# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_MOF-217-100K
_audit_block_doi                 10.5517/ccdc.csd.cc23yntk
_database_code_depnum_ccdc_archive 'CCDC 1964929'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C9SC06500H 2020
loop_
_audit_author_name
_audit_author_address
'Jing Cao'
;Wuhan University
China
;
_audit_update_record             
;
2019-11-10 deposited with the CCDC.	2020-04-02 downloaded from the CCDC.
;
_audit_creation_date             2019-07-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            MOF-217
_chemical_name_systematic        MOF-217
_chemical_formula_moiety         '0.25(C84 H36 N12 O24 Ti4)'
_chemical_formula_sum            'C21 H9 N3 O6 Ti'
_chemical_formula_weight         447.21
_chemical_melting_point          ?
_chemical_oxdiff_formula         ' C N O H Ti'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 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'
'-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'

_cell_length_a                   20.9953(3)
_cell_length_b                   20.9953(3)
_cell_length_c                   20.9953(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9254.8(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5979
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      47.0660
_cell_measurement_theta_min      2.9580
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.741
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.642
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28360
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        50.374
_diffrn_reflns_theta_max         50.373
_diffrn_reflns_theta_min         3.646
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Counting (HPC) detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HyPix-6000HE'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -88.00  31.00   0.50  120.00    --    0.00 -57.00 -30.00  238
  2  ω     -8.00  35.00   0.50   20.00    --    5.00 -57.00-120.00   86
  3  ω    -58.00 -20.00   0.50   20.00    --    5.00 -57.00-120.00   76
  4  ω   -106.00  -2.00   0.50   20.00    --  -78.80  38.00   0.00  208
  5  ω   -106.00  11.00   0.50   20.00    --  -78.80  38.00-120.00  234
  6  ω   -112.00 -15.00   0.50   20.00    --  -78.80  57.00   0.00  194
  7  ω   -140.00 -19.00   0.50   20.00    --  -78.80 -19.00  30.00  242
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       'profile data from ω-scans and φ-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0680601000
_diffrn_orient_matrix_UB_12      0.0206589000
_diffrn_orient_matrix_UB_13      0.0182499000
_diffrn_orient_matrix_UB_21      0.0084688000
_diffrn_orient_matrix_UB_22      -0.0306463000
_diffrn_orient_matrix_UB_23      0.0661221000
_diffrn_orient_matrix_UB_31      0.0261700000
_diffrn_orient_matrix_UB_32      0.0633971000
_diffrn_orient_matrix_UB_33      0.0259453000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'VariMax VHF'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku MicroMax-007HF'
_diffrn_source_voltage           40.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1246
_reflns_number_total             1618
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     39.93
_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 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_computing_data_collection       
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_computing_data_reduction        
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.634
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1618
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1243
_refine_ls_R_factor_gt           0.1140
_refine_ls_restrained_S_all      1.634
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3654
_refine_ls_wR_factor_ref         0.3772
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C5(H5)
;
_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 0.19443(6) 0.30557(6) 0.69443(6) 0.1035(11) Uani 1 3 d S T P . .
O2 O 0.2244(2) 0.36258(18) 0.6273(2) 0.1038(15) Uani 1 1 d . . . . .
O1 O 0.2703(2) 0.2595(2) 0.6666(2) 0.1137(16) Uani 1 1 d . . . . .
N1 N 0.3543(2) 0.4306(3) 0.4346(3) 0.1071(18) Uani 1 1 d . . . . .
C7 C 0.3824(3) 0.3783(3) 0.4575(3) 0.0953(19) Uani 1 1 d . . . . .
C3 C 0.3029(3) 0.3733(3) 0.5428(3) 0.0914(18) Uani 1 1 d . . . . .
H3 H 0.285832 0.411382 0.527868 0.110 Uiso 1 1 calc R . . . .
C2 C 0.2755(3) 0.3422(3) 0.5945(3) 0.100(2) Uani 1 1 d . . . . .
C4 C 0.3547(3) 0.3473(3) 0.5145(3) 0.1023(19) Uani 1 1 d . . . . .
C1 C 0.3022(4) 0.2855(3) 0.6163(3) 0.108(2) Uani 1 1 d . . . . .
C6 C 0.3571(4) 0.2613(3) 0.5891(4) 0.118(2) Uani 1 1 d . . . . .
H6 H 0.376212 0.224875 0.605593 0.141 Uiso 1 1 calc R . . . .
