# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1022957'
_audit_update_record             
;
2015-01-16 deposited with the CCDC.
2015-01-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H48 Cl4 Co2 N8 Si2'
_chemical_formula_weight         872.63

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'
Si Si 0.0817 0.0704 '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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   15.054(3)
_cell_length_b                   15.565(3)
_cell_length_c                   17.937(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.10(3)
_cell_angle_gamma                90.00
_cell_volume                     4017.0(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9522
_cell_measurement_theta_min      1.1878
_cell_measurement_theta_max      27.4700

_exptl_crystal_description       Block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1808
_exptl_absorpt_coefficient_mu    1.187
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.7099
_exptl_absorpt_correction_T_max  0.7887
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27165
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.42
_diffrn_reflns_theta_max         27.47
_reflns_number_total             9171
_reflns_number_gt                7872
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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 > 2sigma(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)+(0.0499P)²+6.7754P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9171
_refine_ls_number_parameters     442
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0633
_refine_ls_wR_factor_ref         0.1496
_refine_ls_wR_factor_gt          0.1408
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Co1 Co 0.26005(3) 0.38951(3) 0.36172(3) 0.02250(13) Uani 1 1 d . . .
Co2 Co 0.21463(3) 0.57287(3) 0.18686(3) 0.02238(13) Uani 1 1 d . . .
Si1 Si 0.04445(7) 0.31804(7) 0.33067(6) 0.0273(2) Uani 1 1 d . . .
Si2 Si 0.34623(7) 0.49346(7) 0.08477(6) 0.0296(2) Uani 1 1 d . . .
N4 N 0.12493(19) 0.38203(18) 0.30249(17) 0.0230(6) Uani 1 1 d . . .
N2 N 0.13280(19) 0.51873(18) 0.24498(17) 0.0213(6) Uani 1 1 d . . .
N1 N 0.2453(2) 0.65821(18) 0.27851(17) 0.0241(6) Uani 1 1 d . . .
N8 N 0.29902(19) 0.48374(19) 0.16242(17) 0.0234(6) Uani 1 1 d . . .
C9 C 0.1345(2) 0.5664(2) 0.3116(2) 0.0224(7) Uani 1 1 d . . .
N5 N 0.3274(2) 0.48859(19) 0.43219(17) 0.0238(6) Uani 1 1 d . . .
N6 N 0.33609(19) 0.43111(19) 0.29299(17) 0.0235(6) Uani 1 1 d . . .
C8 C 0.0771(3) 0.5528(2) 0.3579(2) 0.0291(8) Uani 1 1 d . . .
H8A H 0.0337 0.5069 0.3455 0.035 Uiso 1 1 calc R . .
C27 C 0.3160(2) 0.4187(2) 0.2145(2) 0.0245(7) Uani 1 1 d . . .
C10 C 0.1943(2) 0.6393(2) 0.3284(2) 0.0226(7) Uani 1 1 d . . .
C11 C 0.1041(2) 0.4352(2) 0.2401(2) 0.0212(7) Uani 1 1 d . . .
C26 C 0.3902(2) 0.5281(2) 0.4011(2) 0.0249(7) Uani 1 1 d . . .
N3 N 0.0582(2) 0.4070(2) 0.16786(19) 0.0292(7) Uani 1 1 d . . .
C25 C 0.3952(2) 0.4986(2) 0.3275(2) 0.0251(7) Uani 1 1 d . . .
C24 C 0.4639(3) 0.5323(3) 0.2992(2) 0.0342(9) Uani 1 1 d . . .
H24A H 0.4709 0.5112 0.2516 0.041 Uiso 1 1 calc R . .
C18 C 0.3212(3) 0.5132(3) 0.5017(2) 0.0302(8) Uani 1 1 d . . .
C6 C 0.1411(3) 0.6720(3) 0.4421(2) 0.0352(9) Uani 1 1 d . . .
H6A H 0.1448 0.7055 0.4872 0.042 Uiso 1 1 calc R . .
C2 C 0.3000(2) 0.7275(2) 0.2916(2) 0.0288(8) Uani 1 1 d . . .
C21 C 0.4496(3) 0.5944(2) 0.4412(2) 0.0307(8) Uani 1 1 d . . .
C4 C 0.2594(3) 0.7628(2) 0.4075(2) 0.0353(9) Uani 1 1 d . . .
H4A H 0.2658 0.7985 0.4518 0.042 Uiso 1 1 calc R . .
C7 C 0.0807(3) 0.6046(3) 0.4230(2) 0.0336(9) Uani 1 1 d . . .
H7A H 0.0406 0.5925 0.4539 0.040 Uiso 1 1 calc R . .
N7 N 0.3083(3) 0.3358(2) 0.1911(2) 0.0377(8) Uani 1 1 d . . .
C5 C 0.1980(3) 0.6916(2) 0.3943(2) 0.0292(8) Uani 1 1 d . . .
C16 C 0.0618(3) 0.3324(3) 0.4377(2) 0.0397(10) Uani 1 1 d . . .
H16A H 0.1249 0.3145 0.4668 0.060 Uiso 1 1 calc R . .
H16B H 0.0166 0.2972 0.4537 0.060 Uiso 1 1 calc R . .
H16C H 0.0530 0.3930 0.4486 0.060 Uiso 1 1 calc R . .
C15 C 0.0538(3) 0.2000(3) 0.3172(3) 0.0400(10) Uani 1 1 d . . .
H15A H 0.1174 0.1811 0.3436 0.060 Uiso 1 1 calc R . .
H15B H 0.0386 0.1869 0.2614 0.060 Uiso 1 1 calc R . .
H15C H 0.0103 0.1699 0.3395 0.060 Uiso 1 1 calc R . .
C22 C 0.5155(3) 0.6293(3) 0.4081(3) 0.0413(11) Uani 1 1 d . . .
H22A H 0.5544 0.6752 0.4333 0.050 Uiso 1 1 calc R . .
C32 C 0.4425(3) 0.4143(3) 0.0932(3) 0.0431(10) Uani 1 1 d . . .
H32A H 0.4179 0.3558 0.0912 0.065 Uiso 1 1 calc R . .
H32B H 0.4909 0.4230 0.1428 0.065 Uiso 1 1 calc R . .
H32C H 0.4690 0.4227 0.0500 0.065 Uiso 1 1 calc R . .
C31 C 0.3998(3) 0.6024(3) 0.0891(3) 0.0429(10) Uani 1 1 d . . .
H31A H 0.3520 0.6465 0.0849 0.064 Uiso 1 1 calc R . .
H31B H 0.4268 0.6088 0.0459 0.064 Uiso 1 1 calc R . .
H31C H 0.4487 0.6091 0.1388 0.064 Uiso 1 1 calc R . .
C30 C 0.2588(3) 0.4836(3) -0.0124(2) 0.0434(11) Uani 1 1 d . . .
H30A H 0.2087 0.5252 -0.0165 0.065 Uiso 1 1 calc R . .
H30B H 0.2331 0.4253 -0.0189 0.065 Uiso 1 1 calc R . .
H30C H 0.2885 0.4952 -0.0532 0.065 Uiso 1 1 calc R . .
C20 C 0.4397(3) 0.6202(3) 0.5141(2) 0.0370(10) Uani 1 1 d . . .
H20A H 0.4771 0.6654 0.5425 0.044 Uiso 1 1 calc R . .
C23 C 0.5232(3) 0.5968(3) 0.3394(3) 0.0445(11) Uani 1 1 d . . .
H23A H 0.5699 0.6186 0.3187 0.053 Uiso 1 1 calc R . .
C19 C 0.3771(3) 0.5807(3) 0.5434(2) 0.0371(9) Uani 1 1 d . . .
H19A H 0.3707 0.5984 0.5922 0.045 Uiso 1 1 calc R . .
C17 C 0.2556(3) 0.4666(3) 0.5347(2) 0.0409(10) Uani 1 1 d . . .
H17A H 0.2231 0.4223 0.4979 0.061 Uiso 1 1 calc R . .
H17B H 0.2102 0.5072 0.5441 0.061 Uiso 1 1 calc R . .
H17C H 0.2900 0.4395 0.5841 0.061 Uiso 1 1 calc R . .
C3 C 0.3090(3) 0.7803(3) 0.3575(3) 0.0379(10) Uani 1 1 d . . .
H3A H 0.3499 0.8282 0.3667 0.046 Uiso 1 1 calc R . .
C1 C 0.3502(3) 0.7488(3) 0.2330(3) 0.0405(10) Uani 1 1 d . . .
H1A H 0.3358 0.7053 0.1916 0.061 Uiso 1 1 calc R . .
H1B H 0.4173 0.7495 0.2588 0.061 Uiso 1 1 calc R . .
H1C H 0.3302 0.8054 0.2103 0.061 Uiso 1 1 calc R . .
C14 C -0.0774(3) 0.3536(3) 0.2799(3) 0.0420(10) Uani 1 1 d . . .
H14A H -0.0898 0.3472 0.2234 0.063 Uiso 1 1 calc R . .
H14B H -0.0848 0.4140 0.2924 0.063 Uiso 1 1 calc R . .
H14C H -0.1212 0.3182 0.2975 0.063 Uiso 1 1 calc R . .
Cl2 Cl 0.15040(7) 0.65246(6) 0.07896(6) 0.0352(2) Uani 1 1 d . . .
Cl1 Cl 0.30151(7) 0.26342(6) 0.42643(6) 0.0346(2) Uani 1 1 d . . .
Cl3 Cl 0.66302(10) 0.51251(11) 0.21182(11) 0.0821(5) Uani 1 1 d . . .
C12 C 0.0468(3) 0.3164(3) 0.1487(3) 0.0403(10) Uani 1 1 d . . .
H12A H 0.0758 0.2822 0.1954 0.061 Uiso 1 1 calc R . .
H12B H 0.0763 0.3031 0.1081 0.061 Uiso 1 1 calc R . .
H12C H -0.0196 0.3027 0.1296 0.061 Uiso 1 1 calc R . .
C13 C 0.0178(3) 0.4659(3) 0.1030(2) 0.0431(11) Uani 1 1 d . . .
H13A H 0.0290 0.5253 0.1215 0.065 Uiso 1 1 calc R . .
H13B H -0.0492 0.4557 0.0829 0.065 Uiso 1 1 calc R . .
H13C H 0.0467 0.4561 0.0614 0.065 Uiso 1 1 calc R . .
C28 C 0.2572(4) 0.3087(3) 0.1123(3) 0.0516(13) Uani 1 1 d . . .
H28A H 0.2305 0.3592 0.0811 0.077 Uiso 1 1 calc R . .
H28B H 0.2073 0.2694 0.1146 0.077 Uiso 1 1 calc R . .
H28C H 0.2996 0.2794 0.0884 0.077 Uiso 1 1 calc R . .
C29 C 0.3529(5) 0.2674(3) 0.2455(3) 0.076(2) Uani 1 1 d . . .
H29A H 0.3850 0.2926 0.2964 0.113 Uiso 1 1 calc R . .
H29B H 0.3978 0.2370 0.2252 0.113 Uiso 1 1 calc R . .
H29C H 0.3055 0.2270 0.2514 0.113 Uiso 1 1 calc R . .
C33 C 0.7683(3) 0.5618(3) 0.2147(3) 0.0476(11) Uani 1 1 d . . .
H33A H 0.7558 0.6141 0.1818 0.057 Uiso 1 1 calc R . .
H33B H 0.8058 0.5222 0.1930 0.057 Uiso 1 1 calc R . .
Cl4 Cl 0.83184(9) 0.58999(8) 0.31100(7) 0.0521(3) 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
Co1 N4 2.002(3) . ?
Co1 N6 2.020(3) . ?
Co1 N5 2.062(3) . ?
Co1 Cl1 2.2721(11) . ?
Co2 N8 2.014(3) . ?
Co2 N2 2.017(3) . ?
Co2 N1 2.058(3) . ?
Co2 Cl2 2.2616(11) . ?
Si1 N4 1.754(3) . ?
Si1 C15 1.864(4) . ?
Si1 C16 1.873(4) . ?
Si1 C14 1.875(4) . ?
Si2 N8 1.746(3) . ?
Si2 C30 1.856(4) . ?
Si2 C31 1.870(5) . ?
Si2 C32 1.874(4) . ?
N4 C11 1.352(4) . ?
N2 C11 1.365(4) . ?
N2 C9 1.401(4) . ?
N1 C2 1.335(5) . ?
N1 C10 1.372(5) . ?
N8 C27 1.350(5) . ?
C9 C8 1.379(5) . ?
C9 C10 1.424(5) . ?
N5 C18 1.333(5) . ?
N5 C26 1.376(4) . ?
N6 C27 1.363(5) . ?
N6 C25 1.398(4) . ?
C8 C7 1.406(5) . ?
C27 N7 1.351(5) . ?
C10 C5 1.424(5) . ?
C11 N3 1.350(4) . ?
C26 C21 1.415(5) . ?
C26 C25 1.422(5) . ?
N3 C12 1.449(5) . ?
N3 C13 1.465(5) . ?
C25 C24 1.382(5) . ?
C24 C23 1.394(6) . ?
C18 C19 1.415(5) . ?
C18 C17 1.483(6) . ?
C6 C7 1.365(6) . ?
C6 C5 1.413(6) . ?
C2 C3 1.413(6) . ?
C2 C1 1.501(6) . ?
C21 C22 1.406(6) . ?
C21 C20 1.416(6) . ?
C4 C3 1.353(6) . ?
C4 C5 1.417(5) . ?
N7 C28 1.458(6) . ?
N7 C29 1.467(6) . ?
C22 C23 1.368(7) . ?
C20 C19 1.354(6) . ?
Cl3 C33 1.748(5) . ?
C33 Cl4 1.766(5) . ?

