# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_Ti2Cl5tmeda
_database_code_depnum_ccdc_archive 'CCDC 2045300'
loop_
_audit_author_name
_audit_author_address
'Takashi Kurogi'
;Okayama University
Japan
;
_audit_update_record             
;
2020-11-19 deposited with the CCDC.	2021-01-19 downloaded from the CCDC.
;
_audit_creation_date             2020-05-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_formula_moiety         'C12 H32 Cl5 N4 Ti2'
_chemical_formula_sum            'C12 H32 Cl5 N4 Ti2'
_chemical_formula_weight         505.46

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   19.796(5)
_cell_length_b                   8.413(2)
_cell_length_c                   13.102(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2182.1(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6254
_cell_measurement_temperature    100(2)
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      27.5
_shelx_estimated_absorpt_T_max   0.974
_shelx_estimated_absorpt_T_min   0.900
_exptl_absorpt_coefficient_mu    1.347
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20125
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.056
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support Fiber
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC11 (Right): Eulerian 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_wavelength     0.71075
_reflns_Friedel_coverage         0.915
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                4582
_reflns_number_total             4976
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details 
;
 Flack x determined using 1832 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         4976
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0507
_refine_ls_restrained_S_all      1.096
_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)+(0.0573P)²+2.1194P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1223
_refine_special_details          ?
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.91671(5) 0.48811(14) 0.35848(9) 0.0161(2) Uani 1 1 d . . . . .
Ti2 Ti 0.80223(5) 0.40821(13) 0.26059(9) 0.0177(2) Uani 1 1 d . . . . .
Cl1 Cl 0.91091(8) 0.5236(2) 0.53863(12) 0.0250(4) Uani 1 1 d . . . . .
Cl2 Cl 0.70314(8) 0.3900(2) 0.36186(13) 0.0263(3) Uani 1 1 d . . . . .
Cl3 Cl 0.91087(8) 0.4496(2) 0.17128(11) 0.0213(3) Uani 1 1 d . . . . .
Cl4 Cl 0.82617(8) 0.67778(19) 0.32300(12) 0.0232(3) Uani 1 1 d . . . . .
Cl5 Cl 0.86314(8) 0.22767(19) 0.37245(12) 0.0243(3) Uani 1 1 d . . . . .
N1 N 1.0184(3) 0.3539(6) 0.3578(5) 0.0223(11) Uani 1 1 d . . . . .
N2 N 0.9918(3) 0.6980(6) 0.3445(4) 0.0238(12) Uani 1 1 d . . . . .
N3 N 0.7863(3) 0.1903(7) 0.1569(5) 0.0249(12) Uani 1 1 d . . . . .
N4 N 0.7408(3) 0.5226(7) 0.1302(4) 0.0222(12) Uani 1 1 d . . . . .
C1 C 1.0256(4) 0.2295(8) 0.2792(5) 0.0268(15) Uani 1 1 d . . . . .
H1A H 1.069606 0.177323 0.286756 0.040 Uiso 1 1 calc GR . . . .
H1B H 1.022522 0.277775 0.211272 0.040 Uiso 1 1 calc GR . . . .
H1C H 0.989563 0.150660 0.287280 0.040 Uiso 1 1 calc GR . . . .
C2 C 1.0305(4) 0.2775(9) 0.4579(5) 0.0298(16) Uani 1 1 d . . . . .
H2A H 0.993150 0.204830 0.473462 0.045 Uiso 1 1 calc GR . . . .
H2B H 1.033316 0.359216 0.510996 0.045 Uiso 1 1 calc GR . . . .
H2C H 1.072926 0.217694 0.455502 0.045 Uiso 1 1 calc GR . . . .
C3 C 1.0718(4) 0.4764(9) 0.3345(7) 0.0343(18) Uani 1 1 d . . . . .
H3A H 1.116158 0.437473 0.358797 0.041 Uiso 1 1 calc R . . . .
H3B H 1.074769 0.491709 0.259707 0.041 Uiso 1 1 calc R . . . .
C4 C 1.0563(4) 0.6317(9) 0.3843(6) 0.0344(17) Uani 1 1 d . . . . .
H4A H 1.052850 0.616556 0.459013 0.041 Uiso 1 1 calc R . . . .
H4B H 1.093515 0.707535 0.370824 0.041 Uiso 1 1 calc R . . . .
C5 C 0.9760(5) 0.8335(9) 0.4156(6) 0.043(2) Uani 1 1 d . . . . .
H5A H 0.968883 0.792177 0.484674 0.064 Uiso 1 1 calc GR . . . .
H5B H 0.935078 0.887947 0.392323 0.064 Uiso 1 1 calc GR . . . .
H5C H 1.013903 0.908483 0.416010 0.064 Uiso 1 1 calc GR . . . .
C6 C 0.9969(4) 0.7664(9) 0.2424(6) 0.0332(17) Uani 1 1 d . . . . .
H6A H 1.028375 0.856334 0.243638 0.050 Uiso 1 1 calc GR . . . .
H6B H 0.952329 0.803152 0.220159 0.050 Uiso 1 1 calc GR . . . .
H6C H 1.013592 0.685511 0.194762 0.050 Uiso 1 1 calc GR . . . .
C7 C 0.8457(4) 0.0899(8) 0.1326(6) 0.0296(16) Uani 1 1 d . . . . .
H7A H 0.862511 0.039976 0.195284 0.044 Uiso 1 1 calc GR . . . .
H7B H 0.881371 0.156058 0.102811 0.044 Uiso 1 1 calc GR . . . .
H7C H 0.832597 0.007285 0.083768 0.044 Uiso 1 1 calc GR . . . .
C8 C 0.7344(4) 0.0847(9) 0.2030(6) 0.0327(17) Uani 1 1 d . . . . .
H8A H 0.725865 -0.005349 0.157387 0.049 Uiso 1 1 calc GR . . . .
H8B H 0.692459 0.144536 0.213143 0.049 Uiso 1 1 calc GR . . . .
H8C H 0.750700 0.045327 0.268977 0.049 Uiso 1 1 calc GR . . . .
C9 C 0.7598(4) 0.2532(9) 0.0578(5) 0.0306(16) Uani 1 1 d . . . . .
H9A H 0.737520 0.166351 0.019606 0.037 Uiso 1 1 calc R . . . .
H9B H 0.797885 0.293150 0.016051 0.037 Uiso 1 1 calc R . . . .
C10 C 0.7098(4) 0.3862(9) 0.0760(5) 0.0297(16) Uani 1 1 d . . . . .
H10A H 0.691856 0.422964 0.009534 0.036 Uiso 1 1 calc R . . . .
H10B H 0.671509 0.345185 0.116709 0.036 Uiso 1 1 calc R . . . .
C11 C 0.7824(4) 0.6179(9) 0.0595(5) 0.0322(16) Uani 1 1 d . . . . .
H11A H 0.753247 0.666001 0.007474 0.048 Uiso 1 1 calc GR . . . .
H11B H 0.815775 0.549070 0.026350 0.048 Uiso 1 1 calc GR . . . .
H11C H 0.805677 0.701778 0.097563 0.048 Uiso 1 1 calc GR . . . .
C12 C 0.6846(4) 0.6280(9) 0.1653(6) 0.0308(16) Uani 1 1 d . . . . .
H12A H 0.703361 0.720867 0.200366 0.046 Uiso 1 1 calc GR . . . .
H12B H 0.655294 0.569051 0.212279 0.046 Uiso 1 1 calc GR . . . .
H12C H 0.658127 0.663065 0.106182 0.046 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 Ti2 2.6893(16) . ?
Ti1 Cl1 2.3819(19) . ?
Ti1 Cl3 2.4768(18) . ?
Ti1 Cl4 2.4444(19) . ?
Ti1 Cl5 2.4411(19) . ?
Ti1 N1 2.307(5) . ?
Ti1 N2 2.315(5) . ?
Ti2 Cl2 2.3731(19) . ?
Ti2 Cl3 2.4729(19) . ?
Ti2 Cl4 2.457(2) . ?
Ti2 Cl5 2.4308(19) . ?
Ti2 N3 2.303(6) . ?
Ti2 N4 2.307(5) . ?
N1 C1 1.476(9) . ?
N1 C2 1.480(9) . ?
N1 C3 1.508(9) . ?
N2 C4 1.489(9) . ?
N2 C5 1.504(9) . ?
N2 C6 1.460(9) . ?
N3 C7 1.484(9) . ?
N3 C8 1.486(9) . ?
N3 C9 1.496(9) . ?
N4 C10 1.483(9) . ?
N4 C11 1.476(9) . ?
N4 C12 1.496(9) . ?
C3 C4 1.492(11) . ?
C9 C10 1.512(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Ti1 Ti2 117.60(6) . . ?
Cl1 Ti1 Cl3 174.55(7) . . ?
Cl1 Ti1 Cl4 94.09(7) . . ?
Cl1 Ti1 Cl5 90.99(7) . . ?
Cl3 Ti1 Ti2 57.02(5) . . ?
Cl4 Ti1 Ti2 56.95(5) . . ?
Cl4 Ti1 Cl3 82.12(7) . . ?