C5 C 0.3834(3) 0.2923(3) 0.5369(3) 0.106(2) Uani 1 1 d . . . . .
H5 H 0.419664 0.276276 0.517189 0.127 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O2 1.953(4) 12_565 ?
Ti1 O2 1.953(4) 6_456 ?
Ti1 O2 1.953(4) . ?
Ti1 O1 1.953(4) . ?
Ti1 O1 1.954(4) 12_565 ?
Ti1 O1 1.954(4) 6_456 ?
O2 C2 1.346(7) . ?
O1 C1 1.364(8) . ?
N1 C7 1.331(7) 9 ?
N1 C7 1.337(7) . ?
C7 C4 1.482(8) . ?
C3 H3 0.9300 . ?
C3 C2 1.390(8) . ?
C3 C4 1.356(8) . ?
C2 C1 1.394(9) . ?
C4 C5 1.383(8) . ?
C1 C6 1.384(9) . ?
C6 H6 0.9300 . ?
C6 C5 1.389(8) . ?
C5 H5 0.9300 . ?

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
O2 Ti1 O2 89.3(2) 12_565 6_456 ?
O2 Ti1 O2 89.3(2) . 6_456 ?
O2 Ti1 O2 89.3(2) 12_565 . ?
O1 Ti1 O2 79.96(19) 12_565 12_565 ?
O1 Ti1 O2 162.48(19) 12_565 6_456 ?
O1 Ti1 O2 104.25(19) 6_456 12_565 ?
O1 Ti1 O2 162.47(19) 6_456 . ?
O1 Ti1 O2 162.47(19) . 12_565 ?
O1 Ti1 O2 79.96(19) . . ?
O1 Ti1 O2 104.25(19) 12_565 . ?
O1 Ti1 O2 104.25(19) . 6_456 ?
O1 Ti1 O2 79.96(19) 6_456 6_456 ?
O1 Ti1 O1 89.3(2) . 12_565 ?
O1 Ti1 O1 89.3(2) . 6_456 ?
O1 Ti1 O1 89.3(2) 12_565 6_456 ?
C2 O2 Ti1 115.6(4) . . ?
C1 O1 Ti1 115.7(4) . . ?
C7 N1 C7 118.5(6) 9 . ?
N1 C7 N1 121.5(6) 5 . ?
N1 C7 C4 119.9(7) 5 . ?
N1 C7 C4 118.6(7) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C4 C3 C2 118.9(6) . . ?
O2 C2 C3 125.4(6) . . ?
O2 C2 C1 115.0(7) . . ?
C3 C2 C1 119.5(6) . . ?
C3 C4 C7 119.4(6) . . ?
C3 C4 C5 122.5(6) . . ?
C5 C4 C7 118.1(6) . . ?
O1 C1 C2 113.6(7) . . ?
O1 C1 C6 125.6(7) . . ?
C6 C1 C2 120.8(7) . . ?
C1 C6 H6 120.5 . . ?
C1 C6 C5 119.0(6) . . ?
C5 C6 H6 120.5 . . ?
C4 C5 C6 119.1(6) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?

_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 -0.752 -0.481 -0.808 6499.7 1990.6 ?

_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 2.002
_oxdiff_exptl_absorpt_empirical_full_min 0.322
####################################################################### 
# 
# 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_I
_audit_block_doi                 10.5517/ccdc.csd.cc24wx0z
_database_code_depnum_ccdc_archive 'CCDC 1993021'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C9SC06500H 2020
loop_
_audit_author_name
_audit_author_address
'Hengjiang Cong'
;Wuhan University
China
;
_audit_update_record             
;
2020-03-26 deposited with the CCDC.	2020-04-02 downloaded from the CCDC.
;
_chemical_name_mineral           ??