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
N4 Co1 N6 111.38(12) . . ?
N4 Co1 N5 127.49(12) . . ?
N6 Co1 N5 82.50(12) . . ?
N4 Co1 Cl1 107.72(9) . . ?
N6 Co1 Cl1 117.96(9) . . ?
N5 Co1 Cl1 108.73(9) . . ?
N8 Co2 N2 110.17(12) . . ?
N8 Co2 N1 127.63(12) . . ?
N2 Co2 N1 83.38(12) . . ?
N8 Co2 Cl2 109.23(9) . . ?
N2 Co2 Cl2 119.91(9) . . ?
N1 Co2 Cl2 105.61(9) . . ?
N4 Si1 C15 115.96(17) . . ?
N4 Si1 C16 109.12(17) . . ?
C15 Si1 C16 104.9(2) . . ?
N4 Si1 C14 110.64(18) . . ?
C15 Si1 C14 109.2(2) . . ?
C16 Si1 C14 106.5(2) . . ?
N8 Si2 C30 113.56(18) . . ?
N8 Si2 C31 108.49(18) . . ?
C30 Si2 C31 107.0(2) . . ?
N8 Si2 C32 111.41(18) . . ?
C30 Si2 C32 109.8(2) . . ?
C31 Si2 C32 106.2(2) . . ?
C11 N4 Si1 125.0(2) . . ?
C11 N4 Co1 110.9(2) . . ?
Si1 N4 Co1 124.08(16) . . ?
C11 N2 C9 119.0(3) . . ?
C11 N2 Co2 126.5(2) . . ?
C9 N2 Co2 111.1(2) . . ?
C2 N1 C10 119.6(3) . . ?
C2 N1 Co2 130.1(3) . . ?
C10 N1 Co2 110.2(2) . . ?
C27 N8 Si2 125.3(2) . . ?
C27 N8 Co2 111.6(2) . . ?
Si2 N8 Co2 122.99(16) . . ?
C8 C9 N2 125.1(3) . . ?
C8 C9 C10 117.7(3) . . ?
N2 C9 C10 116.9(3) . . ?
C18 N5 C26 119.7(3) . . ?
C18 N5 Co1 129.1(3) . . ?
C26 N5 Co1 111.0(2) . . ?
C27 N6 C25 118.8(3) . . ?
C27 N6 Co1 126.3(2) . . ?
C25 N6 Co1 111.9(2) . . ?
C9 C8 C7 122.3(4) . . ?
N8 C27 N7 121.2(3) . . ?
N8 C27 N6 123.2(3) . . ?
N7 C27 N6 115.4(3) . . ?
N1 C10 C5 121.7(3) . . ?
N1 C10 C9 118.3(3) . . ?
C5 C10 C9 119.9(3) . . ?
N3 C11 N4 121.6(3) . . ?
N3 C11 N2 115.7(3) . . ?
N4 C11 N2 122.5(3) . . ?
N5 C26 C21 121.8(4) . . ?
N5 C26 C25 117.5(3) . . ?
C21 C26 C25 120.6(3) . . ?
C11 N3 C12 122.4(3) . . ?
C11 N3 C13 122.3(3) . . ?
C12 N3 C13 115.3(3) . . ?
C24 C25 N6 124.9(4) . . ?
C24 C25 C26 117.8(3) . . ?
N6 C25 C26 116.9(3) . . ?
C25 C24 C23 121.2(4) . . ?
N5 C18 C19 120.9(4) . . ?
N5 C18 C17 118.1(3) . . ?
C19 C18 C17 121.0(4) . . ?
C7 C6 C5 119.5(4) . . ?
N1 C2 C3 121.3(4) . . ?
N1 C2 C1 117.8(3) . . ?
C3 C2 C1 120.9(4) . . ?
C22 C21 C26 119.1(4) . . ?
C22 C21 C20 124.0(4) . . ?
C26 C21 C20 117.0(4) . . ?
C3 C4 C5 120.4(4) . . ?
C6 C7 C8 120.6(4) . . ?
C27 N7 C28 123.4(4) . . ?
C27 N7 C29 120.3(4) . . ?
C28 N7 C29 116.3(4) . . ?
C6 C5 C4 123.4(4) . . ?
C6 C5 C10 119.8(3) . . ?
C4 C5 C10 116.8(4) . . ?
C23 C22 C21 119.7(4) . . ?
C19 C20 C21 120.2(4) . . ?
C22 C23 C24 121.4(4) . . ?
C20 C19 C18 120.4(4) . . ?
C4 C3 C2 120.2(4) . . ?
Cl3 C33 Cl4 111.3(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
C15 Si1 N4 C11 110.1(3) . . . . ?
C16 Si1 N4 C11 -131.8(3) . . . . ?
C14 Si1 N4 C11 -14.9(3) . . . . ?
C15 Si1 N4 Co1 -72.6(3) . . . . ?
C16 Si1 N4 Co1 45.5(3) . . . . ?
C14 Si1 N4 Co1 162.4(2) . . . . ?
N6 Co1 N4 C11 -23.9(3) . . . . ?
N5 Co1 N4 C11 73.2(3) . . . . ?
Cl1 Co1 N4 C11 -154.7(2) . . . . ?
N6 Co1 N4 Si1 158.44(17) . . . . ?
N5 Co1 N4 Si1 -104.5(2) . . . . ?
Cl1 Co1 N4 Si1 27.6(2) . . . . ?
N8 Co2 N2 C11 -27.9(3) . . . . ?
N1 Co2 N2 C11 -155.6(3) . . . . ?
Cl2 Co2 N2 C11 100.2(3) . . . . ?
N8 Co2 N2 C9 130.8(2) . . . . ?
N1 Co2 N2 C9 3.0(2) . . . . ?
Cl2 Co2 N2 C9 -101.2(2) . . . . ?
N8 Co2 N1 C2 71.3(3) . . . . ?
N2 Co2 N1 C2 -178.3(3) . . . . ?
Cl2 Co2 N1 C2 -59.0(3) . . . . ?
N8 Co2 N1 C10 -113.2(2) . . . . ?
N2 Co2 N1 C10 -2.8(2) . . . . ?
Cl2 Co2 N1 C10 116.4(2) . . . . ?
C30 Si2 N8 C27 113.3(3) . . . . ?
C31 Si2 N8 C27 -128.0(3) . . . . ?
C32 Si2 N8 C27 -11.4(4) . . . . ?
C30 Si2 N8 Co2 -69.1(3) . . . . ?
C31 Si2 N8 Co2 49.7(2) . . . . ?
C32 Si2 N8 Co2 166.3(2) . . . . ?
N2 Co2 N8 C27 -26.9(3) . . . . ?
N1 Co2 N8 C27 70.4(3) . . . . ?
Cl2 Co2 N8 C27 -160.6(2) . . . . ?
N2 Co2 N8 Si2 155.09(17) . . . . ?
N1 Co2 N8 Si2 -107.6(2) . . . . ?
Cl2 Co2 N8 Si2 21.4(2) . . . . ?
C11 N2 C9 C8 -28.4(5) . . . . ?
Co2 N2 C9 C8 171.1(3) . . . . ?
C11 N2 C9 C10 157.7(3) . . . . ?
Co2 N2 C9 C10 -2.8(4) . . . . ?
N4 Co1 N5 C18 70.0(3) . . . . ?
N6 Co1 N5 C18 -178.8(3) . . . . ?
Cl1 Co1 N5 C18 -61.7(3) . . . . ?
N4 Co1 N5 C26 -114.3(2) . . . . ?
N6 Co1 N5 C26 -3.0(2) . . . . ?
Cl1 Co1 N5 C26 114.0(2) . . . . ?
N4 Co1 N6 C27 -29.5(3) . . . . ?
N5 Co1 N6 C27 -156.9(3) . . . . ?
Cl1 Co1 N6 C27 95.8(3) . . . . ?
N4 Co1 N6 C25 130.2(2) . . . . ?
N5 Co1 N6 C25 2.8(2) . . . . ?
Cl1 Co1 N6 C25 -104.5(2) . . . . ?
N2 C9 C8 C7 -178.2(3) . . . . ?
C10 C9 C8 C7 -4.3(5) . . . . ?
Si2 N8 C27 N7 -50.1(5) . . . . ?
Co2 N8 C27 N7 132.0(3) . . . . ?
Si2 N8 C27 N6 134.2(3) . . . . ?
Co2 N8 C27 N6 -43.7(4) . . . . ?
C25 N6 C27 N8 -40.9(5) . . . . ?
Co1 N6 C27 N8 117.6(3) . . . . ?
C25 N6 C27 N7 143.1(3) . . . . ?
Co1 N6 C27 N7 -58.4(4) . . . . ?
C2 N1 C10 C5 -0.1(5) . . . . ?
Co2 N1 C10 C5 -176.1(3) . . . . ?
C2 N1 C10 C9 178.2(3) . . . . ?
Co2 N1 C10 C9 2.2(4) . . . . ?
C8 C9 C10 N1 -174.0(3) . . . . ?
N2 C9 C10 N1 0.4(5) . . . . ?
C8 C9 C10 C5 4.3(5) . . . . ?
N2 C9 C10 C5 178.7(3) . . . . ?
Si1 N4 C11 N3 -54.0(4) . . . . ?
Co1 N4 C11 N3 128.4(3) . . . . ?
Si1 N4 C11 N2 130.3(3) . . . . ?
Co1 N4 C11 N2 -47.3(4) . . . . ?
C9 N2 C11 N3 146.5(3) . . . . ?
Co2 N2 C11 N3 -56.4(4) . . . . ?
C9 N2 C11 N4 -37.6(5) . . . . ?
Co2 N2 C11 N4 119.6(3) . . . . ?
C18 N5 C26 C21 0.4(5) . . . . ?
Co1 N5 C26 C21 -175.8(3) . . . . ?
C18 N5 C26 C25 179.0(3) . . . . ?
Co1 N5 C26 C25 2.8(4) . . . . ?
N4 C11 N3 C12 -14.2(5) . . . . ?
N2 C11 N3 C12 161.8(3) . . . . ?
N4 C11 N3 C13 166.7(4) . . . . ?
N2 C11 N3 C13 -17.3(5) . . . . ?
C27 N6 C25 C24 -27.6(5) . . . . ?
Co1 N6 C25 C24 171.0(3) . . . . ?
C27 N6 C25 C26 159.3(3) . . . . ?
Co1 N6 C25 C26 -2.2(4) . . . . ?
N5 C26 C25 C24 -174.1(3) . . . . ?
C21 C26 C25 C24 4.4(5) . . . . ?
N5 C26 C25 N6 -0.5(5) . . . . ?
C21 C26 C25 N6 178.1(3) . . . . ?
N6 C25 C24 C23 -176.7(4) . . . . ?
C26 C25 C24 C23 -3.6(6) . . . . ?
C26 N5 C18 C19 1.3(5) . . . . ?
Co1 N5 C18 C19 176.7(3) . . . . ?
C26 N5 C18 C17 -177.5(3) . . . . ?
Co1 N5 C18 C17 -2.1(5) . . . . ?
C10 N1 C2 C3 2.2(5) . . . . ?
Co2 N1 C2 C3 177.3(3) . . . . ?
C10 N1 C2 C1 -176.4(3) . . . . ?
Co2 N1 C2 C1 -1.3(5) . . . . ?
N5 C26 C21 C22 176.9(3) . . . . ?
C25 C26 C21 C22 -1.6(5) . . . . ?
N5 C26 C21 C20 -1.8(5) . . . . ?
C25 C26 C21 C20 179.7(3) . . . . ?
C5 C6 C7 C8 2.3(6) . . . . ?
C9 C8 C7 C6 1.0(6) . . . . ?
N8 C27 N7 C28 -18.3(6) . . . . ?
N6 C27 N7 C28 157.8(4) . . . . ?
N8 C27 N7 C29 161.5(4) . . . . ?
N6 C27 N7 C29 -22.5(6) . . . . ?
C7 C6 C5 C4 176.8(4) . . . . ?
C7 C6 C5 C10 -2.2(6) . . . . ?
C3 C4 C5 C6 -177.0(4) . . . . ?
C3 C4 C5 C10 2.1(6) . . . . ?
N1 C10 C5 C6 177.1(3) . . . . ?
C9 C10 C5 C6 -1.2(5) . . . . ?
N1 C10 C5 C4 -2.0(5) . . . . ?
C9 C10 C5 C4 179.7(3) . . . . ?
C26 C21 C22 C23 -2.2(6) . . . . ?
C20 C21 C22 C23 176.4(4) . . . . ?
C22 C21 C20 C19 -177.1(4) . . . . ?
C26 C21 C20 C19 1.5(6) . . . . ?
C21 C22 C23 C24 3.1(7) . . . . ?
C25 C24 C23 C22 -0.2(7) . . . . ?
C21 C20 C19 C18 0.2(6) . . . . ?
N5 C18 C19 C20 -1.6(6) . . . . ?
C17 C18 C19 C20 177.1(4) . . . . ?
C5 C4 C3 C2 -0.1(6) . . . . ?
N1 C2 C3 C4 -2.1(6) . . . . ?
C1 C2 C3 C4 176.5(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.097

