# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_1b
_database_code_depnum_ccdc_archive 'CCDC 1056534'
_audit_update_record             
;
2015-03-27 deposited with the CCDC.
2015-05-07 downloaded from the CCDC.
;

_audit_creation_date             2012-05-10T18:01:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C32 H42 Cl2 N4 Ti2'
_chemical_formula_sum            'C32 H42 Cl2 N4 Ti2'
_chemical_formula_weight         649.4
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.570(2)
_cell_length_b                   16.1114(13)
_cell_length_c                   10.626(3)
_cell_angle_alpha                90
_cell_angle_beta                 111.075(17)
_cell_angle_gamma                90
_cell_volume                     1528.8(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    245
_cell_measurement_theta_min      3.17
_cell_measurement_theta_max      16.34
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             680
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 1 6 0.103
1 6 3 0.134
-4 -5 1 0.109
0 -4 -3 0.098
19 7 -18 0.128
4 -2 -1 0.108
-4 5 2 0.164
-1 4 -2 0.087
1 -4 2 0.198

_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_type   none

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.1192
_diffrn_reflns_av_unetI/netI     0.1135
_diffrn_reflns_number            10644
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.26
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_full        27.5
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_reflns_number_total             3490
_reflns_number_gt                2031
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0447P)²+3.3846P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3490
_refine_ls_number_parameters     181
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1532
_refine_ls_R_factor_gt           0.0695
_refine_ls_wR_factor_ref         0.1643
_refine_ls_wR_factor_gt          0.1309
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.002
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.108