_cell_length_a                   21.43809
_cell_length_b                   21.43809
_cell_length_c                   21.43809
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9852.765
_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   PA-3
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z '
'-x, y+1/2, -z+1/2 '
'-x+1/2, -y, z+1/2 '
'-x+1/2, y+1/2, z '
'-y, -z, -x '
'-y, z+1/2, -x+1/2 '
'-y+1/2, -z, x+1/2 '
'-y+1/2, z+1/2, x '
'-z, -x, -y '
'-z, x+1/2, -y+1/2 '
'-z+1/2, -x, y+1/2 '
'-z+1/2, x+1/2, y '
'z, -x+1/2, y+1/2 '
'z, x, y '
'z+1/2, -x+1/2, -y '
'z+1/2, x, -y+1/2 '
'y, -z+1/2, x+1/2 '
'y, z, x '
'y+1/2, -z+1/2, -x '
'y+1/2, z, -x+1/2 '
'x, -y+1/2, z+1/2 '
'-x, -y, -z '
'x+1/2, -y+1/2, -z '
'x+1/2, y, -z+1/2 '
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Ti1 Ti 8 0.6706903 0.8293097 0.1706903 1 4
O2 O 24 0.6060165 0.8029801 0.1213706 1 4
O1 O 24 0.6393274 0.8041769 0.2419902 1 4
N1 N 24 0.3965731 0.608349 0.1847051 1 4
C7 C 24 0.4204546 0.6609048 0.1558368 1 4
C4 C 24 0.471278 0.7208544 0.1769708 1 4
C5 C 24 0.4883729 0.7109421 0.2385826 1 4
C3 C 24 0.5086328 0.7582602 0.1379094 1 4
C2 C 24 0.5642762 0.786774 0.1620571 1 4
C1 C 24 0.5826428 0.7760393 0.2226001 1 4
C6 C 24 0.54379 0.7399921 0.2626564 1 4
N2 N 24 0.3163608 0.6245591 0.4002458 1 2
C8 C 24 0.309036 0.6205252 0.4655706 1 2
N3 N 24 0.3141483 0.5575951 0.4830194 1 2
C9 C 24 0.324625 0.5220684 0.4283287 1 2
C10 C 24 0.3257946 0.5639748 0.3769391 1 2
N4 N 24 -0.03945959 0.4463799 -0.6378649 1 2
C11 C 24 -0.08159914 0.4697209 -0.5949921 1 2
C12 C 24 -0.1331066 0.4312325 -0.5949192 1 2
N5 N 24 -0.1230959 0.3845899 -0.6380952 1 2
C13 C 24 -0.06554808 0.3945049 -0.6651178 1 2
O3 O 24 0.3934855 0.807633 0.2651976 1 1
O4 O 24 -0.01219327 0.8303223 0.4802688 1 1
O4 O 24 0.349154 -0.2969259 -0.5321744 1 1
O5 O 24 0.2063566 0.1987815 0.3020605 1 1
O6 O 24 0.316649 -0.09936266 0.4212758 1 1
O7 O 24 0.2448869 0.02013347 0.5680254 1 1
_chemical_name_systematic        'MOF-217 with 28 wt% Imidazole'
####################################################################### 
# 
# 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_MOF-217-250K
_audit_block_doi                 10.5517/ccdc.csd.cc23ynwm
_database_code_depnum_ccdc_archive 'CCDC 1964931'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C9SC06500H 2020
loop_
_audit_author_name
_audit_author_address
'Jing Cao'
;Wuhan University
China
;
_audit_update_record             
;
2019-11-10 deposited with the CCDC.	2020-04-02 downloaded from the CCDC.
;
_audit_creation_date             2019-07-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.04(C84 H36 N12 O24 Ti4)'
_chemical_formula_sum            'C3.50 H1.50 N0.50 O Ti0.17'
_chemical_formula_weight         74.54
_chemical_melting_point          ?
_chemical_oxdiff_formula         'H C N O Ti'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 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'
'-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'

_cell_length_a                   21.1222(4)
_cell_length_b                   21.1222(4)
_cell_length_c                   21.1222(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9423.6(5)
_cell_formula_units_Z            48
_cell_measurement_reflns_used    4198
_cell_measurement_temperature    249.99(10)
_cell_measurement_theta_max      42.8080
_cell_measurement_theta_min      2.9120
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.709
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    0.630
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11570
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        44.287
_diffrn_reflns_theta_max         44.287
_diffrn_reflns_theta_min         3.624
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      249.99(10)
_diffrn_detector                 'Hybrid Pixel Counting (HPC) detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HyPix-6000HE'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  94.00   0.50   60.00    --    5.00  38.00-120.00  252
  2  ω    -90.00  33.00   0.50   60.00    --  -56.20  57.00 -60.00  246
  3  ω   -146.00 -96.00   0.50   60.00    --  -56.20 -38.00 -60.00  100
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       'profile data from ω-scans and φ-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0101795000
_diffrn_orient_matrix_UB_12      0.0722148000
_diffrn_orient_matrix_UB_13      -0.0026532000
_diffrn_orient_matrix_UB_21      0.0657653000
_diffrn_orient_matrix_UB_22      0.0080837000
_diffrn_orient_matrix_UB_23      -0.0305399000
_diffrn_orient_matrix_UB_31      -0.0300866000
_diffrn_orient_matrix_UB_32      -0.0067972000
_diffrn_orient_matrix_UB_33      -0.0660218000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'VariMax VHF'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku MicroMax-007HF'
_diffrn_source_voltage           40.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                885
_reflns_number_total             1231
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     50.38
_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 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_computing_data_collection       
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_computing_data_reduction        
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.0008(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.534
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         1231
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.1201
_refine_ls_R_factor_gt           0.1083
_refine_ls_restrained_S_all      1.495
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3521
_refine_ls_wR_factor_ref         0.3639
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C5(H5)
;
_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 0.68997(7) 0.81003(7) 0.18997(7) 0.1340(17) Uani 1 3 d S TU P . .