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1022958'
_audit_update_record             
;
2015-01-16 deposited with the CCDC.
2015-01-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H46 Cl2 Fe2 N8 Si2, C H2 Cl2'
_chemical_formula_sum            'C33 H48 Cl4 Fe2 N8 Si2'
_chemical_formula_weight         866.47

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   15.103(3)
_cell_length_b                   15.635(3)
_cell_length_c                   17.934(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.776(2)
_cell_angle_gamma                90.00
_cell_volume                     4054.4(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6926
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      27.28

_exptl_crystal_description       Block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1800
_exptl_absorpt_coefficient_mu    1.073
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.7051
_exptl_absorpt_correction_T_max  0.7390
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15089
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         25.05
_reflns_number_total             7026
_reflns_number_gt                5730
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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 > 2sigma(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)+(0.0499P)²+6.7754P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7026
_refine_ls_number_parameters     442
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0439
_refine_ls_wR_factor_ref         0.1303
_refine_ls_wR_factor_gt          0.1109
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Fe1 Fe 0.25860(3) 0.38462(3) 0.36121(3) 0.03026(15) Uani 1 1 d . . .
Fe2 Fe 0.21487(3) 0.57101(3) 0.18369(3) 0.02971(15) Uani 1 1 d . . .
Si1 Si 0.04358(7) 0.31742(7) 0.33033(7) 0.0392(3) Uani 1 1 d . . .
Si2 Si 0.34878(8) 0.49179(8) 0.08538(6) 0.0421(3) Uani 1 1 d . . .
N4 N 0.1232(2) 0.38198(18) 0.30170(17) 0.0316(6) Uani 1 1 d . . .
N2 N 0.13193(19) 0.51839(18) 0.24526(16) 0.0281(6) Uani 1 1 d . . .
N1 N 0.24310(19) 0.65655(18) 0.27949(17) 0.0306(6) Uani 1 1 d . . .
N8 N 0.3016(2) 0.4815(2) 0.16339(17) 0.0337(7) Uani 1 1 d . . .
C9 C 0.1334(2) 0.5649(2) 0.3121(2) 0.0290(7) Uani 1 1 d . . .
N5 N 0.32771(19) 0.48766(19) 0.43130(16) 0.0310(6) Uani 1 1 d . . .
N6 N 0.3382(2) 0.42968(19) 0.29341(17) 0.0310(6) Uani 1 1 d . . .
C8 C 0.0761(3) 0.5513(3) 0.3585(2) 0.0385(8) Uani 1 1 d . . .
H8A H 0.0330 0.5055 0.3465 0.046 Uiso 1 1 calc R . .
C27 C 0.3188(2) 0.4174(2) 0.2151(2) 0.0323(8) Uani 1 1 d . . .
C10 C 0.1923(2) 0.6379(2) 0.3294(2) 0.0299(7) Uani 1 1 d . . .
C11 C 0.1027(2) 0.4357(2) 0.2400(2) 0.0291(7) Uani 1 1 d . . .
C26 C 0.3899(2) 0.5271(2) 0.4005(2) 0.0315(8) Uani 1 1 d . . .
N3 N 0.0559(2) 0.4085(2) 0.16838(18) 0.0374(7) Uani 1 1 d . . .
C25 C 0.3964(2) 0.4973(2) 0.3276(2) 0.0339(8) Uani 1 1 d . . .
C24 C 0.4649(3) 0.5310(3) 0.2995(2) 0.0449(10) Uani 1 1 d . . .
H24A H 0.4725 0.5096 0.2522 0.054 Uiso 1 1 calc R . .
C18 C 0.3213(3) 0.5125(3) 0.5005(2) 0.0401(9) Uani 1 1 d . . .
C6 C 0.1381(3) 0.6694(3) 0.4425(2) 0.0470(10) Uani 1 1 d . . .
H6A H 0.1413 0.7022 0.4877 0.056 Uiso 1 1 calc R . .
C2 C 0.2974(3) 0.7248(2) 0.2929(2) 0.0406(9) Uani 1 1 d . . .
C21 C 0.4485(3) 0.5931(3) 0.4402(2) 0.0412(9) Uani 1 1 d . . .
C4 C 0.2563(3) 0.7598(3) 0.4085(3) 0.0481(10) Uani 1 1 d . . .
H4A H 0.2624 0.7951 0.4529 0.058 Uiso 1 1 calc R . .
C7 C 0.0797(3) 0.6031(3) 0.4228(2) 0.0475(10) Uani 1 1 d . . .
H7A H 0.0394 0.5910 0.4535 0.057 Uiso 1 1 calc R . .
N7 N 0.3116(3) 0.3352(2) 0.1916(2) 0.0517(9) Uani 1 1 d . . .
C5 C 0.1950(3) 0.6893(2) 0.3946(2) 0.0382(9) Uani 1 1 d . . .
C16 C 0.0629(3) 0.3288(3) 0.4379(3) 0.0562(12) Uani 1 1 d . . .
H16A H 0.1259 0.3107 0.4656 0.084 Uiso 1 1 calc R . .
H16B H 0.0185 0.2929 0.4541 0.084 Uiso 1 1 calc R . .
H16C H 0.0544 0.3887 0.4504 0.084 Uiso 1 1 calc R . .
C15 C 0.0542(3) 0.1999(3) 0.3158(3) 0.0529(11) Uani 1 1 d . . .
H15A H 0.1175 0.1815 0.3422 0.079 Uiso 1 1 calc R . .
H15B H 0.0397 0.1876 0.2600 0.079 Uiso 1 1 calc R . .
H15C H 0.0108 0.1692 0.3377 0.079 Uiso 1 1 calc R . .
C22 C 0.5145(3) 0.6279(3) 0.4068(3) 0.0550(12) Uani 1 1 d . . .
H22A H 0.5529 0.6739 0.4317 0.066 Uiso 1 1 calc R . .
C32 C 0.4454(3) 0.4136(3) 0.0930(3) 0.0581(12) Uani 1 1 d . . .
H32A H 0.4215 0.3552 0.0911 0.087 Uiso 1 1 calc R . .
H32B H 0.4936 0.4225 0.1424 0.087 Uiso 1 1 calc R . .
H32C H 0.4716 0.4225 0.0496 0.087 Uiso 1 1 calc R . .
C31 C 0.4005(3) 0.6007(3) 0.0889(3) 0.0573(12) Uani 1 1 d . . .
H31A H 0.3524 0.6440 0.0847 0.086 Uiso 1 1 calc R . .
H31B H 0.4273 0.6073 0.0455 0.086 Uiso 1 1 calc R . .
H31C H 0.4491 0.6080 0.1383 0.086 Uiso 1 1 calc R . .
C30 C 0.2627(4) 0.4825(4) -0.0109(3) 0.0628(13) Uani 1 1 d . . .
H30A H 0.2129 0.5239 -0.0147 0.094 Uiso 1 1 calc R . .
H30B H 0.2369 0.4245 -0.0174 0.094 Uiso 1 1 calc R . .
H30C H 0.2924 0.4941 -0.0517 0.094 Uiso 1 1 calc R . .
C20 C 0.4379(3) 0.6187(3) 0.5120(3) 0.0516(11) Uani 1 1 d . . .
H20A H 0.4749 0.6638 0.5402 0.062 Uiso 1 1 calc R . .
C23 C 0.5228(3) 0.5954(3) 0.3387(3) 0.0557(12) Uani 1 1 d . . .
H23A H 0.5692 0.6172 0.3178 0.067 Uiso 1 1 calc R . .
C19 C 0.3754(3) 0.5800(3) 0.5413(2) 0.0501(11) Uani 1 1 d . . .
H19A H 0.3680 0.5984 0.5896 0.060 Uiso 1 1 calc R . .
C17 C 0.2568(3) 0.4664(3) 0.5344(3) 0.0543(11) Uani 1 1 d . . .
H17A H 0.2243 0.4222 0.4980 0.081 Uiso 1 1 calc R . .
H17B H 0.2119 0.5068 0.5443 0.081 Uiso 1 1 calc R . .
H17C H 0.2916 0.4396 0.5836 0.081 Uiso 1 1 calc R . .
C3 C 0.3061(3) 0.7770(3) 0.3589(3) 0.0494(11) Uani 1 1 d . . .
H3A H 0.3472 0.8244 0.3683 0.059 Uiso 1 1 calc R . .
C1 C 0.3482(3) 0.7465(3) 0.2350(3) 0.0549(11) Uani 1 1 d . . .
H1A H 0.3344 0.7036 0.1934 0.082 Uiso 1 1 calc R . .
H1B H 0.4149 0.7471 0.2611 0.082 Uiso 1 1 calc R . .
H1C H 0.3287 0.8030 0.2127 0.082 Uiso 1 1 calc R . .
C14 C -0.0776(3) 0.3513(3) 0.2816(3) 0.0609(13) Uani 1 1 d . . .
H14A H -0.0905 0.3451 0.2251 0.091 Uiso 1 1 calc R . .
H14B H -0.0856 0.4113 0.2943 0.091 Uiso 1 1 calc R . .
H14C H -0.1203 0.3154 0.2997 0.091 Uiso 1 1 calc R . .
Cl2 Cl 0.14591(7) 0.65284(7) 0.07832(6) 0.0470(3) Uani 1 1 d . . .
Cl1 Cl 0.30793(7) 0.26050(6) 0.42698(6) 0.0469(3) Uani 1 1 d . . .
Cl3 Cl 0.66547(14) 0.51029(14) 0.21237(15) 0.1193(8) Uani 1 1 d . . .
C12 C 0.0457(4) 0.3179(3) 0.1480(3) 0.0533(11) Uani 1 1 d . . .
H12A H 0.0745 0.2834 0.1943 0.080 Uiso 1 1 calc R . .
H12B H 0.0759 0.3059 0.1076 0.080 Uiso 1 1 calc R . .
H12C H -0.0202 0.3036 0.1285 0.080 Uiso 1 1 calc R . .
C13 C 0.0133(3) 0.4674(3) 0.1048(3) 0.0595(13) Uani 1 1 d . . .
H13A H 0.0246 0.5265 0.1234 0.089 Uiso 1 1 calc R . .
H13B H -0.0534 0.4569 0.0865 0.089 Uiso 1 1 calc R . .
H13C H 0.0403 0.4584 0.0618 0.089 Uiso 1 1 calc R . .
C28 C 0.2599(4) 0.3091(4) 0.1145(3) 0.0707(15) Uani 1 1 d . . .
H28A H 0.2335 0.3596 0.0837 0.106 Uiso 1 1 calc R . .
H28B H 0.2100 0.2705 0.1176 0.106 Uiso 1 1 calc R . .
H28C H 0.3010 0.2794 0.0896 0.106 Uiso 1 1 calc R . .
C29 C 0.3584(6) 0.2679(3) 0.2465(4) 0.100(3) Uani 1 1 d . . .
H29A H 0.3901 0.2938 0.2968 0.150 Uiso 1 1 calc R . .
H29B H 0.4036 0.2385 0.2258 0.150 Uiso 1 1 calc R . .
H29C H 0.3124 0.2267 0.2532 0.150 Uiso 1 1 calc R . .
C33 C 0.7700(4) 0.5600(4) 0.2169(3) 0.0708(14) Uani 1 1 d . . .
H33A H 0.8085 0.5207 0.1962 0.085 Uiso 1 1 calc R . .
H33B H 0.7578 0.6116 0.1834 0.085 Uiso 1 1 calc R . .
Cl4 Cl 0.83003(11) 0.58911(11) 0.31033(8) 0.0784(4) 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
Fe1 N4 2.015(3) . ?
Fe1 N6 2.065(3) . ?
Fe1 N5 2.123(3) . ?
Fe1 Cl1 2.2813(11) . ?
Fe2 N8 2.020(3) . ?
Fe2 N2 2.065(3) . ?
Fe2 N1 2.121(3) . ?
Fe2 Cl2 2.2708(11) . ?
Si1 N4 1.757(3) . ?
Si1 C14 1.863(5) . ?
Si1 C15 1.868(4) . ?
Si1 C16 1.875(4) . ?
Si2 N8 1.751(3) . ?
Si2 C30 1.843(5) . ?
Si2 C31 1.867(5) . ?
Si2 C32 1.878(5) . ?
N4 C11 1.353(5) . ?
N2 C11 1.360(4) . ?
N2 C9 1.397(4) . ?
N1 C2 1.325(5) . ?
N1 C10 1.368(5) . ?
N8 C27 1.339(5) . ?
C9 C8 1.379(5) . ?
C9 C10 1.426(5) . ?
N5 C18 1.331(5) . ?
N5 C26 1.367(5) . ?
N6 C27 1.364(5) . ?
N6 C25 1.397(5) . ?
C8 C7 1.396(6) . ?
C27 N7 1.348(5) . ?
C10 C5 1.410(5) . ?
C11 N3 1.344(4) . ?
C26 C21 1.411(5) . ?
C26 C25 1.417(5) . ?
N3 C12 1.460(5) . ?
N3 C13 1.463(5) . ?
C25 C24 1.380(5) . ?
C24 C23 1.385(6) . ?
C18 C19 1.404(6) . ?
C18 C17 1.476(6) . ?
C6 C7 1.341(6) . ?
C6 C5 1.412(6) . ?
C2 C3 1.413(6) . ?
C2 C1 1.497(6) . ?
C21 C20 1.401(6) . ?
C21 C22 1.412(6) . ?
C4 C3 1.349(7) . ?
C4 C5 1.416(6) . ?
N7 C28 1.436(6) . ?
N7 C29 1.474(7) . ?
C22 C23 1.362(7) . ?
C20 C19 1.348(7) . ?
Cl3 C33 1.741(6) . ?
C33 Cl4 1.721(6) . ?