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.53292(9) 0.05127(5) 0.89594(8) 0.0208(2) Uani 1 1 d . . .
Cl1 Cl 0.33622(14) 0.08907(8) 0.69641(13) 0.0338(3) Uani 1 1 d . . .
N1 N 0.5373(4) 0.0555(2) 1.0977(4) 0.0238(8) Uani 1 1 d . . .
N2 N 0.4811(4) 0.1713(2) 0.9740(4) 0.0257(9) Uani 1 1 d . . .
C1 C 0.5219(5) 0.1398(3) 1.0999(5) 0.0247(10) Uani 1 1 d . . .
C2 C 0.5462(5) 0.1921(3) 1.2097(5) 0.0299(11) Uani 1 1 d . . .
H2 H 0.5804 0.1714 1.2973 0.036 Uiso 1 1 calc R . .
C3 C 0.5179(6) 0.2761(3) 1.1847(5) 0.0339(12) Uani 1 1 d . . .
H3 H 0.5328 0.312 1.2569 0.041 Uiso 1 1 calc R . .
C4 C 0.4678(5) 0.3080(3) 1.0544(5) 0.0302(11) Uani 1 1 d . . .
C5 C 0.4527(5) 0.2518(3) 0.9517(5) 0.0276(11) Uani 1 1 d . . .
H5 H 0.4214 0.2712 0.8634 0.033 Uiso 1 1 calc R . .
C6 C 0.7510(5) 0.1350(3) 0.9121(5) 0.0284(11) Uani 1 1 d . . .
C7 C 0.7970(5) 0.0676(3) 1.0029(5) 0.0296(12) Uani 1 1 d . . .
C8 C 0.7701(5) -0.0070(3) 0.9275(5) 0.0276(11) Uani 1 1 d . . .
C9 C 0.7020(5) 0.0147(3) 0.7894(5) 0.0247(10) Uani 1 1 d . . .
C10 C 0.6911(5) 0.1020(3) 0.7805(5) 0.0257(10) Uani 1 1 d . . .
C11 C 0.7791(6) 0.2255(3) 0.9464(7) 0.0486(16) Uani 1 1 d . . .
H11A H 0.8202 0.232 1.0427 0.073 Uiso 1 1 calc R . .
H11B H 0.6866 0.2555 0.9106 0.073 Uiso 1 1 calc R . .
H11C H 0.8487 0.2468 0.908 0.073 Uiso 1 1 calc R . .
C12 C 0.8763(6) 0.0746(4) 1.1530(5) 0.0480(16) Uani 1 1 d . . .
H12A H 0.8944 0.0201 1.192 0.072 Uiso 1 1 calc R . .
H12B H 0.8152 0.1054 1.191 0.072 Uiso 1 1 calc R . .
H12C H 0.97 0.1028 1.1718 0.072 Uiso 1 1 calc R . .
C13 C 0.8185(6) -0.0910(3) 0.9863(6) 0.0403(14) Uani 1 1 d . . .
H13A H 0.8609 -0.0869 1.0828 0.06 Uiso 1 1 calc R . .
H13B H 0.8922 -0.1126 0.9531 0.06 Uiso 1 1 calc R . .
H13C H 0.7336 -0.1275 0.9608 0.06 Uiso 1 1 calc R . .
C14 C 0.6565(6) -0.0440(3) 0.6718(5) 0.0382(13) Uani 1 1 d . . .
H14A H 0.6746 -0.1 0.7042 0.057 Uiso 1 1 calc R . .
H14B H 0.7138 -0.0324 0.616 0.057 Uiso 1 1 calc R . .
H14C H 0.5518 -0.0369 0.6201 0.057 Uiso 1 1 calc R . .
C15 C 0.6359(6) 0.1526(3) 0.6546(6) 0.0428(14) Uani 1 1 d . . .
H15A H 0.6008 0.1165 0.5778 0.064 Uiso 1 1 calc R . .
H15B H 0.7161 0.1864 0.6489 0.064 Uiso 1 1 calc R . .
H15C H 0.5554 0.1876 0.6561 0.064 Uiso 1 1 calc R . .
C16 C 0.4375(6) 0.3991(3) 1.0269(6) 0.0443(15) Uani 1 1 d . . .
H16A H 0.4542 0.4277 1.1103 0.067 Uiso 1 1 calc R . .
H16B H 0.3356 0.4068 0.9678 0.067 Uiso 1 1 calc R . .
H16C H 0.5036 0.4208 0.9851 0.067 Uiso 1 1 calc R . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 1.857(4) 3_657 ?
Ti1 N1 2.131(4) . ?
Ti1 N2 2.229(4) . ?
Ti1 Cl1 2.3536(16) . ?
Ti1 C9 2.359(4) . ?
Ti1 C8 2.366(4) . ?
Ti1 C7 2.383(5) . ?
Ti1 C10 2.409(4) . ?
Ti1 C6 2.439(4) . ?
Ti1 C1 2.628(5) . ?
Ti1 Ti1 3.0030(17) 3_657 ?
N1 C1 1.368(6) . ?
N1 Ti1 1.857(4) 3_657 ?
N2 C5 1.328(6) . ?
N2 C1 1.350(6) . ?
C1 C2 1.389(7) . ?
C2 C3 1.387(7) . ?
C3 C4 1.390(7) . ?
C4 C5 1.386(7) . ?
C4 C16 1.504(6) . ?
C6 C10 1.411(7) . ?
C6 C7 1.414(7) . ?
C6 C11 1.503(7) . ?
C7 C8 1.416(7) . ?
C7 C12 1.505(7) . ?
C8 C9 1.419(7) . ?
C8 C13 1.492(7) . ?
C9 C10 1.412(6) . ?
C9 C14 1.501(7) . ?
C10 C15 1.492(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
N1 Ti1 N1 82.52(16) 3_657 . ?
N1 Ti1 N2 131.21(16) 3_657 . ?
N1 Ti1 N2 61.60(14) . . ?
N1 Ti1 Cl1 95.15(12) 3_657 . ?
N1 Ti1 Cl1 128.17(11) . . ?
N2 Ti1 Cl1 84.13(11) . . ?
N1 Ti1 C9 96.04(16) 3_657 . ?
N1 Ti1 C9 136.25(16) . . ?
N2 Ti1 C9 132.68(15) . . ?
Cl1 Ti1 C9 95.57(12) . . ?
N1 Ti1 C8 88.16(16) 3_657 . ?
N1 Ti1 C8 101.50(16) . . ?
N2 Ti1 C8 128.46(16) . . ?
Cl1 Ti1 C8 130.26(13) . . ?
C9 Ti1 C8 34.94(16) . . ?
N1 Ti1 C7 114.84(17) 3_657 . ?
N1 Ti1 C7 83.29(16) . . ?
N2 Ti1 C7 93.82(16) . . ?
Cl1 Ti1 C7 140.21(13) . . ?
C9 Ti1 C7 57.56(16) . . ?
C8 Ti1 C7 34.68(17) . . ?
N1 Ti1 C10 129.39(17) 3_657 . ?
N1 Ti1 C10 135.50(16) . . ?
N2 Ti1 C10 99.18(15) . . ?
Cl1 Ti1 C10 84.20(12) . . ?
C9 Ti1 C10 34.43(15) . . ?
C8 Ti1 C10 57.35(16) . . ?
C7 Ti1 C10 56.80(16) . . ?
N1 Ti1 C6 145.24(17) 3_657 . ?
N1 Ti1 C6 101.83(16) . . ?
N2 Ti1 C6 78.05(15) . . ?
Cl1 Ti1 C6 107.88(13) . . ?
C9 Ti1 C6 56.95(16) . . ?
C8 Ti1 C6 57.10(16) . . ?
C7 Ti1 C6 34.08(17) . . ?
C10 Ti1 C6 33.83(16) . . ?
N1 Ti1 C1 110.55(16) 3_657 . ?
N1 Ti1 C1 31.23(14) . . ?
N2 Ti1 C1 30.91(14) . . ?
Cl1 Ti1 C1 110.23(11) . . ?
C9 Ti1 C1 140.28(16) . . ?
C8 Ti1 C1 114.81(16) . . ?
C7 Ti1 C1 84.11(16) . . ?
C10 Ti1 C1 117.04(16) . . ?
C6 Ti1 C1 85.92(16) . . ?
N1 Ti1 Ti1 44.71(12) 3_657 3_657 ?
N1 Ti1 Ti1 37.81(10) . 3_657 ?
N2 Ti1 Ti1 94.01(11) . 3_657 ?
Cl1 Ti1 Ti1 119.61(6) . 3_657 ?
C9 Ti1 Ti1 125.28(12) . 3_657 ?
C8 Ti1 Ti1 96.99(12) . 3_657 ?
C7 Ti1 Ti1 100.19(13) . 3_657 ?
C10 Ti1 Ti1 153.97(12) . 3_657 ?
C6 Ti1 Ti1 130.80(13) . 3_657 ?
C1 Ti1 Ti1 67.07(11) . 3_657 ?
C1 N1 Ti1 151.3(3) . 3_657 ?
C1 N1 Ti1 94.9(3) . . ?
Ti1 N1 Ti1 97.48(16) 3_657 . ?
C5 N2 C1 120.7(4) . . ?
C5 N2 Ti1 147.0(3) . . ?
C1 N2 Ti1 91.1(3) . . ?
N2 C1 N1 110.6(4) . . ?
N2 C1 C2 120.4(4) . . ?
N1 C1 C2 129.0(5) . . ?
N2 C1 Ti1 58.0(2) . . ?
N1 C1 Ti1 53.9(2) . . ?
C2 C1 Ti1 167.8(3) . . ?
C1 C2 C3 117.9(5) . . ?
C2 C3 C4 121.7(5) . . ?
C5 C4 C3 116.3(4) . . ?
C5 C4 C16 121.8(5) . . ?
C3 C4 C16 121.8(5) . . ?
N2 C5 C4 122.8(5) . . ?
C10 C6 C7 107.6(4) . . ?
C10 C6 C11 125.4(5) . . ?
C7 C6 C11 126.5(5) . . ?
C10 C6 Ti1 71.9(3) . . ?
C7 C6 Ti1 70.8(3) . . ?
C11 C6 Ti1 128.9(3) . . ?
C8 C7 C6 108.6(4) . . ?
C8 C7 C12 125.7(5) . . ?
C6 C7 C12 125.5(5) . . ?
C8 C7 Ti1 72.0(3) . . ?
C6 C7 Ti1 75.1(3) . . ?
C12 C7 Ti1 123.9(3) . . ?
C7 C8 C9 107.3(4) . . ?
C7 C8 C13 124.6(5) . . ?
C9 C8 C13 127.9(5) . . ?
C7 C8 Ti1 73.3(3) . . ?
C9 C8 Ti1 72.3(3) . . ?
C13 C8 Ti1 123.9(3) . . ?
C10 C9 C8 108.1(4) . . ?
C10 C9 C14 125.4(4) . . ?
C8 C9 C14 126.4(4) . . ?
C10 C9 Ti1 74.7(3) . . ?
C8 C9 Ti1 72.8(3) . . ?
C14 C9 Ti1 120.8(3) . . ?
C6 C10 C9 108.4(4) . . ?
C6 C10 C15 124.7(5) . . ?
C9 C10 C15 126.8(5) . . ?
C6 C10 Ti1 74.3(3) . . ?
C9 C10 Ti1 70.9(3) . . ?
C15 C10 Ti1 123.9(3) . . ?
####################################################################### 
# 
# 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_2a
_database_code_depnum_ccdc_archive 'CCDC 1056535'
_audit_update_record             
;
2015-03-27 deposited with the CCDC.
2015-05-07 downloaded from the CCDC.
;

_audit_creation_date             2013-01-09T12:40:57-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C32 H43 Li1 N6 O1 Ti1'
_chemical_formula_sum            'C32 H43 Li N6 O Ti'
_chemical_formula_weight         582.56
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 1 21/n'
_space_group_name_Hall           '-P 2n'
_space_group_IT_number           14
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                   11.414(8)
_cell_length_b                   15.790(9)
_cell_length_c                   18.041(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                106.06(4)
_cell_volume                     3125(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    68
_cell_measurement_theta_min      3.15
_cell_measurement_theta_max      18.6
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1240
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 12 0.181
0 4 -3 0.134
0 1 -10 0.163
0 -2 -1 0.24
-2 2 -1 0.058
17 -16 6 0.095

_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.308
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_T_max  1.078

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.1
_diffrn_reflns_av_unetI/netI     0.0855
_diffrn_reflns_number            19158
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.43
_diffrn_reflns_theta_max         25.56
_diffrn_reflns_theta_full        25.56
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_reflns_number_total             5822
_reflns_number_gt                3933
_reflns_threshold_expression     >2σ(I)
_diffrn_reflns_reduction_process 
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0380P)²+9.5716P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5822
_refine_ls_number_parameters     402
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1334
_refine_ls_R_factor_gt           0.0844
_refine_ls_wR_factor_ref         0.1793
_refine_ls_wR_factor_gt          0.156
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.078

