# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_s600p
_database_code_depnum_ccdc_archive 'CCDC 1424470'
_audit_update_record             
;
2015-09-15 deposited with the CCDC.
2015-12-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H29 Cl6 N5 Ti2'
_chemical_formula_weight         684.01

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                   11.095(5)
_cell_length_b                   19.886(9)
_cell_length_c                   13.656(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.13(3)
_cell_angle_gamma                90.00
_cell_volume                     2983(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    213(2)
_cell_measurement_reflns_used    3286
_cell_measurement_theta_min      2.445
_cell_measurement_theta_max      23.4335

_exptl_crystal_description       block
_exptl_crystal_colour            red
_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    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1392
_exptl_absorpt_coefficient_mu    1.095
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7347
_exptl_absorpt_correction_T_max  0.8107
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      213(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 scan'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12192
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         25.01
_reflns_number_total             5255
_reflns_number_gt                4611
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       SMART
_computing_cell_refinement       SAINT
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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)+(0.0459P)²+7.0215P] 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         5255
_refine_ls_number_parameters     329
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0736
_refine_ls_wR_factor_ref         0.1553
_refine_ls_wR_factor_gt          0.1495
_refine_ls_goodness_of_fit_ref   1.208
_refine_ls_restrained_S_all      1.208
_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 0.23830(8) 0.24312(4) 0.30260(6) 0.0234(2) Uani 1 1 d . . .
Ti2 Ti 0.26647(9) 0.50100(5) 0.26477(7) 0.0303(3) Uani 1 1 d . . .
Cl1 Cl 0.15488(12) 0.23946(7) 0.13816(10) 0.0375(3) Uani 1 1 d . . .
Cl2 Cl 0.42297(12) 0.27600(7) 0.25649(11) 0.0371(3) Uani 1 1 d . . .
Cl3 Cl 0.14929(14) 0.56980(7) 0.34975(11) 0.0454(4) Uani 1 1 d . . .
Cl4 Cl 0.44177(14) 0.56469(8) 0.26750(13) 0.0535(4) Uani 1 1 d . . .
Cl5 Cl 0.5872(3) 0.37410(16) 0.06758(18) 0.1164(10) Uani 1 1 d . . .
Cl6 Cl 0.7473(3) 0.45399(14) 0.2019(3) 0.1344(12) Uani 1 1 d . . .
N1 N 0.0845(3) 0.2928(2) 0.3368(3) 0.0261(9) Uani 1 1 d . . .
N2 N 0.0971(4) 0.3904(2) 0.4400(3) 0.0295(10) Uani 1 1 d . . .
N3 N 0.2664(3) 0.32705(19) 0.4016(3) 0.0237(9) Uani 1 1 d . . .
N4 N 0.3178(4) 0.4368(2) 0.3518(3) 0.0288(10) Uani 1 1 d . . .
N5 N 0.4571(4) 0.3725(2) 0.4533(3) 0.0323(10) Uani 1 1 d . . .
C1 C -0.0369(4) 0.2723(2) 0.3419(4) 0.0293(12) Uani 1 1 d . . .
C2 C -0.1092(5) 0.2513(3) 0.2570(5) 0.0423(14) Uani 1 1 d . . .
H2 H -0.0799 0.2530 0.1957 0.051 Uiso 1 1 calc R . .
C3 C -0.2263(6) 0.2273(4) 0.2627(6) 0.061(2) Uani 1 1 d . . .
H3 H -0.2758 0.2135 0.2046 0.073 Uiso 1 1 calc R . .
C4 C -0.2697(5) 0.2237(3) 0.3501(6) 0.059(2) Uani 1 1 d . . .
H4 H -0.3486 0.2071 0.3525 0.071 Uiso 1 1 calc R . .
C5 C -0.1992(5) 0.2441(3) 0.4351(5) 0.0538(17) Uani 1 1 d . . .
H5 H -0.2294 0.2415 0.4959 0.065 Uiso 1 1 calc R . .
C6 C -0.0826(5) 0.2686(3) 0.4312(4) 0.0393(14) Uani 1 1 d . . .
H6 H -0.0343 0.2828 0.4896 0.047 Uiso 1 1 calc R . .
C7 C 0.1450(4) 0.3397(2) 0.3944(3) 0.0238(10) Uani 1 1 d . . .
C8 C -0.0235(5) 0.4177(3) 0.4051(5) 0.0441(15) Uani 1 1 d . . .
H8A H -0.0540 0.3983 0.3412 0.066 Uiso 1 1 calc R . .
H8B H -0.0181 0.4661 0.3989 0.066 Uiso 1 1 calc R . .
H8C H -0.0784 0.4067 0.4521 0.066 Uiso 1 1 calc R . .
C9 C 0.1669(5) 0.4253(3) 0.5233(4) 0.0350(13) Uani 1 1 d . . .
H9A H 0.2374 0.3986 0.5490 0.053 Uiso 1 1 calc R . .
H9B H 0.1162 0.4320 0.5748 0.053 Uiso 1 1 calc R . .
H9C H 0.1934 0.4686 0.5015 0.053 Uiso 1 1 calc R . .
C10 C 0.3481(4) 0.3807(2) 0.4014(4) 0.0248(11) Uani 1 1 d . . .
C11 C 0.4881(5) 0.3146(3) 0.5176(4) 0.0441(15) Uani 1 1 d . . .
H11A H 0.4154 0.2982 0.5417 0.066 Uiso 1 1 calc R . .
H11B H 0.5478 0.3278 0.5731 0.066 Uiso 1 1 calc R . .
H11C H 0.5217 0.2793 0.4805 0.066 Uiso 1 1 calc R . .
C12 C 0.5556(5) 0.4189(3) 0.4445(5) 0.0447(15) Uani 1 1 d . . .
H12A H 0.5274 0.4537 0.3970 0.067 Uiso 1 1 calc R . .
H12B H 0.6228 0.3948 0.4224 0.067 Uiso 1 1 calc R . .
H12C H 0.5827 0.4393 0.5084 0.067 Uiso 1 1 calc R . .
C13 C 0.1544(5) 0.1359(3) 0.3138(5) 0.0409(14) Uani 1 1 d . . .
H13 H 0.0786 0.1191 0.2743 0.049 Uiso 1 1 calc R . .
C14 C 0.1644(5) 0.1637(3) 0.4085(4) 0.0380(13) Uani 1 1 d . . .
H14 H 0.0965 0.1709 0.4472 0.046 Uiso 1 1 calc R . .
C15 C 0.2730(5) 0.1276(3) 0.2906(4) 0.0377(14) Uani 1 1 d . . .
H15 H 0.2948 0.1041 0.2316 0.045 Uiso 1 1 calc R . .
C16 C 0.2876(5) 0.1748(3) 0.4421(4) 0.0345(13) Uani 1 1 d . . .
H16 H 0.3218 0.1906 0.5091 0.041 Uiso 1 1 calc R . .
C17 C 0.3550(5) 0.1508(3) 0.3699(4) 0.0354(13) Uani 1 1 d . . .
H17 H 0.4447 0.1470 0.3769 0.042 Uiso 1 1 calc R . .
C18 C 0.2492(8) 0.4271(4) 0.1317(5) 0.064(2) Uani 1 1 d . . .
H18 H 0.2967 0.3853 0.1281 0.076 Uiso 1 1 calc R . .
C19 C 0.1354(7) 0.4317(3) 0.1611(5) 0.0579(19) Uani 1 1 d . . .
H19 H 0.0884 0.3935 0.1830 0.069 Uiso 1 1 calc R . .
C20 C 0.0913(7) 0.4956(4) 0.1416(5) 0.064(2) Uani 1 1 d . . .
H20 H 0.0086 0.5116 0.1490 0.077 Uiso 1 1 calc R . .
C21 C 0.1794(9) 0.5316(4) 0.1004(5) 0.077(3) Uani 1 1 d . . .
H21 H 0.1706 0.5779 0.0735 0.092 Uiso 1 1 calc R . .
C22 C 0.2758(8) 0.4884(5) 0.0940(5) 0.077(2) Uani 1 1 d . . .
