# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1415001'
_audit_update_record             
;
2015-08-26 deposited with the CCDC.
2015-09-16 downloaded from the CCDC.
;

_audit_creation_date             2010-09-17T18:46:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

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

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C30 H47 Cl3 N4 Ti3 Zr'
_chemical_formula_sum            'C30 H47 Cl3 N4 Ti3 Zr'
_chemical_formula_weight         804.99
_chemical_compound_source        'synthesis as described'

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

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

_cell_length_a                   11.065(3)
_cell_length_b                   17.559(4)
_cell_length_c                   18.813(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.44(4)
_cell_angle_gamma                90
_cell_volume                     3648.5(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    243
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_wavelength     0.71073

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

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1648
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
7 0 -6 0.029
-1 1 9 0.109
1 -1 -9 0.096
-11 -1 -1 0.148
0 -1 0 0.052
0 1 0 0.085

_exptl_special_details           
;
 ?
;

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

_exptl_absorpt_coefficient_mu    1.155
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_T_max  0.885

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

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.1480
_diffrn_reflns_av_unetI/netI     0.1105
_diffrn_reflns_number            80915
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         5.04
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_reflns_number_total             8322
_reflns_number_gt                4934
_reflns_threshold_expression     >2sigma(I)
_diffrn_reflns_reduction_process 
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

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

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

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

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 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)+(0.0578P)²+0.0000P] 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_number_reflns         8322
_refine_ls_number_parameters     385
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1139
_refine_ls_R_factor_gt           0.0542
_refine_ls_wR_factor_ref         0.1337
_refine_ls_wR_factor_gt          0.1137
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_restrained_S_all      0.986
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.71
_refine_diff_density_rms         0.108

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

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.1391(4) 0.9463(3) 0.4506(3) 0.0388(11) Uani 1 1 d . . .
C12 C 0.0814(4) 0.9595(2) 0.3816(3) 0.0386(11) Uani 1 1 d . . .
C13 C -0.0264(4) 0.9147(3) 0.3783(2) 0.0384(11) Uani 1 1 d . . .
C14 C -0.0333(4) 0.8744(3) 0.4426(2) 0.0365(11) Uani 1 1 d . . .
C15 C 0.0690(4) 0.8939(3) 0.4884(2) 0.0344(10) Uani 1 1 d . . .
C16 C 0.2535(4) 0.9847(3) 0.4811(3) 0.0705(19) Uani 1 1 d . . .
H16A H 0.2353 1.0142 0.5221 0.106 Uiso 1 1 calc R . .
H16B H 0.2848 1.0176 0.4458 0.106 Uiso 1 1 calc R . .
H16C H 0.3128 0.9467 0.4947 0.106 Uiso 1 1 calc R . .
C17 C 0.1226(6) 1.0137(3) 0.3260(3) 0.0746(19) Uani 1 1 d . . .
H17A H 0.0963 0.9954 0.2795 0.112 Uiso 1 1 calc R . .
H17B H 0.2094 1.0171 0.3296 0.112 Uiso 1 1 calc R . .
H17C H 0.0886 1.0631 0.3333 0.112 Uiso 1 1 calc R . .
C18 C -0.1241(4) 0.9145(4) 0.3179(3) 0.0674(17) Uani 1 1 d . . .
H18A H -0.1411 0.8631 0.3033 0.101 Uiso 1 1 calc R . .
H18B H -0.0967 0.9429 0.2784 0.101 Uiso 1 1 calc R . .
H18C H -0.1964 0.9375 0.3339 0.101 Uiso 1 1 calc R . .
C19 C -0.1370(4) 0.8219(3) 0.4599(3) 0.0581(15) Uani 1 1 d . . .
H19A H -0.1386 0.7788 0.4285 0.087 Uiso 1 1 calc R . .
H19B H -0.2122 0.849 0.4537 0.087 Uiso 1 1 calc R . .
H19C H -0.1256 0.8049 0.5083 0.087 Uiso 1 1 calc R . .
C20 C 0.0983(5) 0.8661(4) 0.5633(3) 0.0624(16) Uani 1 1 d . . .
H20A H 0.1092 0.909 0.5947 0.094 Uiso 1 1 calc R . .
H20B H 0.1713 0.8365 0.5647 0.094 Uiso 1 1 calc R . .
H20C H 0.0329 0.8352 0.5782 0.094 Uiso 1 1 calc R . .
C21 C 0.5627(3) 0.8061(3) 0.3159(2) 0.0284(9) Uani 1 1 d . . .
C22 C 0.5800(3) 0.7304(3) 0.3422(2) 0.0305(10) Uani 1 1 d . . .
C23 C 0.5697(3) 0.7334(2) 0.4185(2) 0.0295(9) Uani 1 1 d . . .
C24 C 0.5439(3) 0.8106(2) 0.4370(2) 0.0282(9) Uani 1 1 d . . .
C25 C 0.5399(3) 0.8551(2) 0.3734(2) 0.0277(9) Uani 1 1 d . . .
C26 C 0.5773(4) 0.8306(3) 0.2393(2) 0.0459(12) Uani 1 1 d . . .
H26A H 0.5003 0.8465 0.2181 0.069 Uiso 1 1 calc R . .
H26B H 0.6071 0.7886 0.2128 0.069 Uiso 1 1 calc R . .
H26C H 0.6335 0.8722 0.2386 0.069 Uiso 1 1 calc R . .
C27 C 0.6100(4) 0.6602(3) 0.2994(3) 0.0525(14) Uani 1 1 d . . .
H27A H 0.5679 0.6626 0.2533 0.079 Uiso 1 1 calc R . .
H27B H 0.5854 0.6153 0.3239 0.079 Uiso 1 1 calc R . .
H27C H 0.6956 0.6583 0.2939 0.079 Uiso 1 1 calc R . .
C28 C 0.5917(4) 0.6704(3) 0.4708(3) 0.0485(13) Uani 1 1 d . . .
H28A H 0.6672 0.6789 0.4975 0.073 Uiso 1 1 calc R . .
H28B H 0.5949 0.6228 0.4458 0.073 Uiso 1 1 calc R . .
H28C H 0.5272 0.669 0.5027 0.073 Uiso 1 1 calc R . .
C29 C 0.5325(4) 0.8382(3) 0.5124(2) 0.0407(11) Uani 1 1 d . . .
H29A H 0.5093 0.8909 0.5116 0.061 Uiso 1 1 calc R . .
H29B H 0.6089 0.8325 0.5388 0.061 Uiso 1 1 calc R . .
H29C H 0.4721 0.8087 0.5345 0.061 Uiso 1 1 calc R . .
C30 C 0.5235(4) 0.9409(3) 0.3675(3) 0.0441(12) Uani 1 1 d . . .
H30A H 0.5129 0.9618 0.4138 0.066 Uiso 1 1 calc R . .
H30B H 0.4535 0.9519 0.3366 0.066 Uiso 1 1 calc R . .
H30C H 0.5939 0.963 0.3483 0.066 Uiso 1 1 calc R . .
C31 C 0.1414(4) 0.5346(2) 0.3899(2) 0.0285(9) Uani 1 1 d . . .
C32 C 0.0398(4) 0.5701(2) 0.4179(2) 0.0316(10) Uani 1 1 d . . .
C33 C 0.0785(4) 0.6022(2) 0.4853(2) 0.0362(11) Uani 1 1 d . . .
C34 C 0.2048(4) 0.5871(3) 0.4979(2) 0.0385(11) Uani 1 1 d . . .
C35 C 0.2427(4) 0.5454(2) 0.4387(2) 0.0347(10) Uani 1 1 d . . .
C36 C 0.1445(5) 0.4881(3) 0.3226(3) 0.0543(14) Uani 1 1 d . . .
H36A H 0.152 0.4351 0.3346 0.081 Uiso 1 1 calc R . .
H36B H 0.2124 0.5035 0.2966 0.081 Uiso 1 1 calc R . .
H36C H 0.071 0.4962 0.2938 0.081 Uiso 1 1 calc R . .
C37 C -0.0886(4) 0.5712(3) 0.3856(3) 0.0555(15) Uani 1 1 d . . .
H37A H -0.089 0.5563 0.3365 0.083 Uiso 1 1 calc R . .
H37B H -0.1212 0.6216 0.389 0.083 Uiso 1 1 calc R . .
H37C H -0.1372 0.5363 0.4109 0.083 Uiso 1 1 calc R . .
C38 C -0.0016(6) 0.6416(3) 0.5363(3) 0.0705(18) Uani 1 1 d . . .
H38A H -0.0157 0.6081 0.5754 0.106 Uiso 1 1 calc R . .
H38B H -0.0776 0.6545 0.5119 0.106 Uiso 1 1 calc R . .
H38C H 0.0374 0.6871 0.5541 0.106 Uiso 1 1 calc R . .
C39 C 0.2808(5) 0.6095(3) 0.5639(2) 0.0661(18) Uani 1 1 d . . .
H39A H 0.3582 0.5849 0.5638 0.099 Uiso 1 1 calc R . .
H39B H 0.2405 0.5942 0.6054 0.099 Uiso 1 1 calc R . .
H39C H 0.2918 0.6637 0.5646 0.099 Uiso 1 1 calc R . .
C40 C 0.3669(4) 0.5136(3) 0.4289(3) 0.0606(16) Uani 1 1 d . . .
H40A H 0.4216 0.5303 0.4673 0.091 Uiso 1 1 calc R . .
H40B H 0.395 0.5312 0.3845 0.091 Uiso 1 1 calc R . .
H40C H 0.3633 0.4589 0.4287 0.091 Uiso 1 1 calc R . .
Cl1 Cl 0.32031(12) 0.73659(8) 0.15511(6) 0.0519(3) Uani 1 1 d . . .
Cl2 Cl 0.04556(12) 0.83882(8) 0.18273(6) 0.0531(3) Uani 1 1 d . . .
Cl3 Cl 0.04844(13) 0.63151(8) 0.20151(6) 0.0558(4) Uani 1 1 d . . .
N1 N 0.2583(3) 0.76034(18) 0.43688(16) 0.0247(7) Uani 1 1 d . . .
N12 N 0.2603(3) 0.83604(19) 0.31406(16) 0.0251(7) Uani 1 1 d . . .
H12 H 0.2605 0.8604 0.2744 0.03 Uiso 1 1 calc R . .
N13 N 0.0655(3) 0.73762(18) 0.34698(17) 0.0259(7) Uani 1 1 d . . .
H13 H 0.0038 0.7305 0.3178 0.031 Uiso 0.5 1 calc PR . .
N23 N 0.2977(3) 0.67563(19) 0.32207(16) 0.0257(7) Uani 1 1 d . . .
H23 H 0.3096 0.6489 0.2848 0.031 Uiso 0.5 1 calc PR . .
Ti1 Ti 0.14408(6) 0.82877(4) 0.38932(4) 0.02580(18) Uani 1 1 d . . .
Ti2 Ti 0.37544(6) 0.76655(4) 0.36426(4) 0.02471(18) Uani 1 1 d . . .
Ti3 Ti 0.18263(6) 0.66893(4) 0.39722(4) 0.02548(18) Uani 1 1 d . . .
Zr1 Zr 0.16826(4) 0.74066(2) 0.244401(19) 0.02696(13) Uani 1 1 d . . .