Cl5 Ti1 Ti2 56.31(5) . . ?
Cl5 Ti1 Cl3 86.36(6) . . ?
Cl5 Ti1 Cl4 106.36(7) . . ?
N1 Ti1 Ti2 127.64(15) . . ?
N1 Ti1 Cl1 96.16(16) . . ?
N1 Ti1 Cl3 88.44(16) . . ?
N1 Ti1 Cl4 163.37(16) . . ?
N1 Ti1 Cl5 86.56(14) . . ?
N1 Ti1 N2 79.2(2) . . ?
N2 Ti1 Ti2 133.93(15) . . ?
N2 Ti1 Cl1 90.78(15) . . ?
N2 Ti1 Cl3 92.95(15) . . ?
N2 Ti1 Cl4 87.57(15) . . ?
N2 Ti1 Cl5 165.78(15) . . ?
Cl2 Ti2 Ti1 116.49(7) . . ?
Cl2 Ti2 Cl3 172.97(8) . . ?
Cl2 Ti2 Cl4 91.89(7) . . ?
Cl2 Ti2 Cl5 91.87(7) . . ?
Cl3 Ti2 Ti1 57.16(5) . . ?
Cl4 Ti2 Ti1 56.50(5) . . ?
Cl4 Ti2 Cl3 81.94(6) . . ?
Cl5 Ti2 Ti1 56.68(5) . . ?
Cl5 Ti2 Cl3 86.67(6) . . ?
Cl5 Ti2 Cl4 106.29(7) . . ?
N3 Ti2 Ti1 126.57(15) . . ?
N3 Ti2 Cl2 99.49(16) . . ?
N3 Ti2 Cl3 87.27(16) . . ?
N3 Ti2 Cl4 163.21(16) . . ?
N3 Ti2 Cl5 85.78(15) . . ?
N3 Ti2 N4 79.8(2) . . ?
N4 Ti2 Ti1 133.85(15) . . ?
N4 Ti2 Cl2 90.32(15) . . ?
N4 Ti2 Cl3 92.81(15) . . ?
N4 Ti2 Cl4 87.87(15) . . ?
N4 Ti2 Cl5 165.59(15) . . ?
Ti2 Cl3 Ti1 65.82(5) . . ?
Ti1 Cl4 Ti2 66.55(6) . . ?
Ti2 Cl5 Ti1 67.01(6) . . ?
C1 N1 Ti1 115.8(4) . . ?
C1 N1 C2 107.1(5) . . ?
C1 N1 C3 106.0(5) . . ?
C2 N1 Ti1 110.5(4) . . ?
C2 N1 C3 111.3(6) . . ?
C3 N1 Ti1 106.1(4) . . ?
C4 N2 Ti1 103.7(4) . . ?
C4 N2 C5 104.2(6) . . ?
C5 N2 Ti1 113.3(4) . . ?
C6 N2 Ti1 114.7(4) . . ?
C6 N2 C4 114.1(6) . . ?
C6 N2 C5 106.5(6) . . ?
C7 N3 Ti2 118.1(4) . . ?
C7 N3 C8 107.2(5) . . ?
C7 N3 C9 107.0(6) . . ?
C8 N3 Ti2 109.3(5) . . ?
C8 N3 C9 108.8(6) . . ?
C9 N3 Ti2 106.1(4) . . ?
C10 N4 Ti2 104.5(4) . . ?
C10 N4 C12 107.3(5) . . ?
C11 N4 Ti2 113.5(4) . . ?
C11 N4 C10 110.5(5) . . ?
C11 N4 C12 106.6(5) . . ?
C12 N4 Ti2 114.3(4) . . ?
C4 C3 N1 111.5(6) . . ?
N2 C4 C3 110.6(6) . . ?
N3 C9 C10 110.7(6) . . ?
N4 C10 C9 112.2(6) . . ?

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 N1 C3 C4 37.3(7) . . . . ?
Ti1 N2 C4 C3 50.0(7) . . . . ?
Ti2 N3 C9 C10 -39.8(6) . . . . ?
Ti2 N4 C10 C9 -45.2(6) . . . . ?
N1 C3 C4 N2 -62.4(8) . . . . ?
N3 C9 C10 N4 61.0(8) . . . . ?
C1 N1 C3 C4 160.9(6) . . . . ?
C2 N1 C3 C4 -82.9(7) . . . . ?
C5 N2 C4 C3 168.8(6) . . . . ?
C6 N2 C4 C3 -75.5(8) . . . . ?
C7 N3 C9 C10 -166.8(6) . . . . ?
C8 N3 C9 C10 77.7(7) . . . . ?
C11 N4 C10 C9 77.1(7) . . . . ?
C12 N4 C10 C9 -167.0(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane/hexane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_TiCl3tmeda_dimer
_database_code_depnum_ccdc_archive 'CCDC 2045302'
loop_
_audit_author_name
_audit_author_address
'Takashi Kurogi'
;Okayama University
Japan
;
_audit_update_record             
;
2020-11-19 deposited with the CCDC.	2021-01-19 downloaded from the CCDC.
;
_audit_creation_date             2020-01-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_formula_moiety         '2(C6 H16 Cl3 N2 Ti), 2(C H2 Cl2)'
_chemical_formula_sum            'C14 H36 Cl10 N4 Ti2'
_chemical_formula_weight         710.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   13.348(3)
_cell_length_b                   13.855(3)
_cell_length_c                   17.166(4)
_cell_angle_alpha                90
_cell_angle_beta                 112.468(4)
_cell_angle_gamma                90
_cell_volume                     2933.6(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7872
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_shelx_estimated_absorpt_T_max   0.904
_shelx_estimated_absorpt_T_min   0.867
_exptl_absorpt_coefficient_mu    1.467
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0433
_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       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45330
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.941
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support Fiber
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC11 (Right): Eulerian 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_wavelength     0.71075
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6256
_reflns_number_total             6710
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         1.060
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         6710
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0562
_refine_ls_restrained_S_all      1.158
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0316P)²+6.2137P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1084
_refine_special_details          ?
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.41345(5) 0.90274(4) -0.01304(4) 0.01348(13) Uani 1 1 d . . . . .
Cl1 Cl 0.56209(7) 0.80345(6) 0.05130(6) 0.02142(19) Uani 1 1 d . . . . .
Cl2 Cl 0.49486(6) 1.02435(6) 0.10016(5) 0.01664(17) Uani 1 1 d . . . . .
Cl3 Cl 0.26221(6) 1.00057(6) -0.07364(5) 0.01936(18) Uani 1 1 d . . . . .
N1 N 0.3313(2) 0.7874(2) -0.11224(18) 0.0182(6) Uani 1 1 d . . . . .
C1 C 0.2686(3) 0.8271(3) -0.1976(2) 0.0252(8) Uani 1 1 d . . . . .
H1A H 0.317729 0.861660 -0.218134 0.038 Uiso 1 1 calc GR . . . .
H1B H 0.213124 0.871622 -0.194658 0.038 Uiso 1 1 calc GR . . . .
H1C H 0.233673 0.774084 -0.236255 0.038 Uiso 1 1 calc GR . . . .
C2 C 0.4066(4) 0.7155(3) -0.1230(3) 0.0331(9) Uani 1 1 d . . . . .
H2A H 0.365782 0.669100 -0.166738 0.050 Uiso 1 1 calc GR . . . .
H2B H 0.443529 0.681297 -0.069652 0.050 Uiso 1 1 calc GR . . . .
H2C H 0.460310 0.748206 -0.139695 0.050 Uiso 1 1 calc GR . . . .
C3 C 0.2507(3) 0.7408(3) -0.0830(2) 0.0320(9) Uani 1 1 d . . . . .
H3A H 0.185376 0.782108 -0.098992 0.038 Uiso 1 1 calc R . . . .
H3B H 0.228547 0.677949 -0.111871 0.038 Uiso 1 1 calc R . . . .
C4 C 0.2944(4) 0.7252(3) 0.0091(3) 0.0314(9) Uani 1 1 d . . . . .
H4A H 0.358712 0.682654 0.024940 0.038 Uiso 1 1 calc R . . . .
H4B H 0.239095 0.692050 0.024727 0.038 Uiso 1 1 calc R . . . .
C5 C 0.2290(3) 0.8647(3) 0.0614(3) 0.0347(10) Uani 1 1 d . . . . .
H5A H 0.196234 0.822254 0.090844 0.052 Uiso 1 1 calc GR . . . .
H5B H 0.176503 0.877109 0.004172 0.052 Uiso 1 1 calc GR . . . .
H5C H 0.249745 0.925891 0.092053 0.052 Uiso 1 1 calc GR . . . .
C6 C 0.3955(3) 0.7929(3) 0.1455(3) 0.0342(10) Uani 1 1 d . . . . .
H6A H 0.417163 0.852154 0.178990 0.051 Uiso 1 1 calc GR . . . .
H6B H 0.460205 0.758837 0.146371 0.051 Uiso 1 1 calc GR . . . .
H6C H 0.355011 0.751355 0.169343 0.051 Uiso 1 1 calc GR . . . .