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.87511(7) 0.92757(5) 0.78338(4) 0.0227(2) Uani 1 1 d . . .
N1 N 0.7367(3) 0.8726(2) 0.82691(19) 0.0277(8) Uani 1 1 d . . .
N2 N 0.8268(3) 0.9363(3) 0.6751(2) 0.0291(9) Uani 1 1 d . . .
N3 N 0.9126(3) 1.0535(3) 0.8214(2) 0.0295(9) Uani 1 1 d . . .
N4 N 0.5968(3) 0.7315(3) 0.8226(2) 0.0341(9) Uani 1 1 d . . .
N5 N 0.6779(4) 1.0076(3) 0.6949(2) 0.0351(9) Uani 1 1 d . . .
N6 N 0.7322(3) 1.0773(3) 0.8644(2) 0.0332(9) Uani 1 1 d . . .
C1 C 0.9641(4) 0.8175(3) 0.8286(3) 0.0283(10) Uani 1 1 d . . .
C2 C 1.0407(4) 0.9013(3) 0.8525(2) 0.0269(10) Uani 1 1 d . . .
C3 C 1.0947(4) 0.9491(3) 0.7886(2) 0.0261(9) Uani 1 1 d . . .
C4 C 1.0518(4) 0.8966(3) 0.7250(2) 0.0266(9) Uani 1 1 d . . .
C5 C 0.9709(4) 0.8159(3) 0.7493(3) 0.0288(10) Uani 1 1 d . . .
C6 C 1.0957(5) 0.9204(4) 0.6472(3) 0.0393(12) Uani 1 1 d . . .
H6A H 1.1817 0.9266 0.6446 0.059 Uiso 1 1 calc R . .
H6B H 1.0802 0.975 0.6335 0.059 Uiso 1 1 calc R . .
H6C H 1.0534 0.8747 0.6139 0.059 Uiso 1 1 calc R . .
C7 C 0.9058(5) 0.7394(3) 0.7010(3) 0.0465(13) Uani 1 1 d . . .
H7A H 0.8546 0.7584 0.6662 0.07 Uiso 1 1 calc R . .
H7B H 0.8567 0.6931 0.7314 0.07 Uiso 1 1 calc R . .
H7C H 0.9646 0.7178 0.6745 0.07 Uiso 1 1 calc R . .
C8 C 0.8992(5) 0.7433(4) 0.8782(3) 0.0466(14) Uani 1 1 d . . .
H8A H 0.9096 0.7623 0.9289 0.07 Uiso 1 1 calc R . .
H8B H 0.9324 0.6942 0.8713 0.07 Uiso 1 1 calc R . .
H8C H 0.8139 0.7257 0.8662 0.07 Uiso 1 1 calc R . .
C9 C 1.0626(5) 0.9308(4) 0.9319(3) 0.0423(13) Uani 1 1 d . . .
H9A H 0.9865 0.9308 0.9546 0.063 Uiso 1 1 calc R . .
H9B H 1.1171 0.9892 0.9335 0.063 Uiso 1 1 calc R . .
H9C H 1.098 0.8911 0.9583 0.063 Uiso 1 1 calc R . .
C10 C 1.1870(4) 1.0378(3) 0.7866(3) 0.0386(11) Uani 1 1 d . . .
H10A H 1.2019 1.0606 0.8361 0.058 Uiso 1 1 calc R . .
H10B H 1.1565 1.0774 0.7569 0.058 Uiso 1 1 calc R . .
H10C H 1.2617 1.032 0.7656 0.058 Uiso 1 1 calc R . .
C11 C 0.6540(4) 0.8038(3) 0.8628(2) 0.0260(9) Uani 1 1 d . . .
C12 C 0.6302(4) 0.8100(3) 0.9401(2) 0.0297(10) Uani 1 1 d . . .
C13 C 0.5478(4) 0.7393(3) 0.9727(3) 0.0360(11) Uani 1 1 d . . .
H13 H 0.5309 0.7414 1.023 0.043 Uiso 1 1 calc R . .
C14 C 0.4890(5) 0.6645(3) 0.9320(3) 0.0400(12) Uani 1 1 d . . .
H14 H 0.4335 0.6166 0.954 0.048 Uiso 1 1 calc R . .
C15 C 0.5171(4) 0.6648(3) 0.8576(3) 0.0406(12) Uani 1 1 d . . .
H15 H 0.4781 0.6155 0.8298 0.049 Uiso 1 1 calc R . .
C16 C 0.6946(5) 0.8899(4) 0.9837(3) 0.0429(13) Uani 1 1 d . . .
H16A H 0.7418 0.8733 1.0223 0.064 Uiso 1 1 calc R . .
H16B H 0.6358 0.9158 1.0053 0.064 Uiso 1 1 calc R . .
H16C H 0.7477 0.9319 0.9515 0.064 Uiso 1 1 calc R . .
C21 C 0.7430(4) 0.9729(3) 0.6459(2) 0.0283(10) Uani 1 1 d . . .
C22 C 0.7229(4) 0.9759(3) 0.5674(2) 0.0306(10) Uani 1 1 d . . .
C23 C 0.6462(5) 1.0231(4) 0.5432(3) 0.0447(13) Uani 1 1 d . . .
H23 H 0.6332 1.0276 0.4926 0.054 Uiso 1 1 calc R . .
C24 C 0.5874(5) 1.0647(4) 0.5934(3) 0.0527(15) Uani 1 1 d . . .
H24 H 0.5377 1.0986 0.577 0.063 Uiso 1 1 calc R . .
C25 C 0.6049(5) 1.0541(4) 0.6671(3) 0.0437(13) Uani 1 1 d . . .
H25 H 0.5639 1.0805 0.7005 0.052 Uiso 1 1 calc R . .
C26 C 0.7871(5) 0.9300(4) 0.5145(3) 0.0402(12) Uani 1 1 d . . .
C31 C 0.8547(4) 1.1067(3) 0.8577(2) 0.0279(10) Uani 1 1 d . . .
C32 C 0.9221(5) 1.1910(3) 0.8868(2) 0.0328(11) Uani 1 1 d . . .
C33 C 0.8567(5) 1.2404(4) 0.9227(3) 0.0438(13) Uani 1 1 d . . .
H33 H 0.8975 1.2955 0.9416 0.053 Uiso 1 1 calc R . .
C34 C 0.7311(5) 1.2093(4) 0.9313(3) 0.0491(14) Uani 1 1 d . . .
H34 H 0.6872 1.242 0.9563 0.059 Uiso 1 1 calc R . .
C35 C 0.6743(5) 1.1282(4) 0.9012(3) 0.0458(13) Uani 1 1 d . . .
H35 H 0.5902 1.1071 0.9065 0.055 Uiso 1 1 calc R . .
C36 C 1.0572(5) 1.2237(4) 0.8787(3) 0.0407(12) Uani 1 1 d . . .
C41 C 0.3873(5) 0.9023(4) 0.8735(3) 0.0463(14) Uani 1 1 d . . .
H41A H 0.3398 0.9445 0.876 0.056 Uiso 1 1 calc R . .
H41B H 0.4333 0.9057 0.9191 0.056 Uiso 1 1 calc R . .
C42 C 0.3049(5) 0.8101(4) 0.8623(3) 0.0533(15) Uani 1 1 d . . .
H42A H 0.224 0.8048 0.8819 0.064 Uiso 1 1 calc R . .
H42B H 0.3381 0.7668 0.8864 0.064 Uiso 1 1 calc R . .
C43 C 0.3012(5) 0.7980(4) 0.7788(3) 0.0557(15) Uani 1 1 d . . .
H43A H 0.2991 0.7379 0.7659 0.067 Uiso 1 1 calc R . .
H43B H 0.2299 0.8112 0.758 0.067 Uiso 1 1 calc R . .
C44 C 0.4144(5) 0.8607(4) 0.7507(3) 0.0529(15) Uani 1 1 d . . .
H44A H 0.471 0.8288 0.734 0.063 Uiso 1 1 calc R . .
H44B H 0.3957 0.8936 0.7091 0.063 Uiso 1 1 calc R . .
O1 O 0.4688(3) 0.9205(2) 0.81020(19) 0.0434(9) Uani 1 1 d . . .
Li1 Li 0.6458(7) 0.9704(6) 0.8036(4) 0.0366(18) Uani 1 1 d . . .
H2 H 0.867(4) 0.915(3) 0.643(3) 0.033(14) Uiso 1 1 d . . .
H3 H 0.992(4) 1.084(3) 0.816(2) 0.010(10) Uiso 1 1 d . . .
H26A H 0.765(6) 0.862(5) 0.526(4) 0.08(2) Uiso 1 1 d . . .
H26B H 0.883(5) 0.961(4) 0.514(3) 0.054(16) Uiso 1 1 d . . .
H26C H 0.756(5) 0.930(4) 0.460(3) 0.050(15) Uiso 1 1 d . . .