H22 H 0.3475 0.4984 0.0608 0.092 Uiso 1 1 calc R . .
C23 C 0.6297(9) 0.4013(5) 0.1854(7) 0.104(3) Uani 1 1 d . . .
H23A H 0.5597 0.4236 0.2079 0.125 Uiso 1 1 calc R . .
H23B H 0.6498 0.3620 0.2278 0.125 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 N1 2.081(4) . ?
Ti1 N3 2.143(4) . ?
Ti1 Cl1 2.3059(19) . ?
Ti1 Cl2 2.3210(17) . ?
Ti1 C15 2.338(5) . ?
Ti1 C13 2.340(5) . ?
Ti1 C16 2.341(5) . ?
Ti1 C17 2.356(5) . ?
Ti1 C14 2.365(5) . ?
Ti1 C7 2.588(5) . ?
Ti2 N4 1.782(4) . ?
Ti2 Cl3 2.3098(18) . ?
Ti2 Cl4 2.3169(19) . ?
Ti2 C18 2.323(7) . ?
Ti2 C19 2.332(6) . ?
Ti2 C22 2.362(7) . ?
Ti2 C20 2.386(7) . ?
Ti2 C21 2.394(7) . ?
Cl5 C23 1.700(9) . ?
Cl6 C23 1.664(9) . ?
N1 C7 1.338(6) . ?
N1 C1 1.419(6) . ?
N2 C7 1.334(6) . ?
N2 C8 1.459(7) . ?
N2 C9 1.459(6) . ?
N3 C7 1.360(6) . ?
N3 C10 1.401(6) . ?
N4 C10 1.323(6) . ?
N5 C10 1.322(6) . ?
N5 C12 1.448(7) . ?
N5 C11 1.460(7) . ?
C1 C2 1.378(7) . ?
C1 C6 1.387(8) . ?
C2 C3 1.396(8) . ?
C2 H2 0.9400 . ?
C3 C4 1.351(10) . ?
C3 H3 0.9400 . ?
C4 C5 1.366(9) . ?
C4 H4 0.9400 . ?
C5 C6 1.390(8) . ?
C5 H5 0.9400 . ?
C6 H6 0.9400 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 H9C 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11C 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C13 C14 1.397(8) . ?
C13 C15 1.406(8) . ?
C13 H13 0.9900 . ?
C14 C16 1.396(8) . ?
C14 H14 0.9900 . ?
C15 C17 1.391(8) . ?
C15 H15 0.9900 . ?
C16 C17 1.403(7) . ?
C16 H16 0.9900 . ?
C17 H17 0.9900 . ?
C18 C22 1.370(11) . ?
C18 C19 1.381(10) . ?
C18 H18 0.9900 . ?
C19 C20 1.374(9) . ?
C19 H19 0.9900 . ?
C20 C21 1.393(11) . ?
C20 H20 0.9900 . ?
C21 C22 1.385(11) . ?
C21 H21 0.9900 . ?
C22 H22 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 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
N1 Ti1 N3 62.57(15) . . ?
N1 Ti1 Cl1 90.26(12) . . ?
N3 Ti1 Cl1 129.90(12) . . ?
N1 Ti1 Cl2 135.27(12) . . ?
N3 Ti1 Cl2 84.06(11) . . ?
Cl1 Ti1 Cl2 89.59(7) . . ?
N1 Ti1 C15 129.08(18) . . ?
N3 Ti1 C15 143.00(18) . . ?
Cl1 Ti1 C15 87.03(15) . . ?
Cl2 Ti1 C15 95.58(15) . . ?
N1 Ti1 C13 94.09(19) . . ?
N3 Ti1 C13 133.81(19) . . ?
Cl1 Ti1 C13 85.76(16) . . ?
Cl2 Ti1 C13 130.47(16) . . ?
C15 Ti1 C13 34.99(19) . . ?
N1 Ti1 C16 101.38(18) . . ?
N3 Ti1 C16 86.67(18) . . ?
Cl1 Ti1 C16 142.18(15) . . ?
Cl2 Ti1 C16 105.71(14) . . ?
C15 Ti1 C16 57.69(19) . . ?
C13 Ti1 C16 57.8(2) . . ?
N1 Ti1 C17 134.83(18) . . ?
N3 Ti1 C17 109.74(18) . . ?
Cl1 Ti1 C17 118.55(15) . . ?
Cl2 Ti1 C17 82.40(14) . . ?
C15 Ti1 C17 34.46(19) . . ?
C13 Ti1 C17 57.8(2) . . ?
C16 Ti1 C17 34.77(18) . . ?
N1 Ti1 C14 79.27(18) . . ?
N3 Ti1 C14 99.58(18) . . ?
Cl1 Ti1 C14 116.65(16) . . ?
Cl2 Ti1 C14 138.55(14) . . ?
C15 Ti1 C14 57.43(19) . . ?
C13 Ti1 C14 34.5(2) . . ?
C16 Ti1 C14 34.51(19) . . ?
C17 Ti1 C14 57.32(19) . . ?
N1 Ti1 C7 30.93(15) . . ?
N3 Ti1 C7 31.67(14) . . ?
Cl1 Ti1 C7 111.24(11) . . ?
Cl2 Ti1 C7 110.58(12) . . ?
C15 Ti1 C7 147.53(18) . . ?
C13 Ti1 C7 117.01(19) . . ?
C16 Ti1 C7 95.70(17) . . ?
C17 Ti1 C7 128.63(18) . . ?
C14 Ti1 C7 90.12(17) . . ?
N4 Ti2 Cl3 103.82(15) . . ?
N4 Ti2 Cl4 101.11(14) . . ?
Cl3 Ti2 Cl4 101.48(7) . . ?
N4 Ti2 C18 93.0(2) . . ?
Cl3 Ti2 C18 141.0(2) . . ?
Cl4 Ti2 C18 109.5(2) . . ?
N4 Ti2 C19 95.4(2) . . ?
Cl3 Ti2 C19 107.9(2) . . ?
Cl4 Ti2 C19 141.5(2) . . ?
C18 Ti2 C19 34.5(3) . . ?
N4 Ti2 C22 121.8(3) . . ?
Cl3 Ti2 C22 131.7(3) . . ?
Cl4 Ti2 C22 85.4(2) . . ?
C18 Ti2 C22 34.0(3) . . ?
C19 Ti2 C22 56.5(3) . . ?
N4 Ti2 C20 126.1(2) . . ?
Cl3 Ti2 C20 85.5(2) . . ?
Cl4 Ti2 C20 129.4(2) . . ?
C18 Ti2 C20 56.7(3) . . ?
C19 Ti2 C20 33.8(2) . . ?
C22 Ti2 C20 56.3(3) . . ?
N4 Ti2 C21 148.9(2) . . ?
Cl3 Ti2 C21 98.0(2) . . ?
Cl4 Ti2 C21 95.9(2) . . ?
C18 Ti2 C21 56.6(3) . . ?
C19 Ti2 C21 56.4(2) . . ?
C22 Ti2 C21 33.9(3) . . ?
C20 Ti2 C21 33.9(3) . . ?
C7 N1 C1 124.9(4) . . ?
C7 N1 Ti1 96.0(3) . . ?
C1 N1 Ti1 133.6(3) . . ?
C7 N2 C8 122.4(4) . . ?
C7 N2 C9 121.4(4) . . ?
C8 N2 C9 116.0(4) . . ?
C7 N3 C10 119.6(4) . . ?
C7 N3 Ti1 92.5(3) . . ?
C10 N3 Ti1 128.9(3) . . ?
C10 N4 Ti2 168.3(4) . . ?
C10 N5 C12 121.4(5) . . ?
C10 N5 C11 122.7(4) . . ?
C12 N5 C11 115.8(4) . . ?
C2 C1 C6 118.8(5) . . ?
C2 C1 N1 119.3(5) . . ?
C6 C1 N1 121.8(5) . . ?
C1 C2 C3 119.4(6) . . ?
C1 C2 H2 120.3 . . ?
C3 C2 H2 120.3 . . ?
C4 C3 C2 121.2(6) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 120.1(6) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 119.7(6) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C1 C6 C5 120.7(6) . . ?