Ti2 Ti 0.09999(5) 0.41300(4) 0.03437(4) 0.01289(13) Uani 1 1 d . . . . .
Cl4 Cl 0.01303(7) 0.33686(6) 0.11109(5) 0.01835(17) Uani 1 1 d . . . . .
Cl5 Cl 0.07465(6) 0.57427(5) 0.08935(5) 0.01481(16) Uani 1 1 d . . . . .
Cl6 Cl 0.19038(7) 0.48554(6) -0.04257(5) 0.01826(17) Uani 1 1 d . . . . .
N2 N 0.2615(2) 0.3891(2) 0.14440(19) 0.0222(6) Uani 1 1 d . . . . .
C7 C 0.3475(3) 0.4575(4) 0.1485(3) 0.0376(10) Uani 1 1 d . . . . .
H7A H 0.323375 0.523443 0.152412 0.056 Uiso 1 1 calc GR . . . .
H7B H 0.363450 0.451223 0.097506 0.056 Uiso 1 1 calc GR . . . .
H7C H 0.412971 0.443331 0.198155 0.056 Uiso 1 1 calc GR . . . .
C8A C 0.2511(8) 0.4045(7) 0.2321(6) 0.0235(18) Uani 0.652(14) 1 d . . P A 1
H8AA H 0.194915 0.361586 0.236075 0.035 Uiso 0.652(14) 1 calc R . P A 1
H8AB H 0.320609 0.389713 0.277715 0.035 Uiso 0.652(14) 1 calc R . P A 1
H8AC H 0.231441 0.471723 0.236915 0.035 Uiso 0.652(14) 1 calc R . P A 1
C8B C 0.2651(14) 0.3679(14) 0.2205(10) 0.026(4) Uani 0.348(14) 1 d . . P A 2
H8BA H 0.206941 0.322307 0.215809 0.039 Uiso 0.348(14) 1 calc R . P A 2
H8BB H 0.335367 0.338710 0.253789 0.039 Uiso 0.348(14) 1 calc R . P A 2
H8BC H 0.255655 0.426999 0.248336 0.039 Uiso 0.348(14) 1 calc R . P A 2
C9A C 0.2858(5) 0.2852(4) 0.1424(4) 0.0200(16) Uani 0.652(14) 1 d . . P A 1
H9AA H 0.238522 0.246734 0.163063 0.024 Uiso 0.652(14) 1 calc R . P A 1
H9AB H 0.362207 0.272493 0.179562 0.024 Uiso 0.652(14) 1 calc R . P A 1
C10A C 0.2667(6) 0.2567(5) 0.0528(4) 0.0193(15) Uani 0.652(14) 1 d . . P A 1
H10A H 0.291172 0.189409 0.051790 0.023 Uiso 0.652(14) 1 calc R . P A 1
H10B H 0.309420 0.299181 0.030738 0.023 Uiso 0.652(14) 1 calc R . P A 1
C9B C 0.3106(9) 0.3055(8) 0.1053(9) 0.023(3) Uani 0.348(14) 1 d . . P A 2
H9BA H 0.333754 0.333177 0.061630 0.027 Uiso 0.348(14) 1 calc R . P A 2
H9BB H 0.375102 0.277274 0.150069 0.027 Uiso 0.348(14) 1 calc R . P A 2
C10B C 0.2297(11) 0.2297(9) 0.0677(8) 0.021(3) Uani 0.348(14) 1 d . . P A 2
H10C H 0.264269 0.174260 0.051447 0.026 Uiso 0.348(14) 1 calc R . P A 2
H10D H 0.200651 0.206971 0.109571 0.026 Uiso 0.348(14) 1 calc R . P A 2
N3 N 0.1442(2) 0.2653(2) -0.00404(18) 0.0182(6) Uani 1 1 d . . . . .
C11 C 0.1453(4) 0.2613(3) -0.0894(2) 0.0295(9) Uani 1 1 d . . . . .
H11A H 0.195391 0.310174 -0.094714 0.044 Uiso 1 1 calc GR . . . .
H11B H 0.072237 0.273839 -0.131074 0.044 Uiso 1 1 calc GR . . . .
H11C H 0.169143 0.197129 -0.099259 0.044 Uiso 1 1 calc GR . . . .
C12A C 0.0889(7) 0.1801(5) 0.0105(5) 0.0194(15) Uani 0.652(14) 1 d . . P A 1
H12A H 0.088276 0.183006 0.067381 0.029 Uiso 0.652(14) 1 calc R . P A 1
H12B H 0.014189 0.178425 -0.031079 0.029 Uiso 0.652(14) 1 calc R . P A 1
H12C H 0.127174 0.121734 0.005019 0.029 Uiso 0.652(14) 1 calc R . P A 1
C12B C 0.0448(13) 0.1938(9) -0.0239(11) 0.025(3) Uani 0.348(14) 1 d . . P A 2
H12D H -0.016105 0.216739 -0.073654 0.037 Uiso 0.348(14) 1 calc R . P A 2
H12E H 0.066071 0.129139 -0.034896 0.037 Uiso 0.348(14) 1 calc R . P A 2
H12F H 0.023082 0.191459 0.024490 0.037 Uiso 0.348(14) 1 calc R . P A 2
C13 C 0.3350(3) 0.0914(3) 0.3221(2) 0.0293(9) Uani 1 1 d . . . . .
H13A H 0.325450 0.161614 0.327221 0.035 Uiso 1 1 calc R . . . .
H13B H 0.265855 0.058980 0.314696 0.035 Uiso 1 1 calc R . . . .
Cl7 Cl 0.36811(10) 0.06849(9) 0.23340(7) 0.0449(3) Uani 1 1 d . . . . .
Cl8 Cl 0.43804(8) 0.04869(7) 0.41392(6) 0.0324(2) Uani 1 1 d . . . . .
C14 C 0.0131(3) 0.5036(3) 0.7363(2) 0.0239(8) Uani 1 1 d . . . . .
H14A H 0.027602 0.503316 0.797340 0.029 Uiso 1 1 calc R . . . .
H14B H -0.061814 0.527167 0.705840 0.029 Uiso 1 1 calc R . . . .
Cl9 Cl 0.10551(9) 0.58221(7) 0.71687(7) 0.0360(2) Uani 1 1 d . . . . .
Cl10 Cl 0.02507(8) 0.38490(7) 0.70294(6) 0.0289(2) Uani 1 1 d . . . . .
N4 N 0.3258(2) 0.8179(2) 0.05732(18) 0.0178(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 Cl1 2.3182(10) . ?
Ti1 Cl2 2.4808(10) 3_675 ?
Ti1 Cl2 2.4864(10) . ?
Ti1 Cl3 2.3216(10) . ?
Ti1 N1 2.286(3) . ?
Ti1 N4 2.299(3) . ?
N1 C1 1.487(4) . ?
N1 C2 1.477(5) . ?
N1 C3 1.496(5) . ?
C3 C4 1.476(6) . ?
C4 N4 1.498(5) . ?
C5 N4 1.472(5) . ?
C6 N4 1.483(5) . ?
Ti2 Cl4 2.3158(10) . ?
Ti2 Cl5 2.4882(10) 3_565 ?
Ti2 Cl5 2.4984(10) . ?
Ti2 Cl6 2.3299(10) . ?
Ti2 N2 2.283(3) . ?
Ti2 N3 2.295(3) . ?
N2 C7 1.469(5) . ?
N2 C8A 1.578(9) . ?
N2 C8B 1.322(17) . ?
N2 C9A 1.479(6) . ?
N2 C9B 1.600(12) . ?
C9A C10A 1.513(10) . ?
C10A N3 1.556(7) . ?
C9B C10B 1.47(2) . ?
C10B N3 1.409(11) . ?
N3 C11 1.473(4) . ?
N3 C12A 1.463(7) . ?
N3 C12B 1.584(14) . ?
C13 Cl7 1.769(4) . ?
C13 Cl8 1.751(4) . ?
C14 Cl9 1.770(4) . ?
C14 Cl10 1.769(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Ti1 Cl2 89.96(4) . 3_675 ?
Cl1 Ti1 Cl2 89.48(4) . . ?
Cl1 Ti1 Cl3 177.87(4) . . ?
Cl2 Ti1 Cl2 91.50(4) 3_675 . ?
Cl3 Ti1 Cl2 92.12(4) . 3_675 ?
Cl3 Ti1 Cl2 90.00(4) . . ?
N1 Ti1 Cl1 91.14(8) . . ?
N1 Ti1 Cl2 92.43(8) . 3_675 ?
N1 Ti1 Cl2 176.02(8) . . ?
N1 Ti1 Cl3 89.23(8) . . ?
N1 Ti1 N4 80.70(10) . . ?
N4 Ti1 Cl1 87.76(8) . . ?
N4 Ti1 Cl2 172.71(8) . 3_675 ?
N4 Ti1 Cl2 95.40(8) . . ?
N4 Ti1 Cl3 90.23(8) . . ?
Ti1 Cl2 Ti1 88.50(4) 3_675 . ?
C1 N1 Ti1 113.9(2) . . ?
C1 N1 C3 106.5(3) . . ?
