . ?
C3 H3 0.9500 . ?
C3 C2 1.347(14) . ?
C3 C1 1.455(15) 27_645 ?
C2 C1 1.455(14) . ?
C1 C4 1.392(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 O1 83.4(4) 9 . ?
O1 Ti1 O1 83.4(4) 5 9 ?
O1 Ti1 O1 83.4(4) 5 . ?
O3 Ti1 O1 170.1(4) . 9 ?
O3 Ti1 O1 95.5(4) 5 9 ?
O3 Ti1 O1 170.1(4) 5 . ?
O3 Ti1 O1 86.7(4) 9 9 ?
O3 Ti1 O1 86.7(4) 5 5 ?
O3 Ti1 O1 95.5(4) 9 . ?
O3 Ti1 O1 95.5(4) . 5 ?
O3 Ti1 O1 86.7(4) . . ?
O3 Ti1 O1 170.1(4) 9 5 ?
O3 Ti1 O3 94.3(4) 9 5 ?
O3 Ti1 O3 94.3(4) . 5 ?
O3 Ti1 O3 94.3(4) . 9 ?
C4 O1 Ti1 128.1(9) . . ?
C2 O3 Ti1 135.2(9) . . ?
C2 C3 H3 118.0 . . ?
C2 C3 C1 124.0(12) . 27_645 ?
C1 C3 H3 118.0 27_645 . ?
O3 C2 C3 120.6(12) . . ?
O3 C2 C1 121.4(15) . . ?
C3 C2 C1 117.9(14) . . ?
C2 C1 C3 118.0(14) . 27_645 ?
C4 C1 C3 117.9(11) . 27_645 ?
C4 C1 C2 122.6(16) . . ?
O2 C4 O1 113.9(15) . . ?
O2 C4 C1 124.9(13) . . ?
C1 C4 O1 121.0(14) . . ?

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 C4 O2 -168.7(10) . . . . ?
Ti1 O1 C4 C1 5.5(18) . . . . ?
Ti1 O3 C2 C3 169.8(7) . . . . ?
Ti1 O3 C2 C1 -6.2(18) . . . . ?
O1 Ti1 O3 C2 19.2(11) . . . . ?
O1 Ti1 O3 C2 102.2(11) 5 . . . ?
O3 Ti1 O3 C2 -76.0(13) 9 . . . ?
O3 Ti1 O3 C2 -170.7(11) 5 . . . ?
O3 C2 C1 C3 177.7(10) . . . 27_645 ?
O3 C2 C1 C4 -16.4(17) . . . . ?
C3 C2 C1 C3 1.6(14) . . . 27_645 ?
C3 C2 C1 C4 167.5(12) . . . . ?
C3 C1 C4 O1 -178.6(11) 27_645 . . . ?
C3 C1 C4 O2 -5(2) 27_645 . . . ?
C2 C1 C4 O1 15.5(18) . . . . ?
C2 C1 C4 O2 -170.9(14) . . . . ?
C1 C3 C2 O3 -173.0(10) 27_645 . . . ?
C1 C3 C2 C1 3.1(14) 27_645 . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.512 -0.332 -0.046 6597.2 1806.9 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
# end Validation Reply Form
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.457
_oxdiff_exptl_absorpt_empirical_full_min 0.706
# start Validation Reply Form
_vrf_PLAT026_hz-17-7-24_auto     
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        28% Check 
RESPONSE: weak diffraction at high 2theta angle
;
_vrf_PLAT029_hz-17-7-24_auto     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.938 Why?  
RESPONSE: weak diffraction at high 2theta angle
;
####################################################################### 
# 
# 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_FIR-118
_database_code_depnum_ccdc_archive 'CCDC 2287494'
loop_
_audit_author_name
_audit_author_address
'Fei Wang'
;fujian institute
China
;
_audit_update_record             
;
2023-08-08 deposited with the CCDC.	2024-04-15 downloaded from the CCDC.