C1 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
N2 C7 N1 127.0(4) . . ?
N2 C7 N3 124.2(4) . . ?
N1 C7 N3 108.8(4) . . ?
N2 C7 Ti1 178.6(4) . . ?
N1 C7 Ti1 53.1(2) . . ?
N3 C7 Ti1 55.8(2) . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N4 C10 N5 121.7(4) . . ?
N4 C10 N3 121.7(4) . . ?
N5 C10 N3 116.6(4) . . ?
N5 C11 H11A 109.5 . . ?
N5 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N5 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N5 C12 H12A 109.5 . . ?
N5 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N5 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C15 107.5(5) . . ?
C14 C13 Ti1 73.7(3) . . ?
C15 C13 Ti1 72.5(3) . . ?
C14 C13 H13 126.0 . . ?
C15 C13 H13 126.0 . . ?
Ti1 C13 H13 126.0 . . ?
C13 C14 C16 108.3(5) . . ?
C13 C14 Ti1 71.7(3) . . ?
C16 C14 Ti1 71.8(3) . . ?
C13 C14 H14 125.8 . . ?
C16 C14 H14 125.8 . . ?
Ti1 C14 H14 125.8 . . ?
C17 C15 C13 108.4(5) . . ?
C17 C15 Ti1 73.5(3) . . ?
C13 C15 Ti1 72.5(3) . . ?
C17 C15 H15 125.6 . . ?
C13 C15 H15 125.6 . . ?
Ti1 C15 H15 125.6 . . ?
C14 C16 C17 108.0(5) . . ?
C14 C16 Ti1 73.7(3) . . ?
C17 C16 Ti1 73.2(3) . . ?
C14 C16 H16 125.7 . . ?
C17 C16 H16 125.7 . . ?
Ti1 C16 H16 125.7 . . ?
C15 C17 C16 107.8(5) . . ?
C15 C17 Ti1 72.1(3) . . ?
C16 C17 Ti1 72.0(3) . . ?
C15 C17 H17 126.0 . . ?
C16 C17 H17 126.0 . . ?
Ti1 C17 H17 126.0 . . ?
C22 C18 C19 107.8(7) . . ?
C22 C18 Ti2 74.6(4) . . ?
C19 C18 Ti2 73.1(4) . . ?
C22 C18 H18 125.7 . . ?
C19 C18 H18 125.7 . . ?
Ti2 C18 H18 125.7 . . ?
C20 C19 C18 108.6(7) . . ?
C20 C19 Ti2 75.2(4) . . ?
C18 C19 Ti2 72.4(4) . . ?
C20 C19 H19 125.4 . . ?
C18 C19 H19 125.4 . . ?
Ti2 C19 H19 125.4 . . ?
C19 C20 C21 107.7(7) . . ?
C19 C20 Ti2 70.9(4) . . ?
C21 C20 Ti2 73.4(4) . . ?
C19 C20 H20 126.0 . . ?
C21 C20 H20 126.0 . . ?
Ti2 C20 H20 126.0 . . ?
C22 C21 C20 107.3(7) . . ?
C22 C21 Ti2 71.8(4) . . ?
C20 C21 Ti2 72.8(4) . . ?
C22 C21 H21 126.1 . . ?
C20 C21 H21 126.1 . . ?
Ti2 C21 H21 126.1 . . ?
C18 C22 C21 108.6(7) . . ?
C18 C22 Ti2 71.5(4) . . ?
C21 C22 Ti2 74.3(4) . . ?
C18 C22 H22 125.5 . . ?
C21 C22 H22 125.5 . . ?
Ti2 C22 H22 125.5 . . ?
Cl6 C23 Cl5 115.8(6) . . ?
Cl6 C23 H23A 108.3 . . ?
Cl5 C23 H23A 108.3 . . ?
Cl6 C23 H23B 108.3 . . ?
Cl5 C23 H23B 108.3 . . ?
H23A C23 H23B 107.4 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.085
####################################################################### 
# 
# 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_s602p
_database_code_depnum_ccdc_archive 'CCDC 1424471'
_audit_update_record             
;
2015-09-15 deposited with the CCDC.
2015-12-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H29 Cl2 N3 Ti'
_chemical_formula_weight         430.26

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                   8.966(9)
_cell_length_b                   14.723(17)
_cell_length_c                   16.566(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.41(7)
_cell_angle_gamma                90.00
_cell_volume                     2151(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    213(2)
_cell_measurement_reflns_used    1198
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      20.7515

_exptl_crystal_description       block
_exptl_crystal_colour            red
_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    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             904
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8277
_exptl_absorpt_correction_T_max  0.8801
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      213(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 scan'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8727
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_av_sigmaI/netI    0.0901
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         25.01
_reflns_number_total             3773
_reflns_number_gt                3252
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       SMART
_computing_cell_refinement       SAINT
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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)+(0.0699P)²+6.4801P] 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         3773
_refine_ls_number_parameters     241
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1294
_refine_ls_R_factor_gt           0.1122
_refine_ls_wR_factor_ref         0.2397
_refine_ls_wR_factor_gt          0.2322
_refine_ls_goodness_of_fit_ref   1.356
_refine_ls_restrained_S_all      1.356
_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
Ti Ti 0.87148(13) 0.15951(9) 0.16253(8) 0.0198(4) Uani 1 1 d . . .
Cl1 Cl 0.8278(2) 0.24144(15) 0.04285(12) 0.0378(6) Uani 1 1 d . . .
Cl2 Cl 1.0527(2) 0.05429(14) 0.13775(15) 0.0446(6) Uani 1 1 d . . .
N1 N 0.4453(6) 0.0932(4) 0.1565(3) 0.0203(13) Uani 1 1 d . . .
H1 H 0.3578 0.0745 0.1323 0.024 Uiso 1 1 calc R . .
N2 N 0.5534(7) -0.0312(4) 0.1051(4) 0.0249(14) Uani 1 1 d . . .
N3 N 0.7047(6) 0.0931(4) 0.1539(3) 0.0208(13) Uani 1 1 d . . .
C1 C 0.4539(7) 0.1682(5) 0.2134(4) 0.0186(15) Uani 1 1 d . . .
C2 C 0.4434(7) 0.2572(5) 0.1844(4) 0.0189(15) Uani 1 1 d . . .
C3 C 0.4461(8) 0.3261(5) 0.2419(4) 0.0231(16) Uani 1 1 d . . .
H3 H 0.4403 0.3863 0.2245 0.028 Uiso 1 1 calc R . .
C4 C 0.4571(7) 0.3073(5) 0.3243(4) 0.0226(16) Uani 1 1 d . . .
H4 H 0.4585 0.3548 0.3615 0.027 Uiso 1 1 calc R . .
C5 C 0.4661(8) 0.2189(5) 0.3522(4) 0.0269(17) Uani 1 1 d . . .
H5 H 0.4725 0.2075 0.4079 0.032 Uiso 1 1 calc R . .
C6 C 0.4657(7) 0.1458(5) 0.2975(4) 0.0219(16) Uani 1 1 d . . .
C7 C 0.4771(8) 0.0491(5) 0.3301(4) 0.0260(17) Uani 1 1 d . . .
H7 H 0.4604 0.0082 0.2826 0.031 Uiso 1 1 calc R . .
C8 C 0.3547(13) 0.0300(7) 0.3794(8) 0.085(4) Uani 1 1 d . . .
H8A H 0.3661 0.0703 0.4256 0.128 Uiso 1 1 calc R . .
H8B H 0.3631 -0.0317 0.3984 0.128 Uiso 1 1 calc R . .
H8C H 0.2571 0.0391 0.3455 0.128 Uiso 1 1 calc R . .
C9 C 0.6314(11) 0.0276(7) 0.3796(6) 0.059(3) Uani 1 1 d . . .
H9A H 0.7074 0.0377 0.3465 0.089 Uiso 1 1 calc R . .
H9B H 0.6342 -0.0347 0.3967 0.089 Uiso 1 1 calc R . .
H9C H 0.6508 0.0662 0.4270 0.089 Uiso 1 1 calc R . .