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

_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
C11 C15 1.421(6) . ?
C11 C12 1.432(6) . ?
C11 C16 1.516(6) . ?
C11 Ti1 2.367(4) . ?
C12 C13 1.427(6) . ?
C12 C17 1.505(6) . ?
C12 Ti1 2.400(4) . ?
C13 C14 1.409(6) . ?
C13 C18 1.521(6) . ?
C13 Ti1 2.414(4) . ?
C14 C15 1.423(6) . ?
C14 C19 1.521(6) . ?
C14 Ti1 2.395(4) . ?
C15 C20 1.509(6) . ?
C15 Ti1 2.378(4) . ?
C21 C25 1.417(6) . ?
C21 C22 1.426(6) . ?
C21 C26 1.523(5) . ?
C21 Ti2 2.414(4) . ?
C22 C23 1.447(6) . ?
C22 C27 1.521(6) . ?
C22 Ti2 2.410(4) . ?
C23 C24 1.431(6) . ?
C23 C28 1.491(6) . ?
C23 Ti2 2.395(4) . ?
C24 C25 1.428(5) . ?
C24 C29 1.511(6) . ?
C24 Ti2 2.374(4) . ?
C25 C30 1.520(6) . ?
C25 Ti2 2.392(4) . ?
C31 C32 1.414(6) . ?
C31 C35 1.419(6) . ?
C31 C36 1.507(6) . ?
C31 Ti3 2.405(4) . ?
C32 C33 1.431(6) . ?
C32 C37 1.512(6) . ?
C32 Ti3 2.395(4) . ?
C33 C34 1.429(6) . ?
C33 C38 1.512(6) . ?
C33 Ti3 2.383(4) . ?
C34 C35 1.417(6) . ?
C34 C39 1.510(6) . ?
C34 Ti3 2.379(4) . ?
C35 C40 1.505(6) . ?
C35 Ti3 2.387(4) . ?
Cl1 Zr1 2.4487(15) . ?
Cl2 Zr1 2.4436(14) . ?
Cl3 Zr1 2.4399(13) . ?
N1 Ti1 1.925(3) . ?
N1 Ti3 1.939(3) . ?
N1 Ti2 1.942(3) . ?
N12 Ti2 1.964(3) . ?
N12 Ti1 1.973(3) . ?
N12 Zr1 2.324(3) . ?
N13 Ti1 1.967(3) . ?
N13 Ti3 1.970(3) . ?
N13 Zr1 2.298(3) . ?
N23 Ti2 1.959(3) . ?
N23 Ti3 1.962(3) . ?
N23 Zr1 2.289(3) . ?
Ti1 Ti3 2.8415(12) . ?
Ti1 Ti2 2.8485(12) . ?
Ti1 Zr1 3.1601(9) . ?
Ti2 Ti3 2.8342(11) . ?
Ti2 Zr1 3.1506(15) . ?
Ti3 Zr1 3.1340(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C15 C11 C12 109.3(4) . . ?
C15 C11 C16 124.6(5) . . ?
C12 C11 C16 126.0(5) . . ?
C15 C11 Ti1 73.0(2) . . ?
C12 C11 Ti1 73.8(2) . . ?
C16 C11 Ti1 121.9(3) . . ?
C13 C12 C11 106.1(4) . . ?
C13 C12 C17 127.3(5) . . ?
C11 C12 C17 126.6(5) . . ?
C13 C12 Ti1 73.3(2) . . ?
C11 C12 Ti1 71.3(2) . . ?
C17 C12 Ti1 123.2(3) . . ?
C14 C13 C12 109.2(4) . . ?
C14 C13 C18 124.6(4) . . ?
C12 C13 C18 126.1(5) . . ?
C14 C13 Ti1 72.2(2) . . ?
C12 C13 Ti1 72.2(2) . . ?
C18 C13 Ti1 125.5(3) . . ?
C13 C14 C15 108.4(4) . . ?
C13 C14 C19 124.6(4) . . ?
C15 C14 C19 126.9(4) . . ?
C13 C14 Ti1 73.7(2) . . ?
C15 C14 Ti1 72.0(2) . . ?
C19 C14 Ti1 122.3(3) . . ?
C11 C15 C14 107.0(4) . . ?
C11 C15 C20 125.7(4) . . ?
C14 C15 C20 127.3(4) . . ?
C11 C15 Ti1 72.2(2) . . ?
C14 C15 Ti1 73.3(2) . . ?
C20 C15 Ti1 120.8(3) . . ?
C25 C21 C22 109.1(3) . . ?
C25 C21 C26 125.7(4) . . ?
C22 C21 C26 124.9(4) . . ?
C25 C21 Ti2 72.0(2) . . ?
C22 C21 Ti2 72.7(2) . . ?
C26 C21 Ti2 125.4(3) . . ?
C21 C22 C23 107.1(4) . . ?
C21 C22 C27 126.9(4) . . ?
C23 C22 C27 126.0(4) . . ?
C21 C22 Ti2 73.0(2) . . ?
C23 C22 Ti2 71.9(2) . . ?
C27 C22 Ti2 122.8(3) . . ?
C24 C23 C22 107.7(4) . . ?
C24 C23 C28 124.7(4) . . ?
C22 C23 C28 127.4(4) . . ?
C24 C23 Ti2 71.7(2) . . ?
C22 C23 Ti2 73.1(2) . . ?
C28 C23 Ti2 124.6(3) . . ?
C25 C24 C23 108.2(4) . . ?
C25 C24 C29 127.6(4) . . ?
C23 C24 C29 124.1(4) . . ?
C25 C24 Ti2 73.3(2) . . ?
C23 C24 Ti2 73.3(2) . . ?
C29 C24 Ti2 122.6(3) . . ?
C21 C25 C24 107.9(4) . . ?
C21 C25 C30 124.9(4) . . ?
C24 C25 C30 127.0(4) . . ?
C21 C25 Ti2 73.7(2) . . ?
C24 C25 Ti2 71.9(2) . . ?
C30 C25 Ti2 123.5(3) . . ?
C32 C31 C35 108.3(4) . . ?
C32 C31 C36 127.5(4) . . ?
C35 C31 C36 124.0(4) . . ?
C32 C31 Ti3 72.5(2) . . ?
C35 C31 Ti3 72.1(2) . . ?
C36 C31 Ti3 124.5(3) . . ?
C31 C32 C33 107.6(4) . . ?
C31 C32 C37 127.2(4) . . ?
C33 C32 C37 125.1(4) . . ?
C31 C32 Ti3 73.3(2) . . ?
C33 C32 Ti3 72.1(2) . . ?
C37 C32 Ti3 122.6(3) . . ?
C34 C33 C32 108.1(4) . . ?
C34 C33 C38 125.8(5) . . ?
C32 C33 C38 126.0(5) . . ?
C34 C33 Ti3 72.4(2) . . ?
C32 C33 Ti3 73.0(2) . . ?
C38 C33 Ti3 122.9(3) . . ?
C35 C34 C33 107.4(4) . . ?
C35 C34 C39 127.2(5) . . ?
C33 C34 C39 125.3(5) . . ?
C35 C34 Ti3 73.0(2) . . ?
C33 C34 Ti3 72.7(2) . . ?
C39 C34 Ti3 121.6(3) . . ?
C34 C35 C31 108.6(4) . . ?
C34 C35 C40 127.1(4) . . ?
C31 C35 C40 124.2(4) . . ?
C34 C35 Ti3 72.4(2) . . ?
C31 C35 Ti3 73.5(2) . . ?
C40 C35 Ti3 122.4(3) . . ?
Ti1 N1 Ti3 94.67(14) . . ?
Ti1 N1 Ti2 94.89(14) . . ?
Ti3 N1 Ti2 93.83(14) . . ?
Ti2 N12 Ti1 92.67(13) . . ?
Ti2 N12 Zr1 94.19(14) . . ?
Ti1 N12 Zr1 94.33(12) . . ?
Ti1 N13 Ti3 92.40(14) . . ?
Ti1 N13 Zr1 95.29(13) . . ?
Ti3 N13 Zr1 94.17(13) . . ?
Ti2 N23 Ti3 92.58(13) . . ?
Ti2 N23 Zr1 95.44(13) . . ?
Ti3 N23 Zr1 94.67(13) . . ?
N1 Ti1 N13 86.69(14) . . ?
N1 Ti1 N12 86.32(13) . . ?
N13 Ti1 N12 93.06(13) . . ?
N1 Ti1 C11 110.59(16) . . ?
N13 Ti1 C11 152.17(14) . . ?
N12 Ti1 C11 109.18(15) . . ?
N1 Ti1 C15 100.74(15) . . ?
N13 Ti1 C15 122.82(14) . . ?
N12 Ti1 C15 143.55(15) . . ?
C11 Ti1 C15 34.84(15) . . ?
N1 Ti1 C14 123.08(15) . . ?
N13 Ti1 C14 95.05(15) . . ?
N12 Ti1 C14 149.85(15) . . ?
C11 Ti1 C14 57.37(15) . . ?
C15 Ti1 C14 34.69(15) . . ?
N1 Ti1 C12 143.56(16) . . ?
N13 Ti1 C12 129.39(16) . . ?
N12 Ti1 C12 95.34(14) . . ?
C11 Ti1 C12 34.94(16) . . ?
C15 Ti1 C12 58.28(16) . . ?
C14 Ti1 C12 57.62(15) . . ?
N1 Ti1 C13 156.60(15) . . ?
N13 Ti1 C13 98.60(15) . . ?
N12 Ti1 C13 115.92(15) . . ?
C11 Ti1 C13 57.05(16) . . ?
C15 Ti1 C13 57.28(15) . . ?
C14 Ti1 C13 34.06(15) . . ?
C12 Ti1 C13 34.48(15) . . ?
N1 Ti1 Ti3 42.85(10) . . ?
N13 Ti1 Ti3 43.84(10) . . ?
N12 Ti1 Ti3 89.95(10) . . ?
C11 Ti1 Ti3 147.54(13) . . ?
C15 Ti1 Ti3 119.50(12) . . ?
C14 Ti1 Ti3 115.63(11) . . ?
C12 Ti1 Ti3 171.85(11) . . ?
C13 Ti1 Ti3 137.37(12) . . ?
N1 Ti1 Ti2 42.78(9) . . ?
N13 Ti1 Ti2 90.04(10) . . ?
N12 Ti1 Ti2 43.54(9) . . ?
C11 Ti1 Ti2 117.56(11) . . ?
C15 Ti1 Ti2 132.35(11) . . ?
C14 Ti1 Ti2 164.76(12) . . ?
C12 Ti1 Ti2 128.04(10) . . ?
C13 Ti1 Ti2 158.52(12) . . ?
Ti3 Ti1 Ti2 59.75(3) . . ?
N1 Ti1 Zr1 90.47(10) . . ?
N13 Ti1 Zr1 46.40(9) . . ?
N12 Ti1 Zr1 47.16(9) . . ?
C11 Ti1 Zr1 148.55(13) . . ?
C15 Ti1 Zr1 164.38(11) . . ?
C14 Ti1 Zr1 129.70(12) . . ?
C12 Ti1 Zr1 117.07(12) . . ?
C13 Ti1 Zr1 109.73(11) . . ?
Ti2 Ti1 Zr1 63.00(4) . . ?
N1 Ti2 N23 86.80(13) . . ?
N1 Ti2 N12 86.12(13) . . ?
N23 Ti2 N12 93.17(14) . . ?
N1 Ti2 C24 98.45(13) . . ?
N23 Ti2 C24 144.02(15) . . ?
N12 Ti2 C24 122.60(15) . . ?
N1 Ti2 C25 121.52(14) . . ?
N23 Ti2 C25 150.77(14) . . ?
N12 Ti2 C25 95.69(14) . . ?
C24 Ti2 C25 34.85(13) . . ?
N1 Ti2 C23 107.83(14) . . ?
N23 Ti2 C23 109.61(15) . . ?
N12 Ti2 C23 153.52(14) . . ?
C24 Ti2 C23 34.93(14) . . ?
C25 Ti2 C23 57.85(14) . . ?
N1 Ti2 C22 141.21(14) . . ?
N23 Ti2 C22 96.30(14) . . ?
N12 Ti2 C22 132.01(14) . . ?
C24 Ti2 C22 58.12(14) . . ?
C25 Ti2 C22 57.68(15) . . ?
C23 Ti2 C22 35.06(14) . . ?
N1 Ti2 C21 154.87(14) . . ?
N23 Ti2 C21 116.58(14) . . ?
N12 Ti2 C21 100.76(13) . . ?
C24 Ti2 C21 57.43(13) . . ?
C25 Ti2 C21 34.29(14) . . ?
C23 Ti2 C21 57.44(14) . . ?
C22 Ti2 C21 34.39(14) . . ?
N1 Ti2 Ti3 43.05(10) . . ?
N23 Ti2 Ti3 43.76(9) . . ?
N12 Ti2 Ti3 90.34(10) . . ?
C24 Ti2 Ti3 130.25(10) . . ?
C25 Ti2 Ti3 163.11(10) . . ?
C23 Ti2 Ti3 115.34(10) . . ?
C22 Ti2 Ti3 127.26(11) . . ?
C21 Ti2 Ti3 158.52(11) . . ?
N1 Ti2 Ti1 42.33(10) . . ?
N23 Ti2 Ti1 90.16(10) . . ?
N12 Ti2 Ti1 43.79(9) . . ?
C24 Ti2 Ti1 117.51(10) . . ?
C25 Ti2 Ti1 115.21(11) . . ?
C23 Ti2 Ti1 144.59(11) . . ?
C22 Ti2 Ti1 172.70(11) . . ?
C21 Ti2 Ti1 138.79(11) . . ?
Ti3 Ti2 Ti1 60.00(3) . . ?
N1 Ti2 Zr1 90.45(10) . . ?
N23 Ti2 Zr1 46.33(9) . . ?
N12 Ti2 Zr1 47.36(10) . . ?
C24 Ti2 Zr1 166.34(11) . . ?
C25 Ti2 Zr1 131.53(10) . . ?
C23 Ti2 Zr1 149.98(11) . . ?
C22 Ti2 Zr1 119.30(10) . . ?
C21 Ti2 Zr1 112.08(10) . . ?
Ti3 Ti2 Zr1 62.89(3) . . ?
Ti1 Ti2 Zr1 63.34(3) . . ?
N1 Ti3 N23 86.77(13) . . ?
N1 Ti3 N13 86.23(14) . . ?
N23 Ti3 N13 93.12(13) . . ?
N1 Ti3 C34 99.91(15) . . ?
N23 Ti3 C34 124.72(16) . . ?
N13 Ti3 C34 141.77(16) . . ?
N1 Ti3 C33 110.80(14) . . ?
N23 Ti3 C33 153.20(15) . . ?
N13 Ti3 C33 107.64(15) . . ?
C34 Ti3 C33 34.92(15) . . ?
N1 Ti3 C35 121.41(15) . . ?
N23 Ti3 C35 96.33(14) . . ?
N13 Ti3 C35 151.14(14) . . ?
C34 Ti3 C35 34.59(15) . . ?
C33 Ti3 C35 57.47(15) . . ?
N1 Ti3 C32 144.25(14) . . ?
N23 Ti3 C32 128.57(15) . . ?
N13 Ti3 C32 95.75(14) . . ?
C34 Ti3 C32 58.02(15) . . ?
C33 Ti3 C32 34.85(15) . . ?
C35 Ti3 C32 57.41(14) . . ?
N1 Ti3 C31 155.52(14) . . ?
N23 Ti3 C31 98.41(14) . . ?
N13 Ti3 C31 117.13(14) . . ?
C34 Ti3 C31 57.55(14) . . ?
C33 Ti3 C31 57.31(14) . . ?
C35 Ti3 C31 34.44(14) . . ?
C32 Ti3 C31 34.28(14) . . ?
N1 Ti3 Ti2 43.12(9) . . ?
N23 Ti3 Ti2 43.66(10) . . ?
N13 Ti3 Ti2 90.39(10) . . ?
C34 Ti3 Ti2 119.77(12) . . ?
C33 Ti3 Ti2 148.36(12) . . ?
C35 Ti3 Ti2 115.02(11) . . ?
C32 Ti3 Ti2 170.60(11) . . ?
C31 Ti3 Ti2 136.32(10) . . ?
N1 Ti3 Ti1 42.48(10) . . ?
N23 Ti3 Ti1 90.29(10) . . ?
N13 Ti3 Ti1 43.76(10) . . ?
C34 Ti3 Ti1 130.27(12) . . ?
C33 Ti3 Ti1 116.40(11) . . ?
C35 Ti3 Ti1 162.36(11) . . ?
C32 Ti3 Ti1 128.76(11) . . ?
C31 Ti3 Ti1 159.80(10) . . ?
Ti2 Ti3 Ti1 60.25(3) . . ?
N1 Ti3 Zr1 90.99(10) . . ?
N23 Ti3 Zr1 46.72(10) . . ?
N13 Ti3 Zr1 47.01(9) . . ?
C34 Ti3 Zr1 166.04(12) . . ?
C33 Ti3 Zr1 146.69(12) . . ?
C35 Ti3 Zr1 131.55(11) . . ?
C32 Ti3 Zr1 116.26(11) . . ?
C31 Ti3 Zr1 110.02(10) . . ?
Ti2 Ti3 Zr1 63.50(4) . . ?
N23 Zr1 N13 76.98(11) . . ?
N23 Zr1 N12 76.30(12) . . ?
N13 Zr1 N12 76.43(11) . . ?
N23 Zr1 Cl3 97.25(9) . . ?
N13 Zr1 Cl3 88.46(9) . . ?
N12 Zr1 Cl3 164.52(8) . . ?
N23 Zr1 Cl2 164.47(9) . . ?
N13 Zr1 Cl2 97.26(9) . . ?
N12 Zr1 Cl2 88.37(9) . . ?
Cl3 Zr1 Cl2 96.99(6) . . ?
N23 Zr1 Cl1 89.65(8) . . ?
N13 Zr1 Cl1 165.95(9) . . ?
N12 Zr1 Cl1 96.42(8) . . ?
Cl3 Zr1 Cl1 97.60(5) . . ?
Cl2 Zr1 Cl1 94.58(5) . . ?
N23 Zr1 Ti3 38.61(8) . . ?
N13 Zr1 Ti3 38.82(8) . . ?
N12 Zr1 Ti3 77.05(8) . . ?
Cl3 Zr1 Ti3 89.10(4) . . ?
Cl2 Zr1 Ti3 135.66(4) . . ?
Cl1 Zr1 Ti3 128.20(4) . . ?
N23 Zr1 Ti2 38.23(8) . . ?
N13 Zr1 Ti2 77.16(8) . . ?
N12 Zr1 Ti2 38.45(8) . . ?
Cl3 Zr1 Ti2 135.04(4) . . ?
Cl2 Zr1 Ti2 126.70(4) . . ?
Cl1 Zr1 Ti2 89.70(4) . . ?
Ti3 Zr1 Ti2 53.61(3) . . ?
N23 Zr1 Ti1 77.03(8) . . ?
N13 Zr1 Ti1 38.30(8) . . ?
N12 Zr1 Ti1 38.51(8) . . ?
Cl3 Zr1 Ti1 126.69(4) . . ?
Cl2 Zr1 Ti1 89.48(4) . . ?
Cl1 Zr1 Ti1 134.69(4) . . ?
Ti3 Zr1 Ti1 53.67(2) . . ?
Ti2 Zr1 Ti1 53.66(3) . . ?
_exptl_crystal_recrystallization_method 
'Slow diffusion of tetrahydrofuran and toluene solutions of starting materials.'
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_8
_database_code_depnum_ccdc_archive 'CCDC 1415002'
_audit_update_record             
;
2015-08-26 deposited with the CCDC.
2015-09-16 downloaded from the CCDC.
;

_audit_creation_date             2014-02-14T15:53:31-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

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

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C36 H63 N5 Si2 Ti4'
_chemical_formula_sum            'C36 H63 N5 Si2 Ti4'
_chemical_formula_weight         813.69
_chemical_compound_source        'synthesis as described'