;
_audit_creation_date             2023-08-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H3 O9 Ti, C4 H12 N'
_chemical_formula_sum            'C16 H15 N O9 Ti'
_chemical_formula_weight         413.19
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ti C H O '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0137 0.0067 '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 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.3343 1.4243 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.5880(2)
_cell_length_b                   10.2373(3)
_cell_length_c                   10.7261(3)
_cell_angle_alpha                103.159(2)
_cell_angle_beta                 94.609(2)
_cell_angle_gamma                90.904(2)
_cell_volume                     1021.23(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9711
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.3090
_cell_measurement_theta_min      3.6860
_shelx_estimated_absorpt_T_max   0.878
_shelx_estimated_absorpt_T_min   0.776
_exptl_absorpt_coefficient_mu    2.669
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21565
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.416
_diffrn_reflns_theta_min         3.693
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -17.00  72.00   0.50    0.31    --   -1.56  40.00-131.00  178
  2  ω     57.00 145.00   0.50    1.27    --   71.86  40.00-131.00  176
  3  ω     -1.00  73.00   0.50    1.27    --   71.86 -40.00  75.00  148
  4  ω   -148.00 -59.00   0.50    1.27    --  -74.99 -40.00  75.00  178
  5  ω    -73.00  -1.00   0.50    1.27    --  -74.99  40.00-131.00  144
  6  ω    -75.00  14.00   0.50    0.31    --   -1.56 -40.00  75.00  178
  7  ω    -16.00  72.00   0.50    0.31    --   -1.56  38.00 -60.00  176
  8  ω     -1.00  88.00   0.50    1.27    --   71.86 -57.00 120.00  178
  9  ω     20.00 112.00   0.50    1.27    --   71.86-125.00-120.00  184
 10  ω     -1.00 105.00   0.50    1.27    --   71.86 -99.00  60.00  212
 11  ω     -1.00  96.00   0.50    1.27    --   71.86 -77.00-180.00  194
 12  ω     57.00 146.00   0.50    1.27    --   71.86  38.00 -60.00  178
 13  ω     -1.00 105.00   0.50    1.27    --   71.86 -99.00-180.00  212
 14  ω     -2.00  71.00   0.50    1.27    --   71.86 -38.00-120.00  146
 15  ω     20.00 112.00   0.50    1.27    --   71.86-125.00  90.00  184
 16  ω   -148.00 -79.00   0.50    1.27    --  -74.99-125.00 120.00  138
 17  ω    -91.00  -2.00   0.50    1.27    --  -74.99  57.00   0.00  178
 18  ω   -148.00 -88.00   0.50    1.27    --  -74.99 -99.00  60.00  120
 19  ω    -99.00  -2.00   0.50    1.27    --  -74.99  77.00 120.00  194
 20  ω    -99.00  -2.00   0.50    1.27    --  -74.99  77.00   0.00  194
 21  ω    -75.00  13.00   0.50    0.31    --   -1.56 -38.00 -30.00  176
 22  ω    -74.00  15.00   0.50    0.31    --   -1.56 -57.00-180.00  178
 23  ω    -16.00  72.00   0.50    0.31    --   -1.56  38.00   0.00  176
 24  ω     56.00 115.00   0.50    1.27    --   71.86  57.00   0.00  118
 25  ω     56.00 145.00   0.50    1.27    --   71.86  57.00 150.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0880115000
_diffrn_orient_matrix_UB_12      0.1029620000
_diffrn_orient_matrix_UB_13      0.0571431000
_diffrn_orient_matrix_UB_21      -0.0927481000
_diffrn_orient_matrix_UB_22      0.0861276000
_diffrn_orient_matrix_UB_23      -0.0313996000
_diffrn_orient_matrix_UB_31      -0.0575485000
_diffrn_orient_matrix_UB_32      0.0071609000
_diffrn_orient_matrix_UB_33      0.1109620000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ga K\a'
_diffrn_radiation_wavelength     1.3405
_diffrn_source                   'micro-focus metaljet'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3712
_reflns_number_total             4554
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         2.228
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         4554
_refine_ls_number_restraints     64
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0895
_refine_ls_restrained_S_all      1.079
_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)+(0.1719P)²+2.2391P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2648
_refine_ls_wR_factor_ref         0.2763
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C18-N14
 1.45 with sigma of 0.02
 N14-C18
 1.48 with sigma of 0.002
 N14-C17
 1.48 with sigma of 0.002
3. Rigid bond restraints
 C19, N14, C17, C18, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N14 \\sim C17 \\sim C18 \\sim C19 \\sim C20: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 1.7A
Uanis(C20) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
5.a Secondary CH2 refined with riding coordinates:
 N14(H14A,H14B), C17(H17A,H17B), C18(H18A,H18B)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C12(H12), C4(H4)
5.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.72272(7) 0.69693(8) 0.76635(7) 0.0283(3) Uani 1 1 d . . . . .
O3 O 0.7562(3) 0.5872(3) 0.6067(3) 0.0302(7) Uani 1 1 d . . . . .
O4 O 0.8272(3) 0.5789(3) 0.8659(3) 0.0290(6) Uani 1 1 d . . . . .