C2 N1 Ti1 114.2(2) . . ?
C2 N1 C1 106.2(3) . . ?
C2 N1 C3 111.2(3) . . ?
C3 N1 Ti1 104.7(2) . . ?
C4 C3 N1 112.5(3) . . ?
C3 C4 N4 112.3(3) . . ?
Cl4 Ti2 Cl5 91.32(4) . . ?
Cl4 Ti2 Cl5 90.46(4) . 3_565 ?
Cl4 Ti2 Cl6 178.34(4) . . ?
Cl5 Ti2 Cl5 92.36(3) 3_565 . ?
Cl6 Ti2 Cl5 90.15(4) . . ?
Cl6 Ti2 Cl5 90.27(4) . 3_565 ?
N2 Ti2 Cl4 89.05(9) . . ?
N2 Ti2 Cl5 175.42(8) . 3_565 ?
N2 Ti2 Cl5 92.21(8) . . ?
N2 Ti2 Cl6 90.10(9) . . ?
N2 Ti2 N3 80.99(11) . . ?
N3 Ti2 Cl4 89.81(8) . . ?
N3 Ti2 Cl5 173.08(8) . . ?
N3 Ti2 Cl5 94.46(8) . 3_565 ?
N3 Ti2 Cl6 88.64(8) . . ?
Ti2 Cl5 Ti2 87.64(3) 3_565 . ?
C7 N2 Ti2 114.8(2) . . ?
C7 N2 C8A 102.7(4) . . ?
C7 N2 C9A 117.0(4) . . ?
C7 N2 C9B 92.8(6) . . ?
C8A N2 Ti2 111.8(4) . . ?
C8B N2 Ti2 121.1(8) . . ?
C8B N2 C7 111.3(8) . . ?
C8B N2 C9B 112.8(9) . . ?
C9A N2 Ti2 105.6(3) . . ?
C9A N2 C8A 104.7(4) . . ?
C9B N2 Ti2 99.6(4) . . ?
N2 C9A C10A 109.0(6) . . ?
C9A C10A N3 110.2(6) . . ?
C10B C9B N2 110.6(11) . . ?
N3 C10B C9B 110.4(12) . . ?
C10A N3 Ti2 102.2(3) . . ?
C10B N3 Ti2 105.8(5) . . ?
C10B N3 C11 122.9(7) . . ?
C10B N3 C12B 107.6(8) . . ?
C11 N3 Ti2 114.9(2) . . ?
C11 N3 C10A 102.3(4) . . ?
C11 N3 C12B 95.1(6) . . ?
C12A N3 Ti2 117.9(3) . . ?
C12A N3 C10A 108.0(4) . . ?
C12A N3 C11 109.7(4) . . ?
C12B N3 Ti2 109.5(5) . . ?
Cl8 C13 Cl7 110.2(2) . . ?
Cl10 C14 Cl9 110.8(2) . . ?
C4 N4 Ti1 103.8(2) . . ?
C5 N4 Ti1 115.6(2) . . ?
C5 N4 C4 109.8(3) . . ?
C5 N4 C6 105.8(3) . . ?
C6 N4 Ti1 114.2(2) . . ?
C6 N4 C4 107.4(3) . . ?

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 N1 C3 C4 -41.2(4) . . . . ?
N1 C3 C4 N4 61.0(5) . . . . ?
C1 N1 C3 C4 -162.2(3) . . . . ?
C2 N1 C3 C4 82.5(4) . . . . ?
C3 C4 N4 Ti1 -43.2(4) . . . . ?
C3 C4 N4 C5 81.0(4) . . . . ?
C3 C4 N4 C6 -164.4(3) . . . . ?
Ti2 N2 C9A C10A 46.3(6) . . . . ?
Ti2 N2 C9B C10B -47.6(13) . . . . ?
N2 C9A C10A N3 -66.1(8) . . . . ?
N2 C9B C10B N3 67.6(17) . . . . ?
C7 N2 C9A C10A -82.8(6) . . . . ?
C7 N2 C9B C10B -163.3(12) . . . . ?
C8A N2 C9A C10A 164.4(6) . . . . ?
C8B N2 C9B C10B 82.1(15) . . . . ?
C9A C10A N3 Ti2 46.0(6) . . . . ?
C9A C10A N3 C11 165.2(6) . . . . ?
C9A C10A N3 C12A -79.0(7) . . . . ?
C9B C10B N3 Ti2 -45.5(14) . . . . ?
C9B C10B N3 C11 89.2(11) . . . . ?
C9B C10B N3 C12B -162.4(12) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane/hexane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_TiCl3tmedathf
_database_code_depnum_ccdc_archive 'CCDC 2045303'
loop_
_audit_author_name
_audit_author_address
'Takashi Kurogi'
;Okayama University
Japan
;
_audit_update_record             
;
2020-11-19 deposited with the CCDC.	2021-01-19 downloaded from the CCDC.
;
_audit_creation_date             2020-01-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_formula_moiety         'C10 H24 Cl3 N2 O Ti'
_chemical_formula_sum            'C10 H24 Cl3 N2 O Ti'
_chemical_formula_weight         342.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.972(4)
_cell_length_b                   12.308(4)
_cell_length_c                   12.075(4)
_cell_angle_alpha                90
_cell_angle_beta                 101.587(6)
_cell_angle_gamma                90
_cell_volume                     1597.4(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4636
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_shelx_estimated_absorpt_T_max   0.932
_shelx_estimated_absorpt_T_min   0.887
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18771
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.458
_diffrn_reflns_theta_min         3.257
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support Fiber
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC11 (Right): Eulerian 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_wavelength     0.71075
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2930
_reflns_number_total             3644
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3644
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0550
_refine_ls_restrained_S_all      1.085
_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)+(0.0633P)²+1.8356P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1447
_refine_special_details          ?
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.13895(5) 0.25396(5) 0.86972(5) 0.03503(18) Uani 1 1 d . . . . .
Cl1 Cl 0.16226(8) 0.35627(9) 1.03904(7) 0.0533(3) Uani 1 1 d . . . . .
Cl2 Cl 0.20747(9) 0.09331(9) 0.96866(11) 0.0704(3) Uani 1 1 d . . . . .
Cl3 Cl 0.12344(7) 0.16421(7) 0.69322(8) 0.0510(3) Uani 1 1 d . . . . .
N1 N -0.0637(3) 0.2165(3) 0.8730(3) 0.0510(7) Uani 1 1 d . . . . .
N2 N 0.0434(3) 0.4033(2) 0.7715(2) 0.0450(7) Uani 1 1 d . . . . .
C1 C -0.0928(4) 0.2125(4) 0.9867(4) 0.0739(14) Uani 1 1 d . . . . .
H1A H -0.077223 0.283809 1.022793 0.111 Uiso 1 1 calc GR . . . .
H1B H -0.040174 0.157904 1.032339 0.111 Uiso 1 1 calc GR . . . .
H1C H -0.180536 0.192991 0.980732 0.111 Uiso 1 1 calc GR . . . .
C2 C -0.1076(3) 0.1100(3) 0.8202(4) 0.0588(10) Uani 1 1 d . . . . .
H2A H -0.057207 0.051227 0.860755 0.088 Uiso 1 1 calc GR . . . .
H2B H -0.099200 0.109915 0.740890 0.088 Uiso 1 1 calc GR . . . .
H2C H -0.195033 0.099131 0.824233 0.088 Uiso 1 1 calc GR . . . .