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
N4 Fe1 N6 111.67(12) . . ?
N4 Fe1 N5 125.40(11) . . ?
N6 Fe1 N5 79.59(12) . . ?
N4 Fe1 Cl1 112.73(9) . . ?
N6 Fe1 Cl1 115.83(9) . . ?
N5 Fe1 Cl1 107.94(8) . . ?
N8 Fe2 N2 110.22(12) . . ?
N8 Fe2 N1 126.40(11) . . ?
N2 Fe2 N1 80.17(11) . . ?
N8 Fe2 Cl2 113.93(9) . . ?
N2 Fe2 Cl2 117.78(8) . . ?
N1 Fe2 Cl2 104.80(8) . . ?
N4 Si1 C14 111.2(2) . . ?
N4 Si1 C15 115.53(18) . . ?
C14 Si1 C15 109.0(2) . . ?
N4 Si1 C16 109.27(18) . . ?
C14 Si1 C16 107.2(2) . . ?
C15 Si1 C16 104.0(2) . . ?
N8 Si2 C30 113.7(2) . . ?
N8 Si2 C31 108.63(19) . . ?
C30 Si2 C31 106.2(2) . . ?
N8 Si2 C32 111.64(19) . . ?
C30 Si2 C32 109.9(2) . . ?
C31 Si2 C32 106.4(2) . . ?
C11 N4 Si1 125.5(2) . . ?
C11 N4 Fe1 112.3(2) . . ?
Si1 N4 Fe1 122.18(16) . . ?
C11 N2 C9 118.6(3) . . ?
C11 N2 Fe2 125.2(2) . . ?
C9 N2 Fe2 113.0(2) . . ?
C2 N1 C10 119.2(3) . . ?
C2 N1 Fe2 128.6(3) . . ?
C10 N1 Fe2 112.1(2) . . ?
C27 N8 Si2 125.4(2) . . ?
C27 N8 Fe2 113.6(2) . . ?
Si2 N8 Fe2 121.01(16) . . ?
C8 C9 N2 125.5(3) . . ?
C8 C9 C10 116.9(3) . . ?
N2 C9 C10 117.2(3) . . ?
C18 N5 C26 119.3(3) . . ?
C18 N5 Fe1 128.2(3) . . ?
C26 N5 Fe1 112.4(2) . . ?
C27 N6 C25 118.7(3) . . ?
C27 N6 Fe1 124.7(2) . . ?
C25 N6 Fe1 113.5(2) . . ?
C9 C8 C7 121.9(4) . . ?
N8 C27 N7 121.1(3) . . ?
N8 C27 N6 123.3(3) . . ?
N7 C27 N6 115.5(3) . . ?
N1 C10 C5 122.3(3) . . ?
N1 C10 C9 117.5(3) . . ?
C5 C10 C9 120.2(3) . . ?
N3 C11 N4 121.2(3) . . ?
N3 C11 N2 116.0(3) . . ?
N4 C11 N2 122.7(3) . . ?
N5 C26 C21 122.0(3) . . ?
N5 C26 C25 117.6(3) . . ?
C21 C26 C25 120.4(3) . . ?
C11 N3 C12 122.3(3) . . ?
C11 N3 C13 122.5(3) . . ?
C12 N3 C13 115.2(3) . . ?
C24 C25 N6 124.8(4) . . ?
C24 C25 C26 118.0(3) . . ?
N6 C25 C26 116.9(3) . . ?
C25 C24 C23 121.5(4) . . ?
N5 C18 C19 121.1(4) . . ?
N5 C18 C17 118.4(4) . . ?
C19 C18 C17 120.4(4) . . ?
C7 C6 C5 118.7(4) . . ?
N1 C2 C3 121.4(4) . . ?
N1 C2 C1 118.1(4) . . ?
C3 C2 C1 120.5(4) . . ?
C20 C21 C26 116.9(4) . . ?
C20 C21 C22 124.1(4) . . ?
C26 C21 C22 119.0(4) . . ?
C3 C4 C5 120.0(4) . . ?
C6 C7 C8 122.0(4) . . ?
C27 N7 C28 122.9(4) . . ?
C27 N7 C29 119.5(4) . . ?
C28 N7 C29 117.6(4) . . ?
C10 C5 C6 120.1(4) . . ?
C10 C5 C4 116.8(4) . . ?
C6 C5 C4 123.1(4) . . ?
C23 C22 C21 119.7(4) . . ?
C19 C20 C21 120.5(4) . . ?
C22 C23 C24 121.3(4) . . ?
C20 C19 C18 120.2(4) . . ?
C4 C3 C2 120.2(4) . . ?
Cl4 C33 Cl3 112.3(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
C14 Si1 N4 C11 -14.7(4) . . . . ?
C15 Si1 N4 C11 110.3(3) . . . . ?
C16 Si1 N4 C11 -132.8(3) . . . . ?
C14 Si1 N4 Fe1 164.1(2) . . . . ?
C15 Si1 N4 Fe1 -70.9(3) . . . . ?
C16 Si1 N4 Fe1 46.0(3) . . . . ?
N6 Fe1 N4 C11 -21.8(3) . . . . ?
N5 Fe1 N4 C11 70.7(3) . . . . ?
Cl1 Fe1 N4 C11 -154.2(2) . . . . ?
N6 Fe1 N4 Si1 159.27(17) . . . . ?
N5 Fe1 N4 Si1 -108.21(19) . . . . ?
Cl1 Fe1 N4 Si1 26.8(2) . . . . ?
N8 Fe2 N2 C11 -31.3(3) . . . . ?
N1 Fe2 N2 C11 -156.6(3) . . . . ?
Cl2 Fe2 N2 C11 101.7(3) . . . . ?
N8 Fe2 N2 C9 127.8(2) . . . . ?
N1 Fe2 N2 C9 2.5(2) . . . . ?
Cl2 Fe2 N2 C9 -99.1(2) . . . . ?
N8 Fe2 N1 C2 73.4(3) . . . . ?
N2 Fe2 N1 C2 -178.6(3) . . . . ?
Cl2 Fe2 N1 C2 -62.3(3) . . . . ?
N8 Fe2 N1 C10 -110.7(2) . . . . ?
N2 Fe2 N1 C10 -2.7(2) . . . . ?
Cl2 Fe2 N1 C10 113.6(2) . . . . ?
C30 Si2 N8 C27 113.7(4) . . . . ?
C31 Si2 N8 C27 -128.3(3) . . . . ?
C32 Si2 N8 C27 -11.3(4) . . . . ?
C30 Si2 N8 Fe2 -67.3(3) . . . . ?
C31 Si2 N8 Fe2 50.6(3) . . . . ?
C32 Si2 N8 Fe2 167.6(2) . . . . ?
N2 Fe2 N8 C27 -24.8(3) . . . . ?
N1 Fe2 N8 C27 67.8(3) . . . . ?
Cl2 Fe2 N8 C27 -159.8(2) . . . . ?
N2 Fe2 N8 Si2 156.07(17) . . . . ?
N1 Fe2 N8 Si2 -111.32(19) . . . . ?
Cl2 Fe2 N8 Si2 21.1(2) . . . . ?
C11 N2 C9 C8 -28.2(5) . . . . ?
Fe2 N2 C9 C8 171.1(3) . . . . ?
C11 N2 C9 C10 158.6(3) . . . . ?
Fe2 N2 C9 C10 -2.0(4) . . . . ?
N4 Fe1 N5 C18 72.4(3) . . . . ?
N6 Fe1 N5 C18 -178.3(3) . . . . ?
Cl1 Fe1 N5 C18 -64.3(3) . . . . ?
N4 Fe1 N5 C26 -112.2(2) . . . . ?
N6 Fe1 N5 C26 -3.0(2) . . . . ?
Cl1 Fe1 N5 C26 111.0(2) . . . . ?
N4 Fe1 N6 C27 -32.6(3) . . . . ?
N5 Fe1 N6 C27 -156.7(3) . . . . ?
Cl1 Fe1 N6 C27 98.2(3) . . . . ?
N4 Fe1 N6 C25 127.1(2) . . . . ?
N5 Fe1 N6 C25 2.9(2) . . . . ?
Cl1 Fe1 N6 C25 -102.1(2) . . . . ?
N2 C9 C8 C7 -177.4(4) . . . . ?
C10 C9 C8 C7 -4.2(5) . . . . ?
Si2 N8 C27 N7 -50.2(5) . . . . ?
Fe2 N8 C27 N7 130.8(3) . . . . ?
Si2 N8 C27 N6 134.4(3) . . . . ?
Fe2 N8 C27 N6 -44.7(4) . . . . ?
C25 N6 C27 N8 -40.9(5) . . . . ?
Fe1 N6 C27 N8 117.8(3) . . . . ?
C25 N6 C27 N7 143.4(3) . . . . ?
Fe1 N6 C27 N7 -57.9(4) . . . . ?
C2 N1 C10 C5 0.5(5) . . . . ?
Fe2 N1 C10 C5 -175.9(3) . . . . ?
C2 N1 C10 C9 178.8(3) . . . . ?
Fe2 N1 C10 C9 2.5(4) . . . . ?
C8 C9 C10 N1 -174.1(3) . . . . ?
N2 C9 C10 N1 -0.4(4) . . . . ?
C8 C9 C10 C5 4.3(5) . . . . ?
N2 C9 C10 C5 178.0(3) . . . . ?
Si1 N4 C11 N3 -52.9(4) . . . . ?
Fe1 N4 C11 N3 128.2(3) . . . . ?
Si1 N4 C11 N2 130.8(3) . . . . ?
Fe1 N4 C11 N2 -48.1(4) . . . . ?
C9 N2 C11 N3 145.3(3) . . . . ?
Fe2 N2 C11 N3 -56.6(4) . . . . ?
C9 N2 C11 N4 -38.2(5) . . . . ?
Fe2 N2 C11 N4 119.9(3) . . . . ?
C18 N5 C26 C21 0.6(5) . . . . ?
Fe1 N5 C26 C21 -175.2(3) . . . . ?
C18 N5 C26 C25 178.3(3) . . . . ?
Fe1 N5 C26 C25 2.5(4) . . . . ?
N4 C11 N3 C12 -16.5(5) . . . . ?
N2 C11 N3 C12 160.0(4) . . . . ?
N4 C11 N3 C13 164.9(4) . . . . ?
N2 C11 N3 C13 -18.6(5) . . . . ?
C27 N6 C25 C24 -28.1(5) . . . . ?
Fe1 N6 C25 C24 170.9(3) . . . . ?
C27 N6 C25 C26 158.5(3) . . . . ?
Fe1 N6 C25 C26 -2.6(4) . . . . ?
N5 C26 C25 C24 -173.9(3) . . . . ?
C21 C26 C25 C24 3.8(5) . . . . ?
N5 C26 C25 N6 0.0(5) . . . . ?
C21 C26 C25 N6 177.7(3) . . . . ?
N6 C25 C24 C23 -176.8(4) . . . . ?
C26 C25 C24 C23 -3.4(6) . . . . ?
C26 N5 C18 C19 1.8(5) . . . . ?
Fe1 N5 C18 C19 176.9(3) . . . . ?
C26 N5 C18 C17 -177.2(4) . . . . ?
Fe1 N5 C18 C17 -2.1(5) . . . . ?
C10 N1 C2 C3 2.1(5) . . . . ?
Fe2 N1 C2 C3 177.8(3) . . . . ?
C10 N1 C2 C1 -176.7(3) . . . . ?
Fe2 N1 C2 C1 -1.0(5) . . . . ?
N5 C26 C21 C20 -2.3(5) . . . . ?
C25 C26 C21 C20 -179.9(3) . . . . ?
N5 C26 C21 C22 176.7(3) . . . . ?
C25 C26 C21 C22 -0.9(5) . . . . ?
C5 C6 C7 C8 2.8(6) . . . . ?
C9 C8 C7 C6 0.7(7) . . . . ?
N8 C27 N7 C28 -19.6(6) . . . . ?
N6 C27 N7 C28 156.2(4) . . . . ?
N8 C27 N7 C29 160.4(5) . . . . ?
N6 C27 N7 C29 -23.8(6) . . . . ?
N1 C10 C5 C6 177.3(3) . . . . ?
C9 C10 C5 C6 -1.0(5) . . . . ?
N1 C10 C5 C4 -2.7(5) . . . . ?
C9 C10 C5 C4 179.0(3) . . . . ?
C7 C6 C5 C10 -2.5(6) . . . . ?
C7 C6 C5 C4 177.4(4) . . . . ?
C3 C4 C5 C10 2.4(6) . . . . ?
C3 C4 C5 C6 -177.6(4) . . . . ?
C20 C21 C22 C23 176.4(4) . . . . ?
C26 C21 C22 C23 -2.5(6) . . . . ?
C26 C21 C20 C19 1.4(6) . . . . ?
C22 C21 C20 C19 -177.5(4) . . . . ?
C21 C22 C23 C24 2.9(7) . . . . ?
C25 C24 C23 C22 0.1(7) . . . . ?
C21 C20 C19 C18 1.0(6) . . . . ?
N5 C18 C19 C20 -2.7(6) . . . . ?
C17 C18 C19 C20 176.3(4) . . . . ?
C5 C4 C3 C2 0.0(6) . . . . ?
N1 C2 C3 C4 -2.4(6) . . . . ?
C1 C2 C3 C4 176.4(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        25.05
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.109