O7 O 0.6121(3) 0.8189(3) 0.6840(3) 0.0320(7) Uani 1 1 d . . . . .
O1 O 0.9084(3) 0.7803(3) 0.7635(3) 0.0319(7) Uani 1 1 d . . . . .
O6 O 0.5615(3) 0.6066(4) 0.7964(3) 0.0343(7) Uani 1 1 d . . . . .
O9 O 0.7124(3) 0.8303(4) 0.9246(3) 0.0403(8) Uani 1 1 d . . . . .
O8 O 0.4597(3) 0.9666(3) 0.6520(3) 0.0358(7) Uani 1 1 d . . . . .
O5 O 0.8789(3) 0.4821(4) 1.0255(4) 0.0462(10) Uani 1 1 d . . . . .
O2 O 1.1335(4) 0.7961(4) 0.7449(4) 0.0603(13) Uani 1 1 d . . . . .
C11 C 0.6064(4) 0.9121(5) 0.9592(4) 0.0295(9) Uani 1 1 d . . . . .
C8 C 0.3951(4) 0.5421(5) 0.9225(4) 0.0283(9) Uani 1 1 d . . . . .
H8 H 0.324491 0.570532 0.871205 0.034 Uiso 1 1 calc R U . . .
C7 C 0.5338(4) 0.5568(5) 0.8977(4) 0.0274(8) Uani 1 1 d . . . . .
C9 C 0.5267(4) 0.9131(4) 0.7272(4) 0.0284(9) Uani 1 1 d . . . . .
C6 C 0.6402(4) 0.5146(4) 0.9772(4) 0.0271(9) Uani 1 1 d . . . . .
C10 C 0.5138(4) 0.9523(4) 0.8684(4) 0.0260(8) Uani 1 1 d . . . . .
C5 C 0.7899(4) 0.5264(5) 0.9540(4) 0.0291(9) Uani 1 1 d . . . . .
C3 C 0.8766(4) 0.5470(4) 0.5557(4) 0.0268(8) Uani 1 1 d . . . . .
C12 C 0.5912(4) 0.9606(4) 1.0890(4) 0.0279(8) Uani 1 1 d . . . . .
H12 H 0.653010 0.934087 1.149206 0.034 Uiso 1 1 calc R U . . .
C4 C 0.8722(4) 0.4368(5) 0.4516(4) 0.0294(9) Uani 1 1 d . . . . .
H4 H 0.786211 0.394521 0.418600 0.035 Uiso 1 1 calc R U . . .
C2 C 1.0072(4) 0.6124(4) 0.6048(4) 0.0285(9) Uani 1 1 d . . . . .
C1 C 1.0215(4) 0.7367(5) 0.7110(5) 0.0351(10) Uani 1 1 d . . . . .
N14 N 0.6230(6) 0.8048(7) 0.4170(7) 0.0887(19) Uani 1 1 d D U . . .
H14A H 0.619382 0.810380 0.500726 0.106 Uiso 1 1 calc R U . . .
H14B H 0.594486 0.882575 0.402032 0.106 Uiso 1 1 calc R U . . .
C17 C 0.7722(7) 0.7936(10) 0.3900(9) 0.086(2) Uani 1 1 d D U . . .
H17A H 0.805643 0.711361 0.410516 0.103 Uiso 1 1 calc R U . . .
H17B H 0.776886 0.784189 0.298422 0.103 Uiso 1 1 calc R U . . .
C20 C 0.3820(10) 0.7262(9) 0.3704(9) 0.089(2) Uani 1 1 d . U . . .
H20A H 0.322023 0.654294 0.319834 0.133 Uiso 1 1 calc R U . . .
H20B H 0.357796 0.808691 0.347192 0.133 Uiso 1 1 calc R U . . .
H20C H 0.370459 0.734154 0.459893 0.133 Uiso 1 1 calc R U . . .
C18 C 0.5190(11) 0.6997(10) 0.3480(11) 0.116(3) Uani 1 1 d D U . . .
H18A H 0.527640 0.686270 0.256508 0.139 Uiso 1 1 calc R U . . .
H18B H 0.541820 0.616237 0.371996 0.139 Uiso 1 1 calc R U . . .
C19 C 0.8603(14) 0.8934(14) 0.4512(14) 0.130(4) Uani 1 1 d . U . . .
H19A H 0.827393 0.976561 0.434889 0.195 Uiso 1 1 calc R U . . .
H19B H 0.951461 0.877787 0.420909 0.195 Uiso 1 1 calc R U . . .
H19C H 0.865569 0.898014 0.541813 0.195 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 1.877(3) . ?