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2



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

_cell_length_a                   11.5966(6)
_cell_length_b                   11.7721(5)
_cell_length_c                   17.3188(19)
_cell_angle_alpha                81.304(5)
_cell_angle_beta                 87.722(6)
_cell_angle_gamma                66.101(4)
_cell_volume                     2136.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    126
_cell_measurement_theta_min      3
_cell_measurement_theta_max      27
_cell_measurement_wavelength     0.71073

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

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.16
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             860
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-7 -4 -5 0.143
-1 0 6 0.254
3 2 4 0.226
1 0 -13 0.199
16 7 -8 0.359
3 -19 -1 0.075
-2 16 1 0.075

_exptl_special_details           
;
 ?
;

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

_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_T_max  0.906

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

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_number            44784
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_full        27.5
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             9792
_reflns_number_gt                7022
_reflns_threshold_expression     >2σ(I)
_diffrn_reflns_reduction_process 
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

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

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

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

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

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

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0739P)²+1.2527P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         9792
_refine_ls_number_parameters     445
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0493
_refine_ls_wR_factor_ref         0.1389
_refine_ls_wR_factor_gt          0.1242
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.084

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

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7449(4) -0.0910(5) 0.0869(3) 0.0728(13) Uani 1 1 d . . .
H1A H 0.7092 -0.0059 0.0576 0.109 Uiso 1 1 calc R . .
H1B H 0.7489 -0.1515 0.0527 0.109 Uiso 1 1 calc R . .
H1C H 0.8301 -0.1099 0.106 0.109 Uiso 1 1 calc R . .
C2 C 0.7037(5) -0.2683(4) 0.2206(3) 0.0753(13) Uani 1 1 d . . .
H2A H 0.7929 -0.2969 0.2352 0.113 Uiso 1 1 calc R . .
H2B H 0.6949 -0.3212 0.1846 0.113 Uiso 1 1 calc R . .
H2C H 0.6552 -0.2744 0.2675 0.113 Uiso 1 1 calc R . .
C3 C 0.4845(4) -0.0637(4) 0.1295(3) 0.0751(15) Uani 1 1 d . . .
H3A H 0.4278 -0.0713 0.1716 0.113 Uiso 1 1 calc R . .
H3B H 0.4915 -0.1221 0.093 0.113 Uiso 1 1 calc R . .
H3C H 0.4506 0.0225 0.1017 0.113 Uiso 1 1 calc R . .
C4 C 0.9140(4) -0.1520(5) 0.2770(4) 0.111(2) Uani 1 1 d . . .
H4A H 0.8912 -0.2218 0.2987 0.166 Uiso 1 1 calc R . .
H4B H 0.9798 -0.1506 0.3102 0.166 Uiso 1 1 calc R . .
H4C H 0.9455 -0.1629 0.2241 0.166 Uiso 1 1 calc R . .
C5 C 0.8074(4) 0.1313(5) 0.2241(3) 0.0751(14) Uani 1 1 d . . .
H5A H 0.8283 0.1201 0.1696 0.113 Uiso 1 1 calc R . .
H5B H 0.8792 0.1337 0.2507 0.113 Uiso 1 1 calc R . .
H5C H 0.7335 0.2103 0.2257 0.113 Uiso 1 1 calc R . .
C6 C 0.7399(5) 0.0234(5) 0.3788(2) 0.0756(14) Uani 1 1 d . . .
H6A H 0.6603 0.0964 0.3817 0.113 Uiso 1 1 calc R . .
H6B H 0.8088 0.0377 0.4006 0.113 Uiso 1 1 calc R . .
H6C H 0.7339 -0.0515 0.4089 0.113 Uiso 1 1 calc R . .
C11 C 0.4409(3) 0.4952(3) 0.11325(16) 0.0317(6) Uani 1 1 d . . .
C12 C 0.4326(3) 0.4048(3) 0.07069(16) 0.0298(6) Uani 1 1 d . . .
C13 C 0.3034(3) 0.4372(3) 0.05431(15) 0.0300(6) Uani 1 1 d . . .
C14 C 0.2321(3) 0.5479(3) 0.08645(16) 0.0320(6) Uani 1 1 d . . .
C15 C 0.3161(3) 0.5839(3) 0.12301(17) 0.0324(6) Uani 1 1 d . . .
C16 C 0.5608(3) 0.4969(3) 0.1398(2) 0.0466(9) Uani 1 1 d . . .
H16A H 0.5436 0.5786 0.1556 0.07 Uiso 1 1 calc R . .
H16B H 0.6204 0.4829 0.0969 0.07 Uiso 1 1 calc R . .
H16C H 0.5973 0.4304 0.1842 0.07 Uiso 1 1 calc R . .
C17 C 0.5419(3) 0.2922(3) 0.0484(2) 0.0474(9) Uani 1 1 d . . .
H17A H 0.5117 0.2294 0.0378 0.071 Uiso 1 1 calc R . .
H17B H 0.6045 0.2559 0.0914 0.071 Uiso 1 1 calc R . .
H17C H 0.5807 0.318 0.0015 0.071 Uiso 1 1 calc R . .
C18 C 0.2526(4) 0.3666(3) 0.00961(18) 0.0442(8) Uani 1 1 d . . .
H18A H 0.2734 0.378 -0.0456 0.066 Uiso 1 1 calc R . .
H18B H 0.1608 0.3987 0.0145 0.066 Uiso 1 1 calc R . .
H18C H 0.2905 0.277 0.0309 0.066 Uiso 1 1 calc R . .
C19 C 0.0908(3) 0.6228(3) 0.0794(2) 0.0518(9) Uani 1 1 d . . .
H19A H 0.0723 0.702 0.0445 0.078 Uiso 1 1 calc R . .
H19B H 0.0572 0.6406 0.1312 0.078 Uiso 1 1 calc R . .
H19C H 0.0513 0.5743 0.0582 0.078 Uiso 1 1 calc R . .
C20 C 0.2786(4) 0.7017(3) 0.1591(2) 0.0511(9) Uani 1 1 d . . .
H20A H 0.3524 0.7012 0.1851 0.077 Uiso 1 1 calc R . .
H20B H 0.2132 0.7057 0.1976 0.077 Uiso 1 1 calc R . .
H20C H 0.2457 0.775 0.1183 0.077 Uiso 1 1 calc R . .
C21 C 0.0054(3) 0.2830(3) 0.30701(17) 0.0308(6) Uani 1 1 d . . .
C22 C 0.0164(2) 0.2807(3) 0.22540(17) 0.0288(6) Uani 1 1 d . . .
C23 C 0.0965(3) 0.1567(3) 0.21348(17) 0.0300(6) Uani 1 1 d . . .
C24 C 0.1349(3) 0.0826(3) 0.28768(17) 0.0302(6) Uani 1 1 d . . .
C25 C 0.0778(3) 0.1611(3) 0.34529(17) 0.0316(6) Uani 1 1 d . . .
C26 C -0.0743(3) 0.3954(3) 0.3448(2) 0.0508(9) Uani 1 1 d . . .
H26A H -0.0602 0.3748 0.4015 0.076 Uiso 1 1 calc R . .
H26B H -0.1635 0.4191 0.3324 0.076 Uiso 1 1 calc R . .
H26C H -0.0511 0.4656 0.325 0.076 Uiso 1 1 calc R . .
C27 C -0.0514(3) 0.3883(3) 0.1625(2) 0.0491(9) Uani 1 1 d . . .
H27A H -0.1345 0.3898 0.1519 0.074 Uiso 1 1 calc R . .
H27B H -0.0022 0.3779 0.1148 0.074 Uiso 1 1 calc R . .
H27C H -0.062 0.4674 0.1798 0.074 Uiso 1 1 calc R . .
C28 C 0.1261(3) 0.1125(4) 0.13514(19) 0.0455(8) Uani 1 1 d . . .
H28A H 0.1893 0.0256 0.1419 0.068 Uiso 1 1 calc R . .
H28B H 0.1592 0.1664 0.1013 0.068 Uiso 1 1 calc R . .
H28C H 0.049 0.1167 0.1112 0.068 Uiso 1 1 calc R . .
C29 C 0.2179(4) -0.0551(3) 0.3033(2) 0.0533(10) Uani 1 1 d . . .
H29A H 0.2358 -0.0893 0.2538 0.08 Uiso 1 1 calc R . .
H29B H 0.175 -0.0987 0.3379 0.08 Uiso 1 1 calc R . .
H29C H 0.2973 -0.0673 0.3283 0.08 Uiso 1 1 calc R . .
C30 C 0.0907(4) 0.1167(4) 0.43165(19) 0.0533(10) Uani 1 1 d . . .
H30A H 0.059 0.1895 0.4597 0.08 Uiso 1 1 calc R . .
H30B H 0.1798 0.0659 0.4459 0.08 Uiso 1 1 calc R . .
H30C H 0.0418 0.0658 0.4458 0.08 Uiso 1 1 calc R . .
C31 C 0.2994(3) 0.3792(3) 0.47993(16) 0.0306(6) Uani 1 1 d . . .
C32 C 0.4288(3) 0.2986(3) 0.48787(16) 0.0330(7) Uani 1 1 d . . .
C33 C 0.4953(3) 0.3637(3) 0.44366(17) 0.0375(7) Uani 1 1 d . . .
C34 C 0.4068(3) 0.4818(3) 0.40877(17) 0.0363(7) Uani 1 1 d . . .
C35 C 0.2851(3) 0.4918(3) 0.43140(16) 0.0334(7) Uani 1 1 d . . .
C36 C 0.1942(4) 0.3503(4) 0.5186(2) 0.0509(9) Uani 1 1 d . . .
H36A H 0.1823 0.3746 0.571 0.076 Uiso 1 1 calc R . .
H36B H 0.2156 0.26 0.5227 0.076 Uiso 1 1 calc R . .
H36C H 0.1162 0.3973 0.4874 0.076 Uiso 1 1 calc R . .
C37 C 0.4838(4) 0.1717(3) 0.5367(2) 0.0526(9) Uani 1 1 d . . .
H37A H 0.4601 0.1795 0.5912 0.079 Uiso 1 1 calc R . .
H37B H 0.576 0.1368 0.5333 0.079 Uiso 1 1 calc R . .
H37C H 0.4515 0.1158 0.5175 0.079 Uiso 1 1 calc R . .
C38 C 0.6361(3) 0.3213(5) 0.4385(2) 0.0643(12) Uani 1 1 d . . .
H38A H 0.6606 0.3154 0.3839 0.096 Uiso 1 1 calc R . .
H38B H 0.6779 0.2388 0.4703 0.096 Uiso 1 1 calc R . .
H38C H 0.6613 0.3822 0.4578 0.096 Uiso 1 1 calc R . .
C39 C 0.4395(5) 0.5806(4) 0.3604(2) 0.0647(12) Uani 1 1 d . . .
H39A H 0.3629 0.6468 0.3348 0.097 Uiso 1 1 calc R . .
H39B H 0.4998 0.543 0.3207 0.097 Uiso 1 1 calc R . .
H39C H 0.4773 0.6167 0.3941 0.097 Uiso 1 1 calc R . .
C40 C 0.1641(4) 0.6031(3) 0.4088(2) 0.0546(10) Uani 1 1 d . . .
H40A H 0.143 0.6585 0.4489 0.082 Uiso 1 1 calc R . .
H40B H 0.0964 0.5748 0.4041 0.082 Uiso 1 1 calc R . .
H40C H 0.1736 0.6491 0.3586 0.082 Uiso 1 1 calc R . .
N1 N 0.2239(2) 0.4008(2) 0.28079(12) 0.0234(5) Uani 1 1 d . . .
N2 N 0.6369(2) -0.0005(2) 0.23533(14) 0.0294(5) Uani 1 1 d . . .
N12 N 0.3359(2) 0.2202(2) 0.19050(12) 0.0214(4) Uani 1 1 d . . .
N13 N 0.4767(2) 0.3032(2) 0.26548(12) 0.0221(4) Uani 1 1 d . . .
N23 N 0.3666(2) 0.1625(2) 0.34601(12) 0.0233(5) Uani 1 1 d . . .
Si1 Si 0.64295(8) -0.10199(8) 0.17186(6) 0.0393(2) Uani 1 1 d . . .
Si2 Si 0.77228(8) -0.00095(9) 0.27338(6) 0.0423(2) Uani 1 1 d . . .
Ti1 Ti 0.33294(4) 0.38671(4) 0.19279(3) 0.02299(12) Uani 1 1 d . . .
Ti2 Ti 0.22004(4) 0.23880(4) 0.27628(3) 0.02326(12) Uani 1 1 d . . .
Ti3 Ti 0.36616(5) 0.32456(5) 0.35448(3) 0.02377(12) Uani 1 1 d . . .
Ti4 Ti 0.47891(4) 0.14224(4) 0.25841(3) 0.02327(12) Uani 1 1 d . . .