####################################################################### 
# 
# 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_2b
_database_code_depnum_ccdc_archive 'CCDC 1022959'
_audit_update_record             
;
2015-01-16 deposited with the CCDC.
2015-01-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H46 Li2 N8 Si2'
_chemical_formula_sum            'C32 H46 Li2 N8 Si2'
_chemical_formula_weight         612.83

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'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbcn

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'
'x-1/2, y-1/2, -z-1/2'

_cell_length_a                   15.4886(7)
_cell_length_b                   19.2519(9)
_cell_length_c                   12.1325(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3617.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1312
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.9473
_exptl_absorpt_correction_T_max  0.9795
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25319
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         28.33
_reflns_number_total             4508
_reflns_number_gt                3539
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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 > 2sigma(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)+(0.0588P)²+0.9704P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4508
_refine_ls_number_parameters     205
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.1138
_refine_ls_wR_factor_gt          0.1021
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.98429(14) 0.29673(11) 0.14775(18) 0.0316(4) Uani 1 1 d . . .
N1 N 0.91858(7) 0.37629(6) 0.08204(8) 0.0303(2) Uani 1 1 d . . .
N2 N 0.89397(6) 0.29899(5) 0.26533(8) 0.0275(2) Uani 1 1 d . . .
N3 N 0.93513(7) 0.22379(5) 0.40187(9) 0.0312(2) Uani 1 1 d . . .
N4 N 0.79183(7) 0.21834(6) 0.33638(10) 0.0383(3) Uani 1 1 d . . .
Si1 Si 0.96958(2) 0.148115(19) 0.45975(3) 0.03199(11) Uani 1 1 d . . .
C1 C 0.99950(12) 0.38420(10) -0.08686(13) 0.0532(4) Uani 1 1 d . . .
H1A H 1.0432 0.3584 -0.0451 0.080 Uiso 1 1 calc R . .
H1B H 1.0271 0.4228 -0.1260 0.080 Uiso 1 1 calc R . .
H1C H 0.9718 0.3531 -0.1402 0.080 Uiso 1 1 calc R . .
C2 C 0.93268(9) 0.41225(8) -0.00906(11) 0.0389(3) Uani 1 1 d . . .
C3 C 0.88474(11) 0.47300(8) -0.03382(12) 0.0474(4) Uani 1 1 d . . .
H3 H 0.8965 0.4984 -0.0992 0.057 Uiso 1 1 calc R . .
C4 C 0.82217(11) 0.49469(8) 0.03593(13) 0.0462(4) Uani 1 1 d . . .
H4 H 0.7904 0.5356 0.0195 0.055 Uiso 1 1 calc R . .
C5 C 0.80377(9) 0.45698(7) 0.13287(12) 0.0370(3) Uani 1 1 d . . .
C6 C 0.73744(10) 0.47525(8) 0.20695(13) 0.0446(4) Uani 1 1 d . . .
H6 H 0.7035 0.5156 0.1943 0.054 Uiso 1 1 calc R . .
C7 C 0.72239(9) 0.43476(8) 0.29655(13) 0.0418(3) Uani 1 1 d . . .
H7 H 0.6770 0.4468 0.3457 0.050 Uiso 1 1 calc R . .
C8 C 0.77243(8) 0.37545(7) 0.31825(11) 0.0349(3) Uani 1 1 d . . .
H8 H 0.7605 0.3488 0.3824 0.042 Uiso 1 1 calc R . .
C9 C 0.83884(7) 0.35451(6) 0.24876(10) 0.0276(2) Uani 1 1 d . . .
C10 C 0.85456(8) 0.39675(6) 0.15297(10) 0.0284(2) Uani 1 1 d . . .
C11 C 0.87392(8) 0.24629(6) 0.33748(10) 0.0277(2) Uani 1 1 d . . .
C12 C 0.73354(9) 0.22421(8) 0.24368(14) 0.0480(4) Uani 1 1 d . . .
H12A H 0.6866 0.2563 0.2623 0.072 Uiso 1 1 calc R . .
H12B H 0.7095 0.1784 0.2264 0.072 Uiso 1 1 calc R . .
H12C H 0.7651 0.2420 0.1796 0.072 Uiso 1 1 calc R . .
C13 C 0.75615(11) 0.18412(10) 0.43207(16) 0.0569(5) Uani 1 1 d . . .
H13A H 0.7954 0.1900 0.4947 0.085 Uiso 1 1 calc R . .
H13B H 0.7489 0.1345 0.4165 0.085 Uiso 1 1 calc R . .
H13C H 0.7000 0.2046 0.4499 0.085 Uiso 1 1 calc R . .
C14 C 0.92232(12) 0.06800(8) 0.39867(16) 0.0563(4) Uani 1 1 d . . .
H14A H 0.8630 0.0622 0.4251 0.084 Uiso 1 1 calc R . .
H14B H 0.9569 0.0277 0.4206 0.084 Uiso 1 1 calc R . .
H14C H 0.9222 0.0720 0.3181 0.084 Uiso 1 1 calc R . .
C15 C 0.95220(15) 0.14768(11) 0.61154(14) 0.0650(5) Uani 1 1 d . . .
H15A H 0.9745 0.1909 0.6432 0.097 Uiso 1 1 calc R . .
H15B H 0.9826 0.1081 0.6442 0.097 Uiso 1 1 calc R . .
H15C H 0.8903 0.1438 0.6272 0.097 Uiso 1 1 calc R . .
C16 C 1.08885(10) 0.14435(9) 0.43700(15) 0.0501(4) Uani 1 1 d . . .
H16A H 1.1010 0.1455 0.3577 0.075 Uiso 1 1 calc R . .
H16B H 1.1118 0.1013 0.4686 0.075 Uiso 1 1 calc R . .
H16C H 1.1163 0.1843 0.4727 0.075 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
Li1 N3 1.973(2) 3_755 ?
Li1 N2 1.998(2) . ?
Li1 N1 2.004(2) . ?
Li1 N2 2.161(2) 3_755 ?
Li1 C11 2.408(2) 3_755 ?
Li1 Li1 2.528(4) 3_755 ?
N1 C2 1.3224(17) . ?
N1 C10 1.3709(16) . ?
N2 C11 1.3756(15) . ?
N2 C9 1.3828(15) . ?
N2 Li1 2.161(2) 3_755 ?
N3 C11 1.3026(16) . ?
N3 Si1 1.7030(11) . ?
N3 Li1 1.973(2) 3_755 ?
N4 C11 1.3808(16) . ?
N4 C13 1.4447(19) . ?
N4 C12 1.4466(19) . ?
Si1 C14 1.8611(16) . ?
Si1 C15 1.8612(17) . ?
Si1 C16 1.8692(17) . ?
C1 C2 1.501(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.417(2) . ?
C3 C4 1.353(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.411(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.410(2) . ?
C5 C10 1.4223(17) . ?
C6 C7 1.358(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.4050(19) . ?
C7 H7 0.9500 . ?
C8 C9 1.3896(17) . ?
C8 H8 0.9500 . ?
C9 C10 1.4392(17) . ?
C11 Li1 2.408(2) 3_755 ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Li1 N2 132.54(12) 3_755 . ?
N3 Li1 N1 138.05(12) 3_755 . ?
N2 Li1 N1 84.94(9) . . ?
N3 Li1 N2 67.13(8) 3_755 3_755 ?
N2 Li1 N2 105.19(10) . 3_755 ?
N1 Li1 N2 128.45(11) . 3_755 ?
N3 Li1 C11 32.72(5) 3_755 3_755 ?
N2 Li1 C11 126.45(11) . 3_755 ?
N1 Li1 C11 143.22(12) . 3_755 ?
N2 Li1 C11 34.51(5) 3_755 3_755 ?
N3 Li1 Li1 100.24(10) 3_755 3_755 ?
N2 Li1 Li1 55.54(8) . 3_755 ?
N1 Li1 Li1 119.21(9) . 3_755 ?
N2 Li1 Li1 49.70(8) 3_755 3_755 ?
C11 Li1 Li1 75.61(9) 3_755 3_755 ?
C2 N1 C10 119.58(12) . . ?
C2 N1 Li1 130.45(12) . . ?
C10 N1 Li1 109.71(10) . . ?
C11 N2 C9 121.55(10) . . ?
C11 N2 Li1 126.60(10) . . ?
C9 N2 Li1 110.20(10) . . ?
C11 N2 Li1 82.62(9) . 3_755 ?
C9 N2 Li1 128.72(10) . 3_755 ?
Li1 N2 Li1 74.76(10) . 3_755 ?
C11 N3 Si1 139.45(9) . . ?
C11 N3 Li1 92.33(10) . 3_755 ?
Si1 N3 Li1 122.45(9) . 3_755 ?
C11 N4 C13 121.47(13) . . ?
C11 N4 C12 123.49(12) . . ?
C13 N4 C12 114.95(12) . . ?
N3 Si1 C14 114.93(7) . . ?
N3 Si1 C15 111.50(8) . . ?
C14 Si1 C15 109.47(9) . . ?
N3 Si1 C16 106.37(6) . . ?
C14 Si1 C16 107.32(9) . . ?
C15 Si1 C16 106.79(9) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 121.51(14) . . ?
N1 C2 C1 116.80(14) . . ?
C3 C2 C1 121.65(14) . . ?
C4 C3 C2 119.83(14) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 120.49(14) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 C4 123.39(13) . . ?
C6 C5 C10 119.81(13) . . ?
C4 C5 C10 116.78(13) . . ?
C7 C6 C5 119.50(13) . . ?
C7 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
C6 C7 C8 121.45(13) . . ?
C6 C7 H7 119.3 . . ?
C8 C7 H7 119.3 . . ?
C9 C8 C7 122.03(13) . . ?
C9 C8 H8 119.0 . . ?
C7 C8 H8 119.0 . . ?
N2 C9 C8 126.38(12) . . ?
N2 C9 C10 116.72(11) . . ?
C8 C9 C10 116.82(11) . . ?
N1 C10 C5 121.79(12) . . ?
N1 C10 C9 117.84(11) . . ?
C5 C10 C9 120.37(12) . . ?
N3 C11 N2 117.56(10) . . ?
N3 C11 N4 123.12(11) . . ?
N2 C11 N4 119.29(11) . . ?
N3 C11 Li1 54.95(8) . 3_755 ?
N2 C11 Li1 62.87(8) . 3_755 ?
N4 C11 Li1 176.18(11) . 3_755 ?
N4 C12 H12A 109.5 . . ?
N4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 H13A 109.5 . . ?
N4 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N4 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si1 C14 H14A 109.5 . . ?
Si1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si1 C15 H15A 109.5 . . ?
Si1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si1 C16 H16A 109.5 . . ?
Si1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.33
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.040
####################################################################### 
# 
# 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_s228b
_database_code_depnum_ccdc_archive 'CCDC 1022960'
_audit_update_record             
;
2015-01-16 deposited with the CCDC.
2015-01-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H22 Cl2 N4 Ti'
_chemical_formula_sum            'C19 H22 Cl2 N4 Ti'
_chemical_formula_weight         425.21