Ti1 O4 2.014(3) . ?
Ti1 O7 1.964(3) . ?
Ti1 O1 1.967(3) . ?
Ti1 O6 1.876(3) . ?
Ti1 O9 1.931(3) . ?
O3 C3 1.347(4) . ?
O4 C5 1.261(5) . ?
O7 C9 1.303(5) . ?
O1 C1 1.300(5) . ?
O6 C7 1.344(5) . ?
O9 C11 1.348(5) . ?
O8 C9 1.222(5) . ?
O5 C5 1.260(5) . ?
O2 C1 1.213(6) . ?
C11 C10 1.401(6) . ?
C11 C12 1.388(6) . ?
C8 H8 0.9300 . ?
C8 C7 1.389(5) . ?
C8 C6 1.395(6) 2_667 ?
C7 C6 1.412(6) . ?
C9 C10 1.491(5) . ?
C6 C5 1.484(5) . ?
C10 C12 1.391(5) 2_677 ?
C3 C4 1.392(6) . ?
C3 C2 1.415(5) . ?
C12 H12 0.9300 . ?
C4 H4 0.9300 . ?
C4 C2 1.395(5) 2_766 ?
C2 C1 1.498(6) . ?
N14 H14A 0.8900 . ?
N14 H14B 0.8900 . ?
N14 C17 1.484(2) . ?
N14 C18 1.478(2) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C19 1.329(15) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C20 C18 1.375(14) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ti1 O4 93.25(13) . . ?
O3 Ti1 O7 91.83(13) . . ?
O3 Ti1 O1 85.92(12) . . ?
O3 Ti1 O6 98.70(14) . . ?
O3 Ti1 O9 170.19(14) . . ?
O7 Ti1 O4 174.59(11) . . ?
O7 Ti1 O1 97.65(14) . . ?
O1 Ti1 O4 84.57(13) . . ?
O6 Ti1 O4 85.18(13) . . ?
O6 Ti1 O7 92.23(14) . . ?
O6 Ti1 O1 168.97(14) . . ?
O6 Ti1 O9 90.95(15) . . ?
O9 Ti1 O4 89.32(14) . . ?
O9 Ti1 O7 85.98(13) . . ?
O9 Ti1 O1 84.90(14) . . ?
C3 O3 Ti1 131.2(3) . . ?
C5 O4 Ti1 130.4(2) . . ?
C9 O7 Ti1 132.9(3) . . ?
C1 O1 Ti1 133.3(3) . . ?
C7 O6 Ti1 130.1(3) . . ?
C11 O9 Ti1 127.9(3) . . ?
O9 C11 C10 122.0(4) . . ?
O9 C11 C12 118.8(4) . . ?
C12 C11 C10 119.2(4) . . ?
C7 C8 H8 119.4 . . ?
C7 C8 C6 121.2(4) . 2_667 ?
C6 C8 H8 119.4 2_667 . ?
O6 C7 C8 118.7(4) . . ?
O6 C7 C6 122.4(3) . . ?
C8 C7 C6 118.9(4) . . ?
O7 C9 C10 118.5(4) . . ?
O8 C9 O7 119.7(4) . . ?
O8 C9 C10 121.8(4) . . ?
C8 C6 C7 119.9(3) 2_667 . ?
C8 C6 C5 118.9(4) 2_667 . ?
C7 C6 C5 121.1(4) . . ?
C11 C10 C9 123.3(4) . . ?
C12 C10 C11 119.0(4) 2_677 . ?
C12 C10 C9 117.6(4) 2_677 . ?
O4 C5 O5 120.9(3) . . ?
O4 C5 C6 121.3(4) . . ?
O5 C5 C6 117.8(4) . . ?
O3 C3 C4 118.8(3) . . ?
O3 C3 C2 122.2(4) . . ?
C4 C3 C2 118.9(4) . . ?
C11 C12 C10 121.9(4) . 2_677 ?
C11 C12 H12 119.1 . . ?
C10 C12 H12 119.1 2_677 . ?
C3 C4 H4 118.9 . . ?
C3 C4 C2 122.1(4) . 2_766 ?
C2 C4 H4 118.9 2_766 . ?
C3 C2 C1 122.9(4) . . ?
C4 C2 C3 118.9(4) 2_766 . ?
C4 C2 C1 118.2(4) 2_766 . ?
O1 C1 C2 117.4(4) . . ?
O2 C1 O1 121.2(4) . . ?
O2 C1 C2 121.4(4) . . ?
H14A N14 H14B 106.9 . . ?