H36A H 1.083(5) 1.228(4) 0.828(3) 0.044(15) Uiso 1 1 d . . .
H36B H 1.095(5) 1.186(4) 0.905(3) 0.058(18) Uiso 1 1 d . . .
H36C H 1.097(6) 1.283(5) 0.905(3) 0.069(19) Uiso 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 1.763(4) . ?
Ti1 N3 2.033(4) . ?
Ti1 N2 2.045(4) . ?
Ti1 C1 2.387(4) . ?
Ti1 C2 2.395(4) . ?
Ti1 C5 2.398(5) . ?
Ti1 C3 2.436(4) . ?
Ti1 C4 2.441(4) . ?
Ti1 Li1 2.902(8) . ?
N1 C11 1.386(6) . ?
N1 Li1 2.127(9) . ?
N2 C21 1.354(6) . ?
N3 C31 1.371(6) . ?
N4 C15 1.344(6) . ?
N4 C11 1.359(6) . ?
N5 C25 1.350(6) . ?
N5 C21 1.363(6) . ?
N5 Li1 2.052(9) . ?
N6 C35 1.347(6) . ?
N6 C31 1.351(6) . ?
N6 Li1 2.026(9) . ?
C1 C5 1.434(6) . ?
C1 C2 1.436(6) . ?
C1 C8 1.497(6) . ?
C2 C3 1.422(6) . ?
C2 C9 1.505(6) . ?
C3 C4 1.420(6) . ?
C3 C10 1.502(6) . ?
C4 C5 1.420(6) . ?
C4 C6 1.503(6) . ?
C5 C7 1.509(7) . ?
C11 C12 1.429(6) . ?
C12 C13 1.378(6) . ?
C12 C16 1.496(7) . ?
C13 C14 1.394(7) . ?
C14 C15 1.379(7) . ?
C21 C22 1.438(6) . ?
C22 C23 1.368(7) . ?
C22 C26 1.505(7) . ?
C23 C24 1.394(8) . ?
C24 C25 1.363(8) . ?
C31 C32 1.440(6) . ?
C32 C33 1.381(7) . ?
C32 C36 1.493(7) . ?
C33 C34 1.389(8) . ?
C34 C35 1.377(8) . ?
C41 O1 1.451(6) . ?
C41 C42 1.512(8) . ?
C42 C43 1.518(8) . ?
C43 C44 1.483(8) . ?
C44 O1 1.451(6) . ?
O1 Li1 1.958(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
N1 Ti1 N3 104.43(17) . . ?
N1 Ti1 N2 103.74(16) . . ?
N3 Ti1 N2 104.10(16) . . ?
N1 Ti1 C1 89.59(17) . . ?
N3 Ti1 C1 125.46(16) . . ?
N2 Ti1 C1 123.55(16) . . ?
N1 Ti1 C2 108.98(17) . . ?
N3 Ti1 C2 91.80(16) . . ?
N2 Ti1 C2 138.56(15) . . ?
C1 Ti1 C2 34.95(16) . . ?
N1 Ti1 C5 106.31(17) . . ?
N3 Ti1 C5 142.18(16) . . ?
N2 Ti1 C5 89.48(16) . . ?
C1 Ti1 C5 34.87(15) . . ?
C2 Ti1 C5 57.57(16) . . ?
N1 Ti1 C3 143.01(16) . . ?
N3 Ti1 C3 85.42(15) . . ?
N2 Ti1 C3 108.27(16) . . ?
C1 Ti1 C3 57.31(15) . . ?
C2 Ti1 C3 34.23(15) . . ?
C5 Ti1 C3 56.76(15) . . ?
N1 Ti1 C4 140.43(17) . . ?
N3 Ti1 C4 112.26(16) . . ?
N2 Ti1 C4 81.64(16) . . ?
C1 Ti1 C4 57.31(15) . . ?
C2 Ti1 C4 56.94(15) . . ?
C5 Ti1 C4 34.12(15) . . ?
C3 Ti1 C4 33.86(15) . . ?
N1 Ti1 Li1 46.8(2) . . ?
N3 Ti1 Li1 71.9(2) . . ?
N2 Ti1 Li1 80.1(2) . . ?
C1 Ti1 Li1 136.0(2) . . ?
C2 Ti1 Li1 141.34(19) . . ?
C5 Ti1 Li1 145.9(2) . . ?
C3 Ti1 Li1 157.2(2) . . ?
C4 Ti1 Li1 161.68(19) . . ?
C11 N1 Ti1 156.5(3) . . ?
C11 N1 Li1 107.3(3) . . ?
Ti1 N1 Li1 96.0(3) . . ?
C21 N2 Ti1 129.5(3) . . ?
C31 N3 Ti1 138.9(3) . . ?
C15 N4 C11 118.1(4) . . ?
C25 N5 C21 117.7(4) . . ?
C25 N5 Li1 115.0(4) . . ?
C21 N5 Li1 125.4(4) . . ?
C35 N6 C31 118.1(4) . . ?
C35 N6 Li1 123.9(4) . . ?
C31 N6 Li1 117.1(4) . . ?
C5 C1 C2 107.1(4) . . ?
C5 C1 C8 126.9(5) . . ?
C2 C1 C8 125.8(4) . . ?
C5 C1 Ti1 73.0(3) . . ?
C2 C1 Ti1 72.8(2) . . ?
C8 C1 Ti1 123.8(3) . . ?
C3 C2 C1 108.0(4) . . ?
C3 C2 C9 126.6(4) . . ?
C1 C2 C9 125.3(4) . . ?
C3 C2 Ti1 74.4(2) . . ?
C1 C2 Ti1 72.2(2) . . ?
C9 C2 Ti1 120.9(3) . . ?
C4 C3 C2 108.4(4) . . ?
C4 C3 C10 124.4(4) . . ?
C2 C3 C10 127.1(4) . . ?
C4 C3 Ti1 73.3(2) . . ?
C2 C3 Ti1 71.3(2) . . ?
C10 C3 Ti1 124.0(3) . . ?
C3 C4 C5 108.0(4) . . ?
C3 C4 C6 124.8(4) . . ?
C5 C4 C6 126.9(4) . . ?
C3 C4 Ti1 72.9(2) . . ?
C5 C4 Ti1 71.3(2) . . ?
C6 C4 Ti1 126.2(3) . . ?
C4 C5 C1 108.5(4) . . ?
C4 C5 C7 126.5(4) . . ?
C1 C5 C7 125.0(4) . . ?
C4 C5 Ti1 74.6(3) . . ?
C1 C5 Ti1 72.1(3) . . ?
C7 C5 Ti1 120.9(3) . . ?
N4 C11 N1 118.2(4) . . ?
N4 C11 C12 121.5(4) . . ?
N1 C11 C12 120.3(4) . . ?
C13 C12 C11 117.5(4) . . ?
C13 C12 C16 121.7(4) . . ?
C11 C12 C16 120.8(4) . . ?
C12 C13 C14 121.5(5) . . ?
C15 C14 C13 116.9(5) . . ?
N4 C15 C14 124.5(5) . . ?
N2 C21 N5 116.6(4) . . ?
N2 C21 C22 122.3(4) . . ?
N5 C21 C22 121.1(4) . . ?
C23 C22 C21 117.6(4) . . ?
C23 C22 C26 122.0(4) . . ?
C21 C22 C26 120.3(4) . . ?
C22 C23 C24 120.9(5) . . ?
C25 C24 C23 118.0(5) . . ?
N5 C25 C24 124.2(5) . . ?
N6 C31 N3 117.5(4) . . ?
N6 C31 C32 121.4(4) . . ?
N3 C31 C32 121.1(4) . . ?
C33 C32 C31 117.4(5) . . ?
C33 C32 C36 121.3(5) . . ?
C31 C32 C36 121.3(4) . . ?
C32 C33 C34 121.2(5) . . ?
C35 C34 C33 117.3(5) . . ?
N6 C35 C34 124.5(5) . . ?
O1 C41 C42 106.3(4) . . ?
C41 C42 C43 104.0(5) . . ?
C44 C43 C42 105.5(5) . . ?
O1 C44 C43 108.6(5) . . ?
C41 O1 C44 108.5(4) . . ?
C41 O1 Li1 131.4(4) . . ?
C44 O1 Li1 115.2(4) . . ?
O1 Li1 N6 120.8(4) . . ?
O1 Li1 N5 104.8(4) . . ?
N6 Li1 N5 105.8(4) . . ?
O1 Li1 N1 110.6(4) . . ?
N6 Li1 N1 106.0(4) . . ?
N5 Li1 N1 108.2(4) . . ?
O1 Li1 Ti1 144.1(4) . . ?
N6 Li1 Ti1 90.0(3) . . ?
N5 Li1 Ti1 81.1(3) . . ?
N1 Li1 Ti1 37.17(16) . . ?
####################################################################### 
# 
# 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_3a
_database_code_depnum_ccdc_archive 'CCDC 1056536'
_audit_update_record             
;
2015-03-27 deposited with the CCDC.
2015-05-07 downloaded from the CCDC.
;