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

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 Si1 1.873(4) . ?
C2 Si1 1.864(4) . ?
C3 Si1 1.858(4) . ?
C4 Si2 1.863(4) . ?
C5 Si2 1.845(4) . ?
C6 Si2 1.891(4) . ?
C11 C12 1.418(4) . ?
C11 C15 1.422(4) . ?
C11 C16 1.491(4) . ?
C11 Ti1 2.392(3) . ?
C12 C13 1.418(4) . ?
C12 C17 1.506(4) . ?
C12 Ti1 2.392(3) . ?
C13 C14 1.415(4) . ?
C13 C18 1.505(4) . ?
C13 Ti1 2.386(3) . ?
C14 C15 1.412(4) . ?
C14 C19 1.514(4) . ?
C14 Ti1 2.382(3) . ?
C15 C20 1.502(4) . ?
C15 Ti1 2.385(3) . ?
C21 C25 1.408(4) . ?
C21 C22 1.417(4) . ?
C21 C26 1.502(4) . ?
C21 Ti2 2.384(3) . ?
C22 C23 1.419(4) . ?
C22 C27 1.501(4) . ?
C22 Ti2 2.384(3) . ?
C23 C24 1.415(4) . ?
C23 C28 1.504(4) . ?
C23 Ti2 2.394(3) . ?
C24 C25 1.421(4) . ?
C24 C29 1.500(4) . ?
C24 Ti2 2.397(3) . ?
C25 C30 1.500(4) . ?
C25 Ti2 2.392(3) . ?
C31 C35 1.409(4) . ?
C31 C32 1.412(4) . ?
C31 C36 1.502(4) . ?
C31 Ti3 2.370(3) . ?
C32 C33 1.422(4) . ?
C32 C37 1.497(4) . ?
C32 Ti3 2.387(3) . ?
C33 C34 1.411(5) . ?
C33 C38 1.504(5) . ?
C33 Ti3 2.408(3) . ?
C34 C35 1.412(4) . ?
C34 C39 1.495(5) . ?
C34 Ti3 2.408(3) . ?
C35 C40 1.496(5) . ?
C35 Ti3 2.394(3) . ?
N1 Ti1 1.924(2) . ?
N1 Ti2 1.939(2) . ?
N1 Ti3 1.944(2) . ?
N2 Si1 1.722(2) . ?
N2 Si2 1.724(2) . ?
N2 Ti4 1.998(2) . ?
N12 Ti4 1.890(2) . ?
N12 Ti2 1.940(2) . ?
N12 Ti1 1.953(2) . ?
N13 Ti4 1.907(2) . ?
N13 Ti3 1.944(2) . ?
N13 Ti1 1.948(2) . ?
N23 Ti3 1.934(2) . ?
N23 Ti2 1.937(2) . ?
N23 Ti4 1.938(2) . ?
Ti1 Ti4 2.7669(7) . ?
Ti1 Ti3 2.7863(7) . ?
Ti1 Ti2 2.7879(6) . ?
Ti2 Ti4 2.7691(7) . ?
Ti2 Ti3 2.7762(6) . ?
Ti3 Ti4 2.7780(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C12 C11 C15 107.7(3) . . ?
C12 C11 C16 125.0(3) . . ?
C15 C11 C16 127.2(3) . . ?
C12 C11 Ti1 72.75(15) . . ?
C15 C11 Ti1 72.42(16) . . ?
C16 C11 Ti1 122.10(19) . . ?
C13 C12 C11 108.2(3) . . ?
C13 C12 C17 125.9(3) . . ?
C11 C12 C17 125.9(3) . . ?
C13 C12 Ti1 72.50(16) . . ?
C11 C12 Ti1 72.77(15) . . ?
C17 C12 Ti1 119.50(19) . . ?
C14 C13 C12 107.7(2) . . ?
C14 C13 C18 126.6(3) . . ?
C12 C13 C18 125.7(3) . . ?
C14 C13 Ti1 72.61(16) . . ?
C12 C13 Ti1 72.98(15) . . ?
C18 C13 Ti1 120.78(19) . . ?
C15 C14 C13 108.5(3) . . ?
C15 C14 C19 124.2(3) . . ?
C13 C14 C19 127.2(3) . . ?
C15 C14 Ti1 72.88(16) . . ?
C13 C14 Ti1 72.87(16) . . ?
C19 C14 Ti1 123.3(2) . . ?
C14 C15 C11 107.9(3) . . ?
C14 C15 C20 125.1(3) . . ?
C11 C15 C20 126.9(3) . . ?
C14 C15 Ti1 72.66(16) . . ?
C11 C15 Ti1 72.96(16) . . ?
C20 C15 Ti1 124.1(2) . . ?
C25 C21 C22 108.0(3) . . ?
C25 C21 C26 126.7(3) . . ?
C22 C21 C26 125.3(3) . . ?
C25 C21 Ti2 73.19(16) . . ?
C22 C21 Ti2 72.73(15) . . ?
C26 C21 Ti2 121.7(2) . . ?
C21 C22 C23 108.0(2) . . ?
C21 C22 C27 126.0(3) . . ?
C23 C22 C27 125.8(3) . . ?
C21 C22 Ti2 72.68(15) . . ?
C23 C22 Ti2 73.11(15) . . ?
C27 C22 Ti2 123.1(2) . . ?
C24 C23 C22 107.9(3) . . ?
C24 C23 C28 127.0(3) . . ?
C22 C23 C28 125.0(3) . . ?
C24 C23 Ti2 72.92(15) . . ?
C22 C23 Ti2 72.34(15) . . ?
C28 C23 Ti2 123.78(19) . . ?
C23 C24 C25 107.8(3) . . ?
C23 C24 C29 126.4(3) . . ?
C25 C24 C29 125.8(3) . . ?
C23 C24 Ti2 72.72(15) . . ?
C25 C24 Ti2 72.57(15) . . ?
C29 C24 Ti2 121.6(2) . . ?
C21 C25 C24 108.3(3) . . ?
C21 C25 C30 127.3(3) . . ?
C24 C25 C30 124.4(3) . . ?
C21 C25 Ti2 72.52(15) . . ?
C24 C25 Ti2 72.91(15) . . ?
C30 C25 Ti2 122.3(2) . . ?
C35 C31 C32 109.2(3) . . ?
C35 C31 C36 125.5(3) . . ?
C32 C31 C36 125.2(3) . . ?
C35 C31 Ti3 73.69(16) . . ?
C32 C31 Ti3 73.37(16) . . ?
C36 C31 Ti3 120.3(2) . . ?
C31 C32 C33 106.8(3) . . ?
C31 C32 C37 125.9(3) . . ?
C33 C32 C37 127.3(3) . . ?
C31 C32 Ti3 72.10(16) . . ?
C33 C32 Ti3 73.56(16) . . ?
C37 C32 Ti3 121.7(2) . . ?
C34 C33 C32 108.4(3) . . ?
C34 C33 C38 124.3(3) . . ?
C32 C33 C38 127.2(3) . . ?
C34 C33 Ti3 72.98(16) . . ?
C32 C33 Ti3 71.93(16) . . ?
C38 C33 Ti3 124.5(2) . . ?
C33 C34 C35 108.2(3) . . ?
C33 C34 C39 124.9(3) . . ?
C35 C34 C39 126.9(3) . . ?
C33 C34 Ti3 72.94(16) . . ?
C35 C34 Ti3 72.32(16) . . ?
C39 C34 Ti3 123.4(2) . . ?
C31 C35 C34 107.4(3) . . ?
C31 C35 C40 126.8(3) . . ?
C34 C35 C40 125.8(3) . . ?
C31 C35 Ti3 71.90(16) . . ?
C34 C35 Ti3 73.47(16) . . ?
C40 C35 Ti3 121.1(2) . . ?
Ti1 N1 Ti2 92.37(9) . . ?
Ti1 N1 Ti3 92.15(9) . . ?
Ti2 N1 Ti3 91.28(9) . . ?
Si1 N2 Si2 121.53(14) . . ?
Si1 N2 Ti4 123.75(13) . . ?
Si2 N2 Ti4 114.10(12) . . ?
Ti4 N12 Ti2 92.61(9) . . ?
Ti4 N12 Ti1 92.12(9) . . ?
Ti2 N12 Ti1 91.49(9) . . ?
Ti4 N13 Ti3 92.31(9) . . ?
Ti4 N13 Ti1 91.73(9) . . ?
Ti3 N13 Ti1 91.43(9) . . ?
Ti3 N23 Ti2 91.65(9) . . ?
Ti3 N23 Ti4 91.71(9) . . ?
Ti2 N23 Ti4 91.22(9) . . ?
N2 Si1 C3 111.57(15) . . ?
N2 Si1 C2 112.17(18) . . ?
C3 Si1 C2 107.1(2) . . ?
N2 Si1 C1 111.17(17) . . ?
C3 Si1 C1 106.0(2) . . ?
C2 Si1 C1 108.6(2) . . ?
N2 Si2 C5 111.59(16) . . ?
N2 Si2 C4 115.20(19) . . ?
C5 Si2 C4 110.8(3) . . ?
N2 Si2 C6 106.51(18) . . ?
C5 Si2 C6 107.0(2) . . ?
C4 Si2 C6 105.1(3) . . ?
N1 Ti1 N13 88.39(9) . . ?
N1 Ti1 N12 88.04(9) . . ?
N13 Ti1 N12 86.55(9) . . ?
N1 Ti1 C14 111.10(10) . . ?
N13 Ti1 C14 147.90(9) . . ?
N12 Ti1 C14 118.19(10) . . ?
N1 Ti1 C15 113.89(10) . . ?
N13 Ti1 C15 114.83(10) . . ?
N12 Ti1 C15 148.65(10) . . ?
C14 Ti1 C15 34.46(10) . . ?
N1 Ti1 C13 135.48(10) . . ?
N13 Ti1 C13 136.01(10) . . ?
N12 Ti1 C13 91.18(9) . . ?
C14 Ti1 C13 34.52(10) . . ?
C15 Ti1 C13 57.48(10) . . ?
N1 Ti1 C12 168.34(10) . . ?
N13 Ti1 C12 102.26(10) . . ?
N12 Ti1 C12 97.24(9) . . ?
C14 Ti1 C12 57.24(10) . . ?
C15 Ti1 C12 57.38(10) . . ?
C13 Ti1 C12 34.52(10) . . ?
N1 Ti1 C11 142.17(10) . . ?
N13 Ti1 C11 91.47(9) . . ?
N12 Ti1 C11 129.72(10) . . ?
C14 Ti1 C11 57.34(10) . . ?
C15 Ti1 C11 34.62(10) . . ?
C13 Ti1 C11 57.47(10) . . ?
C12 Ti1 C11 34.48(10) . . ?
N1 Ti1 Ti4 88.79(7) . . ?
N13 Ti1 Ti4 43.55(6) . . ?
N12 Ti1 Ti4 43.03(6) . . ?
C14 Ti1 Ti4 153.86(8) . . ?
C15 Ti1 Ti4 150.25(8) . . ?
C13 Ti1 Ti4 119.39(7) . . ?
C12 Ti1 Ti4 102.18(7) . . ?
C11 Ti1 Ti4 116.22(8) . . ?
N1 Ti1 Ti3 44.20(7) . . ?
N13 Ti1 Ti3 44.24(6) . . ?
N12 Ti1 Ti3 87.92(6) . . ?
C14 Ti1 Ti3 146.02(8) . . ?
C15 Ti1 Ti3 123.43(7) . . ?
C13 Ti1 Ti3 179.04(7) . . ?
C12 Ti1 Ti3 145.94(7) . . ?
C11 Ti1 Ti3 123.41(7) . . ?
Ti4 Ti1 Ti3 60.033(18) . . ?
N1 Ti1 Ti2 44.02(6) . . ?
N13 Ti1 Ti2 88.12(6) . . ?
N12 Ti1 Ti2 44.07(6) . . ?
C14 Ti1 Ti2 123.74(7) . . ?
C15 Ti1 Ti2 149.84(8) . . ?
C13 Ti1 Ti2 119.35(7) . . ?
C12 Ti1 Ti2 139.77(7) . . ?
C11 Ti1 Ti2 173.79(8) . . ?
Ti4 Ti1 Ti2 59.800(17) . . ?
Ti3 Ti1 Ti2 59.742(17) . . ?
N23 Ti2 N1 88.50(9) . . ?
N23 Ti2 N12 87.36(9) . . ?
N1 Ti2 N12 88.00(9) . . ?
N23 Ti2 C21 128.16(10) . . ?
N1 Ti2 C21 100.46(10) . . ?
N12 Ti2 C21 143.27(10) . . ?
N23 Ti2 C22 158.08(9) . . ?
N1 Ti2 C22 106.39(10) . . ?
N12 Ti2 C22 108.71(9) . . ?
C21 Ti2 C22 34.59(10) . . ?
N23 Ti2 C25 101.16(10) . . ?
N1 Ti2 C25 125.37(10) . . ?
N12 Ti2 C25 145.35(10) . . ?
C21 Ti2 C25 34.29(10) . . ?
C22 Ti2 C25 57.16(10) . . ?
N23 Ti2 C23 133.54(10) . . ?
N1 Ti2 C23 137.95(10) . . ?
N12 Ti2 C23 92.68(9) . . ?
C21 Ti2 C23 57.43(10) . . ?
C22 Ti2 C23 34.55(10) . . ?
C25 Ti2 C23 57.19(10) . . ?
N23 Ti2 C24 103.60(9) . . ?
N1 Ti2 C24 157.72(10) . . ?
N12 Ti2 C24 110.88(10) . . ?
C21 Ti2 C24 57.34(10) . . ?
C22 Ti2 C24 57.29(10) . . ?
C25 Ti2 C24 34.52(10) . . ?
C23 Ti2 C24 34.36(10) . . ?
N23 Ti2 Ti4 44.40(6) . . ?
N1 Ti2 Ti4 88.44(7) . . ?
N12 Ti2 Ti4 42.97(6) . . ?
C21 Ti2 Ti4 168.71(8) . . ?
C22 Ti2 Ti4 148.62(7) . . ?
C25 Ti2 Ti4 134.41(8) . . ?
C23 Ti2 Ti4 119.46(7) . . ?
C24 Ti2 Ti4 113.35(7) . . ?
N23 Ti2 Ti3 44.13(6) . . ?
N1 Ti2 Ti3 44.43(7) . . ?
N12 Ti2 Ti3 88.46(6) . . ?
C21 Ti2 Ti3 122.40(7) . . ?
C22 Ti2 Ti3 146.87(7) . . ?
C25 Ti2 Ti3 120.96(7) . . ?
C23 Ti2 Ti3 177.37(7) . . ?
C24 Ti2 Ti3 143.04(7) . . ?
Ti4 Ti2 Ti3 60.129(17) . . ?
N23 Ti2 Ti1 88.76(6) . . ?
N1 Ti2 Ti1 43.61(6) . . ?
N12 Ti2 Ti1 44.44(6) . . ?
C21 Ti2 Ti1 131.55(8) . . ?
C22 Ti2 Ti1 113.13(7) . . ?
C25 Ti2 Ti1 165.56(8) . . ?
C23 Ti2 Ti1 122.21(7) . . ?
C24 Ti2 Ti1 152.61(8) . . ?
Ti4 Ti2 Ti1 59.724(17) . . ?
Ti3 Ti2 Ti1 60.101(17) . . ?
N23 Ti3 N1 88.46(9) . . ?
N23 Ti3 N13 87.51(9) . . ?
N1 Ti3 N13 87.93(9) . . ?
N23 Ti3 C31 110.26(10) . . ?
N1 Ti3 C31 109.81(10) . . ?
N13 Ti3 C31 154.62(10) . . ?
N23 Ti3 C32 102.23(10) . . ?
N1 Ti3 C32 144.31(10) . . ?
N13 Ti3 C32 126.02(10) . . ?
C31 Ti3 C32 34.53(10) . . ?
N23 Ti3 C35 142.03(10) . . ?
N1 Ti3 C35 93.43(10) . . ?
N13 Ti3 C35 130.44(10) . . ?
C31 Ti3 C35 34.41(10) . . ?
C32 Ti3 C35 57.53(10) . . ?
N23 Ti3 C33 125.72(11) . . ?
N1 Ti3 C33 145.32(11) . . ?
N13 Ti3 C33 98.22(10) . . ?
C31 Ti3 C33 56.85(10) . . ?
C32 Ti3 C33 34.50(11) . . ?
C35 Ti3 C33 56.88(11) . . ?
N23 Ti3 C34 158.83(10) . . ?
N1 Ti3 C34 111.25(11) . . ?
N13 Ti3 C34 100.40(10) . . ?
C31 Ti3 C34 56.84(10) . . ?
C32 Ti3 C34 57.27(10) . . ?
C35 Ti3 C34 34.21(11) . . ?
C33 Ti3 C34 34.08(11) . . ?
N23 Ti3 Ti2 44.23(6) . . ?
N1 Ti3 Ti2 44.29(6) . . ?
N13 Ti3 Ti2 88.52(6) . . ?
C31 Ti3 Ti2 116.86(7) . . ?
C32 Ti3 Ti2 134.24(8) . . ?
C35 Ti3 Ti2 125.00(8) . . ?
C33 Ti3 Ti2 167.96(9) . . ?
C34 Ti3 Ti2 154.11(9) . . ?
N23 Ti3 Ti4 44.20(6) . . ?
N1 Ti3 Ti4 88.08(6) . . ?
N13 Ti3 Ti4 43.31(6) . . ?
C31 Ti3 Ti4 149.90(8) . . ?
C32 Ti3 Ti4 123.22(8) . . ?
C35 Ti3 Ti4 173.57(8) . . ?
C33 Ti3 Ti4 119.50(8) . . ?
C34 Ti3 Ti4 139.71(8) . . ?
Ti2 Ti3 Ti4 59.808(17) . . ?
N23 Ti3 Ti1 88.88(6) . . ?
N1 Ti3 Ti1 43.65(6) . . ?
N13 Ti3 Ti1 44.34(6) . . ?
C31 Ti3 Ti1 148.37(8) . . ?
C32 Ti3 Ti1 165.56(8) . . ?
C35 Ti3 Ti1 117.85(7) . . ?
C33 Ti3 Ti1 131.07(8) . . ?
C34 Ti3 Ti1 110.55(7) . . ?
Ti2 Ti3 Ti1 60.157(17) . . ?
Ti4 Ti3 Ti1 59.638(18) . . ?
N12 Ti4 N13 89.54(9) . . ?
N12 Ti4 N23 88.78(9) . . ?
N13 Ti4 N23 88.46(9) . . ?
N12 Ti4 N2 124.10(9) . . ?
N13 Ti4 N2 121.52(9) . . ?
N23 Ti4 N2 132.16(10) . . ?
N12 Ti4 Ti1 44.85(6) . . ?
N13 Ti4 Ti1 44.72(7) . . ?
N23 Ti4 Ti1 89.36(7) . . ?
N2 Ti4 Ti1 138.42(7) . . ?
N12 Ti4 Ti2 44.41(6) . . ?
N13 Ti4 Ti2 89.48(7) . . ?
N23 Ti4 Ti2 44.38(6) . . ?
N2 Ti4 Ti2 148.66(7) . . ?
Ti1 Ti4 Ti2 60.475(17) . . ?
N12 Ti4 Ti3 89.42(7) . . ?
N13 Ti4 Ti3 44.38(6) . . ?
N23 Ti4 Ti3 44.09(6) . . ?
N2 Ti4 Ti3 145.87(7) . . ?
Ti1 Ti4 Ti3 60.329(18) . . ?
Ti2 Ti4 Ti3 60.063(17) . . ?
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Toluene'
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_13
_database_code_depnum_ccdc_archive 'CCDC 1415003'
_audit_update_record             
;
2015-08-26 deposited with the CCDC.
2015-09-16 downloaded from the CCDC.
;