C10 C 0.4273(8) 0.2758(5) 0.0924(4) 0.0252(16) Uani 1 1 d . . .
H10 H 0.4875 0.2301 0.0695 0.030 Uiso 1 1 calc R . .
C11 C 0.2604(8) 0.2639(5) 0.0499(5) 0.0300(18) Uani 1 1 d . . .
H11A H 0.2269 0.2037 0.0599 0.045 Uiso 1 1 calc R . .
H11B H 0.2520 0.2732 -0.0081 0.045 Uiso 1 1 calc R . .
H11C H 0.1984 0.3075 0.0716 0.045 Uiso 1 1 calc R . .
C12 C 0.4847(9) 0.3697(6) 0.0720(5) 0.038(2) Uani 1 1 d . . .
H12A H 0.4263 0.4159 0.0929 0.057 Uiso 1 1 calc R . .
H12B H 0.4741 0.3760 0.0136 0.057 Uiso 1 1 calc R . .
H12C H 0.5895 0.3759 0.0969 0.057 Uiso 1 1 calc R . .
C13 C 0.5708(7) 0.0517(5) 0.1402(4) 0.0199(15) Uani 1 1 d . . .
C14 C 0.4094(8) -0.0814(5) 0.0921(5) 0.0306(18) Uani 1 1 d . . .
H14A H 0.3656 -0.0781 0.1407 0.046 Uiso 1 1 calc R . .
H14B H 0.4278 -0.1438 0.0801 0.046 Uiso 1 1 calc R . .
H14C H 0.3409 -0.0551 0.0469 0.046 Uiso 1 1 calc R . .
C15 C 0.6846(9) -0.0765(5) 0.0815(5) 0.0336(19) Uani 1 1 d . . .
H15A H 0.7722 -0.0382 0.0950 0.050 Uiso 1 1 calc R . .
H15B H 0.6646 -0.0881 0.0235 0.050 Uiso 1 1 calc R . .
H15C H 0.7029 -0.1330 0.1106 0.050 Uiso 1 1 calc R . .
C16 C 1.0750(9) 0.2164(6) 0.2643(5) 0.042(2) Uani 1 1 d . . .
H16 H 1.1821 0.1995 0.2702 0.050 Uiso 1 1 calc R . .
C17 C 1.0079(9) 0.2913(6) 0.2240(5) 0.039(2) Uani 1 1 d . . .
H17 H 1.0584 0.3369 0.1952 0.047 Uiso 1 1 calc R . .
C18 C 0.8574(9) 0.2949(6) 0.2366(5) 0.036(2) Uani 1 1 d . . .
H18 H 0.7865 0.3448 0.2194 0.043 Uiso 1 1 calc R . .
C19 C 0.8325(8) 0.2241(5) 0.2864(4) 0.0286(18) Uani 1 1 d . . .
H19 H 0.7429 0.2157 0.3118 0.034 Uiso 1 1 calc R . .
C20 C 0.9655(10) 0.1728(6) 0.3025(5) 0.038(2) Uani 1 1 d . . .
H20 H 0.9852 0.1223 0.3415 0.046 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
Ti N3 1.771(6) . ?
Ti Cl1 2.293(3) . ?
Ti C20 2.328(8) . ?
Ti Cl2 2.335(3) . ?
Ti C19 2.344(7) . ?
Ti C18 2.356(8) . ?
Ti C16 2.401(8) . ?
Ti C17 2.418(8) . ?
N1 C13 1.350(8) . ?
N1 C1 1.445(8) . ?
N1 H1 0.8600 . ?
N2 C13 1.348(9) . ?
N2 C15 1.466(9) . ?
N2 C14 1.469(9) . ?
N3 C13 1.329(9) . ?
C1 C2 1.394(10) . ?
C1 C6 1.416(10) . ?
C2 C3 1.390(10) . ?
C2 C10 1.530(10) . ?
C3 C4 1.378(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.378(10) . ?
C4 H4 0.9300 . ?
C5 C6 1.406(10) . ?
C5 H5 0.9300 . ?
C6 C7 1.520(10) . ?
C7 C8 1.508(12) . ?
C7 C9 1.509(11) . ?
C7 H7 0.9800 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C12 1.533(10) . ?
C10 C11 1.544(10) . ?
C10 H10 0.9800 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.371(12) . ?
C16 C20 1.414(12) . ?
C16 H16 0.9800 . ?
C17 C18 1.403(11) . ?
C17 H17 0.9800 . ?
C18 C19 1.373(11) . ?
C18 H18 0.9800 . ?
C19 C20 1.395(11) . ?
C19 H19 0.9800 . ?
C20 H20 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 Ti Cl1 102.2(2) . . ?
N3 Ti C20 106.0(3) . . ?
Cl1 Ti C20 142.3(2) . . ?
N3 Ti Cl2 102.9(2) . . ?
Cl1 Ti Cl2 102.27(11) . . ?
C20 Ti Cl2 95.3(2) . . ?
N3 Ti C19 92.1(3) . . ?
Cl1 Ti C19 121.0(2) . . ?
C20 Ti C19 34.7(3) . . ?
Cl2 Ti C19 129.9(2) . . ?
N3 Ti C18 112.7(3) . . ?
Cl1 Ti C18 89.3(2) . . ?
C20 Ti C18 56.9(3) . . ?
Cl2 Ti C18 139.2(2) . . ?
C19 Ti C18 34.0(3) . . ?
N3 Ti C16 140.6(3) . . ?
Cl1 Ti C16 114.4(3) . . ?
C20 Ti C16 34.7(3) . . ?
Cl2 Ti C16 83.7(2) . . ?
C19 Ti C16 57.2(3) . . ?
C18 Ti C16 56.2(3) . . ?
N3 Ti C17 146.4(3) . . ?
Cl1 Ti C17 86.3(2) . . ?
C20 Ti C17 56.5(3) . . ?
Cl2 Ti C17 106.9(2) . . ?
C19 Ti C17 56.7(3) . . ?
C18 Ti C17 34.2(3) . . ?
C16 Ti C17 33.1(3) . . ?
C13 N1 C1 121.9(6) . . ?
C13 N1 H1 119.0 . . ?
C1 N1 H1 119.0 . . ?
C13 N2 C15 119.4(6) . . ?
C13 N2 C14 123.3(6) . . ?
C15 N2 C14 117.2(6) . . ?
C13 N3 Ti 172.2(5) . . ?
C2 C1 C6 123.2(6) . . ?
C2 C1 N1 120.0(6) . . ?
C6 C1 N1 116.7(6) . . ?
C3 C2 C1 117.3(6) . . ?
C3 C2 C10 122.7(6) . . ?
C1 C2 C10 120.0(6) . . ?
C4 C3 C2 121.4(7) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 120.7(7) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C6 120.9(7) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C1 116.5(7) . . ?
C5 C6 C7 119.8(6) . . ?
C1 C6 C7 123.7(6) . . ?
C8 C7 C9 110.6(8) . . ?
C8 C7 C6 111.0(7) . . ?
C9 C7 C6 112.7(6) . . ?
C8 C7 H7 107.4 . . ?
C9 C7 H7 107.4 . . ?
C6 C7 H7 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C2 C10 C12 113.9(6) . . ?
C2 C10 C11 110.0(6) . . ?
C12 C10 C11 109.7(6) . . ?
C2 C10 H10 107.7 . . ?
C12 C10 H10 107.7 . . ?
C11 C10 H10 107.7 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 N2 121.3(6) . . ?
N3 C13 N1 121.2(6) . . ?
N2 C13 N1 117.4(6) . . ?
N2 C14 H14A 109.5 . . ?
N2 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N2 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C15 H15A 109.5 . . ?
N2 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N2 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C20 107.7(7) . . ?
C17 C16 Ti 74.2(5) . . ?
C20 C16 Ti 69.8(5) . . ?
C17 C16 H16 126.0 . . ?
C20 C16 H16 126.0 . . ?
Ti C16 H16 126.0 . . ?
C16 C17 C18 107.8(8) . . ?
C16 C17 Ti 72.8(5) . . ?
C18 C17 Ti 70.5(4) . . ?
C16 C17 H17 126.0 . . ?