C3A C -0.1412(10) 0.2934(10) 0.7817(9) 0.046(2) Uani 0.456(10) 1 d . U P A 1
H3A H -0.193857 0.247275 0.724010 0.055 Uiso 0.456(10) 1 calc R . P A 1
H3B H -0.197838 0.336457 0.818840 0.055 Uiso 0.456(10) 1 calc R . P A 1
C4A C -0.0853(7) 0.3558(8) 0.7332(8) 0.053(3) Uani 0.456(10) 1 d . U P A 1
H4A H -0.141003 0.419434 0.715372 0.063 Uiso 0.456(10) 1 calc R . P A 1
H4B H -0.083647 0.320577 0.659861 0.063 Uiso 0.456(10) 1 calc R . P A 1
C5A C 0.0497(12) 0.4988(10) 0.8261(10) 0.046(3) Uani 0.456(10) 1 d . U P A 1
H5A H 0.136702 0.522093 0.846977 0.069 Uiso 0.456(10) 1 calc R . P A 1
H5B H 0.001593 0.553435 0.776704 0.069 Uiso 0.456(10) 1 calc R . P A 1
H5C H 0.015352 0.490546 0.894566 0.069 Uiso 0.456(10) 1 calc R . P A 1
C6A C 0.0962(15) 0.4135(9) 0.6641(9) 0.063(3) Uani 0.456(10) 1 d . U P A 1
H6A H 0.090787 0.343106 0.625580 0.095 Uiso 0.456(10) 1 calc R . P A 1
H6B H 0.048227 0.467646 0.613902 0.095 Uiso 0.456(10) 1 calc R . P A 1
H6C H 0.183421 0.436379 0.684044 0.095 Uiso 0.456(10) 1 calc R . P A 1
C3B C -0.1320(9) 0.3158(11) 0.8315(12) 0.070(3) Uani 0.544(10) 1 d . U P A 2
H3C H -0.193779 0.293410 0.763873 0.084 Uiso 0.544(10) 1 calc R . P A 2
H3D H -0.180377 0.335111 0.889672 0.084 Uiso 0.544(10) 1 calc R . P A 2
C4B C -0.0863(6) 0.4054(6) 0.8045(8) 0.056(2) Uani 0.544(10) 1 d . U P A 2
H4C H -0.081320 0.456003 0.868952 0.067 Uiso 0.544(10) 1 calc R . P A 2
H4D H -0.146204 0.436805 0.740174 0.067 Uiso 0.544(10) 1 calc R . P A 2
C5B C 0.0994(10) 0.5160(10) 0.8174(13) 0.066(3) Uani 0.544(10) 1 d . U P A 2
H5D H 0.114990 0.515757 0.900217 0.099 Uiso 0.544(10) 1 calc R . P A 2
H5E H 0.177717 0.528460 0.792167 0.099 Uiso 0.544(10) 1 calc R . P A 2
H5F H 0.040324 0.573963 0.788468 0.099 Uiso 0.544(10) 1 calc R . P A 2
C6B C 0.0254(8) 0.4156(6) 0.6494(7) 0.0471(19) Uani 0.544(10) 1 d . U P A 2
H6D H 0.106416 0.414481 0.626859 0.071 Uiso 0.544(10) 1 calc R . P A 2
H6E H -0.025954 0.355700 0.612282 0.071 Uiso 0.544(10) 1 calc R . P A 2
H6F H -0.016259 0.484849 0.626748 0.071 Uiso 0.544(10) 1 calc R . P A 2
O1 O 0.31734(18) 0.3074(2) 0.85541(18) 0.0420(5) Uani 1 1 d . . . . .
C7A C 0.3938(8) 0.3900(7) 0.9148(8) 0.037(2) Uani 0.372(6) 1 d . U P B 1
H7A H 0.419527 0.372768 0.996259 0.045 Uiso 0.372(6) 1 calc R . P B 1
H7B H 0.352027 0.461728 0.905849 0.045 Uiso 0.372(6) 1 calc R . P B 1
C8A C 0.5042(11) 0.3856(8) 0.8541(13) 0.045(2) Uani 0.372(6) 1 d . U P B 1
H8A H 0.480081 0.406691 0.773551 0.055 Uiso 0.372(6) 1 calc R . P B 1
H8B H 0.574947 0.430891 0.892164 0.055 Uiso 0.372(6) 1 calc R . P B 1
C9A C 0.5313(7) 0.2667(7) 0.8685(9) 0.041(2) Uani 0.372(6) 1 d . U P B 1
H9A H 0.565071 0.248219 0.948539 0.049 Uiso 0.372(6) 1 calc R . P B 1
H9B H 0.590541 0.242590 0.821530 0.049 Uiso 0.372(6) 1 calc R . P B 1
C10A C 0.4015(7) 0.2168(7) 0.8271(8) 0.038(2) Uani 0.372(6) 1 d . U P B 1
H10A H 0.385431 0.201726 0.744902 0.046 Uiso 0.372(6) 1 calc R . P B 1
H10B H 0.391046 0.148947 0.868298 0.046 Uiso 0.372(6) 1 calc R . P B 1
C7B C 0.4202(5) 0.3169(8) 0.9458(5) 0.0583(19) Uani 0.628(6) 1 d . U P B 2
H7C H 0.440514 0.245315 0.982300 0.070 Uiso 0.628(6) 1 calc R . P B 2
H7D H 0.401161 0.368236 1.003044 0.070 Uiso 0.628(6) 1 calc R . P B 2
C8B C 0.5293(7) 0.3583(10) 0.8978(7) 0.069(2) Uani 0.628(6) 1 d . U P B 2
H8C H 0.540375 0.437402 0.911089 0.083 Uiso 0.628(6) 1 calc R . P B 2
H8D H 0.606928 0.320837 0.933973 0.083 Uiso 0.628(6) 1 calc R . P B 2
C9B C 0.5004(5) 0.3357(6) 0.7798(5) 0.0500(15) Uani 0.628(6) 1 d . U P B 2
H9C H 0.528993 0.262080 0.764127 0.060 Uiso 0.628(6) 1 calc R . P B 2
H9D H 0.540290 0.389450 0.737408 0.060 Uiso 0.628(6) 1 calc R . P B 2
C10B C 0.3620(4) 0.3436(5) 0.7476(4) 0.0407(13) Uani 0.628(6) 1 d . U P B 2
H10C H 0.328945 0.294933 0.683268 0.049 Uiso 0.628(6) 1 calc R . P B 2
H10D H 0.335504 0.419022 0.726718 0.049 Uiso 0.628(6) 1 calc R . P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 Cl1 2.3709(11) . ?
Ti1 Cl2 2.3539(13) . ?
Ti1 Cl3 2.3760(11) . ?
Ti1 N1 2.279(3) . ?
Ti1 N2 2.321(3) . ?
Ti1 O1 2.105(2) . ?
N1 C1 1.472(5) . ?
N1 C2 1.494(5) . ?
N1 C3A 1.568(12) . ?
N1 C3B 1.469(12) . ?
N2 C4A 1.513(9) . ?
N2 C5A 1.343(12) . ?
N2 C6A 1.527(10) . ?
N2 C4B 1.553(7) . ?
N2 C5B 1.572(11) . ?
N2 C6B 1.456(9) . ?
C3A C4A 1.205(15) . ?
C3B C4B 1.281(14) . ?
O1 C7A 1.418(8) . ?
O1 C10A 1.530(8) . ?
O1 C7B 1.408(6) . ?
O1 C10B 1.546(5) . ?
C7A C8A 1.539(15) . ?
C8A C9A 1.496(14) . ?
C9A C10A 1.540(11) . ?
C7B C8B 1.518(10) . ?
C8B C9B 1.424(10) . ?
C9B C10B 1.493(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Ti1 Cl3 175.07(4) . . ?
Cl2 Ti1 Cl1 92.31(5) . . ?
Cl2 Ti1 Cl3 91.31(5) . . ?
N1 Ti1 Cl1 91.67(9) . . ?
N1 Ti1 Cl2 91.97(9) . . ?
N1 Ti1 Cl3 91.56(9) . . ?
N1 Ti1 N2 80.06(11) . . ?
N2 Ti1 Cl1 88.82(8) . . ?
N2 Ti1 Cl2 171.98(8) . . ?
N2 Ti1 Cl3 88.06(8) . . ?
O1 Ti1 Cl1 87.93(6) . . ?
O1 Ti1 Cl2 95.55(8) . . ?
O1 Ti1 Cl3 88.39(6) . . ?
O1 Ti1 N1 172.49(11) . . ?
O1 Ti1 N2 92.43(10) . . ?
C1 N1 Ti1 114.7(2) . . ?
C1 N1 C2 104.9(3) . . ?
C1 N1 C3A 119.2(5) . . ?
C2 N1 Ti1 113.7(2) . . ?
C2 N1 C3A 98.4(5) . . ?
C3A N1 Ti1 105.0(5) . . ?
C3B N1 Ti1 105.0(5) . . ?
C3B N1 C1 98.9(6) . . ?
C3B N1 C2 119.1(6) . . ?
C4A N2 Ti1 98.5(4) . . ?
C4A N2 C6A 105.2(7) . . ?
C5A N2 Ti1 118.0(6) . . ?
C5A N2 C4A 116.1(6) . . ?
C5A N2 C6A 110.8(7) . . ?
C6A N2 Ti1 106.8(5) . . ?
C4B N2 Ti1 103.0(3) . . ?
C4B N2 C5B 102.0(5) . . ?
C5B N2 Ti1 114.5(5) . . ?
C6B N2 Ti1 123.7(4) . . ?
C6B N2 C4B 108.3(5) . . ?
C6B N2 C5B 103.3(7) . . ?
C4A C3A N1 118.0(8) . . ?
C3A C4A N2 129.3(8) . . ?
C4B C3B N1 127.2(8) . . ?
C3B C4B N2 118.5(6) . . ?
C7A O1 Ti1 130.4(4) . . ?
C7A O1 C10A 108.3(5) . . ?
C10A O1 Ti1 113.8(3) . . ?
C7B O1 Ti1 125.2(3) . . ?
C7B O1 C10B 106.8(3) . . ?
C10B O1 Ti1 128.1(2) . . ?
O1 C7A C8A 100.1(7) . . ?
C9A C8A C7A 97.8(8) . . ?
C8A C9A C10A 101.8(7) . . ?
O1 C10A C9A 101.3(6) . . ?
O1 C7B C8B 107.6(5) . . ?
C9B C8B C7B 106.4(6) . . ?
C8B C9B C10B 105.0(5) . . ?
C9B C10B O1 103.9(4) . . ?

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 N1 C3A C4A -2.4(11) . . . . ?
Ti1 N1 C3B C4B -2.9(14) . . . . ?