_audit_creation_date             2013-11-08T15:16:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

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

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C40 H56 Cl2 Mg N4 Ti3 Zr, C7 H8'
_chemical_formula_sum            'C47 H64 Cl2 Mg N4 Ti3 Zr'
_chemical_formula_weight         1015.15
_chemical_compound_source        'synthesis as described'

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

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'
_space_group_IT_number           14



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

_cell_length_a                   23.940(5)
_cell_length_b                   18.507(2)
_cell_length_c                   21.328(3)
_cell_angle_alpha                90
_cell_angle_beta                 97.630(10)
_cell_angle_gamma                90
_cell_volume                     9366(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    271
_cell_measurement_theta_min      3
_cell_measurement_theta_max      27
_cell_measurement_wavelength     0.71073

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

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_exptl_crystal_density_diffrn    1.44
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4208
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
10 0 1 0.118
0 0 1 0.138
-16 0 1 0.167
0 0 -1 0.128
0 -4 1 0.17
-1 3 7 0.081
1 2 -7 0.112

_exptl_special_details           
;
 ?
;

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

_exptl_absorpt_coefficient_mu    0.874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_T_max  0.893

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

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.0946
_diffrn_reflns_av_unetI/netI     0.1229
_diffrn_reflns_number            198900
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             21487
_reflns_number_gt                11234
_reflns_threshold_expression     >2sigma(I)
_diffrn_reflns_reduction_process 
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

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

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

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

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 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.
 DFIX and DELU instructions were used for the toluene molecule C110-C116.
;
_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)+(0.0759P)²+0.0000P] 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_number_reflns         21487
_refine_ls_number_parameters     1062
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.1399
_refine_ls_R_factor_gt           0.0547
_refine_ls_wR_factor_ref         0.16
_refine_ls_wR_factor_gt          0.126
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.116