C18 C17 H17 126.0 . . ?
Ti C17 H17 126.0 . . ?
C19 C18 C17 109.1(8) . . ?
C19 C18 Ti 72.6(5) . . ?
C17 C18 Ti 75.4(5) . . ?
C19 C18 H18 125.2 . . ?
C17 C18 H18 125.2 . . ?
Ti C18 H18 125.2 . . ?
C18 C19 C20 107.4(7) . . ?
C18 C19 Ti 73.5(4) . . ?
C20 C19 Ti 72.0(4) . . ?
C18 C19 H19 126.1 . . ?
C20 C19 H19 126.1 . . ?
Ti C19 H19 126.1 . . ?
C19 C20 C16 107.9(8) . . ?
C19 C20 Ti 73.3(4) . . ?
C16 C20 Ti 75.4(5) . . ?
C19 C20 H20 125.6 . . ?
C16 C20 H20 125.6 . . ?
Ti C20 H20 125.6 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.123
####################################################################### 
# 
# 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_s826b
_database_code_depnum_ccdc_archive 'CCDC 1424472'
_audit_update_record             
;
2015-09-15 deposited with the CCDC.
2015-12-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C53 H98 Cl N15 O2 Si3 Zr'
_chemical_formula_weight         1188.40

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'
O O 0.0106 0.0060 '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'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.6863(19)
_cell_length_b                   14.732(2)
_cell_length_c                   18.976(3)
_cell_angle_alpha                87.593(4)
_cell_angle_beta                 76.510(3)
_cell_angle_gamma                82.086(4)
_cell_volume                     3415.7(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    2603
_cell_measurement_theta_min      2.2065
_cell_measurement_theta_max      21.7115

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1272
_exptl_absorpt_coefficient_mu    0.299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9026
_exptl_absorpt_correction_T_max  0.9399
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      200(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  'Smart apec ccd'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19339
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0896
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.10
_diffrn_reflns_theta_max         25.05
_reflns_number_total             12078
_reflns_number_gt                7669
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       SMART
_computing_cell_refinement       SAINT
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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)+(0.0358P)²+1.3130P] 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         12078
_refine_ls_number_parameters     676
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_ref         0.1201
_refine_ls_wR_factor_gt          0.0997
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.009
_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
Zr1 Zr 0.57855(3) 0.71518(2) 0.74647(2) 0.03351(11) Uani 1 1 d . . .
Cl1 Cl 0.74234(8) 0.60279(7) 0.72408(6) 0.0517(3) Uani 1 1 d . . .
N1 N 0.5287(2) 0.82525(19) 0.67047(15) 0.0339(7) Uani 1 1 d . . .
N2 N 0.6434(2) 0.9347(2) 0.61183(17) 0.0455(8) Uani 1 1 d . . .
N3 N 0.6929(2) 0.81637(19) 0.69270(15) 0.0341(7) Uani 1 1 d . . .
N4 N 0.8695(2) 0.7952(2) 0.70916(17) 0.0457(8) Uani 1 1 d . . .
N5 N 0.8408(2) 0.7911(2) 0.59127(17) 0.0460(8) Uani 1 1 d . . .
Si1 Si 0.93426(9) 0.77713(9) 0.51369(7) 0.0569(4) Uani 1 1 d . . .
C1 C 0.4288(3) 0.8659(3) 0.65283(19) 0.0363(9) Uani 1 1 d . . .
C2 C 0.3771(3) 0.9515(3) 0.6787(2) 0.0446(10) Uani 1 1 d . . .
H2 H 0.4095 0.9858 0.7073 0.054 Uiso 1 1 calc R . .
C3 C 0.2786(3) 0.9861(3) 0.6627(2) 0.0543(11) Uani 1 1 d . . .
H3 H 0.2431 1.0443 0.6809 0.065 Uiso 1 1 calc R . .
C4 C 0.2311(3) 0.9380(3) 0.6208(2) 0.0580(12) Uani 1 1 d . . .
H4 H 0.1638 0.9630 0.6095 0.070 Uiso 1 1 calc R . .
C5 C 0.2819(3) 0.8533(3) 0.5953(2) 0.0549(12) Uani 1 1 d . . .
H5 H 0.2495 0.8193 0.5665 0.066 Uiso 1 1 calc R . .
C6 C 0.3800(3) 0.8175(3) 0.6116(2) 0.0455(10) Uani 1 1 d . . .
H6 H 0.4143 0.7588 0.5941 0.055 Uiso 1 1 calc R . .
C7 C 0.6216(3) 0.8619(2) 0.65544(19) 0.0342(9) Uani 1 1 d . . .
C8 C 0.5934(4) 0.9588(3) 0.5507(2) 0.0660(13) Uani 1 1 d . . .
H8A H 0.5545 0.9089 0.5420 0.099 Uiso 1 1 calc R . .
H8B H 0.6504 0.9687 0.5074 0.099 Uiso 1 1 calc R . .
H8C H 0.5418 1.0151 0.5616 0.099 Uiso 1 1 calc R . .
C9 C 0.7301(3) 0.9887(3) 0.6166(2) 0.0592(12) Uani 1 1 d . . .
H9A H 0.7510 0.9757 0.6629 0.089 Uiso 1 1 calc R . .
H9B H 0.7035 1.0541 0.6134 0.089 Uiso 1 1 calc R . .
H9C H 0.7937 0.9724 0.5766 0.089 Uiso 1 1 calc R . .
C10 C 0.8064(3) 0.8005(2) 0.6592(2) 0.0402(9) Uani 1 1 d . . .
C11 C 0.8253(3) 0.8054(3) 0.7866(2) 0.0564(12) Uani 1 1 d . . .
H11A H 0.7547 0.8446 0.7953 0.085 Uiso 1 1 calc R . .
H11B H 0.8762 0.8334 0.8080 0.085 Uiso 1 1 calc R . .
H11C H 0.8153 0.7450 0.8089 0.085 Uiso 1 1 calc R . .
C12 C 0.9833(3) 0.7542(4) 0.6887(2) 0.0723(15) Uani 1 1 d . . .
H12A H 0.9897 0.7014 0.6576 0.108 Uiso 1 1 calc R . .
H12B H 1.0091 0.7341 0.7324 0.108 Uiso 1 1 calc R . .
H12C H 1.0279 0.7996 0.6623 0.108 Uiso 1 1 calc R . .
C13 C 1.0090(5) 0.6592(4) 0.5051(3) 0.127(3) Uani 1 1 d . . .
H13A H 1.0582 0.6510 0.5384 0.190 Uiso 1 1 calc R . .
H13B H 1.0518 0.6497 0.4552 0.190 Uiso 1 1 calc R . .
H13C H 0.9565 0.6148 0.5171 0.190 Uiso 1 1 calc R . .
C14 C 1.0352(4) 0.8606(5) 0.5011(3) 0.119(2) Uani 1 1 d . . .
H14A H 1.0019 0.9204 0.4868 0.178 Uiso 1 1 calc R . .
H14B H 1.0997 0.8387 0.4633 0.178 Uiso 1 1 calc R . .
H14C H 1.0572 0.8666 0.5468 0.178 Uiso 1 1 calc R . .
C15 C 0.8644(4) 0.7975(3) 0.4376(2) 0.0726(14) Uani 1 1 d . . .
H15A H 0.8100 0.7551 0.4420 0.109 Uiso 1 1 calc R . .
H15B H 0.9183 0.7874 0.3915 0.109 Uiso 1 1 calc R . .
H15C H 0.8279 0.8607 0.4392 0.109 Uiso 1 1 calc R . .
N6 N 0.5287(2) 0.82270(19) 0.83300(15) 0.0344(7) Uani 1 1 d . . .
N7 N 0.5135(3) 0.7908(2) 0.95883(17) 0.0455(8) Uani 1 1 d . . .
N8 N 0.5665(2) 0.6786(2) 0.86515(16) 0.0367(7) Uani 1 1 d . . .
N9 N 0.7120(3) 0.6483(2) 0.92357(18) 0.0488(9) Uani 1 1 d . . .