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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                   12.856(2)
_cell_length_b                   7.1985(11)
_cell_length_c                   21.868(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.232(2)
_cell_angle_gamma                90.00
_cell_volume                     1977.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    3751
_cell_measurement_theta_min      2.97
_cell_measurement_theta_max      27.33

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             880
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.843
_exptl_absorpt_correction_T_max  0.867
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7528
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3395
_reflns_number_gt                3134
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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 > 2sigma(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)+(0.0903P)²+8.9253P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3395
_refine_ls_number_parameters     235
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0999
_refine_ls_wR_factor_ref         0.2416
_refine_ls_wR_factor_gt          0.2328
_refine_ls_goodness_of_fit_ref   1.275
_refine_ls_restrained_S_all      1.274
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 1.03996(8) 1.00311(16) 0.19822(5) 0.0238(4) Uani 1 1 d . . .
Cl1 Cl 1.10916(14) 0.9045(3) 0.29903(8) 0.0414(5) Uani 1 1 d . . .
Cl2 Cl 1.04659(15) 1.3188(2) 0.21371(9) 0.0422(5) Uani 1 1 d . . .
N1 N 0.7449(5) 0.9193(8) 0.1100(3) 0.0350(14) Uani 1 1 d . . .
H1 H 0.7091 0.8389 0.0889 0.042 Uiso 1 1 d R . .
N2 N 0.7767(4) 0.7206(8) 0.1933(3) 0.0316(13) Uani 1 1 d . . .
N3 N 0.9006(4) 0.9500(7) 0.1868(2) 0.0259(12) Uani 1 1 d . . .
C1 C 0.7519(5) 1.0705(10) 0.0708(3) 0.0311(15) Uani 1 1 d . . .
C2 C 0.8070(5) 1.2307(10) 0.0861(3) 0.0363(16) Uani 1 1 d . . .
H2A H 0.8487 1.2468 0.1266 0.044 Uiso 1 1 calc R . .
C3 C 0.8014(6) 1.3721(11) 0.0414(4) 0.049(2) Uani 1 1 d . . .
H3A H 0.8400 1.4823 0.0524 0.059 Uiso 1 1 calc R . .
C4 C 0.7405(6) 1.3534(11) -0.0183(4) 0.0428(18) Uani 1 1 d . . .
H4A H 0.7396 1.4487 -0.0478 0.051 Uiso 1 1 calc R . .
C5 C 0.6802(5) 1.1926(10) -0.0348(3) 0.0336(15) Uani 1 1 d . . .
C6 C 0.6124(6) 1.1631(11) -0.0947(3) 0.0380(17) Uani 1 1 d . . .
H6A H 0.6071 1.2532 -0.1263 0.046 Uiso 1 1 calc R . .
C7 C 0.5561(6) 1.0041(11) -0.1053(3) 0.0398(17) Uani 1 1 d . . .
H7A H 0.5116 0.9833 -0.1447 0.048 Uiso 1 1 calc R . .
C8 C 0.5631(5) 0.8671(10) -0.0576(3) 0.0311(15) Uani 1 1 d . . .
N4 N 0.6278(4) 0.8891(8) -0.0020(2) 0.0295(12) Uani 1 1 d . . .
C9 C 0.6841(5) 1.0491(9) 0.0094(3) 0.0258(13) Uani 1 1 d . . .
C10 C 0.8110(5) 0.8657(9) 0.1635(3) 0.0249(13) Uani 1 1 d . . .
C11 C 0.6744(6) 0.6314(11) 0.1710(4) 0.045(2) Uani 1 1 d D . .
H11A H 0.6226 0.7202 0.1594 0.068 Uiso 1 1 d RD . .
H11B H 0.6549 0.5681 0.2035 0.068 Uiso 1 1 d RD . .
H11C H 0.6774 0.5570 0.1369 0.068 Uiso 1 1 d RD . .
C12 C 0.8427(6) 0.6441(10) 0.2501(3) 0.0402(17) Uani 1 1 d . . .
H12A H 0.9088 0.7134 0.2608 0.060 Uiso 1 1 calc R . .
H12B H 0.8581 0.5148 0.2433 0.060 Uiso 1 1 calc R . .
H12C H 0.8051 0.6532 0.2841 0.060 Uiso 1 1 calc R . .
C13 C 1.1206(6) 1.0553(10) 0.1100(3) 0.0404(18) Uani 1 1 d . . .
C14 C 1.0386(6) 0.9211(11) 0.0937(3) 0.0399(17) Uani 1 1 d . . .
H14A H 0.9765 0.9310 0.0582 0.048 Uiso 1 1 calc R . .
C15 C 1.0660(7) 0.7641(11) 0.1313(4) 0.0459(19) Uani 1 1 d . . .
H15A H 1.0280 0.6436 0.1263 0.055 Uiso 1 1 calc R . .
C16 C 1.1651(7) 0.7977(12) 0.1706(4) 0.051(2) Uani 1 1 d . . .
H16A H 1.2077 0.7054 0.1988 0.061 Uiso 1 1 calc R . .
C17 C 1.1989(6) 0.9763(12) 0.1589(4) 0.046(2) Uani 1 1 d . . .
H17A H 1.2687 1.0321 0.1779 0.055 Uiso 1 1 calc R . .
C18 C 1.1287(10) 1.2388(13) 0.0789(5) 0.072(3) Uani 1 1 d . . .
H18A H 1.1648 1.2224 0.0446 0.108 Uiso 1 1 calc R . .
H18B H 1.1685 1.3251 0.1091 0.108 Uiso 1 1 calc R . .
H18C H 1.0578 1.2877 0.0630 0.108 Uiso 1 1 calc R . .
C19 C 0.5007(6) 0.6912(11) -0.0681(4) 0.0428(18) Uani 1 1 d . . .
H19A H 0.5161 0.6166 -0.0303 0.064 Uiso 1 1 calc R . .
H19B H 0.5201 0.6226 -0.1022 0.064 Uiso 1 1 calc R . .
H19C H 0.4253 0.7199 -0.0786 0.064 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 N3 1.797(5) . ?
Ti1 Cl2 2.297(2) . ?
Ti1 Cl1 2.307(2) . ?
Ti1 C15 2.328(7) . ?
Ti1 C16 2.356(8) . ?
Ti1 C14 2.358(7) . ?
Ti1 C17 2.386(7) . ?
Ti1 C13 2.406(7) . ?
N1 C10 1.348(8) . ?
N1 C1 1.400(9) . ?
N1 H1 0.8182 . ?
N2 C10 1.354(8) . ?
N2 C11 1.452(9) . ?
N2 C12 1.456(9) . ?
N3 C10 1.306(8) . ?
C1 C2 1.358(10) . ?
C1 C9 1.445(9) . ?
C2 C3 1.403(11) . ?
C2 H2A 0.9400 . ?
C3 C4 1.378(11) . ?
C3 H3A 0.9400 . ?
C4 C5 1.397(11) . ?
C4 H4A 0.9400 . ?
C5 C9 1.409(9) . ?
C5 C6 1.426(10) . ?
C6 C7 1.348(11) . ?
C6 H6A 0.9400 . ?
C7 C8 1.425(10) . ?
C7 H7A 0.9400 . ?
C8 N4 1.329(8) . ?
C8 C19 1.491(10) . ?
N4 C9 1.355(8) . ?
C11 H11A 0.9191 . ?
C11 H11B 0.9221 . ?
C11 H11C 0.9263 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C13 C14 1.419(11) . ?
C13 C17 1.423(12) . ?
C13 C18 1.499(12) . ?
C14 C15 1.399(11) . ?
C14 H14A 0.9900 . ?
C15 C16 1.397(13) . ?
C15 H15A 0.9900 . ?
C16 C17 1.398(13) . ?
C16 H16A 0.9900 . ?
C17 H17A 0.9900 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 H19C 0.9700 . ?