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

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.66803(19) 0.9887(2) 0.3961(2) 0.0421(12) Uani 1 1 d . . .
C12 C 0.71179(18) 0.9371(3) 0.4073(2) 0.0391(12) Uani 1 1 d . . .
C13 C 0.71653(17) 0.9007(2) 0.3501(2) 0.0325(10) Uani 1 1 d . . .
C14 C 0.67484(19) 0.9290(3) 0.3026(2) 0.0387(12) Uani 1 1 d . . .
C15 C 0.64515(19) 0.9838(2) 0.3313(3) 0.0424(12) Uani 1 1 d . . .
C16 C 0.6531(2) 1.0458(3) 0.4412(3) 0.0657(17) Uani 1 1 d . . .
H16A H 0.6158 1.037 0.4515 0.099 Uiso 1 1 calc R . .
H16B H 0.6543 1.0925 0.4218 0.099 Uiso 1 1 calc R . .
H16C H 0.6795 1.0444 0.4792 0.099 Uiso 1 1 calc R . .
C17 C 0.7528(2) 0.9275(4) 0.4666(3) 0.0657(18) Uani 1 1 d . . .
H17A H 0.7477 0.8805 0.4841 0.099 Uiso 1 1 calc R . .
H17B H 0.7461 0.9639 0.4968 0.099 Uiso 1 1 calc R . .
H17C H 0.7906 0.9319 0.4567 0.099 Uiso 1 1 calc R . .
C18 C 0.76247(19) 0.8492(3) 0.3415(3) 0.0519(14) Uani 1 1 d . . .
H18A H 0.7979 0.8742 0.3473 0.078 Uiso 1 1 calc R . .
H18B H 0.7561 0.8292 0.2996 0.078 Uiso 1 1 calc R . .
H18C H 0.7631 0.8111 0.372 0.078 Uiso 1 1 calc R . .
C19 C 0.6688(2) 0.9097(3) 0.2343(2) 0.0536(14) Uani 1 1 d . . .
H19A H 0.6591 0.8595 0.2293 0.08 Uiso 1 1 calc R . .
H19B H 0.7037 0.9185 0.2182 0.08 Uiso 1 1 calc R . .
H19C H 0.6396 0.9386 0.2115 0.08 Uiso 1 1 calc R . .
C20 C 0.6061(2) 1.0383(3) 0.2970(3) 0.0647(17) Uani 1 1 d . . .
H20A H 0.6277 1.0755 0.2801 0.097 Uiso 1 1 calc R . .
H20B H 0.5831 1.0593 0.3258 0.097 Uiso 1 1 calc R . .
H20C H 0.5824 1.015 0.2631 0.097 Uiso 1 1 calc R . .
C21 C 0.68738(17) 0.6451(2) 0.3780(2) 0.0309(10) Uani 1 1 d . . .
C22 C 0.64724(18) 0.6028(2) 0.4044(2) 0.0314(10) Uani 1 1 d . . .
C23 C 0.60097(17) 0.5899(2) 0.3567(2) 0.0291(10) Uani 1 1 d . . .
C24 C 0.61236(18) 0.6263(2) 0.3014(2) 0.0314(10) Uani 1 1 d . . .
C25 C 0.66619(18) 0.6586(2) 0.3141(2) 0.0299(10) Uani 1 1 d . . .
C26 C 0.74425(18) 0.6650(3) 0.4119(2) 0.0404(12) Uani 1 1 d . . .
H26A H 0.7399 0.7 0.4441 0.061 Uiso 1 1 calc R . .
H26B H 0.7668 0.6851 0.3822 0.061 Uiso 1 1 calc R . .
H26C H 0.7624 0.6226 0.4309 0.061 Uiso 1 1 calc R . .
C27 C 0.6548(2) 0.5735(3) 0.4711(2) 0.0425(12) Uani 1 1 d . . .
H27A H 0.6819 0.535 0.4745 0.064 Uiso 1 1 calc R . .
H27B H 0.6194 0.5555 0.4809 0.064 Uiso 1 1 calc R . .
H27C H 0.6679 0.6113 0.5001 0.064 Uiso 1 1 calc R . .
C28 C 0.55245(19) 0.5411(2) 0.3619(2) 0.0421(12) Uani 1 1 d . . .
H28A H 0.5188 0.5617 0.3395 0.063 Uiso 1 1 calc R . .
H28B H 0.5479 0.535 0.4056 0.063 Uiso 1 1 calc R . .
H28C H 0.5594 0.4949 0.3439 0.063 Uiso 1 1 calc R . .
C29 C 0.5774(2) 0.6251(3) 0.2374(2) 0.0434(12) Uani 1 1 d . . .
H29A H 0.5899 0.5864 0.2127 0.065 Uiso 1 1 calc R . .
H29B H 0.5814 0.6702 0.2163 0.065 Uiso 1 1 calc R . .
H29C H 0.5385 0.6178 0.2424 0.065 Uiso 1 1 calc R . .
C30 C 0.6950(2) 0.6959(3) 0.2652(2) 0.0434(12) Uani 1 1 d . . .
H30A H 0.7331 0.707 0.2826 0.065 Uiso 1 1 calc R . .
H30B H 0.6753 0.7398 0.2525 0.065 Uiso 1 1 calc R . .
H30C H 0.6951 0.6649 0.2292 0.065 Uiso 1 1 calc R . .
C31 C 0.5539(2) 0.8669(3) 0.5698(2) 0.0383(12) Uani 1 1 d . . .
C32 C 0.52964(19) 0.7989(3) 0.57423(19) 0.0373(12) Uani 1 1 d . . .
C33 C 0.5723(2) 0.7465(3) 0.5806(2) 0.0406(12) Uani 1 1 d . . .
C34 C 0.6235(2) 0.7819(3) 0.5817(2) 0.0427(13) Uani 1 1 d . . .
C35 C 0.6135(2) 0.8577(3) 0.5762(2) 0.0429(13) Uani 1 1 d . . .
C36 C 0.5227(3) 0.9370(3) 0.5643(3) 0.0652(17) Uani 1 1 d . . .
H36A H 0.4936 0.935 0.5288 0.098 Uiso 1 1 calc R . .
H36B H 0.5484 0.9754 0.5582 0.098 Uiso 1 1 calc R . .
H36C H 0.5063 0.9455 0.6022 0.098 Uiso 1 1 calc R . .
C37 C 0.4688(2) 0.7871(3) 0.5813(2) 0.0576(15) Uani 1 1 d . . .
H37A H 0.4624 0.8006 0.6233 0.086 Uiso 1 1 calc R . .
H37B H 0.4595 0.737 0.5744 0.086 Uiso 1 1 calc R . .
H37C H 0.4456 0.8161 0.551 0.086 Uiso 1 1 calc R . .
C38 C 0.5644(3) 0.6671(3) 0.5889(3) 0.0648(17) Uani 1 1 d . . .
H38A H 0.6004 0.6435 0.5938 0.097 Uiso 1 1 calc R . .
H38B H 0.5412 0.6481 0.5525 0.097 Uiso 1 1 calc R . .
H38C H 0.5464 0.6588 0.6259 0.097 Uiso 1 1 calc R . .
C39 C 0.6824(2) 0.7481(4) 0.5898(3) 0.0706(19) Uani 1 1 d . . .
H39A H 0.7029 0.7632 0.6294 0.106 Uiso 1 1 calc R . .
H39B H 0.7022 0.7634 0.5558 0.106 Uiso 1 1 calc R . .
H39C H 0.6791 0.6964 0.5892 0.106 Uiso 1 1 calc R . .
C40 C 0.6566(2) 0.9167(4) 0.5807(3) 0.077(2) Uani 1 1 d . . .
H40A H 0.6566 0.9421 0.6199 0.116 Uiso 1 1 calc R . .
H40B H 0.6477 0.9497 0.546 0.116 Uiso 1 1 calc R . .
H40C H 0.6932 0.8962 0.579 0.116 Uiso 1 1 calc R . .
C41 C 0.43406(19) 0.9214(3) 0.3076(2) 0.0416(12) Uani 1 1 d . . .
H41 H 0.4126 0.9415 0.3364 0.05 Uiso 1 1 calc R . .
C42 C 0.48692(19) 0.9444(2) 0.2966(2) 0.0358(11) Uani 1 1 d . . .
H42 H 0.5072 0.9826 0.3169 0.043 Uiso 1 1 calc R . .
C43 C 0.5046(2) 0.9006(3) 0.2500(2) 0.0421(12) Uani 1 1 d . . .
H43 H 0.5387 0.9042 0.2338 0.051 Uiso 1 1 calc R . .
C44 C 0.4619(2) 0.8503(3) 0.2319(2) 0.0507(14) Uani 1 1 d . . .
H44 H 0.4623 0.8147 0.2012 0.061 Uiso 1 1 calc R . .
C45 C 0.4187(2) 0.8631(3) 0.2680(2) 0.0450(13) Uani 1 1 d . . .
H45 H 0.3853 0.8371 0.2661 0.054 Uiso 1 1 calc R . .
C46 C 0.4184(4) 0.6199(5) 0.4987(3) 0.090(3) Uani 1 1 d . . .
H46 H 0.428 0.6358 0.5401 0.108 Uiso 1 1 calc R . .
C47 C 0.4460(3) 0.5712(5) 0.4684(6) 0.101(3) Uani 1 1 d . . .
H47 H 0.4793 0.5485 0.4851 0.121 Uiso 1 1 calc R . .
C48 C 0.4193(4) 0.5603(4) 0.4120(5) 0.090(3) Uani 1 1 d . . .
H48 H 0.4299 0.5272 0.3829 0.108 Uiso 1 1 calc R . .
C49 C 0.3741(3) 0.6038(5) 0.4020(3) 0.088(3) Uani 1 1 d . . .
H49 H 0.3486 0.607 0.3651 0.105 Uiso 1 1 calc R . .
C50 C 0.3726(3) 0.6424(4) 0.4564(5) 0.091(3) Uani 1 1 d . . .
H50 H 0.3461 0.677 0.4636 0.11 Uiso 1 1 calc R . .
Cl1 Cl 0.42667(5) 0.81042(7) 0.42132(6) 0.0409(3) Uani 1 1 d . . .
Cl2 Cl 0.45861(5) 0.69775(6) 0.30254(5) 0.0383(3) Uani 1 1 d . . .
Mg1 Mg 0.45813(6) 0.68123(8) 0.41731(7) 0.0361(4) Uani 1 1 d . . .
N1 N 0.64138(14) 0.78802(19) 0.43803(16) 0.0293(8) Uani 1 1 d . . .
N12 N 0.58740(13) 0.79784(19) 0.32105(16) 0.0281(8) Uani 1 1 d . . .
N13 N 0.55724(13) 0.88212(18) 0.41769(15) 0.0271(8) Uani 1 1 d . . .
H13 H 0.5472 0.9266 0.4306 0.033 Uiso 1 1 calc R . .
N23 N 0.53955(13) 0.72917(19) 0.42257(15) 0.0277(8) Uani 1 1 d . . .
Ti1 Ti 0.62618(3) 0.86743(4) 0.38076(4) 0.02972(19) Uani 1 1 d . . .
Ti2 Ti 0.60450(3) 0.71687(4) 0.38059(3) 0.02620(18) Uani 1 1 d . . .
Ti3 Ti 0.57400(3) 0.80197(4) 0.47798(3) 0.02853(19) Uani 1 1 d . . .
Zr1 Zr 0.502859(16) 0.82068(2) 0.345059(19) 0.02581(11) Uani 1 1 d . . .
C51 C 0.19523(18) 0.6117(2) 0.1391(2) 0.0379(11) Uani 1 1 d . . .
C52 C 0.2003(2) 0.6503(3) 0.0842(2) 0.0414(12) Uani 1 1 d . . .
C53 C 0.2476(2) 0.6957(2) 0.0972(2) 0.0412(12) Uani 1 1 d . . .
C54 C 0.27116(19) 0.6857(2) 0.1607(2) 0.0396(12) Uani 1 1 d . . .
C55 C 0.2377(2) 0.6330(3) 0.1866(2) 0.0387(12) Uani 1 1 d . . .
C56 C 0.1553(2) 0.5490(3) 0.1426(3) 0.0738(19) Uani 1 1 d . . .
H56A H 0.1197 0.56 0.1181 0.111 Uiso 1 1 calc R . .
H56B H 0.1499 0.541 0.1859 0.111 Uiso 1 1 calc R . .
H56C H 0.1708 0.5064 0.1261 0.111 Uiso 1 1 calc R . .
C57 C 0.1644(3) 0.6421(4) 0.0214(3) 0.080(2) Uani 1 1 d . . .
H57A H 0.1792 0.6038 -0.002 0.119 Uiso 1 1 calc R . .
H57B H 0.1647 0.6864 -0.002 0.119 Uiso 1 1 calc R . .
H57C H 0.1265 0.6307 0.0279 0.119 Uiso 1 1 calc R . .
C58 C 0.2703(3) 0.7404(3) 0.0482(3) 0.085(2) Uani 1 1 d . . .
H58A H 0.2706 0.7124 0.0104 0.127 Uiso 1 1 calc R . .
H58B H 0.308 0.7554 0.0637 0.127 Uiso 1 1 calc R . .
H58C H 0.247 0.7823 0.039 0.127 Uiso 1 1 calc R . .
C59 C 0.3225(2) 0.7222(3) 0.1932(3) 0.0736(19) Uani 1 1 d . . .
H59A H 0.3552 0.7038 0.1768 0.11 Uiso 1 1 calc R . .
H59B H 0.3258 0.7129 0.2378 0.11 Uiso 1 1 calc R . .
H59C H 0.3197 0.7733 0.1857 0.11 Uiso 1 1 calc R . .
C60 C 0.2494(3) 0.5997(4) 0.2514(3) 0.080(2) Uani 1 1 d . . .
H60A H 0.2148 0.5949 0.2691 0.119 Uiso 1 1 calc R . .
H60B H 0.2749 0.6301 0.2782 0.119 Uiso 1 1 calc R . .
H60C H 0.2661 0.5529 0.2482 0.119 Uiso 1 1 calc R . .
C61 C 0.18913(19) 1.0207(2) 0.1568(2) 0.0375(11) Uani 1 1 d . . .
C62 C 0.16747(19) 1.0048(2) 0.0942(2) 0.0413(12) Uani 1 1 d . . .
C63 C 0.2069(2) 0.9602(3) 0.0684(2) 0.0498(14) Uani 1 1 d . . .
C64 C 0.2530(2) 0.9498(2) 0.1170(3) 0.0417(12) Uani 1 1 d . . .
C65 C 0.24251(18) 0.9872(2) 0.1702(2) 0.0379(12) Uani 1 1 d . . .
C66 C 0.1633(2) 1.0721(3) 0.1991(3) 0.0581(15) Uani 1 1 d . . .
H66A H 0.1475 1.1126 0.1747 0.087 Uiso 1 1 calc R . .
H66B H 0.1918 1.0888 0.2319 0.087 Uiso 1 1 calc R . .
H66C H 0.1341 1.0479 0.2177 0.087 Uiso 1 1 calc R . .
C67 C 0.1183(2) 1.0428(3) 0.0570(3) 0.076(2) Uani 1 1 d . . .
H67A H 0.0922 1.0577 0.0851 0.114 Uiso 1 1 calc R . .
H67B H 0.0997 1.0106 0.0257 0.114 Uiso 1 1 calc R . .
H67C H 0.1315 1.0845 0.0366 0.114 Uiso 1 1 calc R . .
C68 C 0.2023(3) 0.9338(3) 0.0020(3) 0.087(2) Uani 1 1 d . . .
H68A H 0.2045 0.882 0.0018 0.131 Uiso 1 1 calc R . .
H68B H 0.2325 0.9536 -0.018 0.131 Uiso 1 1 calc R . .
H68C H 0.1668 0.9488 -0.0207 0.131 Uiso 1 1 calc R . .
C69 C 0.3083(2) 0.9125(3) 0.1106(3) 0.082(2) Uani 1 1 d . . .
H69A H 0.339 0.9452 0.123 0.122 Uiso 1 1 calc R . .
H69B H 0.3087 0.8982 0.0674 0.122 Uiso 1 1 calc R . .
H69C H 0.3123 0.8706 0.1373 0.122 Uiso 1 1 calc R . .
C70 C 0.2841(2) 0.9936(3) 0.2291(3) 0.0654(17) Uani 1 1 d . . .
H70A H 0.2855 0.9489 0.252 0.098 Uiso 1 1 calc R . .
H70B H 0.2727 1.0318 0.2551 0.098 Uiso 1 1 calc R . .
H70C H 0.3207 1.0042 0.2178 0.098 Uiso 1 1 calc R . .
C71 C 0.12700(19) 0.8747(3) 0.3594(2) 0.0422(12) Uani 1 1 d . . .
C72 C 0.1822(2) 0.8962(3) 0.3561(2) 0.0405(12) Uani 1 1 d . . .
C73 C 0.2169(2) 0.8350(3) 0.3611(2) 0.0490(14) Uani 1 1 d . . .
C74 C 0.1818(2) 0.7752(3) 0.3689(2) 0.0496(14) Uani 1 1 d . . .
C75 C 0.1270(2) 0.8007(3) 0.3700(2) 0.0435(13) Uani 1 1 d . . .
C76 C 0.0768(2) 0.9237(4) 0.3590(3) 0.079(2) Uani 1 1 d . . .
H76A H 0.0462 0.9056 0.3295 0.118 Uiso 1 1 calc R . .
H76B H 0.0865 0.9715 0.3466 0.118 Uiso 1 1 calc R . .
H76C H 0.0656 0.9253 0.4005 0.118 Uiso 1 1 calc R . .
C77 C 0.2008(3) 0.9742(3) 0.3545(3) 0.082(2) Uani 1 1 d . . .
H77A H 0.1796 0.9982 0.3191 0.123 Uiso 1 1 calc R . .
H77B H 0.2402 0.9761 0.3503 0.123 Uiso 1 1 calc R . .
H77C H 0.1944 0.9978 0.393 0.123 Uiso 1 1 calc R . .
C78 C 0.2801(2) 0.8329(5) 0.3623(3) 0.094(3) Uani 1 1 d . . .
H78A H 0.2898 0.7963 0.3337 0.141 Uiso 1 1 calc R . .
H78B H 0.2976 0.8221 0.4044 0.141 Uiso 1 1 calc R . .
H78C H 0.2931 0.8791 0.3496 0.141 Uiso 1 1 calc R . .
C79 C 0.1998(4) 0.6977(4) 0.3805(3) 0.111(3) Uani 1 1 d . . .
H79A H 0.1974 0.6853 0.4238 0.166 Uiso 1 1 calc R . .
H79B H 0.2379 0.6919 0.372 0.166 Uiso 1 1 calc R . .
H79C H 0.1755 0.6666 0.3531 0.166 Uiso 1 1 calc R . .
C80 C 0.0775(3) 0.7591(4) 0.3885(3) 0.089(2) Uani 1 1 d . . .
H80A H 0.0671 0.7785 0.427 0.134 Uiso 1 1 calc R . .
H80B H 0.0878 0.7092 0.3947 0.134 Uiso 1 1 calc R . .
H80C H 0.0463 0.763 0.3555 0.134 Uiso 1 1 calc R . .
C81 C 0.0187(2) 0.9286(3) 0.1001(3) 0.0552(15) Uani 1 1 d . . .
H81 H 0.0343 0.9715 0.1168 0.066 Uiso 1 1 calc R . .
C82 C 0.0356(2) 0.8910(3) 0.0489(3) 0.0496(14) Uani 1 1 d . . .
H82 H 0.0641 0.9048 0.0258 0.06 Uiso 1 1 calc R . .
C83 C 0.0022(2) 0.8294(3) 0.0387(3) 0.0519(14) Uani 1 1 d . . .
H83 H 0.0045 0.7945 0.0078 0.062 Uiso 1 1 calc R . .
C84 C -0.0352(2) 0.8295(3) 0.0834(3) 0.0581(16) Uani 1 1 d . . .
H84 H -0.0625 0.7948 0.0876 0.07 Uiso 1 1 calc R . .
C85 C -0.0244(2) 0.8918(4) 0.1214(3) 0.0651(17) Uani 1 1 d . . .
H85 H -0.0433 0.9054 0.1549 0.078 Uiso 1 1 calc R . .
C86 C 0.0267(3) 0.5420(3) 0.2260(3) 0.0730(19) Uani 1 1 d . . .
H86 H 0.0252 0.5177 0.1876 0.088 Uiso 1 1 calc R . .
C87 C -0.0164(2) 0.5811(3) 0.2471(3) 0.0619(16) Uani 1 1 d . . .
H87 H -0.0521 0.5884 0.225 0.074 Uiso 1 1 calc R . .
C88 C 0.0032(3) 0.6078(3) 0.3078(3) 0.0710(19) Uani 1 1 d . . .
H88 H -0.0173 0.6352 0.3333 0.085 Uiso 1 1 calc R . .
C89 C 0.0574(3) 0.5861(4) 0.3222(3) 0.079(2) Uani 1 1 d . . .
H89 H 0.0807 0.5967 0.3595 0.095 Uiso 1 1 calc R . .
C90 C 0.0724(3) 0.5460(3) 0.2727(4) 0.079(2) Uani 1 1 d . . .
H90 H 0.1075 0.5251 0.271 0.094 Uiso 1 1 calc R . .
N2 N 0.21149(14) 0.82050(18) 0.21150(16) 0.0296(8) Uani 1 1 d . . .
N56 N 0.14043(14) 0.81014(19) 0.10572(17) 0.0315(9) Uani 1 1 d . . .
N57 N 0.12390(13) 0.73529(19) 0.22043(16) 0.0308(8) Uani 1 1 d . . .
N67 N 0.11307(13) 0.88999(18) 0.20636(16) 0.0294(8) Uani 1 1 d . . .
H67 H 0.0984 0.9316 0.2199 0.035 Uiso 1 1 calc R . .
Mg2 Mg 0.05676(6) 0.66569(8) 0.23080(8) 0.0399(4) Uani 1 1 d . . .
Cl3 Cl 0.00199(5) 0.77866(7) 0.23412(6) 0.0458(3) Uani 1 1 d . . .
Cl4 Cl 0.03798(5) 0.67765(7) 0.11213(6) 0.0461(3) Uani 1 1 d . . .
Ti5 Ti 0.17897(3) 0.73796(4) 0.16282(4) 0.02821(19) Uani 1 1 d . . .
Ti6 Ti 0.17526(3) 0.88928(4) 0.15273(4) 0.02967(19) Uani 1 1 d . . .
Ti7 Ti 0.15373(3) 0.81840(4) 0.26586(4) 0.02931(19) Uani 1 1 d . . .
Zr2 Zr 0.061643(17) 0.81126(2) 0.14385(2) 0.03130(12) Uani 1 1 d . . .
C100 C 0.0755(2) 0.4400(3) -0.0169(2) 0.102(3) Uani 1 1 d G . .
H10A H 0.0621 0.4846 -0.0014 0.153 Uiso 1 1 calc R . .
H10B H 0.0497 0.4235 -0.0523 0.153 Uiso 1 1 calc R . .
H10C H 0.1119 0.4477 -0.0301 0.153 Uiso 1 1 calc R . .
C101 C 0.08017(12) 0.38403(19) 0.03479(15) 0.0673(17) Uani 1 1 d G . .
C102 C 0.06713(14) 0.4011(2) 0.09524(18) 0.0683(18) Uani 1 1 d G . .
H102 H 0.0546 0.4474 0.1032 0.082 Uiso 1 1 calc R . .
C103 C 0.07262(16) 0.3499(3) 0.14369(16) 0.078(2) Uani 1 1 d G . .
H103 H 0.0638 0.3622 0.1835 0.093 Uiso 1 1 calc R . .
C104 C 0.09130(16) 0.2801(2) 0.1325(2) 0.080(2) Uani 1 1 d G . .
H104 H 0.0951 0.2459 0.1647 0.096 Uiso 1 1 calc R . .
C105 C 0.10428(17) 0.26221(18) 0.0725(3) 0.091(2) Uani 1 1 d G . .
H105 H 0.1167 0.2159 0.0646 0.109 Uiso 1 1 calc R . .
C106 C 0.09869(16) 0.3137(2) 0.02422(19) 0.081(2) Uani 1 1 d G . .
H106 H 0.1074 0.3012 -0.0156 0.097 Uiso 1 1 calc R . .
C110 C 0.1690(2) 0.2697(4) 0.3570(3) 0.086(2) Uani 1 1 d DU . .
C111 C 0.1853(2) 0.3054(4) 0.4136(3) 0.0713(17) Uani 1 1 d DU . .
H111 H 0.1891 0.2795 0.4513 0.086 Uiso 1 1 calc R . .
C112 C 0.1960(3) 0.3791(4) 0.4150(3) 0.087(2) Uani 1 1 d DU . .
H112 H 0.2073 0.4015 0.4537 0.104 Uiso 1 1 calc R . .
C113 C 0.1903(3) 0.4201(4) 0.3601(3) 0.094(2) Uani 1 1 d DU . .
H113 H 0.1977 0.4695 0.361 0.112 Uiso 1 1 calc R . .
C114 C 0.1731(3) 0.3842(5) 0.3040(4) 0.118(3) Uani 1 1 d DU . .
H114 H 0.1683 0.4103 0.2664 0.141 Uiso 1 1 calc R . .
C115 C 0.1627(3) 0.3101(4) 0.3020(3) 0.097(2) Uani 1 1 d DU . .
H115 H 0.1513 0.2877 0.2634 0.116 Uiso 1 1 calc R . .
C116 C 0.1576(3) 0.1922(5) 0.3551(5) 0.127(3) Uani 1 1 d U . .
H11A H 0.1679 0.1723 0.3167 0.191 Uiso 1 1 calc R . .
H11B H 0.1182 0.1842 0.3566 0.191 Uiso 1 1 calc R . .
H11C H 0.1792 0.1693 0.3908 0.191 Uiso 1 1 calc R . .