O2 O 0.6232(2) 0.7800(3) 0.1358(2) 0.134(2) Uani 1 1 d . U . . .
O1 O 0.6625(3) 0.7357(3) 0.2385(2) 0.137(2) Uani 1 1 d . U . . .
N1 N 0.4284(4) 0.5686(4) 0.1479(3) 0.129(2) Uani 1 1 d . U . . .
C7 C 0.4557(4) 0.6197(4) 0.1220(5) 0.123(3) Uani 1 1 d . U . . .
C4 C 0.5114(4) 0.6472(4) 0.1534(4) 0.125(3) Uani 1 1 d . U . . .
C3 C 0.5393(4) 0.7029(4) 0.1263(4) 0.126(3) Uani 1 1 d . U . . .
H3 H 0.522943 0.720884 0.089654 0.151 Uiso 1 1 calc R . . . .
C2 C 0.5912(4) 0.7288(4) 0.1564(4) 0.121(3) Uani 1 1 d . U . . .
C1 C 0.6138(4) 0.7035(4) 0.2125(4) 0.128(3) Uani 1 1 d . U . . .
C6 C 0.5854(4) 0.6485(5) 0.2377(4) 0.153(3) Uani 1 1 d . U . . .
H6 H 0.600708 0.631071 0.275142 0.184 Uiso 1 1 calc R . . . .
C5 C 0.5373(4) 0.6217(4) 0.2084(4) 0.131(3) Uani 1 1 d . U . . .
H5 H 0.520122 0.584728 0.224976 0.158 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O2 1.923(5) 6_566 ?
Ti1 O2 1.923(5) 12_664 ?
Ti1 O2 1.923(5) . ?
Ti1 O1 1.963(5) 6_566 ?
Ti1 O1 1.963(5) 12_664 ?
Ti1 O1 1.963(5) . ?
O2 C2 1.347(8) . ?
O1 C1 1.349(9) . ?
N1 C7 1.341(8) . ?
N1 C7 1.323(8) 7_564 ?
C7 C4 1.470(10) . ?
C4 C3 1.434(9) . ?
C4 C5 1.392(10) . ?
C3 H3 0.9300 . ?
C3 C2 1.381(10) . ?
C2 C1 1.386(10) . ?
C1 C6 1.412(11) . ?
C6 H6 0.9300 . ?
C6 C5 1.317(10) . ?
C5 H5 0.9300 . ?

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
O2 Ti1 O2 90.1(3) 6_566 12_664 ?
O2 Ti1 O2 90.1(3) 6_566 . ?
O2 Ti1 O2 90.1(3) 12_664 . ?
O2 Ti1 O1 103.8(2) . 12_664 ?
O2 Ti1 O1 163.0(2) 6_566 12_664 ?
O2 Ti1 O1 163.0(2) 12_664 . ?
O2 Ti1 O1 80.2(2) 6_566 6_566 ?
O2 Ti1 O1 80.2(2) 12_664 12_664 ?
O2 Ti1 O1 163.0(2) . 6_566 ?
O2 Ti1 O1 80.2(2) . . ?
O2 Ti1 O1 103.8(2) 6_566 . ?
O2 Ti1 O1 103.8(2) 12_664 6_566 ?
O1 Ti1 O1 88.5(2) 6_566 . ?
O1 Ti1 O1 88.5(2) 6_566 12_664 ?
O1 Ti1 O1 88.5(2) 12_664 . ?
C2 O2 Ti1 116.2(5) . . ?
C1 O1 Ti1 114.6(5) . . ?