Ti1 N2 C4A C3A 35.3(12) . . . . ?
Ti1 N2 C4B C3B -27.4(9) . . . . ?
Ti1 O1 C7A C8A -177.0(5) . . . . ?
Ti1 O1 C10A C9A -158.3(5) . . . . ?
Ti1 O1 C7B C8B -179.9(5) . . . . ?
Ti1 O1 C10B C9B -161.4(3) . . . . ?
N1 C3A C4A N2 -25.0(16) . . . . ?
N1 C3B C4B N2 22.7(17) . . . . ?
C1 N1 C3A C4A 127.8(9) . . . . ?
C1 N1 C3B C4B 115.8(13) . . . . ?
C2 N1 C3A C4A -119.8(9) . . . . ?
C2 N1 C3B C4B -131.5(11) . . . . ?
C5A N2 C4A C3A -91.7(13) . . . . ?
C6A N2 C4A C3A 145.4(12) . . . . ?
C5B N2 C4B C3B -146.4(10) . . . . ?
C6B N2 C4B C3B 105.1(10) . . . . ?
O1 C7A C8A C9A -53.3(10) . . . . ?
O1 C7B C8B C9B -19.9(11) . . . . ?
C7A O1 C10A C9A -5.3(8) . . . . ?
C7A C8A C9A C10A 49.9(10) . . . . ?
C8A C9A C10A O1 -28.7(10) . . . . ?
C10A O1 C7A C8A 36.0(8) . . . . ?
C7B O1 C10B C9B 18.7(6) . . . . ?
C7B C8B C9B C10B 31.5(10) . . . . ?
C8B C9B C10B O1 -31.0(8) . . . . ?
C10B O1 C7B C8B 0.0(8) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF/hexane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_Ti2CH2Cl4tmeda
_database_code_depnum_ccdc_archive 'CCDC 2045301'
loop_
_audit_author_name
_audit_author_address
'Takashi Kurogi'
;Okayama University
Japan
;
_audit_update_record             
;
2020-11-19 deposited with the CCDC.	2021-01-19 downloaded from the CCDC.
;
_audit_creation_date             2020-01-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_formula_moiety         'C13 H34 Cl4 N4 Ti2'
_chemical_formula_sum            'C13 H34 Cl4 N4 Ti2'
_chemical_formula_weight         484.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.348(11)
_cell_length_b                   8.843(4)
_cell_length_c                   12.648(6)
_cell_angle_alpha                90
_cell_angle_beta                 121.198(6)
_cell_angle_gamma                90
_cell_volume                     2233.7(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3252
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_shelx_estimated_absorpt_T_max   0.988
_shelx_estimated_absorpt_T_min   0.890
_exptl_absorpt_coefficient_mu    1.196
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9148
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.465
_diffrn_reflns_theta_min         3.223
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support Fiber
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC11 (Right): Eulerian 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_wavelength     0.71075
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2217
_reflns_number_total             2548
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         4.149
_refine_diff_density_min         -1.211
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         2548
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0768
_refine_ls_restrained_S_all      1.055
_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)+(0.0970P)²+30.5438P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1988
_refine_ls_wR_factor_ref         0.2057
_refine_special_details          ?
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.43505(4) 0.20539(10) 0.20584(8) 0.0196(3) Uani 1 1 d . . . . .
Cl1 Cl 0.35324(6) 0.30492(14) 0.00614(11) 0.0265(3) Uani 1 1 d . . . . .
Cl2 Cl 0.51717(6) 0.06513(14) 0.39285(11) 0.0240(3) Uani 1 1 d . . . . .
C1 C 0.500000 0.3880(8) 0.250000 0.0252(14) Uani 1 2 d S T P . .
H1 H 0.468(4) 0.458(8) 0.178(7) 0.05(2) Uiso 1 1 d . . . . .
N1 N 0.3879(2) 0.3057(5) 0.3081(4) 0.0247(9) Uani 1 1 d . . . . .
N2 N 0.3591(2) 0.0065(5) 0.1875(4) 0.0237(9) Uani 1 1 d . . . . .
C2 C 0.3246(3) 0.2189(7) 0.2688(6) 0.0375(13) Uani 1 1 d . . . . .
H2A H 0.307803 0.244242 0.324236 0.045 Uiso 1 1 calc R . . . .
H2B H 0.289943 0.248805 0.183698 0.045 Uiso 1 1 calc R . . . .
C3 C 0.3364(3) 0.0534(7) 0.2728(7) 0.0396(14) Uani 1 1 d . . . . .
H3A H 0.370719 0.023914 0.358245 0.047 Uiso 1 1 calc R . . . .
H3B H 0.294479 -0.000740 0.250370 0.047 Uiso 1 1 calc R . . . .
C4 C 0.3650(3) 0.4640(7) 0.2650(6) 0.0394(14) Uani 1 1 d . . . . .
H4A H 0.339302 0.501091 0.301118 0.059 Uiso 1 1 calc GR . . . .
H4B H 0.336736 0.465347 0.174694 0.059 Uiso 1 1 calc GR . . . .
H4C H 0.404057 0.529251 0.291156 0.059 Uiso 1 1 calc GR . . . .
C5 C 0.4321(3) 0.3153(7) 0.4440(5) 0.0355(13) Uani 1 1 d . . . . .
H5A H 0.409574 0.372996 0.478246 0.053 Uiso 1 1 calc GR . . . .
H5B H 0.473925 0.365970 0.464543 0.053 Uiso 1 1 calc GR . . . .
H5C H 0.441944 0.213130 0.479132 0.053 Uiso 1 1 calc GR . . . .
C6 C 0.3019(3) -0.0085(7) 0.0601(6) 0.0406(14) Uani 1 1 d . . . . .
H6A H 0.272317 -0.089609 0.056641 0.061 Uiso 1 1 calc GR . . . .
H6B H 0.318232 -0.032895 0.004728 0.061 Uiso 1 1 calc GR . . . .
H6C H 0.276949 0.086905 0.034133 0.061 Uiso 1 1 calc GR . . . .
C7 C 0.3890(3) -0.1467(6) 0.2273(7) 0.0413(15) Uani 1 1 d . . . . .
H7A H 0.354537 -0.218127 0.217754 0.062 Uiso 1 1 calc GR . . . .
H7B H 0.425205 -0.143426 0.314141 0.062 Uiso 1 1 calc GR . . . .
H7C H 0.406977 -0.179528 0.176112 0.062 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 Ti1 2.634(2) 2_655 ?
Ti1 Cl1 2.4093(16) . ?
Ti1 Cl2 2.4049(15) 2_655 ?
Ti1 Cl2 2.4720(15) . ?
Ti1 C1 2.084(6) . ?
Ti1 N1 2.268(4) . ?
Ti1 N2 2.422(4) . ?
N1 C2 1.504(7) . ?
N1 C4 1.497(7) . ?
N1 C5 1.479(7) . ?
N2 C3 1.486(7) . ?
N2 C6 1.473(7) . ?
N2 C7 1.488(7) . ?
C2 C3 1.486(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Ti1 Ti1 123.92(6) . 2_655 ?
Cl1 Ti1 Cl2 170.81(6) . . ?
Cl1 Ti1 N2 91.22(11) . . ?
Cl2 Ti1 Ti1 58.55(4) 2_655 2_655 ?
Cl2 Ti1 Ti1 56.09(4) . 2_655 ?
Cl2 Ti1 Cl1 88.47(6) 2_655 . ?
Cl2 Ti1 Cl2 84.23(7) 2_655 . ?
Cl2 Ti1 N2 95.14(11) 2_655 . ?
C1 Ti1 Ti1 50.81(13) . 2_655 ?
C1 Ti1 Cl1 93.98(10) . . ?
C1 Ti1 Cl2 94.01(11) . 2_655 ?
C1 Ti1 Cl2 92.08(11) . . ?
C1 Ti1 N1 92.55(15) . . ?
C1 Ti1 N2 169.59(12) . . ?
N1 Ti1 Ti1 123.39(12) . 2_655 ?
N1 Ti1 Cl1 95.71(13) . . ?
N1 Ti1 Cl2 171.96(12) . 2_655 ?
N1 Ti1 Cl2 90.90(12) . . ?
N1 Ti1 N2 77.94(15) . . ?
N2 Ti1 Ti1 131.76(10) . 2_655 ?
N2 Ti1 Cl2 83.91(11) . . ?
Ti1 Cl2 Ti1 65.36(6) 2_655 . ?
Ti1 C1 Ti1 78.4(3) 2_655 . ?
C2 N1 Ti1 107.2(3) . . ?
C4 N1 Ti1 110.2(3) . . ?
C4 N1 C2 104.6(5) . . ?
C5 N1 Ti1 115.7(3) . . ?
C5 N1 C2 112.8(5) . . ?
C5 N1 C4 105.8(4) . . ?
C3 N2 Ti1 104.3(3) . . ?
C3 N2 C7 106.9(5) . . ?
C6 N2 Ti1 112.0(3) . . ?
C6 N2 C3 111.0(5) . . ?
C6 N2 C7 106.8(5) . . ?