N10 N 0.6259(3) 0.5284(2) 0.89257(19) 0.0498(9) Uani 1 1 d . . .
Si2 Si 0.81043(10) 0.63440(9) 0.96999(7) 0.0564(3) Uani 1 1 d . . .
C16 C 0.4770(3) 0.9153(2) 0.83802(19) 0.0373(9) Uani 1 1 d . . .
C17 C 0.3668(3) 0.9387(3) 0.8686(2) 0.0458(10) Uani 1 1 d . . .
H17 H 0.3237 0.8923 0.8896 0.055 Uiso 1 1 calc R . .
C18 C 0.3190(4) 1.0286(3) 0.8688(2) 0.0559(12) Uani 1 1 d . . .
H18 H 0.2432 1.0438 0.8896 0.067 Uiso 1 1 calc R . .
C19 C 0.3811(4) 1.0970(3) 0.8390(2) 0.0562(12) Uani 1 1 d . . .
H19 H 0.3482 1.1590 0.8393 0.067 Uiso 1 1 calc R . .
C20 C 0.4907(4) 1.0742(3) 0.8090(2) 0.0528(11) Uani 1 1 d . . .
H20 H 0.5338 1.1208 0.7885 0.063 Uiso 1 1 calc R . .
C21 C 0.5390(3) 0.9841(3) 0.8082(2) 0.0433(10) Uani 1 1 d . . .
H21 H 0.6148 0.9692 0.7873 0.052 Uiso 1 1 calc R . .
C22 C 0.5360(3) 0.7663(3) 0.8886(2) 0.0370(9) Uani 1 1 d . . .
C23 C 0.5277(4) 0.8801(3) 0.9818(2) 0.0636(13) Uani 1 1 d . . .
H23A H 0.5697 0.9122 0.9406 0.095 Uiso 1 1 calc R . .
H23B H 0.5671 0.8725 1.0208 0.095 Uiso 1 1 calc R . .
H23C H 0.4559 0.9159 0.9994 0.095 Uiso 1 1 calc R . .
C24 C 0.4898(4) 0.7236(3) 1.0174(2) 0.0613(12) Uani 1 1 d . . .
H24A H 0.4742 0.6676 0.9978 0.092 Uiso 1 1 calc R . .
H24B H 0.4261 0.7489 1.0544 0.092 Uiso 1 1 calc R . .
H24C H 0.5531 0.7091 1.0390 0.092 Uiso 1 1 calc R . .
C25 C 0.6405(3) 0.6184(3) 0.8970(2) 0.0435(10) Uani 1 1 d . . .
C26 C 0.5405(4) 0.4988(3) 0.8628(3) 0.0656(13) Uani 1 1 d . . .
H26A H 0.4769 0.5463 0.8708 0.098 Uiso 1 1 calc R . .
H26B H 0.5191 0.4418 0.8869 0.098 Uiso 1 1 calc R . .
H26C H 0.5679 0.4884 0.8107 0.098 Uiso 1 1 calc R . .
C27 C 0.7133(4) 0.4570(3) 0.8998(3) 0.0815(16) Uani 1 1 d . . .
H27A H 0.7830 0.4820 0.8880 0.122 Uiso 1 1 calc R . .
H27B H 0.7162 0.4071 0.8665 0.122 Uiso 1 1 calc R . .
H27C H 0.6998 0.4334 0.9497 0.122 Uiso 1 1 calc R . .
C28 C 0.9458(4) 0.5889(4) 0.9122(3) 0.0867(17) Uani 1 1 d . . .
H28A H 0.9465 0.5241 0.9022 0.130 Uiso 1 1 calc R . .
H28B H 1.0034 0.5951 0.9376 0.130 Uiso 1 1 calc R . .
H28C H 0.9587 0.6236 0.8665 0.130 Uiso 1 1 calc R . .
C29 C 0.7782(4) 0.5622(4) 1.0538(3) 0.104(2) Uani 1 1 d . . .
H29A H 0.7046 0.5840 1.0821 0.156 Uiso 1 1 calc R . .
H29B H 0.8316 0.5665 1.0830 0.156 Uiso 1 1 calc R . .
H29C H 0.7814 0.4982 1.0402 0.156 Uiso 1 1 calc R . .
C30 C 0.8237(4) 0.7508(4) 0.9995(3) 0.0842(17) Uani 1 1 d . . .
H30A H 0.8388 0.7912 0.9570 0.126 Uiso 1 1 calc R . .
H30B H 0.8839 0.7464 1.0243 0.126 Uiso 1 1 calc R . .
H30C H 0.7554 0.7759 1.0327 0.126 Uiso 1 1 calc R . .
N11 N 0.4027(2) 0.6874(2) 0.77490(16) 0.0367(7) Uani 1 1 d . . .
N12 N 0.3291(2) 0.5931(2) 0.70366(17) 0.0438(8) Uani 1 1 d . . .
N13 N 0.5150(2) 0.6247(2) 0.67703(16) 0.0382(8) Uani 1 1 d . . .
N14 N 0.6434(3) 0.5498(2) 0.58345(18) 0.0505(9) Uani 1 1 d . . .
N15 N 0.5393(3) 0.4628(2) 0.67517(19) 0.0522(9) Uani 1 1 d . . .
Si3 Si 0.54670(12) 0.34997(9) 0.66710(8) 0.0680(4) Uani 1 1 d . . .
C31 C 0.3029(3) 0.7267(3) 0.8204(2) 0.0416(10) Uani 1 1 d . . .
C32 C 0.2259(3) 0.7860(3) 0.7942(2) 0.0497(11) Uani 1 1 d . . .
H32 H 0.2372 0.7994 0.7438 0.060 Uiso 1 1 calc R . .
C33 C 0.1322(3) 0.8258(3) 0.8417(3) 0.0653(14) Uani 1 1 d . . .
H33 H 0.0795 0.8661 0.8235 0.078 Uiso 1 1 calc R . .
C34 C 0.1145(4) 0.8075(4) 0.9152(3) 0.0707(15) Uani 1 1 d . . .
H34 H 0.0503 0.8355 0.9473 0.085 Uiso 1 1 calc R . .
C35 C 0.1906(4) 0.7483(3) 0.9415(3) 0.0652(13) Uani 1 1 d . . .
H35 H 0.1783 0.7346 0.9919 0.078 Uiso 1 1 calc R . .
C36 C 0.2847(3) 0.7088(3) 0.8948(2) 0.0501(11) Uani 1 1 d . . .
H36 H 0.3375 0.6691 0.9135 0.060 Uiso 1 1 calc R . .
C37 C 0.4111(3) 0.6328(2) 0.7194(2) 0.0387(9) Uani 1 1 d . . .
C38 C 0.2369(3) 0.5684(3) 0.7593(2) 0.0622(13) Uani 1 1 d . . .
H38A H 0.2517 0.5741 0.8073 0.093 Uiso 1 1 calc R . .
H38B H 0.2263 0.5051 0.7523 0.093 Uiso 1 1 calc R . .
H38C H 0.1706 0.6096 0.7558 0.093 Uiso 1 1 calc R . .
C39 C 0.3334(3) 0.5625(3) 0.6314(2) 0.0587(12) Uani 1 1 d . . .
H39A H 0.3935 0.5869 0.5969 0.088 Uiso 1 1 calc R . .
H39B H 0.2641 0.5846 0.6181 0.088 Uiso 1 1 calc R . .
H39C H 0.3456 0.4954 0.6303 0.088 Uiso 1 1 calc R . .
C40 C 0.5653(3) 0.5389(3) 0.6458(2) 0.0429(10) Uani 1 1 d . . .
C41 C 0.6649(3) 0.6384(3) 0.5513(2) 0.0579(12) Uani 1 1 d . . .
H41A H 0.5967 0.6810 0.5603 0.087 Uiso 1 1 calc R . .
H41B H 0.6940 0.6317 0.4989 0.087 Uiso 1 1 calc R . .
H41C H 0.7184 0.6623 0.5729 0.087 Uiso 1 1 calc R . .
C42 C 0.7341(4) 0.4768(3) 0.5612(3) 0.0771(16) Uani 1 1 d . . .