C7 N1 C7 118.3(9) . 7_564 ?
N1 C7 N1 121.6(9) . 10_655 ?
N1 C7 C4 118.5(9) . . ?
N1 C7 C4 119.7(10) 10_655 . ?
C3 C4 C7 118.2(8) . . ?
C5 C4 C7 122.6(8) . . ?
C5 C4 C3 119.2(7) . . ?
C4 C3 H3 121.0 . . ?
C2 C3 C4 118.0(8) . . ?
C2 C3 H3 121.0 . . ?
O2 C2 C3 124.7(8) . . ?
O2 C2 C1 114.3(8) . . ?
C3 C2 C1 120.9(8) . . ?
O1 C1 C2 114.6(8) . . ?
O1 C1 C6 125.9(8) . . ?
C2 C1 C6 119.5(8) . . ?
C1 C6 H6 119.9 . . ?
C5 C6 C1 120.3(8) . . ?
C5 C6 H6 119.9 . . ?
C4 C5 H5 119.0 . . ?
C6 C5 C4 122.0(8) . . ?
C6 C5 H5 119.0 . . ?

_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 -0.967 -0.382 -0.624 6755.9 1843.0 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.607
_oxdiff_exptl_absorpt_empirical_full_min 0.668
####################################################################### 
# 
# 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_MOF-217-200K
_audit_block_doi                 10.5517/ccdc.csd.cc23ynvl
_database_code_depnum_ccdc_archive 'CCDC 1964930'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C9SC06500H 2020
loop_
_audit_author_name
_audit_author_address
'Jing Cao'
;Wuhan University
China
;
_audit_update_record             
;
2019-11-10 deposited with the CCDC.	2020-04-02 downloaded from the CCDC.
;
_audit_creation_date             2019-07-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.02(C84 H36 N12 O24 Ti4)'
_chemical_formula_sum            'C H N O Ti'
_chemical_formula_weight         90.93
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O Ti'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 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'
'-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'

_cell_length_a                   21.1205(3)
_cell_length_b                   21.1205(3)
_cell_length_c                   21.1205(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9421.3(4)
_cell_formula_units_Z            131
_cell_measurement_reflns_used    5189
_cell_measurement_temperature    199.99(10)
_cell_measurement_theta_max      51.4260
_cell_measurement_theta_min      2.9220
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    22.897
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    2.099
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5764
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18218
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        51.054
_diffrn_reflns_theta_max         51.054
_diffrn_reflns_theta_min         3.625
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      199.99(10)
_diffrn_detector                 'Hybrid Pixel Counting (HPC) detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HyPix-6000HE'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -168.00  11.00   0.50   30.00    --  -78.80 -14.00-139.00  358
  2  ω    -32.00  55.00   0.50  120.00    --    0.00  57.00-180.00  174
  3  ω     24.00  55.00   0.50  120.00    --    0.00  57.00-180.00   62
  4  ω   -111.00 -10.00   0.50   30.00    --  -78.80  57.00-180.00  202
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       'profile data from ω-scans and φ-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0169371000
_diffrn_orient_matrix_UB_12      0.0516807000
_diffrn_orient_matrix_UB_13      0.0486711000
_diffrn_orient_matrix_UB_21      0.0638283000
_diffrn_orient_matrix_UB_22      -0.0106820000
_diffrn_orient_matrix_UB_23      0.0335968000
_diffrn_orient_matrix_UB_31      0.0310179000
_diffrn_orient_matrix_UB_32      0.0503678000
_diffrn_orient_matrix_UB_33      -0.0426484000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'VariMax VHF'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku MicroMax-007HF'
_diffrn_source_voltage           40.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1309
_reflns_number_total             1699
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     39.93
_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 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_computing_data_collection       
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_computing_data_reduction        
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.0007(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.624
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         1699
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1197
_refine_ls_R_factor_gt           0.1096
_refine_ls_restrained_S_all      1.624
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3658
_refine_ls_wR_factor_ref         0.3770
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C4(H4)
;
_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 0.80841(5) 0.19159(5) 0.69159(5) 0.0995(12) Uani 1 3 d S T P . .
O1 O 0.7785(2) 0.13611(17) 0.6243(2) 0.1026(15) Uani 1 1 d . . . . .
O2 O 0.7335(2) 0.23846(19) 0.6640(2) 0.1077(16) Uani 1 1 d . . . . .
N1 N 0.6466(2) 0.0712(3) 0.4328(3) 0.1056(18) Uani 1 1 d . . . . .