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

_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
C11 C12 1.414(6) . ?
C11 C15 1.420(7) . ?
C11 C16 1.506(7) . ?
C11 Ti1 2.461(4) . ?
C12 C13 1.412(6) . ?
C12 C17 1.505(7) . ?
C12 Ti1 2.424(4) . ?
C13 C14 1.424(6) . ?
C13 C18 1.484(6) . ?
C13 Ti1 2.421(4) . ?
C14 C15 1.422(6) . ?
C14 C19 1.488(7) . ?
C14 Ti1 2.440(4) . ?
C15 C20 1.500(7) . ?
C15 Ti1 2.467(5) . ?
C21 C22 1.412(6) . ?
C21 C25 1.411(6) . ?
C21 C26 1.500(6) . ?
C21 Ti2 2.395(4) . ?
C22 C23 1.421(6) . ?
C22 C27 1.511(6) . ?
C22 Ti2 2.371(4) . ?
C23 C24 1.416(6) . ?
C23 C28 1.488(6) . ?
C23 Ti2 2.403(4) . ?
C24 C25 1.414(6) . ?
C24 C29 1.502(6) . ?
C24 Ti2 2.405(4) . ?
C25 C30 1.494(6) . ?
C25 Ti2 2.431(4) . ?
C31 C32 1.395(7) . ?
C31 C35 1.426(6) . ?
C31 C36 1.492(7) . ?
C31 Ti3 2.401(4) . ?
C32 C33 1.401(6) . ?
C32 C37 1.500(6) . ?
C32 Ti3 2.434(4) . ?
C33 C34 1.388(7) . ?
C33 C38 1.495(7) . ?
C33 Ti3 2.424(5) . ?
C34 C35 1.426(7) . ?
C34 C39 1.532(6) . ?
C34 Ti3 2.396(4) . ?
C35 C40 1.496(7) . ?
C35 Ti3 2.413(4) . ?
C41 C45 1.389(7) . ?
C41 C42 1.384(6) . ?
C41 Zr1 2.545(4) . ?
C42 C43 1.390(6) . ?
C42 Zr1 2.521(4) . ?
C43 C44 1.400(7) . ?
C43 Zr1 2.514(5) . ?
C44 C45 1.389(7) . ?
C44 Zr1 2.542(5) . ?
C45 Zr1 2.548(4) . ?
C46 C47 1.335(11) . ?
C46 C50 1.388(10) . ?
C46 Mg1 2.376(6) . ?
C47 C48 1.302(10) . ?
C47 Mg1 2.346(7) . ?
C48 C49 1.344(10) . ?
C48 Mg1 2.421(6) . ?
C49 C50 1.368(10) . ?
C49 Mg1 2.457(6) . ?
C50 Mg1 2.420(6) . ?
Cl1 Mg1 2.5115(19) . ?
Cl1 Zr1 2.6069(12) . ?
Cl2 Mg1 2.469(2) . ?
Cl2 Zr1 2.6202(12) . ?
Mg1 N23 2.131(4) . ?
Mg1 Zr1 3.2588(15) . ?
N1 Ti1 1.915(4) . ?
N1 Ti2 1.931(3) . ?
N1 Ti3 1.939(3) . ?
N12 Ti1 1.957(3) . ?
N12 Ti2 1.972(4) . ?
N12 Zr1 2.194(3) . ?
N13 Ti1 1.940(3) . ?
N13 Ti3 1.969(3) . ?
N13 Zr1 2.203(3) . ?
N23 Ti3 1.906(3) . ?
N23 Ti2 1.908(3) . ?
N23 Zr1 2.447(3) . ?
Ti1 Ti3 2.8312(11) . ?
Ti1 Ti2 2.8342(11) . ?
Ti1 Zr1 3.0736(10) . ?
Ti2 Ti3 2.7804(11) . ?
Ti2 Zr1 3.1141(9) . ?
Ti3 Zr1 3.1265(9) . ?
C51 C52 1.391(7) . ?
C51 C55 1.393(6) . ?
C51 C56 1.512(7) . ?
C51 Ti5 2.433(4) . ?
C52 C53 1.406(7) . ?
C52 C57 1.501(7) . ?
C52 Ti5 2.435(4) . ?
C53 C54 1.409(7) . ?
C53 C58 1.491(7) . ?
C53 Ti5 2.425(4) . ?
C54 C55 1.420(7) . ?
C54 C59 1.491(7) . ?
C54 Ti5 2.416(4) . ?
C55 C60 1.505(7) . ?
C55 Ti5 2.412(4) . ?
C61 C62 1.397(7) . ?
C61 C65 1.415(6) . ?
C61 C66 1.500(6) . ?
C61 Ti6 2.455(4) . ?
C62 C63 1.419(7) . ?
C62 C67 1.504(7) . ?
C62 Ti6 2.471(5) . ?
C63 C64 1.425(7) . ?
C63 C68 1.488(7) . ?
C63 Ti6 2.428(5) . ?
C64 C65 1.379(7) . ?
C64 C69 1.515(7) . ?
C64 Ti6 2.383(4) . ?
C65 C70 1.501(7) . ?
C65 Ti6 2.420(4) . ?
C71 C75 1.388(7) . ?
C71 C72 1.391(6) . ?
C71 C76 1.505(7) . ?
C71 Ti7 2.412(5) . ?
C72 C73 1.401(7) . ?
C72 C77 1.512(7) . ?
C72 Ti7 2.427(5) . ?
C73 C74 1.412(7) . ?
C73 C78 1.512(7) . ?
C73 Ti7 2.386(5) . ?
C74 C75 1.398(7) . ?
C74 C79 1.509(8) . ?
C74 Ti7 2.352(5) . ?
C75 C80 1.508(7) . ?
C75 Ti7 2.415(5) . ?
C81 C85 1.363(8) . ?
C81 C82 1.397(7) . ?
C81 Zr2 2.527(5) . ?
C82 C83 1.392(7) . ?
C82 Zr2 2.516(5) . ?
C83 C84 1.393(8) . ?
C83 Zr2 2.513(5) . ?
C84 C85 1.412(8) . ?
C84 Zr2 2.521(5) . ?
C85 Zr2 2.536(5) . ?
C86 C87 1.382(8) . ?
C86 C90 1.381(9) . ?
C86 Mg2 2.398(6) . ?
C87 C88 1.407(8) . ?
C87 Mg2 2.408(5) . ?
C88 C89 1.354(9) . ?
C88 Mg2 2.460(5) . ?
C89 C90 1.377(9) . ?
C89 Mg2 2.441(6) . ?
C90 Mg2 2.399(6) . ?
N2 Ti6 1.912(3) . ?
N2 Ti7 1.919(3) . ?
N2 Ti5 1.950(3) . ?
N56 Ti6 1.904(4) . ?
N56 Ti5 1.955(4) . ?
N56 Zr2 2.151(3) . ?
N57 Ti7 1.906(4) . ?
N57 Ti5 1.918(3) . ?
N57 Mg2 2.094(4) . ?
N57 Zr2 2.494(3) . ?
N67 Ti6 1.994(3) . ?
N67 Ti7 1.996(3) . ?
N67 Zr2 2.232(3) . ?
Mg2 Cl3 2.474(2) . ?
Mg2 Cl4 2.521(2) . ?
Mg2 Zr2 3.2814(17) . ?
Cl3 Zr2 2.6153(13) . ?
Cl4 Zr2 2.6060(13) . ?
Ti5 Ti7 2.7862(11) . ?
Ti5 Ti6 2.8092(11) . ?
Ti5 Zr2 3.0970(10) . ?
Ti6 Ti7 2.8528(11) . ?
Ti6 Zr2 3.0631(10) . ?
Ti7 Zr2 3.1820(10) . ?
C100 C101 1.5071 . ?
C101 C102 1.4022 . ?
C101 C106 1.4022 . ?
C102 C103 1.3963 . ?
C103 C104 1.3965 . ?
C104 C105 1.3965 . ?
C105 C106 1.3964 . ?
C110 C115 1.383(5) . ?
C110 C111 1.385(4) . ?
C110 C116 1.459(10) . ?
C111 C112 1.388(4) . ?
C112 C113 1.388(4) . ?
C113 C114 1.384(5) . ?
C114 C115 1.392(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
C12 C11 C15 107.6(4) . . ?
C12 C11 C16 126.9(5) . . ?
C15 C11 C16 125.0(5) . . ?
C12 C11 Ti1 71.7(3) . . ?
C15 C11 Ti1 73.5(3) . . ?
C16 C11 Ti1 126.8(3) . . ?
C13 C12 C11 108.6(4) . . ?
C13 C12 C17 123.5(4) . . ?
C11 C12 C17 127.4(5) . . ?
C13 C12 Ti1 73.0(2) . . ?
C11 C12 Ti1 74.6(2) . . ?
C17 C12 Ti1 124.8(3) . . ?
C12 C13 C14 108.0(4) . . ?
C12 C13 C18 123.9(4) . . ?
C14 C13 C18 127.6(4) . . ?
C12 C13 Ti1 73.2(2) . . ?
C14 C13 Ti1 73.7(2) . . ?
C18 C13 Ti1 125.0(3) . . ?
C15 C14 C13 107.4(4) . . ?
C15 C14 C19 127.1(5) . . ?
C13 C14 C19 125.1(4) . . ?
C15 C14 Ti1 74.2(3) . . ?
C13 C14 Ti1 72.2(2) . . ?
C19 C14 Ti1 124.2(3) . . ?
C11 C15 C14 108.3(4) . . ?
C11 C15 C20 124.6(5) . . ?
C14 C15 C20 125.8(5) . . ?
C11 C15 Ti1 73.0(3) . . ?
C14 C15 Ti1 72.1(3) . . ?
C20 C15 Ti1 131.2(3) . . ?
C22 C21 C25 107.8(4) . . ?
C22 C21 C26 124.5(4) . . ?
C25 C21 C26 127.5(4) . . ?
C22 C21 Ti2 71.8(2) . . ?
C25 C21 Ti2 74.4(2) . . ?
C26 C21 Ti2 123.7(3) . . ?
C21 C22 C23 108.4(4) . . ?
C21 C22 C27 124.9(4) . . ?
C23 C22 C27 126.7(4) . . ?
C21 C22 Ti2 73.7(2) . . ?
C23 C22 Ti2 73.9(2) . . ?
C27 C22 Ti2 121.1(3) . . ?
C24 C23 C22 107.4(4) . . ?
C24 C23 C28 126.1(4) . . ?
C22 C23 C28 126.2(4) . . ?
C24 C23 Ti2 73.0(2) . . ?
C22 C23 Ti2 71.5(2) . . ?
C28 C23 Ti2 125.8(3) . . ?
C25 C24 C23 108.2(4) . . ?
C25 C24 C29 124.5(4) . . ?
C23 C24 C29 127.1(4) . . ?
C25 C24 Ti2 74.0(2) . . ?
C23 C24 Ti2 72.8(2) . . ?
C29 C24 Ti2 124.2(3) . . ?
C21 C25 C24 108.2(4) . . ?
C21 C25 C30 128.0(4) . . ?
C24 C25 C30 123.7(4) . . ?
C21 C25 Ti2 71.6(2) . . ?
C24 C25 Ti2 72.0(2) . . ?
C30 C25 Ti2 125.1(3) . . ?
C32 C31 C35 107.8(4) . . ?
C32 C31 C36 125.6(5) . . ?
C35 C31 C36 126.4(5) . . ?
C32 C31 Ti3 74.5(3) . . ?
C35 C31 Ti3 73.2(2) . . ?
C36 C31 Ti3 121.5(3) . . ?
C31 C32 C33 109.1(4) . . ?
C31 C32 C37 123.8(4) . . ?
C33 C32 C37 126.5(5) . . ?
C31 C32 Ti3 71.9(2) . . ?
C33 C32 Ti3 72.8(3) . . ?
C37 C32 Ti3 128.8(3) . . ?
C34 C33 C32 107.8(5) . . ?
C34 C33 C38 126.0(5) . . ?
C32 C33 C38 126.1(5) . . ?
C34 C33 Ti3 72.2(3) . . ?
C32 C33 Ti3 73.6(3) . . ?
C38 C33 Ti3 122.8(3) . . ?
C33 C34 C35 109.0(4) . . ?
C33 C34 C39 127.4(5) . . ?
C35 C34 C39 123.6(5) . . ?
C33 C34 Ti3 74.3(3) . . ?
C35 C34 Ti3 73.4(3) . . ?
C39 C34 Ti3 120.2(3) . . ?
C34 C35 C31 106.2(4) . . ?
C34 C35 C40 127.3(5) . . ?
C31 C35 C40 126.3(5) . . ?
C34 C35 Ti3 72.1(3) . . ?
C31 C35 Ti3 72.3(2) . . ?
C40 C35 Ti3 123.7(3) . . ?
C45 C41 C42 108.0(4) . . ?
C45 C41 Zr1 74.3(3) . . ?
C42 C41 Zr1 73.2(2) . . ?
C43 C42 C41 108.3(4) . . ?
C43 C42 Zr1 73.7(3) . . ?
C41 C42 Zr1 75.1(3) . . ?
C42 C43 C44 107.8(5) . . ?
C42 C43 Zr1 74.2(3) . . ?
C44 C43 Zr1 75.0(3) . . ?
C45 C44 C43 107.6(5) . . ?
C45 C44 Zr1 74.4(3) . . ?
C43 C44 Zr1 72.8(3) . . ?
C41 C45 C44 108.3(5) . . ?
C41 C45 Zr1 74.1(2) . . ?
C44 C45 Zr1 73.9(3) . . ?
C47 C46 C50 106.7(7) . . ?
C47 C46 Mg1 72.3(4) . . ?
C50 C46 Mg1 74.9(4) . . ?
C48 C47 C46 109.8(7) . . ?
C48 C47 Mg1 77.4(5) . . ?
C46 C47 Mg1 74.8(4) . . ?
C47 C48 C49 109.9(7) . . ?
C47 C48 Mg1 71.0(4) . . ?
C49 C48 Mg1 75.5(4) . . ?
C48 C49 C50 106.8(6) . . ?
C48 C49 Mg1 72.5(4) . . ?
C50 C49 Mg1 72.2(4) . . ?
C49 C50 C46 106.8(7) . . ?
C49 C50 Mg1 75.2(3) . . ?
C46 C50 Mg1 71.4(4) . . ?
Mg1 Cl1 Zr1 79.07(5) . . ?
Mg1 Cl2 Zr1 79.58(5) . . ?
N23 Mg1 C47 120.4(2) . . ?
N23 Mg1 C46 127.8(2) . . ?
C47 Mg1 C46 32.8(3) . . ?
N23 Mg1 C50 156.3(3) . . ?
C47 Mg1 C50 54.5(2) . . ?
C46 Mg1 C50 33.6(2) . . ?
N23 Mg1 C48 136.9(3) . . ?
C47 Mg1 C48 31.7(3) . . ?
C46 Mg1 C48 53.4(3) . . ?
C50 Mg1 C48 53.4(2) . . ?
N23 Mg1 C49 167.7(3) . . ?
C47 Mg1 C49 53.6(3) . . ?
C46 Mg1 C49 54.5(2) . . ?
C50 Mg1 C49 32.6(2) . . ?
C48 Mg1 C49 32.0(3) . . ?
N23 Mg1 Cl2 82.87(10) . . ?
C47 Mg1 Cl2 125.8(4) . . ?
C46 Mg1 Cl2 147.02(18) . . ?
C50 Mg1 Cl2 119.6(3) . . ?
C48 Mg1 Cl2 96.9(2) . . ?
C49 Mg1 Cl2 92.96(18) . . ?
N23 Mg1 Cl1 83.01(11) . . ?
C47 Mg1 Cl1 139.0(3) . . ?
C46 Mg1 Cl1 106.2(3) . . ?
C50 Mg1 Cl1 89.98(17) . . ?
C48 Mg1 Cl1 140.1(2) . . ?
C49 Mg1 Cl1 108.4(3) . . ?
Cl2 Mg1 Cl1 87.52(6) . . ?
N23 Mg1 Zr1 48.66(9) . . ?
C47 Mg1 Zr1 167.4(2) . . ?
C46 Mg1 Zr1 155.8(3) . . ?
C50 Mg1 Zr1 138.09(18) . . ?
C48 Mg1 Zr1 149.1(2) . . ?
C49 Mg1 Zr1 135.53(18) . . ?
Cl2 Mg1 Zr1 52.26(4) . . ?
Cl1 Mg1 Zr1 51.76(4) . . ?