_audit_creation_date             2014-10-20T12:19:25-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C18 H32 Cl2 Li2 N2 O3'
_chemical_formula_sum            'C18 H32 Cl2 Li2 N2 O3'
_chemical_formula_weight         409.24
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
loop_
_symmetry_equiv_pos_as_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                   8.7259(8)
_cell_length_b                   18.065(2)
_cell_length_c                   15.231(2)
_cell_angle_alpha                90
_cell_angle_beta                 101.634(9)
_cell_angle_gamma                90
_cell_volume                     2351.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    213
_cell_measurement_theta_min      3.45
_cell_measurement_theta_max      16.34
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 3 -7 0.326
-1 -5 1 0.236
0 3 -1 0.417
4 0 5 0.278
1 16 -6 0.432
-1 -8 2 0.287
1 -4 -3 0.172
-1 6 3 0.251
1 2 -2 0.444

_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.293
_exptl_absorpt_correction_type   none

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.1556
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_number            41232
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.18
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_full        27.5
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_reflns_number_total             5380
_reflns_number_gt                4067
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0913P)²+2.6229P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5380
_refine_ls_number_parameters     252
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.075
_refine_ls_wR_factor_ref         0.2235
_refine_ls_wR_factor_gt          0.1965
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.074

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 '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 0.006 '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'