C7 N2 Ti1 115.9(3) . . ?
C3 C2 N1 111.0(5) . . ?
N2 C3 C2 112.3(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 N1 C2 C3 47.0(6) . . . . ?
Ti1 N2 C3 C2 39.5(6) . . . . ?
N1 C2 C3 N2 -61.5(7) . . . . ?
C4 N1 C2 C3 164.1(5) . . . . ?
C5 N1 C2 C3 -81.5(6) . . . . ?
C6 N2 C3 C2 -81.2(6) . . . . ?
C7 N2 C3 C2 162.7(5) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF/hexane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_ZnICltmeda
_database_code_depnum_ccdc_archive 'CCDC 2045305'
loop_
_audit_author_name
_audit_author_address
'Takashi Kurogi'
;Okayama University
Japan
;
_audit_update_record             
;
2020-11-19 deposited with the CCDC.	2021-01-19 downloaded from the CCDC.
;
_audit_creation_date             2020-01-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_formula_moiety         'C6 H16 Cl I N2 Zn'
_chemical_formula_sum            'C6 H16 Cl I N2 Zn'
_chemical_formula_weight         343.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.149(11)
_cell_length_b                   7.256(3)
_cell_length_c                   15.032(7)
_cell_angle_alpha                90
_cell_angle_beta                 111.169(6)
_cell_angle_gamma                90
_cell_volume                     2354.5(18)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    4087
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.8
_shelx_estimated_absorpt_T_max   0.696
_shelx_estimated_absorpt_T_min   0.548
_exptl_absorpt_coefficient_mu    4.888
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11250
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.511
_diffrn_reflns_theta_min         2.837
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support Fiber
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC11 (Right): Eulerian 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_wavelength     0.71075
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2415
_reflns_number_total             2707
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         0.843
_refine_diff_density_min         -1.159
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         2707
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0227
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0294P)²+4.3358P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0613
_refine_special_details          ?
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Zn1 Zn 0.36176(2) 0.26973(4) 0.42111(2) 0.01428(9) Uani 1 1 d . . . . .
I1 I 0.43597(2) 0.18268(3) 0.33833(2) 0.02463(8) Uani 1 1 d . . . . .
Cl1 Cl 0.28013(3) 0.08628(9) 0.39951(5) 0.01768(15) Uani 1 1 d . . . . .
N1 N 0.33551(11) 0.5473(3) 0.40732(17) 0.0169(5) Uani 1 1 d . . . . .
N2 N 0.40531(11) 0.3170(3) 0.56806(17) 0.0162(5) Uani 1 1 d . . . . .
C1 C 0.26790(13) 0.5657(4) 0.3860(2) 0.0214(6) Uani 1 1 d . . . . .
H1A H 0.257120 0.696387 0.385313 0.032 Uiso 1 1 calc GR . . . .
H1B H 0.256988 0.501576 0.435153 0.032 Uiso 1 1 calc GR . . . .
H1C H 0.245011 0.511077 0.323529 0.032 Uiso 1 1 calc GR . . . .
C2 C 0.35074(15) 0.6468(4) 0.3329(2) 0.0224(6) Uani 1 1 d . . . . .
H2A H 0.395242 0.636241 0.345794 0.027 Uiso 1 1 calc R . . . .
H2B H 0.327454 0.593144 0.270350 0.027 Uiso 1 1 calc R . . . .
H2C H 0.339640 0.777094 0.333195 0.027 Uiso 1 1 calc R . . . .
C3 C 0.37153(15) 0.6280(4) 0.5023(2) 0.0229(6) Uani 1 1 d . . . . .
H3A H 0.350838 0.741800 0.511725 0.027 Uiso 1 1 calc R . . . .
H3B H 0.413502 0.661507 0.504620 0.027 Uiso 1 1 calc R . . . .
C4 C 0.37677(15) 0.4930(4) 0.5816(2) 0.0227(7) Uani 1 1 d . . . . .
H4A H 0.402292 0.548012 0.643633 0.027 Uiso 1 1 calc R . . . .
H4B H 0.335035 0.468221 0.582895 0.027 Uiso 1 1 calc R . . . .
C5 C 0.47286(14) 0.3358(4) 0.5961(2) 0.0227(7) Uani 1 1 d . . . . .
H5A H 0.482129 0.433307 0.558163 0.034 Uiso 1 1 calc GR . . . .
H5B H 0.490385 0.219017 0.584981 0.034 Uiso 1 1 calc GR . . . .
H5C H 0.491061 0.367741 0.663967 0.034 Uiso 1 1 calc GR . . . .
C6 C 0.39246(16) 0.1712(4) 0.6271(2) 0.0251(7) Uani 1 1 d . . . . .
H6A H 0.347581 0.157034 0.609186 0.030 Uiso 1 1 calc R . . . .
H6B H 0.410369 0.054532 0.616608 0.030 Uiso 1 1 calc R . . . .
H6C H 0.410915 0.205356 0.694585 0.030 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
Zn1 I1 2.5380(9) . ?
Zn1 Cl1 2.2372(11) . ?
Zn1 N1 2.093(3) . ?
Zn1 N2 2.099(3) . ?
N1 C1 1.486(4) . ?
N1 C2 1.477(4) . ?
N1 C3 1.489(4) . ?
N2 C4 1.485(4) . ?
N2 C5 1.472(4) . ?
N2 C6 1.479(4) . ?
C3 C4 1.513(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Zn1 I1 117.81(3) . . ?
N1 Zn1 I1 114.50(7) . . ?
N1 Zn1 Cl1 111.01(7) . . ?
N1 Zn1 N2 87.64(9) . . ?
N2 Zn1 I1 113.82(7) . . ?
N2 Zn1 Cl1 108.03(7) . . ?
C1 N1 Zn1 110.68(18) . . ?
C1 N1 C3 110.7(2) . . ?
C2 N1 Zn1 113.91(19) . . ?
C2 N1 C1 108.3(2) . . ?
C2 N1 C3 109.3(2) . . ?
C3 N1 Zn1 103.97(18) . . ?
C4 N2 Zn1 102.50(17) . . ?
C5 N2 Zn1 111.95(18) . . ?
C5 N2 C4 111.1(2) . . ?
C5 N2 C6 108.5(2) . . ?
C6 N2 Zn1 112.97(18) . . ?
C6 N2 C4 109.7(2) . . ?
N1 C3 C4 111.0(2) . . ?
N2 C4 C3 111.2(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zn1 N1 C3 C4 -36.8(3) . . . . ?
Zn1 N2 C4 C3 -42.3(3) . . . . ?
N1 C3 C4 N2 56.8(3) . . . . ?
C1 N1 C3 C4 82.1(3) . . . . ?
C2 N1 C3 C4 -158.7(3) . . . . ?
C5 N2 C4 C3 77.4(3) . . . . ?
C6 N2 C4 C3 -162.6(3) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Zn2CH2I2tmeda
_database_code_depnum_ccdc_archive 'CCDC 2045304'
loop_
_audit_author_name
_audit_author_address
'Takashi Kurogi'
;Okayama University
Japan
;
_audit_update_record             
;
2020-11-19 deposited with the CCDC.	2021-01-19 downloaded from the CCDC.
;
_audit_creation_date             2020-01-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_formula_moiety         'C13 H34 I2 N4 Zn2'
_chemical_formula_sum            'C13 H34 I2 N4 Zn2'
_chemical_formula_weight         630.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   11.494(2)
_cell_length_b                   13.090(2)
_cell_length_c                   14.921(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2245.0(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7777
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.7
_shelx_estimated_absorpt_T_max   0.867
_shelx_estimated_absorpt_T_min   0.696
_exptl_absorpt_coefficient_mu    4.887
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12448
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         2.730
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.984
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support Fiber
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC11 (Right): Eulerian 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_wavelength     0.71075
_reflns_Friedel_coverage         0.762
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                4216
_reflns_number_total             5031
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.157
_refine_ls_abs_structure_details 
;
 Flack x determined using 1511 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(19)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         5031
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0315
_refine_ls_restrained_S_all      1.008
_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)+(0.0173P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0630
_refine_special_details          ?
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Zn1 Zn 0.96818(6) 0.19977(6) 0.19202(5) 0.01694(18) Uani 1 1 d . . . . .
Zn2 Zn 0.73399(6) 0.26089(6) 0.29787(5) 0.01715(18) Uani 1 1 d . . . . .
I1 I 0.88773(4) 0.04537(4) 0.09611(3) 0.02683(12) Uani 1 1 d . . . . .
I2 I 0.63551(4) 0.37174(4) 0.16960(3) 0.02422(12) Uani 1 1 d . . . . .
C1 C 0.9031(6) 0.2409(5) 0.3094(5) 0.0181(15) Uani 1 1 d . . . . .
H1A H 0.944(6) 0.308(5) 0.330(5) 0.022(18) Uiso 1 1 d . . . . .
H1B H 0.914(6) 0.188(5) 0.352(5) 0.03(2) Uiso 1 1 d . . . . .
N1 N 1.1586(4) 0.1798(4) 0.1891(4) 0.0191(13) Uani 1 1 d . . . . .