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
N3 Ti1 Cl2 103.65(18) . . ?
N3 Ti1 Cl1 103.79(17) . . ?
Cl2 Ti1 Cl1 99.71(8) . . ?
N3 Ti1 C15 91.6(3) . . ?
Cl2 Ti1 C15 144.9(2) . . ?
Cl1 Ti1 C15 107.2(2) . . ?
N3 Ti1 C16 123.0(3) . . ?
Cl2 Ti1 C16 130.8(2) . . ?
Cl1 Ti1 C16 84.6(2) . . ?
C15 Ti1 C16 34.7(3) . . ?
N3 Ti1 C14 90.5(3) . . ?
Cl2 Ti1 C14 112.5(2) . . ?
Cl1 Ti1 C14 140.5(2) . . ?
C15 Ti1 C14 34.7(3) . . ?
C16 Ti1 C14 57.3(3) . . ?
N3 Ti1 C17 146.9(3) . . ?
Cl2 Ti1 C17 97.2(2) . . ?
Cl1 Ti1 C17 97.6(2) . . ?
C15 Ti1 C17 57.7(3) . . ?
C16 Ti1 C17 34.3(3) . . ?
C14 Ti1 C17 57.4(3) . . ?
N3 Ti1 C13 120.6(3) . . ?
Cl2 Ti1 C13 87.41(19) . . ?
Cl1 Ti1 C13 132.1(2) . . ?
C15 Ti1 C13 57.8(3) . . ?
C16 Ti1 C13 57.2(3) . . ?
C14 Ti1 C13 34.6(3) . . ?
C17 Ti1 C13 34.6(3) . . ?
C10 N1 C1 130.0(6) . . ?
C10 N1 H1 117.6 . . ?
C1 N1 H1 107.8 . . ?
C10 N2 C11 122.9(5) . . ?
C10 N2 C12 120.9(5) . . ?
C11 N2 C12 116.2(5) . . ?
C10 N3 Ti1 157.5(5) . . ?
C2 C1 N1 127.4(6) . . ?
C2 C1 C9 120.0(6) . . ?
N1 C1 C9 112.4(6) . . ?
C1 C2 C3 119.8(6) . . ?
C1 C2 H2A 120.1 . . ?
C3 C2 H2A 120.1 . . ?
C4 C3 C2 121.6(7) . . ?
C4 C3 H3A 119.2 . . ?
C2 C3 H3A 119.2 . . ?
C3 C4 C5 119.9(7) . . ?
C3 C4 H4A 120.1 . . ?
C5 C4 H4A 120.1 . . ?
C4 C5 C9 119.5(6) . . ?
C4 C5 C6 124.0(7) . . ?
C9 C5 C6 116.5(6) . . ?
C7 C6 C5 119.1(7) . . ?
C7 C6 H6A 120.4 . . ?
C5 C6 H6A 120.4 . . ?
C6 C7 C8 120.8(6) . . ?
C6 C7 H7A 119.6 . . ?
C8 C7 H7A 119.6 . . ?
N4 C8 C7 121.2(6) . . ?
N4 C8 C19 117.0(6) . . ?
C7 C8 C19 121.8(6) . . ?
C8 N4 C9 118.4(6) . . ?
N4 C9 C5 123.8(6) . . ?
N4 C9 C1 117.1(6) . . ?
C5 C9 C1 119.1(6) . . ?
N3 C10 N1 123.2(6) . . ?
N3 C10 N2 121.3(5) . . ?
N1 C10 N2 115.4(5) . . ?
N2 C11 H11A 109.6 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 104.9 . . ?
N2 C11 H11C 109.7 . . ?
H11A C11 H11C 109.4 . . ?
H11B C11 H11C 113.5 . . ?
N2 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C17 106.6(7) . . ?
C14 C13 C18 127.3(8) . . ?
C17 C13 C18 126.0(8) . . ?
C14 C13 Ti1 70.8(4) . . ?
C17 C13 Ti1 72.0(4) . . ?
C18 C13 Ti1 125.7(5) . . ?
C15 C14 C13 108.7(7) . . ?
C15 C14 Ti1 71.5(4) . . ?
C13 C14 Ti1 74.6(4) . . ?
C15 C14 H14A 125.5 . . ?
C13 C14 H14A 125.5 . . ?
Ti1 C14 H14A 125.5 . . ?
C16 C15 C14 107.7(7) . . ?
C16 C15 Ti1 73.8(4) . . ?
C14 C15 Ti1 73.8(4) . . ?
C16 C15 H15A 125.8 . . ?
C14 C15 H15A 125.8 . . ?
Ti1 C15 H15A 125.8 . . ?
C15 C16 C17 109.0(7) . . ?
C15 C16 Ti1 71.5(4) . . ?
C17 C16 Ti1 74.0(4) . . ?
C15 C16 H16A 125.4 . . ?
C17 C16 H16A 125.4 . . ?
Ti1 C16 H16A 125.4 . . ?
C16 C17 C13 107.9(7) . . ?
C16 C17 Ti1 71.7(4) . . ?
C13 C17 Ti1 73.5(4) . . ?
C16 C17 H17A 125.9 . . ?
C13 C17 H17A 125.9 . . ?
Ti1 C17 H17A 125.9 . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C8 C19 H19A 109.5 . . ?
C8 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C8 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl2 Ti1 N3 C10 144.1(12) . . . . ?
Cl1 Ti1 N3 C10 -112.1(12) . . . . ?
C15 Ti1 N3 C10 -4.0(12) . . . . ?
C16 Ti1 N3 C10 -19.6(13) . . . . ?
C14 Ti1 N3 C10 30.7(12) . . . . ?
C17 Ti1 N3 C10 16.7(15) . . . . ?
C13 Ti1 N3 C10 49.0(13) . . . . ?
C10 N1 C1 C2 -22.6(12) . . . . ?
C10 N1 C1 C9 162.5(7) . . . . ?
N1 C1 C2 C3 -177.2(7) . . . . ?
C9 C1 C2 C3 -2.7(11) . . . . ?
C1 C2 C3 C4 0.3(12) . . . . ?
C2 C3 C4 C5 1.8(12) . . . . ?
C3 C4 C5 C9 -1.4(11) . . . . ?
C3 C4 C5 C6 178.0(7) . . . . ?
C4 C5 C6 C7 -178.7(7) . . . . ?
C9 C5 C6 C7 0.7(10) . . . . ?
C5 C6 C7 C8 0.4(11) . . . . ?
C6 C7 C8 N4 -2.2(10) . . . . ?
C6 C7 C8 C19 179.4(7) . . . . ?
C7 C8 N4 C9 2.8(9) . . . . ?
C19 C8 N4 C9 -178.8(6) . . . . ?
C8 N4 C9 C5 -1.6(9) . . . . ?
C8 N4 C9 C1 178.6(6) . . . . ?
C4 C5 C9 N4 179.3(6) . . . . ?
C6 C5 C9 N4 -0.1(9) . . . . ?
C4 C5 C9 C1 -0.9(10) . . . . ?
C6 C5 C9 C1 179.6(6) . . . . ?
C2 C1 C9 N4 -177.2(6) . . . . ?
N1 C1 C9 N4 -1.9(8) . . . . ?
C2 C1 C9 C5 3.0(10) . . . . ?
N1 C1 C9 C5 178.3(6) . . . . ?
Ti1 N3 C10 N1 -86.4(13) . . . . ?
Ti1 N3 C10 N2 95.9(13) . . . . ?
C1 N1 C10 N3 -3.3(11) . . . . ?
C1 N1 C10 N2 174.5(7) . . . . ?
C11 N2 C10 N3 175.8(7) . . . . ?
C12 N2 C10 N3 -4.9(10) . . . . ?
C11 N2 C10 N1 -2.0(9) . . . . ?
C12 N2 C10 N1 177.3(6) . . . . ?
N3 Ti1 C13 C14 -33.4(6) . . . . ?
Cl2 Ti1 C13 C14 -137.8(5) . . . . ?
Cl1 Ti1 C13 C14 121.5(4) . . . . ?
C15 Ti1 C13 C14 37.1(5) . . . . ?
C16 Ti1 C13 C14 78.5(5) . . . . ?
C17 Ti1 C13 C14 115.6(7) . . . . ?
N3 Ti1 C13 C17 -149.0(5) . . . . ?
Cl2 Ti1 C13 C17 106.6(4) . . . . ?
Cl1 Ti1 C13 C17 5.9(6) . . . . ?
C15 Ti1 C13 C17 -78.5(5) . . . . ?
C16 Ti1 C13 C17 -37.1(5) . . . . ?
C14 Ti1 C13 C17 -115.6(7) . . . . ?
N3 Ti1 C13 C18 89.2(8) . . . . ?
Cl2 Ti1 C13 C18 -15.1(8) . . . . ?
Cl1 Ti1 C13 C18 -115.9(8) . . . . ?
C15 Ti1 C13 C18 159.7(9) . . . . ?
C16 Ti1 C13 C18 -158.9(9) . . . . ?
C14 Ti1 C13 C18 122.6(10) . . . . ?
C17 Ti1 C13 C18 -121.8(10) . . . . ?
C17 C13 C14 C15 -0.3(8) . . . . ?
C18 C13 C14 C15 175.4(7) . . . . ?
Ti1 C13 C14 C15 -63.8(5) . . . . ?
C17 C13 C14 Ti1 63.5(5) . . . . ?
C18 C13 C14 Ti1 -120.8(8) . . . . ?
N3 Ti1 C14 C15 -91.9(5) . . . . ?
Cl2 Ti1 C14 C15 163.0(4) . . . . ?
Cl1 Ti1 C14 C15 20.8(6) . . . . ?
C16 Ti1 C14 C15 38.0(5) . . . . ?
C17 Ti1 C14 C15 79.0(5) . . . . ?
C13 Ti1 C14 C15 116.4(7) . . . . ?
N3 Ti1 C14 C13 151.7(5) . . . . ?
Cl2 Ti1 C14 C13 46.7(5) . . . . ?
Cl1 Ti1 C14 C13 -95.6(5) . . . . ?
C15 Ti1 C14 C13 -116.4(7) . . . . ?
C16 Ti1 C14 C13 -78.3(5) . . . . ?
C17 Ti1 C14 C13 -37.4(5) . . . . ?
C13 C14 C15 C16 -0.7(8) . . . . ?
Ti1 C14 C15 C16 -66.5(5) . . . . ?
C13 C14 C15 Ti1 65.8(5) . . . . ?
N3 Ti1 C15 C16 -156.8(5) . . . . ?
Cl2 Ti1 C15 C16 86.5(6) . . . . ?
Cl1 Ti1 C15 C16 -51.8(5) . . . . ?
C14 Ti1 C15 C16 114.5(7) . . . . ?
C17 Ti1 C15 C16 36.4(5) . . . . ?
C13 Ti1 C15 C16 77.5(5) . . . . ?
N3 Ti1 C15 C14 88.7(5) . . . . ?
Cl2 Ti1 C15 C14 -28.0(7) . . . . ?
Cl1 Ti1 C15 C14 -166.3(4) . . . . ?
C16 Ti1 C15 C14 -114.5(7) . . . . ?
C17 Ti1 C15 C14 -78.1(5) . . . . ?
C13 Ti1 C15 C14 -37.0(5) . . . . ?
C14 C15 C16 C17 1.5(8) . . . . ?
Ti1 C15 C16 C17 -65.1(5) . . . . ?
C14 C15 C16 Ti1 66.5(5) . . . . ?
N3 Ti1 C16 C15 28.1(6) . . . . ?
Cl2 Ti1 C16 C15 -130.8(5) . . . . ?
Cl1 Ti1 C16 C15 131.1(5) . . . . ?
C14 Ti1 C16 C15 -38.0(5) . . . . ?
C17 Ti1 C16 C15 -116.9(7) . . . . ?
C13 Ti1 C16 C15 -79.5(5) . . . . ?
N3 Ti1 C16 C17 145.0(5) . . . . ?
Cl2 Ti1 C16 C17 -13.8(6) . . . . ?
Cl1 Ti1 C16 C17 -112.0(5) . . . . ?
C15 Ti1 C16 C17 116.9(7) . . . . ?
C14 Ti1 C16 C17 78.9(5) . . . . ?
C13 Ti1 C16 C17 37.4(5) . . . . ?
C15 C16 C17 C13 -1.6(8) . . . . ?
Ti1 C16 C17 C13 -65.1(5) . . . . ?
C15 C16 C17 Ti1 63.5(5) . . . . ?
C14 C13 C17 C16 1.2(8) . . . . ?
C18 C13 C17 C16 -174.6(7) . . . . ?
Ti1 C13 C17 C16 63.9(5) . . . . ?
C14 C13 C17 Ti1 -62.7(5) . . . . ?
C18 C13 C17 Ti1 121.5(8) . . . . ?
N3 Ti1 C17 C16 -61.6(7) . . . . ?
Cl2 Ti1 C17 C16 169.5(5) . . . . ?
Cl1 Ti1 C17 C16 68.6(5) . . . . ?
C15 Ti1 C17 C16 -36.9(5) . . . . ?
C14 Ti1 C17 C16 -78.3(5) . . . . ?
C13 Ti1 C17 C16 -115.8(7) . . . . ?
N3 Ti1 C17 C13 54.2(7) . . . . ?
Cl2 Ti1 C17 C13 -74.7(4) . . . . ?
Cl1 Ti1 C17 C13 -175.6(4) . . . . ?
C15 Ti1 C17 C13 78.9(5) . . . . ?
C16 Ti1 C17 C13 115.8(7) . . . . ?
C14 Ti1 C17 C13 37.5(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.132

####################################################################### 
# 
# 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_sa354
_database_code_depnum_ccdc_archive 'CCDC 1022961'
_audit_update_record             
;
2015-01-16 deposited with the CCDC.
2015-01-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H38 Cl2 N8 Ti2 '
_chemical_formula_sum            'C36 H38 Cl2 N8 Ti2'
_chemical_formula_weight         749.38

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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                   9.3921(19)
_cell_length_b                   18.774(4)
_cell_length_c                   12.411(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.67(3)
_cell_angle_gamma                90.00
_cell_volume                     2033.8(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5977
_cell_measurement_theta_min      2.0723
_cell_measurement_theta_max      27.5319

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             776.0
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7656
_exptl_absorpt_correction_T_max  0.9305
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            4648
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         27.47
_reflns_number_total             4648
_reflns_number_gt                3905
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Siemens SMART'
_computing_cell_refinement       'Siemens SMART & SAINT'
_computing_data_reduction        'Siemens XPREP'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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 > 2sigma(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)+(0.0813P)²+1.6743P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4648
_refine_ls_number_parameters     220
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0605
_refine_ls_wR_factor_ref         0.1704
_refine_ls_wR_factor_gt          0.1657
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_restrained_S_all      1.130
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.001