C17 N14 H14A 107.3 . . ?
C17 N14 H14B 107.3 . . ?
C18 N14 H14A 107.3 . . ?
C18 N14 H14B 107.3 . . ?
C18 N14 C17 119.9(8) . . ?
N14 C17 H17A 107.9 . . ?
N14 C17 H17B 107.9 . . ?
H17A C17 H17B 107.2 . . ?
C19 C17 N14 117.4(9) . . ?
C19 C17 H17A 107.9 . . ?
C19 C17 H17B 107.9 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
N14 C18 H18A 108.5 . . ?
N14 C18 H18B 108.5 . . ?
C20 C18 N14 115.3(9) . . ?
C20 C18 H18A 108.5 . . ?
C20 C18 H18B 108.5 . . ?
H18A C18 H18B 107.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 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 C3 C4 162.1(3) . . . . ?
Ti1 O3 C3 C2 -17.5(6) . . . . ?
Ti1 O4 C5 O5 -163.1(3) . . . . ?
Ti1 O4 C5 C6 16.8(6) . . . . ?
Ti1 O7 C9 O8 -172.9(3) . . . . ?
Ti1 O7 C9 C10 7.0(6) . . . . ?
Ti1 O1 C1 O2 -163.5(4) . . . . ?
Ti1 O1 C1 C2 18.1(7) . . . . ?
Ti1 O6 C7 C8 155.1(3) . . . . ?
Ti1 O6 C7 C6 -27.1(6) . . . . ?
Ti1 O9 C11 C10 -27.3(6) . . . . ?
Ti1 O9 C11 C12 154.4(3) . . . . ?
O3 Ti1 O6 C7 125.8(4) . . . . ?
O3 C3 C4 C2 -178.7(4) . . . 2_766 ?
O3 C3 C2 C4 178.7(4) . . . 2_766 ?
O3 C3 C2 C1 -4.3(7) . . . . ?
O4 Ti1 O3 C3 -57.6(4) . . . . ?
O4 Ti1 O6 C7 33.2(4) . . . . ?
O7 Ti1 O3 C3 124.3(4) . . . . ?
O7 Ti1 O6 C7 -142.0(4) . . . . ?
O7 C9 C10 C11 12.3(6) . . . . ?
O7 C9 C10 C12 -171.4(4) . . . 2_677 ?
O1 Ti1 O3 C3 26.8(4) . . . . ?
O1 Ti1 O6 C7 11.6(9) . . . . ?
O6 Ti1 O3 C3 -143.2(4) . . . . ?
O6 C7 C6 C8 -177.1(4) . . . 2_667 ?
O6 C7 C6 C5 1.4(7) . . . . ?
O9 Ti1 O6 C7 -56.0(4) . . . . ?
O9 C11 C10 C9 -2.3(7) . . . . ?
O9 C11 C10 C12 -178.5(4) . . . 2_677 ?
O9 C11 C12 C10 178.6(4) . . . 2_677 ?
O8 C9 C10 C11 -167.7(4) . . . . ?
O8 C9 C10 C12 8.6(6) . . . 2_677 ?
C8 C7 C6 C8 0.7(7) . . . 2_667 ?
C8 C7 C6 C5 179.2(4) . . . . ?
C8 C6 C5 O4 -178.8(4) 2_667 . . . ?
C8 C6 C5 O5 1.1(6) 2_667 . . . ?
C7 C6 C5 O4 2.7(7) . . . . ?
C7 C6 C5 O5 -177.3(4) . . . . ?
C6 C8 C7 O6 177.1(4) 2_667 . . . ?
C6 C8 C7 C6 -0.7(7) 2_667 . . . ?
C10 C11 C12 C10 0.2(7) . . . 2_677 ?
C3 C2 C1 O1 3.8(7) . . . . ?
C3 C2 C1 O2 -174.6(5) . . . . ?
C12 C11 C10 C9 176.0(4) . . . . ?
C12 C11 C10 C12 -0.2(7) . . . 2_677 ?
C4 C3 C2 C4 -0.8(7) . . . 2_766 ?
C4 C3 C2 C1 176.2(4) . . . . ?
C4 C2 C1 O1 -179.2(4) 2_766 . . . ?
C4 C2 C1 O2 2.4(8) 2_766 . . . ?
C2 C3 C4 C2 0.8(7) . . . 2_766 ?
C17 N14 C18 C20 -173.7(9) . . . . ?
C18 N14 C17 C19 177.5(11) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 197.6 36.4 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.376
_oxdiff_exptl_absorpt_empirical_full_min 0.419