N2 N 1.0057(5) 0.3214(4) 0.0972(4) 0.0188(12) Uani 1 1 d . . . . .
N3 N 0.6425(5) 0.3080(4) 0.4211(4) 0.0214(13) Uani 1 1 d . . . . .
N4 N 0.6255(5) 0.1278(4) 0.3085(4) 0.0204(12) Uani 1 1 d . . . . .
C2 C 1.1989(6) 0.1691(6) 0.2824(5) 0.0290(18) Uani 1 1 d . . . . .
H2A H 1.171301 0.103971 0.306842 0.044 Uiso 1 1 calc GR . . . .
H2B H 1.168075 0.225476 0.318450 0.044 Uiso 1 1 calc GR . . . .
H2C H 1.284130 0.170640 0.283855 0.044 Uiso 1 1 calc GR . . . .
C3 C 1.2002(6) 0.0934(6) 0.1361(5) 0.0264(17) Uani 1 1 d . . . . .
H3A H 1.285155 0.089265 0.140461 0.040 Uiso 1 1 calc GR . . . .
H3B H 1.177716 0.102883 0.073298 0.040 Uiso 1 1 calc GR . . . .
H3C H 1.165679 0.030158 0.159012 0.040 Uiso 1 1 calc GR . . . .
C4 C 1.2007(6) 0.2774(5) 0.1511(5) 0.0233(17) Uani 1 1 d . . . . .
H4A H 1.283060 0.269880 0.132836 0.028 Uiso 1 1 calc R . . . .
H4B H 1.196519 0.331343 0.197485 0.028 Uiso 1 1 calc R . . . .
C5 C 1.1287(6) 0.3086(6) 0.0710(5) 0.0242(16) Uani 1 1 d . . . . .
H5A H 1.158771 0.373686 0.046362 0.029 Uiso 1 1 calc R . . . .
H5B H 1.134761 0.255821 0.023762 0.029 Uiso 1 1 calc R . . . .
C6 C 0.9879(6) 0.4198(5) 0.1450(5) 0.0258(17) Uani 1 1 d . . . . .
H6A H 1.012799 0.476407 0.106478 0.039 Uiso 1 1 calc GR . . . .
H6B H 1.033820 0.420155 0.200317 0.039 Uiso 1 1 calc GR . . . .
H6C H 0.905277 0.427850 0.159662 0.039 Uiso 1 1 calc GR . . . .
C7 C 0.9328(6) 0.3208(6) 0.0159(5) 0.0273(18) Uani 1 1 d . . . . .
H7A H 0.956603 0.376804 -0.023700 0.041 Uiso 1 1 calc GR . . . .
H7B H 0.851032 0.329676 0.032695 0.041 Uiso 1 1 calc GR . . . .
H7C H 0.942417 0.255547 -0.015456 0.041 Uiso 1 1 calc GR . . . .
C8 C 0.7301(8) 0.3516(6) 0.4844(5) 0.036(2) Uani 1 1 d . . . . .
H8A H 0.760699 0.415645 0.459883 0.053 Uiso 1 1 calc GR . . . .
H8B H 0.794008 0.302844 0.492319 0.053 Uiso 1 1 calc GR . . . .
H8C H 0.693106 0.364824 0.542372 0.053 Uiso 1 1 calc GR . . . .
C9 C 0.5463(6) 0.3814(5) 0.4101(5) 0.0306(18) Uani 1 1 d . . . . .
H9A H 0.505365 0.389420 0.467326 0.046 Uiso 1 1 calc GR . . . .
H9B H 0.491914 0.355946 0.364692 0.046 Uiso 1 1 calc GR . . . .
H9C H 0.577507 0.447561 0.391080 0.046 Uiso 1 1 calc GR . . . .
C10 C 0.5977(6) 0.2092(5) 0.4565(5) 0.0220(16) Uani 1 1 d . . . . .
H10A H 0.540300 0.222457 0.504625 0.026 Uiso 1 1 calc R . . . .
H10B H 0.662693 0.169378 0.482533 0.026 Uiso 1 1 calc R . . . .
C11 C 0.5410(6) 0.1485(5) 0.3824(5) 0.0238(17) Uani 1 1 d . . . . .
H11A H 0.511811 0.082951 0.406684 0.029 Uiso 1 1 calc R . . . .
H11B H 0.473753 0.187054 0.358380 0.029 Uiso 1 1 calc R . . . .
C12 C 0.7003(6) 0.0390(5) 0.3333(5) 0.0256(16) Uani 1 1 d . . . . .
H12A H 0.651051 -0.020223 0.346542 0.038 Uiso 1 1 calc GR . . . .
H12B H 0.746552 0.056292 0.386359 0.038 Uiso 1 1 calc GR . . . .
H12C H 0.752415 0.022629 0.283351 0.038 Uiso 1 1 calc GR . . . .
C13 C 0.5633(6) 0.1014(6) 0.2251(5) 0.0272(17) Uani 1 1 d . . . . .
H13A H 0.619837 0.083674 0.178462 0.041 Uiso 1 1 calc GR . . . .
H13B H 0.516866 0.159991 0.205461 0.041 Uiso 1 1 calc GR . . . .
H13C H 0.512019 0.042921 0.236144 0.041 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 I1 2.6434(9) . ?
Zn1 C1 1.979(7) . ?
Zn1 N1 2.205(5) . ?
Zn1 N2 2.173(6) . ?
Zn2 I2 2.6551(10) . ?
Zn2 C1 1.969(7) . ?
Zn2 N3 2.206(5) . ?
Zn2 N4 2.149(5) . ?
N1 C2 1.474(9) . ?
N1 C3 1.460(9) . ?
N1 C4 1.478(8) . ?
N2 C5 1.476(8) . ?
N2 C6 1.487(9) . ?
N2 C7 1.475(8) . ?
N3 C8 1.494(9) . ?
N3 C9 1.474(9) . ?
N3 C10 1.489(8) . ?
N4 C11 1.495(8) . ?
N4 C12 1.492(8) . ?
N4 C13 1.475(8) . ?
C4 C5 1.510(9) . ?
C10 C11 1.511(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Zn1 I1 123.7(2) . . ?
C1 Zn1 N1 115.2(2) . . ?
C1 Zn1 N2 116.9(3) . . ?
N1 Zn1 I1 104.24(15) . . ?
N2 Zn1 I1 106.10(16) . . ?
N2 Zn1 N1 82.9(2) . . ?
C1 Zn2 I2 123.8(2) . . ?
C1 Zn2 N3 115.8(3) . . ?
C1 Zn2 N4 117.3(3) . . ?
N3 Zn2 I2 104.16(16) . . ?
N4 Zn2 I2 104.41(15) . . ?
N4 Zn2 N3 83.6(2) . . ?
Zn2 C1 Zn1 109.4(3) . . ?
C2 N1 Zn1 107.7(4) . . ?
C2 N1 C4 110.0(6) . . ?
C3 N1 Zn1 115.3(4) . . ?
C3 N1 C2 109.5(6) . . ?
C3 N1 C4 110.8(5) . . ?
C4 N1 Zn1 103.3(4) . . ?
C5 N2 Zn1 106.2(4) . . ?
C5 N2 C6 110.9(5) . . ?
C6 N2 Zn1 107.2(4) . . ?
C7 N2 Zn1 114.8(4) . . ?
C7 N2 C5 109.0(5) . . ?
C7 N2 C6 108.7(5) . . ?
C8 N3 Zn2 108.2(4) . . ?
C9 N3 Zn2 116.6(4) . . ?
C9 N3 C8 109.1(6) . . ?
C9 N3 C10 110.3(5) . . ?
C10 N3 Zn2 102.6(4) . . ?
C10 N3 C8 109.9(5) . . ?
C11 N4 Zn2 106.5(4) . . ?
C12 N4 Zn2 108.4(4) . . ?
C12 N4 C11 109.4(5) . . ?
C13 N4 Zn2 114.1(4) . . ?
C13 N4 C11 110.4(5) . . ?
C13 N4 C12 107.8(5) . . ?
N1 C4 C5 111.0(5) . . ?
N2 C5 C4 110.3(5) . . ?
N3 C10 C11 110.2(6) . . ?
N4 C11 C10 110.8(6) . . ?

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
Zn1 N1 C4 C5 -45.0(6) . . . . ?
Zn1 N2 C5 C4 -38.9(6) . . . . ?
Zn2 N3 C10 C11 -46.8(6) . . . . ?
Zn2 N4 C11 C10 -36.1(6) . . . . ?
N1 C4 C5 N2 59.8(8) . . . . ?
N3 C10 C11 N4 59.0(7) . . . . ?
C2 N1 C4 C5 -159.7(6) . . . . ?
C3 N1 C4 C5 79.1(7) . . . . ?
C6 N2 C5 C4 77.3(7) . . . . ?
C7 N2 C5 C4 -163.0(6) . . . . ?
C8 N3 C10 C11 -161.6(6) . . . . ?
C9 N3 C10 C11 78.1(7) . . . . ?
C12 N4 C11 C10 80.9(7) . . . . ?
C13 N4 C11 C10 -160.5(6) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