H42A H 0.7260 0.4258 0.5960 0.116 Uiso 1 1 calc R . .
H42B H 0.8033 0.5003 0.5596 0.116 Uiso 1 1 calc R . .
H42C H 0.7341 0.4554 0.5130 0.116 Uiso 1 1 calc R . .
C43 C 0.6629(5) 0.2880(4) 0.7016(4) 0.114(2) Uani 1 1 d . . .
H43A H 0.7319 0.3039 0.6715 0.172 Uiso 1 1 calc R . .
H43B H 0.6618 0.2218 0.6996 0.172 Uiso 1 1 calc R . .
H43C H 0.6561 0.3057 0.7518 0.172 Uiso 1 1 calc R . .
C44 C 0.5573(6) 0.3084(4) 0.5736(3) 0.131(3) Uani 1 1 d . . .
H44A H 0.5210 0.3560 0.5465 0.197 Uiso 1 1 calc R . .
H44B H 0.5220 0.2528 0.5766 0.197 Uiso 1 1 calc R . .
H44C H 0.6346 0.2947 0.5488 0.197 Uiso 1 1 calc R . .
C45 C 0.4189(5) 0.3144(3) 0.7244(4) 0.117(2) Uani 1 1 d . . .
H45A H 0.4145 0.3274 0.7752 0.175 Uiso 1 1 calc R . .
H45B H 0.4190 0.2485 0.7188 0.175 Uiso 1 1 calc R . .
H45C H 0.3557 0.3483 0.7093 0.175 Uiso 1 1 calc R . .
O1 O 0.8912(5) 0.0400(4) 0.8280(4) 0.161(2) Uani 1 1 d . . .
C46 C 0.8132(11) 0.0697(9) 0.8912(6) 0.249(7) Uani 1 1 d D . .
H46A H 0.8060 0.1371 0.8957 0.299 Uiso 1 1 calc R . .
H46B H 0.7408 0.0522 0.8905 0.299 Uiso 1 1 calc R . .
C47 C 0.8519(13) 0.0265(8) 0.9477(5) 0.308(10) Uani 1 1 d D . .
H47A H 0.8451 -0.0390 0.9477 0.462 Uiso 1 1 calc R . .
H47B H 0.8091 0.0533 0.9937 0.462 Uiso 1 1 calc R . .
H47C H 0.9289 0.0344 0.9419 0.462 Uiso 1 1 calc R . .
C48 C 0.8608(7) 0.0807(7) 0.7678(6) 0.158(3) Uani 1 1 d . . .
H48A H 0.8540 0.1482 0.7712 0.189 Uiso 1 1 calc R . .
H48B H 0.7893 0.0638 0.7645 0.189 Uiso 1 1 calc R . .
C49 C 0.9434(7) 0.0494(6) 0.7051(4) 0.163(4) Uani 1 1 d . . .
H49A H 1.0156 0.0568 0.7126 0.244 Uiso 1 1 calc R . .
H49B H 0.9305 0.0854 0.6626 0.244 Uiso 1 1 calc R . .
H49C H 0.9405 -0.0155 0.6972 0.244 Uiso 1 1 calc R . .
O2 O 0.9379(7) 0.6368(6) 0.2576(5) 0.210(3) Uani 1 1 d . . .
C50 C 1.0213(10) 0.5851(8) 0.2801(7) 0.196(5) Uani 1 1 d . . .
H50A H 1.0673 0.6251 0.2965 0.235 Uiso 1 1 calc R . .
H50B H 1.0676 0.5470 0.2398 0.235 Uiso 1 1 calc R . .
C51 C 0.9753(7) 0.5291(7) 0.3375(6) 0.175(4) Uani 1 1 d . . .
H51A H 0.9227 0.5670 0.3744 0.263 Uiso 1 1 calc R . .
H51B H 1.0332 0.4966 0.3588 0.263 Uiso 1 1 calc R . .
H51C H 0.9377 0.4845 0.3192 0.263 Uiso 1 1 calc R . .
C52 C 0.9777(12) 0.6982(7) 0.2031(8) 0.252(7) Uani 1 1 d . . .
H52A H 1.0383 0.7245 0.2161 0.302 Uiso 1 1 calc R . .
H52B H 1.0081 0.6641 0.1574 0.302 Uiso 1 1 calc R . .
C53 C 0.9004(9) 0.7685(8) 0.1914(6) 0.242(6) Uani 1 1 d . . .
H53A H 0.8416 0.7433 0.1765 0.363 Uiso 1 1 calc R . .
H53B H 0.9343 0.8093 0.1532 0.363 Uiso 1 1 calc R . .
H53C H 0.8703 0.8031 0.2362 0.363 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
Zr1 N1 2.249(3) . ?
Zr1 N6 2.250(3) . ?
Zr1 N13 2.259(3) . ?
Zr1 N11 2.260(3) . ?
Zr1 N3 2.268(3) . ?
Zr1 N8 2.268(3) . ?
Zr1 Cl1 2.4371(10) . ?
Zr1 C22 2.741(4) . ?
Zr1 C37 2.742(4) . ?
Zr1 C7 2.743(4) . ?
N1 C7 1.330(4) . ?
N1 C1 1.432(4) . ?
N2 C7 1.346(4) . ?
N2 C8 1.456(5) . ?
N2 C9 1.464(5) . ?
N3 C7 1.363(4) . ?
N3 C10 1.423(4) . ?
N4 C10 1.370(5) . ?
N4 C12 1.456(5) . ?
N4 C11 1.452(5) . ?
N5 C10 1.267(4) . ?
N5 Si1 1.661(3) . ?
Si1 C13 1.855(5) . ?
Si1 C15 1.857(5) . ?
Si1 C14 1.865(5) . ?
C1 C6 1.377(5) . ?
C1 C2 1.390(5) . ?
C2 C3 1.380(5) . ?
C3 C4 1.375(5) . ?
C4 C5 1.375(5) . ?
C5 C6 1.381(5) . ?
N6 C22 1.328(4) . ?
N6 C16 1.427(4) . ?
N7 C22 1.350(4) . ?
N7 C23 1.450(5) . ?
N7 C24 1.462(5) . ?
N8 C22 1.360(4) . ?
N8 C25 1.422(5) . ?
N9 C25 1.271(5) . ?
N9 Si2 1.675(3) . ?
N10 C25 1.372(5) . ?
N10 C27 1.447(5) . ?
N10 C26 1.456(5) . ?
Si2 C28 1.862(5) . ?
Si2 C29 1.871(5) . ?
Si2 C30 1.867(5) . ?
C16 C17 1.385(5) . ?
C16 C21 1.389(5) . ?
C17 C18 1.379(5) . ?
C18 C19 1.385(6) . ?
C19 C20 1.375(6) . ?
C20 C21 1.383(5) . ?
N11 C37 1.328(4) . ?
N11 C31 1.418(4) . ?
N12 C37 1.356(4) . ?
N12 C39 1.448(5) . ?
N12 C38 1.458(5) . ?
N13 C37 1.367(4) . ?
N13 C40 1.421(4) . ?
N14 C40 1.373(5) . ?
N14 C41 1.451(5) . ?
N14 C42 1.460(5) . ?
N15 C40 1.281(5) . ?
N15 Si3 1.663(3) . ?
Si3 C45 1.857(5) . ?
Si3 C43 1.861(5) . ?
Si3 C44 1.870(6) . ?
C31 C32 1.386(5) . ?
C31 C36 1.397(5) . ?
C32 C33 1.386(5) . ?
C33 C34 1.380(6) . ?
C34 C35 1.378(6) . ?
C35 C36 1.380(5) . ?
O1 C48 1.377(9) . ?
O1 C46 1.407(10) . ?
C46 C47 1.378(13) . ?
C48 C49 1.435(10) . ?
O2 C50 1.357(11) . ?
O2 C52 1.395(13) . ?
C50 C51 1.403(12) . ?
C52 C53 1.374(12) . ?

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 Zr1 N6 86.51(10) . . ?
N1 Zr1 N13 82.75(11) . . ?
N6 Zr1 N13 144.16(10) . . ?
N1 Zr1 N11 87.29(10) . . ?