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.16409(8) 0.97771(4) 0.09135(5) 0.0414(2) Uani 1 1 d . . .
Cl2 Cl 0.91437(12) 0.92032(5) 0.54485(6) 0.0589(3) Uani 1 1 d . . .
O1 O 0.1872(3) 1.13147(13) -0.03680(17) 0.0497(6) Uani 1 1 d . . .
C5 C -0.0369(4) 1.15059(17) 0.1934(2) 0.0422(7) Uani 1 1 d . . .
C6 C -0.1558(4) 1.22699(18) -0.0365(2) 0.0437(7) Uani 1 1 d . . .
H6A H -0.108 1.1842 -0.06 0.065 Uiso 1 1 calc R . .
H6C H -0.1056 1.2725 -0.0515 0.065 Uiso 1 1 calc R . .
H6B H -0.2678 1.2286 -0.0632 0.065 Uiso 1 1 calc R . .
C2 C -0.1920(4) 1.27431(18) 0.1141(2) 0.0483(8) Uani 1 1 d . . .
H2 H -0.2436 1.3169 0.0858 0.058 Uiso 1 1 calc R . .
N2 N -0.0560(3) 1.15907(13) 0.10320(16) 0.0349(5) Uani 1 1 d . . .
O2 O 0.8142(3) 1.1048(2) 0.5973(2) 0.0787(10) Uani 1 1 d . . .
C1 C -0.1341(3) 1.22029(16) 0.0647(2) 0.0360(6) Uani 1 1 d . . .
O3 O 0.6678(4) 1.0491(2) 0.4007(2) 0.0919(12) Uani 1 1 d . . .
C3 C -0.1719(4) 1.2640(2) 0.2077(3) 0.0573(9) Uani 1 1 d . . .
H3 H -0.2117 1.2997 0.2431 0.069 Uiso 1 1 calc R . .
C4 C -0.0958(4) 1.2032(2) 0.2473(2) 0.0512(8) Uani 1 1 d . . .
H4 H -0.0822 1.1961 0.3102 0.061 Uiso 1 1 calc R . .
N1 N 0.0391(5) 1.0893(2) 0.2313(2) 0.0724(12) Uani 1 1 d . . .
C15 C 0.6686(6) 1.0130(3) 0.3166(3) 0.0784(13) Uani 1 1 d . . .
H15A H 0.6342 0.9609 0.3185 0.094 Uiso 1 1 calc R . .
H15B H 0.7752 1.0135 0.3035 0.094 Uiso 1 1 calc R . .
C10 C 0.2721(5) 1.0863(2) -0.0902(3) 0.0596(9) Uani 1 1 d U . .
H10B H 0.2332 1.0952 -0.1549 0.072 Uiso 1 1 calc R . .
H10A H 0.2604 1.033 -0.0777 0.072 Uiso 1 1 calc R . .
C13 C 0.7304(7) 1.1659(4) 0.7135(3) 0.099(2) Uani 1 1 d U . .
H13B H 0.6808 1.2152 0.7022 0.119 Uiso 1 1 calc R . .
H13A H 0.6978 1.1436 0.7662 0.119 Uiso 1 1 calc R . .
C7 C 0.2959(6) 1.1769(4) 0.0213(5) 0.102(2) Uani 1 1 d . . .
H7A H 0.2958 1.1642 0.0845 0.122 Uiso 1 1 calc R . .
H7B H 0.2662 1.2296 0.0117 0.122 Uiso 1 1 calc R . .
Li1 Li 0.8516(7) 1.0421(4) 0.4986(4) 0.0582(15) Uani 1 1 d . . .
C12 C 0.9017(6) 1.1724(3) 0.7291(3) 0.0815(14) Uani 1 1 d U . .
H12B H 0.9332 1.2237 0.7179 0.098 Uiso 1 1 calc R . .
H12A H 0.9498 1.1585 0.7914 0.098 Uiso 1 1 calc R . .
C11 C 0.9473(6) 1.1217(5) 0.6661(4) 0.116(3) Uani 1 1 d U . .
H11B H 1.0305 1.1441 0.6392 0.14 Uiso 1 1 calc R . .
H11A H 0.9891 1.0757 0.6973 0.14 Uiso 1 1 calc R . .
Li2 Li 0.0246(6) 1.0823(3) 0.0173(3) 0.0379(10) Uani 1 1 d . . .
C16 C 0.5587(8) 1.0548(4) 0.2467(4) 0.108(2) Uani 1 1 d . . .
H16B H 0.6155 1.0782 0.2039 0.129 Uiso 1 1 calc R . .
H16A H 0.4775 1.0214 0.2131 0.129 Uiso 1 1 calc R . .
C18 C 0.5450(9) 1.1014(5) 0.3873(5) 0.144(4) Uani 1 1 d . . .
H18A H 0.4597 1.084 0.4162 0.173 Uiso 1 1 calc R . .
H18B H 0.5838 1.1493 0.4148 0.173 Uiso 1 1 calc R . .
C8 C 0.4498(7) 1.1649(6) 0.0026(6) 0.161(4) Uani 1 1 d U . .
H8B H 0.4895 1.2112 -0.0194 0.193 Uiso 1 1 calc R . .
H8A H 0.5232 1.1494 0.0579 0.193 Uiso 1 1 calc R . .
C9 C 0.4386(6) 1.1096(4) -0.0626(6) 0.123(3) Uani 1 1 d U . .
H9A H 0.504 1.0667 -0.0381 0.148 Uiso 1 1 calc R . .
H9B H 0.4769 1.1287 -0.1151 0.148 Uiso 1 1 calc R . .
C14 C 0.6840(7) 1.1172(6) 0.6330(6) 0.145(3) Uani 1 1 d U . .
H14A H 0.6423 1.0696 0.6505 0.174 Uiso 1 1 calc R . .
H14B H 0.6015 1.1415 0.5881 0.174 Uiso 1 1 calc R . .
C17 C 0.4881(10) 1.1108(5) 0.2947(6) 0.146(3) Uani 1 1 d . . .
H17A H 0.515 1.1609 0.2761 0.176 Uiso 1 1 calc R . .
H17B H 0.3727 1.1056 0.2808 0.176 Uiso 1 1 calc R . .
H1B H 0.075(5) 1.085(2) 0.289(3) 0.062(12) Uiso 1 1 d . . .
H1A H 0.074(5) 1.056(2) 0.200(3) 0.060(12) Uiso 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
Cl1 Li2 2.350(5) 3_575 ?
Cl1 Li2 2.402(5) . ?
Cl2 Li1 2.341(7) . ?
Cl2 Li1 2.369(7) 3_776 ?
O1 C7 1.420(5) . ?
O1 C10 1.456(4) . ?
O1 Li2 1.988(5) . ?
C5 N1 1.358(5) . ?
C5 N2 1.359(4) . ?
C5 C4 1.419(4) . ?
C6 C1 1.519(4) . ?
C2 C1 1.388(4) . ?
C2 C3 1.414(5) . ?
N2 C1 1.368(4) . ?
N2 Li2 2.122(5) . ?
O2 C14 1.374(6) . ?
O2 C11 1.432(6) . ?
O2 Li1 1.960(7) . ?
O3 C18 1.413(6) . ?
O3 C15 1.439(6) . ?
O3 Li1 1.962(7) . ?
C3 C4 1.359(5) . ?
C15 C16 1.487(8) . ?
C10 C9 1.490(7) . ?
C13 C12 1.470(8) . ?
C13 C14 1.497(9) . ?
C7 C8 1.444(8) . ?
Li1 Cl2 2.369(7) 3_776 ?
Li1 Li1 2.996(12) 3_776 ?
C12 C11 1.440(6) . ?
Li2 Cl1 2.350(5) 3_575 ?
Li2 Li2 3.034(10) 3_575 ?
C16 C17 1.457(10) . ?
C18 C17 1.407(10) . ?
C8 C9 1.397(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
Li2 Cl1 Li2 79.35(18) 3_575 . ?
Li1 Cl2 Li1 79.0(2) . 3_776 ?
C7 O1 C10 108.7(3) . . ?
C7 O1 Li2 116.3(3) . . ?
C10 O1 Li2 117.8(3) . . ?
N1 C5 N2 118.1(3) . . ?
N1 C5 C4 120.2(3) . . ?
N2 C5 C4 121.7(3) . . ?
C1 C2 C3 118.0(3) . . ?
C5 N2 C1 118.3(2) . . ?
C5 N2 Li2 124.2(2) . . ?
C1 N2 Li2 117.5(2) . . ?
C14 O2 C11 106.8(4) . . ?
C14 O2 Li1 132.6(4) . . ?
C11 O2 Li1 116.7(3) . . ?
N2 C1 C2 122.7(3) . . ?
N2 C1 C6 116.7(2) . . ?
C2 C1 C6 120.6(3) . . ?
C18 O3 C15 108.3(4) . . ?
C18 O3 Li1 129.2(4) . . ?
C15 O3 Li1 119.9(3) . . ?
C4 C3 C2 120.3(3) . . ?
C3 C4 C5 119.1(3) . . ?
O3 C15 C16 106.8(4) . . ?
O1 C10 C9 105.1(4) . . ?
C12 C13 C14 106.1(4) . . ?
O1 C7 C8 108.8(5) . . ?
O2 Li1 O3 108.0(3) . . ?
O2 Li1 Cl2 112.2(3) . . ?
O3 Li1 Cl2 113.2(3) . . ?
O2 Li1 Cl2 109.6(3) . 3_776 ?
O3 Li1 Cl2 112.8(3) . 3_776 ?
Cl2 Li1 Cl2 101.0(2) . 3_776 ?
O2 Li1 Li1 124.0(4) . 3_776 ?
O3 Li1 Li1 127.9(4) . 3_776 ?
Cl2 Li1 Li1 50.9(2) . 3_776 ?
Cl2 Li1 Li1 50.1(2) 3_776 3_776 ?
C11 C12 C13 104.4(4) . . ?
O2 C11 C12 109.4(4) . . ?
O1 Li2 N2 108.4(2) . . ?
O1 Li2 Cl1 111.8(2) . 3_575 ?
N2 Li2 Cl1 117.6(2) . 3_575 ?
O1 Li2 Cl1 102.1(2) . . ?
N2 Li2 Cl1 115.1(2) . . ?
Cl1 Li2 Cl1 100.65(18) 3_575 . ?
O1 Li2 Li2 117.0(3) . 3_575 ?
N2 Li2 Li2 134.0(3) . 3_575 ?
Cl1 Li2 Li2 51.07(15) 3_575 3_575 ?
Cl1 Li2 Li2 49.58(14) . 3_575 ?
C17 C16 C15 105.7(5) . . ?
C17 C18 O3 109.3(6) . . ?
C9 C8 C7 108.2(5) . . ?
C8 C9 C10 109.1(5) . . ?
O2 C14 C13 108.2(5) . . ?
C18 C17 C16 108.6(5) . . ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3b
_database_code_depnum_ccdc_archive 'CCDC 1056537'
_audit_update_record             
;
2015-03-27 deposited with the CCDC.
2015-05-07 downloaded from the CCDC.
;