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 0.84352(5) 0.01203(3) 0.90885(4) 0.02780(17) Uani 1 1 d . . .
Cl1 Cl 0.79931(9) 0.09243(4) 0.74987(6) 0.0387(2) Uani 1 1 d . . .
N1 N 0.8746(3) -0.06654(14) 0.7925(2) 0.0334(5) Uani 1 1 d . . .
N2 N 1.0000(3) -0.17514(14) 0.8819(2) 0.0379(6) Uani 1 1 d . . .
N3 N 1.0945(3) -0.08352(14) 0.6936(2) 0.0370(6) Uani 1 1 d . . .
N4 N 0.9941(3) 0.06851(13) 1.0179(2) 0.0299(5) Uani 1 1 d . . .
C1 C 0.7064(4) -0.0498(3) 1.0089(3) 0.0500(10) Uani 1 1 d . . .
C2 C 0.7106(5) 0.0219(3) 1.0362(4) 0.0704(15) Uani 1 1 d . . .
H2A H 0.7532 0.0416 1.1148 0.085 Uiso 1 1 calc R . .
C3 C 0.6294(4) 0.0602(2) 0.9375(4) 0.0640(12) Uani 1 1 d . . .
H3A H 0.6031 0.1108 0.9347 0.077 Uiso 1 1 calc R . .
C4 C 0.5735(4) 0.0117(2) 0.8453(3) 0.0438(8) Uani 1 1 d . . .
H4A H 0.5025 0.0230 0.7668 0.053 Uiso 1 1 calc R . .
C5 C 0.6197(3) -0.05545(19) 0.8881(3) 0.0382(7) Uani 1 1 d . . .
H5A H 0.5887 -0.1000 0.8445 0.046 Uiso 1 1 calc R . .
C6 C 0.7707(5) -0.1123(4) 1.0885(5) 0.114(3) Uani 1 1 d . . .
H6A H 0.7181 -0.1168 1.1413 0.171 Uiso 1 1 calc R . .
H6B H 0.8779 -0.1048 1.1314 0.171 Uiso 1 1 calc R . .
H6C H 0.7571 -0.1551 1.0433 0.171 Uiso 1 1 calc R . .
C7 C 0.9637(3) -0.10593(16) 0.8813(2) 0.0303(6) Uani 1 1 d . . .
C8 C 1.0879(5) -0.21174(19) 0.9907(3) 0.0528(9) Uani 1 1 d . . .
H8A H 1.1274 -0.1773 1.0517 0.079 Uiso 1 1 calc R . .
H8B H 1.1713 -0.2373 0.9817 0.079 Uiso 1 1 calc R . .
H8C H 1.0223 -0.2445 1.0098 0.079 Uiso 1 1 calc R . .
C9 C 0.9383(5) -0.22186(19) 0.7798(3) 0.0515(9) Uani 1 1 d . . .
H9A H 0.8501 -0.1998 0.7231 0.077 Uiso 1 1 calc R . .
H9B H 0.9093 -0.2668 0.8027 0.077 Uiso 1 1 calc R . .
H9C H 1.0151 -0.2295 0.7472 0.077 Uiso 1 1 calc R . .
C10 C 0.8296(4) -0.07661(16) 0.6732(3) 0.0348(6) Uani 1 1 d . . .
C11 C 0.6791(4) -0.07299(19) 0.6022(3) 0.0401(7) Uani 1 1 d . . .
H11A H 0.6054 -0.0661 0.6347 0.048 Uiso 1 1 calc R . .
C12 C 0.6326(4) -0.0794(2) 0.4817(3) 0.0462(8) Uani 1 1 d . . .
H12A H 0.5289 -0.0778 0.4358 0.055 Uiso 1 1 calc R . .
C13 C 0.7387(4) -0.08806(19) 0.4309(3) 0.0432(8) Uani 1 1 d . . .
H13A H 0.7069 -0.0929 0.3509 0.052 Uiso 1 1 calc R . .
C14 C 0.8964(4) -0.08957(16) 0.5006(3) 0.0361(7) Uani 1 1 d . . .
C15 C 1.0107(4) -0.09416(17) 0.4521(3) 0.0398(7) Uani 1 1 d . . .
H15A H 0.9840 -0.0980 0.3723 0.048 Uiso 1 1 calc R . .
C16 C 1.1602(4) -0.09289(18) 0.5243(3) 0.0438(8) Uani 1 1 d . . .
H16A H 1.2373 -0.0954 0.4942 0.053 Uiso 1 1 calc R . .
C17 C 1.1978(4) -0.08767(18) 0.6448(3) 0.0409(7) Uani 1 1 d . . .
H17A H 1.3008 -0.0871 0.6927 0.049 Uiso 1 1 calc R . .
C18 C 0.9433(4) -0.08368(16) 0.6217(3) 0.0344(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 N4 1.882(3) . ?
Ti1 N4 2.101(2) 3_757 ?
Ti1 N1 2.159(3) . ?
Ti1 C3 2.348(3) . ?
Ti1 C2 2.355(3) . ?
Ti1 C4 2.361(3) . ?
Ti1 C5 2.386(3) . ?
Ti1 C1 2.394(3) . ?
Ti1 Cl1 2.3956(10) . ?
Ti1 C7 2.565(3) . ?
Ti1 Ti1 3.0086(15) 3_757 ?
N1 C7 1.334(4) . ?
N1 C10 1.394(4) . ?
N2 C7 1.343(4) . ?
N2 C8 1.467(4) . ?
N2 C9 1.473(4) . ?
N3 C17 1.321(4) . ?
N3 C18 1.370(4) . ?
N4 C7 1.361(4) 3_757 ?
N4 Ti1 2.101(2) 3_757 ?
C1 C2 1.385(7) . ?
C1 C5 1.422(5) . ?
C1 C6 1.508(6) . ?
C2 C3 1.382(7) . ?
C3 C4 1.402(6) . ?
C4 C5 1.375(5) . ?
C7 N4 1.361(4) 3_757 ?
C10 C11 1.364(4) . ?
C10 C18 1.439(4) . ?
C11 C12 1.399(4) . ?
C12 C13 1.372(5) . ?
C13 C14 1.414(5) . ?
C14 C18 1.406(4) . ?
C14 C15 1.414(5) . ?
C15 C16 1.359(5) . ?
C16 C17 1.409(5) . ?

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
N4 Ti1 N4 82.04(11) . 3_757 ?
N4 Ti1 N1 127.92(10) . . ?
N4 Ti1 N1 62.74(10) 3_757 . ?
N4 Ti1 C3 97.62(13) . . ?
N4 Ti1 C3 137.44(15) 3_757 . ?
N1 Ti1 C3 134.37(13) . . ?
N4 Ti1 C2 85.26(13) . . ?
N4 Ti1 C2 104.22(17) 3_757 . ?
N1 Ti1 C2 137.63(15) . . ?
C3 Ti1 C2 34.17(17) . . ?
N4 Ti1 C4 132.11(12) . . ?
N4 Ti1 C4 131.39(11) 3_757 . ?
N1 Ti1 C4 99.74(12) . . ?
C3 Ti1 C4 34.65(14) . . ?
C2 Ti1 C4 56.92(15) . . ?
N4 Ti1 C5 140.83(11) . . ?
N4 Ti1 C5 97.73(11) 3_757 . ?
N1 Ti1 C5 84.05(11) . . ?
C3 Ti1 C5 56.70(14) . . ?
C2 Ti1 C5 56.62(13) . . ?
C4 Ti1 C5 33.67(12) . . ?
N4 Ti1 C1 107.80(12) . . ?
N4 Ti1 C1 82.52(12) 3_757 . ?
N1 Ti1 C1 104.32(13) . . ?
C3 Ti1 C1 56.87(16) . . ?
C2 Ti1 C1 33.89(17) . . ?
C4 Ti1 C1 56.98(12) . . ?
C5 Ti1 C1 34.62(11) . . ?
N4 Ti1 Cl1 95.33(8) . . ?
N4 Ti1 Cl1 133.42(7) 3_757 . ?
N1 Ti1 Cl1 84.52(7) . . ?
C3 Ti1 Cl1 89.11(13) . . ?
C2 Ti1 Cl1 121.99(16) . . ?
C4 Ti1 Cl1 83.59(10) . . ?
C5 Ti1 Cl1 111.58(9) . . ?
C1 Ti1 Cl1 140.37(9) . . ?
N4 Ti1 C7 109.35(10) . . ?
N4 Ti1 C7 31.98(9) 3_757 . ?
N1 Ti1 C7 31.33(9) . . ?
C3 Ti1 C7 142.75(13) . . ?
C2 Ti1 C7 121.70(17) . . ?
C4 Ti1 C7 115.13(11) . . ?
C5 Ti1 C7 86.60(11) . . ?
C1 Ti1 C7 89.89(13) . . ?
Cl1 Ti1 C7 112.64(7) . . ?
N4 Ti1 Ti1 43.76(8) . 3_757 ?
N4 Ti1 Ti1 38.28(7) 3_757 3_757 ?
N1 Ti1 Ti1 93.70(7) . 3_757 ?
C3 Ti1 Ti1 126.68(13) . 3_757 ?
C2 Ti1 Ti1 96.89(12) . 3_757 ?
C4 Ti1 Ti1 151.80(9) . 3_757 ?
C5 Ti1 Ti1 125.37(8) . 3_757 ?
C1 Ti1 Ti1 95.76(8) . 3_757 ?
Cl1 Ti1 Ti1 122.55(4) . 3_757 ?
C7 Ti1 Ti1 67.35(7) . 3_757 ?
C7 N1 C10 130.8(3) . . ?
C7 N1 Ti1 91.40(17) . . ?
C10 N1 Ti1 137.8(2) . . ?
C7 N2 C8 121.0(3) . . ?
C7 N2 C9 123.5(3) . . ?
C8 N2 C9 114.9(3) . . ?
C17 N3 C18 117.5(3) . . ?
C7 N4 Ti1 147.0(2) 3_757 . ?
C7 N4 Ti1 93.15(17) 3_757 3_757 ?
Ti1 N4 Ti1 97.96(11) . 3_757 ?
C2 C1 C5 106.5(4) . . ?
C2 C1 C6 128.9(5) . . ?
C5 C1 C6 124.6(5) . . ?
C2 C1 Ti1 71.5(2) . . ?
C5 C1 Ti1 72.36(17) . . ?
C6 C1 Ti1 123.7(3) . . ?
C3 C2 C1 109.4(4) . . ?
C3 C2 Ti1 72.6(2) . . ?
C1 C2 Ti1 74.6(2) . . ?
C2 C3 C4 107.7(4) . . ?
C2 C3 Ti1 73.2(2) . . ?
C4 C3 Ti1 73.2(2) . . ?
C5 C4 C3 108.1(4) . . ?
C5 C4 Ti1 74.14(18) . . ?
C3 C4 Ti1 72.17(19) . . ?
C4 C5 C1 108.4(3) . . ?
C4 C5 Ti1 72.19(18) . . ?
C1 C5 Ti1 73.01(18) . . ?
N1 C7 N2 128.5(3) . . ?
N1 C7 N4 110.8(3) . 3_757 ?
N2 C7 N4 120.5(3) . 3_757 ?
N1 C7 Ti1 57.27(15) . . ?
N2 C7 Ti1 163.3(2) . . ?
N4 C7 Ti1 54.87(14) 3_757 . ?
C11 C10 N1 121.0(3) . . ?
C11 C10 C18 118.7(3) . . ?
N1 C10 C18 120.0(3) . . ?
C10 C11 C12 121.8(3) . . ?
C13 C12 C11 120.6(3) . . ?
C12 C13 C14 119.7(3) . . ?
C18 C14 C13 119.8(3) . . ?
C18 C14 C15 118.2(3) . . ?
C13 C14 C15 122.0(3) . . ?
C16 C15 C14 118.7(3) . . ?
C15 C16 C17 119.6(3) . . ?
N3 C17 C16 123.5(3) . . ?
N3 C18 C14 122.4(3) . . ?
N3 C18 C10 118.1(3) . . ?
C14 C18 C10 119.4(3) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.399
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.134
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.505 0.250 0.078 255 133 ' '
2 0.495 0.750 0.323 255 133 ' '
_platon_squeeze_details          
;
;