N6 Zr1 N11 86.95(10) . . ?
N13 Zr1 N11 58.54(10) . . ?
N1 Zr1 N3 58.45(10) . . ?
N6 Zr1 N3 82.15(10) . . ?
N13 Zr1 N3 119.50(11) . . ?
N11 Zr1 N3 144.45(10) . . ?
N1 Zr1 N8 143.63(10) . . ?
N6 Zr1 N8 58.38(10) . . ?
N13 Zr1 N8 119.35(11) . . ?
N11 Zr1 N8 82.07(10) . . ?
N3 Zr1 N8 119.06(10) . . ?
N1 Zr1 Cl1 127.60(8) . . ?
N6 Zr1 Cl1 127.26(8) . . ?
N13 Zr1 Cl1 85.29(8) . . ?
N11 Zr1 Cl1 127.39(8) . . ?
N3 Zr1 Cl1 85.01(7) . . ?
N8 Zr1 Cl1 85.23(8) . . ?
N1 Zr1 C22 114.86(11) . . ?
N6 Zr1 C22 28.76(10) . . ?
N13 Zr1 C22 138.58(11) . . ?
N11 Zr1 C22 83.99(10) . . ?
N3 Zr1 C22 101.07(10) . . ?
N8 Zr1 C22 29.62(10) . . ?
Cl1 Zr1 C22 107.57(8) . . ?
N1 Zr1 C37 84.63(11) . . ?
N6 Zr1 C37 115.31(11) . . ?
N13 Zr1 C37 29.76(10) . . ?
N11 Zr1 C37 28.78(10) . . ?
N3 Zr1 C37 138.97(11) . . ?
N8 Zr1 C37 101.10(11) . . ?
Cl1 Zr1 C37 107.68(8) . . ?
C22 Zr1 C37 111.14(11) . . ?
N1 Zr1 C7 28.77(9) . . ?
N6 Zr1 C7 83.76(10) . . ?
N13 Zr1 C7 101.65(11) . . ?
N11 Zr1 C7 115.64(11) . . ?
N3 Zr1 C7 29.68(9) . . ?
N8 Zr1 C7 138.11(10) . . ?
Cl1 Zr1 C7 107.64(8) . . ?
C22 Zr1 C7 110.86(11) . . ?
C37 Zr1 C7 111.74(11) . . ?
C7 N1 C1 125.1(3) . . ?
C7 N1 Zr1 96.7(2) . . ?
C1 N1 Zr1 136.6(2) . . ?
C7 N2 C8 123.0(3) . . ?
C7 N2 C9 122.0(3) . . ?
C8 N2 C9 114.5(3) . . ?
C7 N3 C10 119.7(3) . . ?
C7 N3 Zr1 94.9(2) . . ?
C10 N3 Zr1 129.4(2) . . ?
C10 N4 C12 119.3(3) . . ?
C10 N4 C11 123.9(3) . . ?
C12 N4 C11 114.8(3) . . ?
C10 N5 Si1 156.0(3) . . ?
N5 Si1 C13 111.9(2) . . ?
N5 Si1 C15 108.64(19) . . ?
C13 Si1 C15 107.9(2) . . ?
N5 Si1 C14 112.8(2) . . ?
C13 Si1 C14 108.9(3) . . ?
C15 Si1 C14 106.4(3) . . ?
C6 C1 C2 119.0(3) . . ?
C6 C1 N1 119.2(3) . . ?
C2 C1 N1 121.8(3) . . ?
C3 C2 C1 119.6(4) . . ?
C4 C3 C2 121.1(4) . . ?
C5 C4 C3 119.3(4) . . ?
C4 C5 C6 120.1(4) . . ?
C1 C6 C5 120.9(4) . . ?
N1 C7 N2 126.2(3) . . ?
N1 C7 N3 110.0(3) . . ?
N2 C7 N3 123.8(3) . . ?
N1 C7 Zr1 54.50(18) . . ?
N2 C7 Zr1 178.8(3) . . ?
N3 C7 Zr1 55.47(18) . . ?
N5 C10 N4 126.2(3) . . ?
N5 C10 N3 122.1(3) . . ?
N4 C10 N3 111.6(3) . . ?
C22 N6 C16 125.6(3) . . ?
C22 N6 Zr1 96.6(2) . . ?
C16 N6 Zr1 135.9(2) . . ?
C22 N7 C23 123.0(3) . . ?
C22 N7 C24 121.3(3) . . ?
C23 N7 C24 114.9(3) . . ?
C22 N8 C25 120.1(3) . . ?
C22 N8 Zr1 94.8(2) . . ?
C25 N8 Zr1 128.7(2) . . ?
C25 N9 Si2 152.2(3) . . ?
C25 N10 C27 119.3(3) . . ?
C25 N10 C26 123.9(3) . . ?
C27 N10 C26 114.9(3) . . ?
N9 Si2 C28 112.0(2) . . ?
N9 Si2 C29 113.8(2) . . ?
C28 Si2 C29 110.2(3) . . ?
N9 Si2 C30 106.7(2) . . ?
C28 Si2 C30 106.7(2) . . ?
C29 Si2 C30 107.1(3) . . ?
C17 C16 C21 118.9(4) . . ?
C17 C16 N6 122.6(4) . . ?
C21 C16 N6 118.5(3) . . ?
C18 C17 C16 120.6(4) . . ?
C17 C18 C19 120.3(4) . . ?
C20 C19 C18 119.3(4) . . ?
C19 C20 C21 120.6(4) . . ?
C16 C21 C20 120.3(4) . . ?
N6 C22 N7 125.7(3) . . ?
N6 C22 N8 110.2(3) . . ?
N7 C22 N8 124.1(4) . . ?
N6 C22 Zr1 54.63(18) . . ?
N7 C22 Zr1 179.0(3) . . ?
N8 C22 Zr1 55.55(18) . . ?
N9 C25 N10 126.7(4) . . ?
N9 C25 N8 121.4(4) . . ?
N10 C25 N8 111.9(3) . . ?
C37 N11 C31 125.2(3) . . ?
C37 N11 Zr1 96.2(2) . . ?
C31 N11 Zr1 136.7(2) . . ?
C37 N12 C39 122.1(3) . . ?
C37 N12 C38 122.6(3) . . ?
C39 N12 C38 114.9(3) . . ?
C37 N13 C40 120.0(3) . . ?
C37 N13 Zr1 95.1(2) . . ?
C40 N13 Zr1 128.4(2) . . ?
C40 N14 C41 123.5(3) . . ?
C40 N14 C42 119.3(4) . . ?
C41 N14 C42 113.7(3) . . ?
C40 N15 Si3 147.7(3) . . ?
N15 Si3 C45 107.5(2) . . ?
N15 Si3 C43 111.4(2) . . ?
C45 Si3 C43 107.4(3) . . ?
N15 Si3 C44 115.7(2) . . ?
C45 Si3 C44 106.4(3) . . ?
C43 Si3 C44 108.1(3) . . ?
C32 C31 C36 118.9(4) . . ?
C32 C31 N11 122.4(4) . . ?
C36 C31 N11 118.6(4) . . ?
C31 C32 C33 119.9(4) . . ?
C34 C33 C32 120.9(5) . . ?
C35 C34 C33 119.5(4) . . ?
C34 C35 C36 120.2(5) . . ?
C35 C36 C31 120.6(4) . . ?
N11 C37 N12 126.2(3) . . ?
N11 C37 N13 110.1(3) . . ?
N12 C37 N13 123.6(3) . . ?
N11 C37 Zr1 55.03(18) . . ?
N12 C37 Zr1 178.1(3) . . ?
N13 C37 Zr1 55.12(18) . . ?
N15 C40 N14 126.5(4) . . ?
N15 C40 N13 121.9(4) . . ?
N14 C40 N13 111.6(3) . . ?
C48 O1 C46 110.1(9) . . ?
C47 C46 O1 105.4(11) . . ?
O1 C48 C49 108.0(8) . . ?
C50 O2 C52 110.7(11) . . ?
O2 C50 C51 107.6(11) . . ?
C53 C52 O2 114.0(14) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.05
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.060