_audit_creation_date             2014-10-20T12:57:23-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C22 H32 Cl2 Li2 N6 O1'
_chemical_formula_sum            'C22 H32 Cl2 Li2 N6 O'
_chemical_formula_weight         481.32
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.457(11)
_cell_length_b                   28.056(8)
_cell_length_c                   9.083(7)
_cell_angle_alpha                90
_cell_angle_beta                 100.46(8)
_cell_angle_gamma                90
_cell_volume                     2621(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    234
_cell_measurement_theta_min      3.13
_cell_measurement_theta_max      25.5
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.514
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.201
_exptl_crystal_density_diffrn    1.22
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1016
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 -2 0.065
3 0 1 0.251
-8 -5 6 0.265
1 -4 7 0.099
0 9 -10 0.127
4 -12 13 0.14
0 -1 -7 0.1
0 1 7 0.068

_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_type   none

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.1527
_diffrn_reflns_av_unetI/netI     0.0684
_diffrn_reflns_number            37790
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.1
_diffrn_reflns_theta_max         25.57
_diffrn_reflns_theta_full        25.57
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_reflns_number_total             4882
_reflns_number_gt                3274
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0670P)²+2.8382P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4882
_refine_ls_number_parameters     390
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0685
_refine_ls_wR_factor_ref         0.1797
_refine_ls_wR_factor_gt          0.1516
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.104
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.003
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.081