C7 C 0.6191(3) 0.1214(3) 0.4565(3) 0.0945(19) Uani 1 1 d . . . . .
C6 C 0.7000(3) 0.1257(3) 0.5412(3) 0.0933(19) Uani 1 1 d . . . . .
H6 H 0.717582 0.088003 0.526658 0.112 Uiso 1 1 calc R . . . .
C5 C 0.6471(3) 0.1520(3) 0.5114(3) 0.0934(18) Uani 1 1 d . . . . .
C1 C 0.7256(3) 0.1569(3) 0.5928(3) 0.0925(18) Uani 1 1 d . . . . .
C2 C 0.7007(3) 0.2125(3) 0.6148(3) 0.098(2) Uani 1 1 d . . . . .
C3 C 0.6474(3) 0.2367(3) 0.5878(3) 0.113(2) Uani 1 1 d . . . . .
H3 H 0.628777 0.273074 0.604326 0.135 Uiso 1 1 calc R . . . .
C4 C 0.6213(3) 0.2074(3) 0.5365(3) 0.105(2) Uani 1 1 d . . . . .
H4 H 0.585457 0.224754 0.517817 0.126 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O1 1.947(4) . ?
Ti1 O1 1.947(4) 7_665 ?
Ti1 O1 1.947(4) 10_646 ?
Ti1 O2 1.955(4) . ?
Ti1 O2 1.955(4) 10_646 ?
Ti1 O2 1.955(4) 7_665 ?
O1 C1 1.373(7) . ?
O2 C2 1.363(7) . ?
N1 C7 1.308(7) . ?
N1 C7 1.351(7) 11_556 ?
C7 C5 1.453(8) . ?
C6 H6 0.9300 . ?
C6 C5 1.399(8) . ?
C6 C1 1.384(8) . ?
C5 C4 1.394(8) . ?
C1 C2 1.369(8) . ?
C2 C3 1.362(8) . ?
C3 H3 0.9300 . ?
C3 C4 1.364(8) . ?
C4 H4 0.9300 . ?

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 89.5(2) . 7_665 ?
O1 Ti1 O1 89.5(2) . 10_646 ?
O1 Ti1 O1 89.5(2) 7_665 10_646 ?
O1 Ti1 O2 79.91(19) . . ?
O1 Ti1 O2 104.31(18) 7_665 . ?
O1 Ti1 O2 162.39(18) 10_646 . ?
O1 Ti1 O2 79.90(19) 7_665 7_665 ?
O1 Ti1 O2 104.31(18) 10_646 7_665 ?
O1 Ti1 O2 104.31(18) . 10_646 ?
O1 Ti1 O2 162.38(18) . 7_665 ?
O1 Ti1 O2 162.39(18) 7_665 10_646 ?
O1 Ti1 O2 79.90(19) 10_646 10_646 ?
O2 Ti1 O2 89.0(2) . 10_646 ?
O2 Ti1 O2 89.0(2) 7_665 10_646 ?
O2 Ti1 O2 89.0(2) . 7_665 ?
C1 O1 Ti1 115.1(4) . . ?
C2 O2 Ti1 115.8(4) . . ?
C7 N1 C7 119.2(6) . 11_556 ?
N1 C7 N1 120.8(6) . 8_645 ?
N1 C7 C5 120.1(7) 8_645 . ?
N1 C7 C5 119.1(6) . . ?
C5 C6 H6 120.8 . . ?
C1 C6 H6 120.8 . . ?
C1 C6 C5 118.5(6) . . ?
C6 C5 C7 120.4(6) . . ?
C4 C5 C7 121.2(6) . . ?
C4 C5 C6 118.3(5) . . ?
O1 C1 C6 123.2(5) . . ?
C2 C1 O1 115.0(6) . . ?
C2 C1 C6 121.7(6) . . ?
O2 C2 C1 114.1(6) . . ?
C3 C2 O2 126.0(6) . . ?
C3 C2 C1 119.9(6) . . ?
C2 C3 H3 120.2 . . ?
C2 C3 C4 119.7(6) . . ?
C4 C3 H3 120.2 . . ?
C5 C4 H4 119.1 . . ?
C3 C4 C5 121.8(6) . . ?
C3 C4 H4 119.1 . . ?

_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 -0.421 -0.629 -0.490 6683.0 1970.5 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.075
_oxdiff_exptl_absorpt_empirical_full_min 0.679