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
Li Li -0.0003 0.0001 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Li1 Li -0.2874(6) -0.3713(2) 0.9306(7) 0.0345(13) Uani 1 1 d . . .
Li2 Li -0.0379(6) -0.3725(2) 0.8148(6) 0.0324(13) Uani 1 1 d . . .
Cl1 Cl -0.15774(9) -0.30601(3) 0.88123(10) 0.0385(3) Uani 1 1 d . . .
Cl2 Cl -0.17896(9) -0.43598(3) 0.84699(10) 0.0353(3) Uani 1 1 d . . .
N3 N -0.0025(3) -0.36214(10) 0.6052(3) 0.0289(6) Uani 1 1 d . . .
N5 N 0.1361(3) -0.38017(10) 0.9540(3) 0.0316(7) Uani 1 1 d . . .
O1 O -0.4535(3) -0.36981(9) 0.8003(3) 0.0476(7) Uani 1 1 d . . .
N6 N 0.1412(3) -0.46233(11) 0.9501(3) 0.0423(8) Uani 1 1 d . . .
H6A H 0.0747 -0.4621 0.8788 0.051 Uiso 1 1 calc R . .
H6B H 0.1753 -0.489 0.9835 0.051 Uiso 1 1 calc R . .
N4 N 0.0071(3) -0.27955(12) 0.6102(4) 0.0426(8) Uani 1 1 d . . .
N1 N -0.3065(3) -0.37066(10) 1.1507(3) 0.0349(7) Uani 1 1 d . . .
N2 N -0.2983(4) -0.28858(13) 1.1760(5) 0.0450(9) Uani 1 1 d . . .
C7 C 0.0100(3) -0.32184(12) 0.5327(4) 0.0304(8) Uani 1 1 d . . .
C11 C 0.0025(4) -0.40329(13) 0.5316(4) 0.0327(8) Uani 1 1 d . . .
C13 C 0.1928(4) -0.42034(12) 1.0102(4) 0.0329(8) Uani 1 1 d . . .
C17 C 0.1899(4) -0.33883(14) 1.0082(4) 0.0378(9) Uani 1 1 d . . .
C8 C 0.0292(4) -0.32205(14) 0.3858(4) 0.0392(9) Uani 1 1 d . . .
C14 C 0.3030(4) -0.41980(16) 1.1224(5) 0.0428(10) Uani 1 1 d . . .
C10 C 0.0185(4) -0.40701(13) 0.3861(4) 0.0377(9) Uani 1 1 d . . .
C9 C 0.0311(4) -0.36456(15) 0.3141(5) 0.0425(10) Uani 1 1 d . . .
C16 C 0.2957(4) -0.33473(14) 1.1184(5) 0.0451(10) Uani 1 1 d . . .
C15 C 0.3526(4) -0.37713(16) 1.1761(5) 0.0492(11) Uani 1 1 d . . .
C19 C -0.5329(5) -0.41100(19) 0.7652(7) 0.0597(13) Uani 1 1 d . . .
C22 C -0.5295(5) -0.3287(2) 0.7574(7) 0.0671(15) Uani 1 1 d . . .
C21 C -0.6379(5) -0.34394(19) 0.6433(7) 0.0844(18) Uani 1 1 d . . .
H21A H -0.628 -0.3317 0.5461 0.101 Uiso 1 1 calc R . .
H21B H -0.7192 -0.3321 0.6662 0.101 Uiso 1 1 calc R . .
C20 C -0.6376(5) -0.39647(18) 0.6421(7) 0.0815(18) Uani 1 1 d . . .
H20A H -0.7208 -0.4088 0.6579 0.098 Uiso 1 1 calc R . .
H20B H -0.6209 -0.4084 0.5471 0.098 Uiso 1 1 calc R . .
C12 C 0.0182(6) -0.45445(18) 0.3095(6) 0.0587(12) Uani 1 1 d . . .
C18 C 0.3470(5) -0.28653(16) 1.1759(7) 0.0732(15) Uani 1 1 d . . .
H18A H 0.4218 -0.2908 1.2534 0.11 Uiso 1 1 calc R . .
H18B H 0.2807 -0.2697 1.2154 0.11 Uiso 1 1 calc R . .
H18C H 0.3711 -0.2685 1.0953 0.11 Uiso 1 1 calc R . .
C5 C -0.3045(3) -0.33238(13) 1.2398(4) 0.0343(8) Uani 1 1 d . . .
C1 C -0.3166(4) -0.41357(14) 1.2116(5) 0.0386(9) Uani 1 1 d . . .
C4 C -0.3123(4) -0.33739(16) 1.3900(4) 0.0430(10) Uani 1 1 d . . .
C2 C -0.3243(4) -0.42180(15) 1.3575(4) 0.0433(10) Uani 1 1 d . . .
C3 C -0.3212(4) -0.38196(17) 1.4476(5) 0.0464(11) Uani 1 1 d . . .
C6 C -0.3328(8) -0.4713(2) 1.4175(8) 0.0704(16) Uani 1 1 d . . .
H11 H -0.010(4) -0.4313(13) 0.588(4) 0.036(10) Uiso 1 1 d . . .
H9 H 0.040(5) -0.3668(16) 0.218(6) 0.074(16) Uiso 1 1 d . . .
H4 H -0.315(4) -0.3086(14) 1.444(4) 0.044(11) Uiso 1 1 d . . .
H1 H -0.318(4) -0.4381(13) 1.144(4) 0.036(10) Uiso 1 1 d . . .
H3 H -0.326(4) -0.3878(14) 1.546(5) 0.046(11) Uiso 1 1 d . . .
H14 H 0.331(4) -0.4496(15) 1.161(4) 0.046(11) Uiso 1 1 d . . .
H4B H -0.020(5) -0.2543(17) 0.546(5) 0.064(14) Uiso 1 1 d . . .
H17 H 0.146(4) -0.3112(13) 0.968(4) 0.034(10) Uiso 1 1 d . . .
H4A H -0.029(4) -0.2789(14) 0.687(5) 0.039(12) Uiso 1 1 d . . .
H2B H -0.276(4) -0.2659(15) 1.230(5) 0.044(13) Uiso 1 1 d . . .
H2A H -0.267(5) -0.2880(15) 1.087(5) 0.060(14) Uiso 1 1 d . . .
H8 H 0.039(4) -0.2907(14) 0.341(4) 0.038(10) Uiso 1 1 d . . .
H6D H -0.305(7) -0.496(2) 1.354(8) 0.11(2) Uiso 1 1 d . . .
H6E H -0.270(8) -0.473(3) 1.518(9) 0.15(3) Uiso 1 1 d . . .
H6C H -0.406(7) -0.481(3) 1.412(8) 0.12(3) Uiso 1 1 d . . .
H12C H -0.035(5) -0.4780(19) 0.350(6) 0.081(17) Uiso 1 1 d . . .
H12B H -0.022(7) -0.452(2) 0.193(8) 0.13(2) Uiso 1 1 d . . .
H12A H 0.107(7) -0.468(2) 0.324(7) 0.12(2) Uiso 1 1 d . . .
H22A H -0.483(7) -0.303(3) 0.743(8) 0.13(3) Uiso 1 1 d . . .
H19A H -0.484(5) -0.4376(19) 0.746(6) 0.078(17) Uiso 1 1 d . . .
H22B H -0.562(6) -0.318(2) 0.855(7) 0.11(2) Uiso 1 1 d . . .
H19B H -0.567(7) -0.415(2) 0.854(7) 0.11(2) Uiso 1 1 d . . .
H15 H 0.432(6) -0.3765(18) 1.267(6) 0.093(17) Uiso 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
Li1 O1 1.916(7) . ?
Li1 N1 2.045(7) . ?
Li1 Cl2 2.338(6) . ?
Li1 Cl1 2.370(6) . ?
Li1 Li2 2.985(9) . ?
Li2 N3 2.025(6) . ?
Li2 N5 2.030(7) . ?
Li2 Cl2 2.363(6) . ?
Li2 Cl1 2.386(6) . ?
N3 C7 1.327(4) . ?
N3 C11 1.340(4) . ?
N5 C13 1.331(4) . ?
N5 C17 1.343(5) . ?
O1 C22 1.416(5) . ?
O1 C19 1.425(5) . ?
N6 C13 1.368(5) . ?
N4 C7 1.383(5) . ?
N1 C1 1.337(5) . ?
N1 C5 1.342(5) . ?
N2 C5 1.365(5) . ?
C7 C8 1.385(5) . ?
C11 C10 1.366(5) . ?
C13 C14 1.393(6) . ?
C17 C16 1.356(6) . ?
C8 C9 1.361(6) . ?
C14 C15 1.360(6) . ?
C10 C9 1.377(6) . ?
C10 C12 1.502(6) . ?
C16 C15 1.389(6) . ?
C16 C18 1.513(6) . ?
C19 C20 1.473(7) . ?
C22 C21 1.454(7) . ?
C21 C20 1.474(7) . ?
C5 C4 1.389(5) . ?
C1 C2 1.362(6) . ?
C4 C3 1.365(6) . ?
C2 C3 1.383(6) . ?
C2 C6 1.502(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
O1 Li1 N1 111.4(3) . . ?
O1 Li1 Cl2 104.8(3) . . ?
N1 Li1 Cl2 117.6(3) . . ?
O1 Li1 Cl1 110.6(3) . . ?
N1 Li1 Cl1 109.8(3) . . ?
Cl2 Li1 Cl1 102.1(2) . . ?
O1 Li1 Li2 122.3(3) . . ?
N1 Li1 Li2 126.2(3) . . ?
Cl2 Li1 Li2 50.95(16) . . ?
Cl1 Li1 Li2 51.36(16) . . ?
N3 Li2 N5 107.7(3) . . ?
N3 Li2 Cl2 116.7(3) . . ?
N5 Li2 Cl2 110.6(3) . . ?
N3 Li2 Cl1 108.6(3) . . ?
N5 Li2 Cl1 112.2(3) . . ?
Cl2 Li2 Cl1 100.9(2) . . ?
N3 Li2 Li1 130.5(3) . . ?
N5 Li2 Li1 121.6(3) . . ?
Cl2 Li2 Li1 50.22(16) . . ?
Cl1 Li2 Li1 50.89(16) . . ?
Li1 Cl1 Li2 77.8(2) . . ?
Li1 Cl2 Li2 78.8(2) . . ?
C7 N3 C11 118.0(3) . . ?
C7 N3 Li2 129.9(3) . . ?
C11 N3 Li2 112.0(3) . . ?
C13 N5 C17 117.6(3) . . ?
C13 N5 Li2 127.9(3) . . ?
C17 N5 Li2 113.9(3) . . ?
C22 O1 C19 108.9(4) . . ?
C22 O1 Li1 126.1(3) . . ?
C19 O1 Li1 123.1(3) . . ?
C1 N1 C5 117.7(3) . . ?
C1 N1 Li1 115.2(3) . . ?
C5 N1 Li1 127.1(3) . . ?
N3 C7 N4 117.7(3) . . ?
N3 C7 C8 121.3(3) . . ?
N4 C7 C8 121.0(3) . . ?
N3 C11 C10 124.9(3) . . ?
N5 C13 N6 117.4(3) . . ?
N5 C13 C14 121.5(3) . . ?
N6 C13 C14 121.0(3) . . ?
N5 C17 C16 125.1(4) . . ?
C9 C8 C7 118.8(4) . . ?
C15 C14 C13 118.9(4) . . ?
C11 C10 C9 115.6(3) . . ?
C11 C10 C12 121.7(4) . . ?
C9 C10 C12 122.6(4) . . ?
C8 C9 C10 121.3(4) . . ?
C17 C16 C15 116.2(4) . . ?
C17 C16 C18 121.4(4) . . ?
C15 C16 C18 122.3(4) . . ?
C14 C15 C16 120.6(4) . . ?
O1 C19 C20 105.6(4) . . ?
O1 C22 C21 106.4(4) . . ?
C22 C21 C20 107.3(4) . . ?
C19 C20 C21 105.9(4) . . ?
N1 C5 N2 117.5(3) . . ?
N1 C5 C4 120.9(4) . . ?
N2 C5 C4 121.6(4) . . ?
N1 C1 C2 125.3(4) . . ?
C3 C4 C5 119.3(4) . . ?
C1 C2 C3 116.1(4) . . ?
C1 C2 C6 121.9(4) . . ?
C3 C2 C6 122.0(4) . . ?
C4 C3 C2 120.6(4) . . ?

# END of CIF