Ti1 N1 Ti2 94.96(15) . . ?
Ti1 N1 Ti3 94.55(15) . . ?
Ti2 N1 Ti3 91.86(14) . . ?
Ti1 N12 Ti2 92.35(14) . . ?
Ti1 N12 Zr1 95.39(14) . . ?
Ti2 N12 Zr1 96.62(14) . . ?
Ti1 N13 Ti3 92.81(14) . . ?
Ti1 N13 Zr1 95.58(14) . . ?
Ti3 N13 Zr1 96.92(14) . . ?
Ti3 N23 Ti2 93.60(15) . . ?
Ti3 N23 Mg1 130.11(17) . . ?
Ti2 N23 Mg1 136.25(19) . . ?
Ti3 N23 Zr1 90.95(13) . . ?
Ti2 N23 Zr1 90.43(13) . . ?
Mg1 N23 Zr1 90.50(12) . . ?
N1 Ti1 N13 87.05(14) . . ?
N1 Ti1 N12 86.77(15) . . ?
N13 Ti1 N12 90.05(14) . . ?
N1 Ti1 C12 100.13(15) . . ?
N13 Ti1 C12 124.70(16) . . ?
N12 Ti1 C12 144.63(15) . . ?
N1 Ti1 C13 105.45(15) . . ?
N13 Ti1 C13 155.91(15) . . ?
N12 Ti1 C13 110.79(15) . . ?
C12 Ti1 C13 33.89(15) . . ?
N1 Ti1 C14 136.64(15) . . ?
N13 Ti1 C14 136.15(15) . . ?
N12 Ti1 C14 95.24(15) . . ?
C12 Ti1 C14 56.31(16) . . ?
C13 Ti1 C14 34.07(15) . . ?
N1 Ti1 C11 125.12(16) . . ?
N13 Ti1 C11 99.88(15) . . ?
N12 Ti1 C11 146.73(16) . . ?
C12 Ti1 C11 33.65(15) . . ?
C13 Ti1 C11 56.06(15) . . ?
C14 Ti1 C11 56.07(16) . . ?
N1 Ti1 C15 155.88(16) . . ?
N13 Ti1 C15 105.44(15) . . ?
N12 Ti1 C15 113.25(16) . . ?
C12 Ti1 C15 55.78(16) . . ?
C13 Ti1 C15 55.99(15) . . ?
C14 Ti1 C15 33.69(15) . . ?
C11 Ti1 C15 33.50(16) . . ?
N1 Ti1 Ti3 43.06(10) . . ?
N13 Ti1 Ti3 44.00(10) . . ?
N12 Ti1 Ti3 88.72(10) . . ?
C12 Ti1 Ti3 119.88(12) . . ?
C13 Ti1 Ti3 143.48(11) . . ?
C14 Ti1 Ti3 176.03(12) . . ?
C11 Ti1 Ti3 120.28(12) . . ?
C15 Ti1 Ti3 144.20(12) . . ?
N1 Ti1 Ti2 42.73(10) . . ?
N13 Ti1 Ti2 88.44(10) . . ?
N12 Ti1 Ti2 44.04(10) . . ?
C12 Ti1 Ti2 132.23(12) . . ?
C13 Ti1 Ti2 114.80(11) . . ?
C14 Ti1 Ti2 124.23(12) . . ?
C11 Ti1 Ti2 165.37(12) . . ?
C15 Ti1 Ti2 154.41(13) . . ?
Ti3 Ti1 Ti2 58.78(3) . . ?
N1 Ti1 Zr1 92.12(10) . . ?
N13 Ti1 Zr1 45.50(10) . . ?
N12 Ti1 Zr1 45.28(9) . . ?
C12 Ti1 Zr1 164.20(12) . . ?
C13 Ti1 Zr1 150.20(11) . . ?
C14 Ti1 Zr1 119.50(11) . . ?
C11 Ti1 Zr1 130.56(12) . . ?
C15 Ti1 Zr1 111.42(11) . . ?
Ti3 Ti1 Zr1 63.79(2) . . ?
Ti2 Ti1 Zr1 63.47(2) . . ?
N23 Ti2 N1 87.33(14) . . ?
N23 Ti2 N12 95.68(14) . . ?
N1 Ti2 N12 85.91(15) . . ?
N23 Ti2 C22 111.18(15) . . ?
N1 Ti2 C22 108.87(15) . . ?
N12 Ti2 C22 149.45(14) . . ?
N23 Ti2 C21 143.74(15) . . ?
N1 Ti2 C21 94.74(14) . . ?
N12 Ti2 C21 120.58(15) . . ?
C22 Ti2 C21 34.47(15) . . ?
N23 Ti2 C23 102.01(15) . . ?
N1 Ti2 C23 143.29(15) . . ?
N12 Ti2 C23 127.44(14) . . ?
C22 Ti2 C23 34.63(14) . . ?
C21 Ti2 C23 57.22(14) . . ?
N23 Ti2 C24 123.88(15) . . ?
N1 Ti2 C24 148.14(15) . . ?
N12 Ti2 C24 96.08(14) . . ?
C22 Ti2 C24 57.20(14) . . ?
C21 Ti2 C24 56.96(14) . . ?
C23 Ti2 C24 34.27(14) . . ?
N23 Ti2 C25 157.30(15) . . ?
N1 Ti2 C25 114.24(15) . . ?
N12 Ti2 C25 92.98(14) . . ?
C22 Ti2 C25 56.73(14) . . ?
C21 Ti2 C25 34.00(14) . . ?
C23 Ti2 C25 56.61(14) . . ?
C24 Ti2 C25 33.99(14) . . ?
N23 Ti2 Ti3 43.17(10) . . ?
N1 Ti2 Ti3 44.19(10) . . ?
N12 Ti2 Ti3 89.88(10) . . ?
C22 Ti2 Ti3 119.54(11) . . ?
C21 Ti2 Ti3 129.21(11) . . ?
C23 Ti2 Ti3 134.98(11) . . ?
C24 Ti2 Ti3 166.51(11) . . ?
C25 Ti2 Ti3 157.98(11) . . ?
N23 Ti2 Ti1 92.44(11) . . ?
N1 Ti2 Ti1 42.30(10) . . ?
N12 Ti2 Ti1 43.61(10) . . ?
C22 Ti2 Ti1 143.24(11) . . ?
C21 Ti2 Ti1 113.17(11) . . ?
C23 Ti2 Ti1 164.30(11) . . ?
C24 Ti2 Ti1 130.89(11) . . ?
C25 Ti2 Ti1 108.16(11) . . ?
Ti3 Ti2 Ti1 60.55(3) . . ?
N23 Ti2 Zr1 51.79(10) . . ?
N1 Ti2 Zr1 90.59(10) . . ?
N12 Ti2 Zr1 44.41(9) . . ?
C22 Ti2 Zr1 154.48(11) . . ?
C21 Ti2 Zr1 163.70(11) . . ?
C23 Ti2 Zr1 123.17(10) . . ?
C24 Ti2 Zr1 112.98(10) . . ?
C25 Ti2 Zr1 130.35(11) . . ?
Ti3 Ti2 Zr1 63.77(2) . . ?
Ti1 Ti2 Zr1 62.01(2) . . ?
N23 Ti3 N1 87.14(14) . . ?
N23 Ti3 N13 95.38(14) . . ?
N1 Ti3 N13 85.56(14) . . ?
N23 Ti3 C34 125.68(17) . . ?
N1 Ti3 C34 92.68(15) . . ?
N13 Ti3 C34 138.81(17) . . ?
N23 Ti3 C31 137.96(16) . . ?
N1 Ti3 C31 133.93(16) . . ?
N13 Ti3 C31 96.32(15) . . ?
C34 Ti3 C31 56.80(15) . . ?
N23 Ti3 C35 158.15(16) . . ?
N1 Ti3 C35 100.67(15) . . ?
N13 Ti3 C35 105.48(16) . . ?
C34 Ti3 C35 34.50(17) . . ?
C31 Ti3 C35 34.46(15) . . ?
N23 Ti3 C33 101.70(16) . . ?
N1 Ti3 C33 117.09(16) . . ?
N13 Ti3 C33 151.96(15) . . ?
C34 Ti3 C33 33.47(16) . . ?
C31 Ti3 C33 56.34(16) . . ?
C35 Ti3 C33 56.55(17) . . ?
N23 Ti3 C32 107.75(16) . . ?
N1 Ti3 C32 148.11(15) . . ?
N13 Ti3 C32 119.65(15) . . ?
C34 Ti3 C32 55.62(15) . . ?
C31 Ti3 C32 33.54(16) . . ?
C35 Ti3 C32 56.13(16) . . ?
C33 Ti3 C32 33.53(15) . . ?
N23 Ti3 Ti2 43.23(10) . . ?
N1 Ti3 Ti2 43.95(10) . . ?
N13 Ti3 Ti2 89.42(10) . . ?
C34 Ti3 Ti2 117.08(12) . . ?
C31 Ti3 Ti2 173.77(12) . . ?
C35 Ti3 Ti2 141.19(12) . . ?
C33 Ti3 Ti2 118.20(12) . . ?
C32 Ti3 Ti2 143.51(13) . . ?
N23 Ti3 Ti1 92.58(10) . . ?
N1 Ti3 Ti1 42.39(11) . . ?
N13 Ti3 Ti1 43.19(10) . . ?
C34 Ti3 Ti1 122.02(13) . . ?
C31 Ti3 Ti1 122.62(13) . . ?
C35 Ti3 Ti1 107.00(12) . . ?
C33 Ti3 Ti1 154.82(12) . . ?
C32 Ti3 Ti1 155.81(13) . . ?
Ti2 Ti3 Ti1 60.66(3) . . ?
N23 Ti3 Zr1 51.49(10) . . ?
N1 Ti3 Zr1 90.07(10) . . ?
N13 Ti3 Zr1 44.38(9) . . ?
C34 Ti3 Zr1 175.97(14) . . ?
C31 Ti3 Zr1 122.70(11) . . ?
C35 Ti3 Zr1 147.49(14) . . ?
C33 Ti3 Zr1 142.52(12) . . ?
C32 Ti3 Zr1 121.41(11) . . ?
Ti2 Ti3 Zr1 63.31(2) . . ?
Ti1 Ti3 Zr1 61.88(3) . . ?
N12 Zr1 N13 77.65(12) . . ?
N12 Zr1 N23 76.39(12) . . ?
N13 Zr1 N23 75.91(12) . . ?
N12 Zr1 C43 79.10(15) . . ?
N13 Zr1 C43 101.05(15) . . ?
N23 Zr1 C43 155.39(14) . . ?
N12 Zr1 C42 99.98(14) . . ?
N13 Zr1 C42 82.10(14) . . ?
N23 Zr1 C42 157.99(13) . . ?
C43 Zr1 C42 32.05(14) . . ?
N12 Zr1 C44 94.11(16) . . ?
N13 Zr1 C44 132.40(15) . . ?
N23 Zr1 C44 148.15(14) . . ?
C43 Zr1 C44 32.14(15) . . ?
C42 Zr1 C44 52.87(15) . . ?
N12 Zr1 C41 130.27(15) . . ?
N13 Zr1 C41 98.05(14) . . ?
N23 Zr1 C41 151.47(14) . . ?
C43 Zr1 C41 52.76(16) . . ?
C42 Zr1 C41 31.71(14) . . ?
C44 Zr1 C41 52.53(16) . . ?
N12 Zr1 C45 125.70(15) . . ?
N13 Zr1 C45 129.58(15) . . ?
N23 Zr1 C45 146.20(14) . . ?
C43 Zr1 C45 52.77(16) . . ?
C42 Zr1 C45 52.55(15) . . ?
C44 Zr1 C45 31.66(16) . . ?
C41 Zr1 C45 31.65(15) . . ?
N12 Zr1 Cl1 151.07(9) . . ?
N13 Zr1 Cl1 89.77(9) . . ?
N23 Zr1 Cl1 75.30(8) . . ?
C43 Zr1 Cl1 129.31(12) . . ?
C42 Zr1 Cl1 103.99(11) . . ?
C44 Zr1 Cl1 113.22(14) . . ?
C41 Zr1 Cl1 76.83(12) . . ?
C45 Zr1 Cl1 82.31(13) . . ?
N12 Zr1 Cl2 95.45(9) . . ?
N13 Zr1 Cl2 149.96(9) . . ?
N23 Zr1 Cl2 74.05(8) . . ?
C43 Zr1 Cl2 106.33(12) . . ?
C42 Zr1 Cl2 127.92(11) . . ?
C44 Zr1 Cl2 76.76(12) . . ?
C41 Zr1 Cl2 108.20(12) . . ?
C45 Zr1 Cl2 78.21(12) . . ?
Cl1 Zr1 Cl2 82.44(4) . . ?
N12 Zr1 Ti1 39.33(9) . . ?
N13 Zr1 Ti1 38.92(8) . . ?
N23 Zr1 Ti1 77.33(8) . . ?
C43 Zr1 Ti1 85.18(12) . . ?
C42 Zr1 Ti1 86.21(11) . . ?
C44 Zr1 Ti1 114.31(13) . . ?
C41 Zr1 Ti1 115.58(11) . . ?
C45 Zr1 Ti1 136.38(12) . . ?
Cl1 Zr1 Ti1 126.48(3) . . ?
Cl2 Zr1 Ti1 131.38(3) . . ?
N12 Zr1 Ti2 38.97(9) . . ?
N13 Zr1 Ti2 77.15(9) . . ?
N23 Zr1 Ti2 37.79(8) . . ?
C43 Zr1 Ti2 117.61(11) . . ?
C42 Zr1 Ti2 136.98(11) . . ?
C44 Zr1 Ti2 123.69(13) . . ?
C41 Zr1 Ti2 168.67(11) . . ?
C45 Zr1 Ti2 150.71(12) . . ?
Cl1 Zr1 Ti2 113.08(3) . . ?
Cl2 Zr1 Ti2 79.37(3) . . ?
Ti1 Zr1 Ti2 54.52(2) . . ?
C52 C51 C55 109.3(4) . . ?
C52 C51 C56 124.2(5) . . ?
C55 C51 C56 125.9(5) . . ?
C52 C51 Ti5 73.5(3) . . ?
C55 C51 Ti5 72.4(3) . . ?
C56 C51 Ti5 127.4(3) . . ?
C51 C52 C53 107.4(4) . . ?
C51 C52 C57 126.6(5) . . ?
C53 C52 C57 125.9(5) . . ?
C51 C52 Ti5 73.3(3) . . ?
C53 C52 Ti5 72.8(3) . . ?
C57 C52 Ti5 122.4(4) . . ?
C52 C53 C54 108.6(4) . . ?
C52 C53 C58 123.6(5) . . ?
C54 C53 C58 127.6(5) . . ?
C52 C53 Ti5 73.6(3) . . ?
C54 C53 Ti5 72.7(2) . . ?
C58 C53 Ti5 124.4(3) . . ?
C53 C54 C55 106.9(4) . . ?
C53 C54 C59 126.0(5) . . ?
C55 C54 C59 127.2(5) . . ?
C53 C54 Ti5 73.4(3) . . ?
C55 C54 Ti5 72.7(2) . . ?
C59 C54 Ti5 120.6(3) . . ?
C51 C55 C54 107.8(4) . . ?
C51 C55 C60 125.5(5) . . ?
C54 C55 C60 126.3(5) . . ?
C51 C55 Ti5 74.1(3) . . ?
C54 C55 Ti5 73.1(3) . . ?
C60 C55 Ti5 123.7(3) . . ?
C62 C61 C65 108.1(4) . . ?
C62 C61 C66 125.3(5) . . ?
C65 C61 C66 126.1(5) . . ?
C62 C61 Ti6 74.1(3) . . ?
C65 C61 Ti6 71.8(3) . . ?
C66 C61 Ti6 125.8(3) . . ?
C61 C62 C63 108.2(4) . . ?
C61 C62 C67 124.8(5) . . ?
C63 C62 C67 125.6(5) . . ?
C61 C62 Ti6 72.9(3) . . ?
C63 C62 Ti6 71.5(3) . . ?
C67 C62 Ti6 132.2(3) . . ?
C62 C63 C64 106.7(4) . . ?
C62 C63 C68 126.3(6) . . ?
C64 C63 C68 126.9(5) . . ?
C62 C63 Ti6 74.8(3) . . ?
C64 C63 Ti6 71.0(3) . . ?
C68 C63 Ti6 122.5(4) . . ?
C65 C64 C63 108.8(4) . . ?
C65 C64 C69 124.0(5) . . ?
C63 C64 C69 126.7(5) . . ?
C65 C64 Ti6 74.8(2) . . ?
C63 C64 Ti6 74.5(3) . . ?
C69 C64 Ti6 123.0(3) . . ?
C64 C65 C61 108.2(4) . . ?
C64 C65 C70 123.7(5) . . ?
C61 C65 C70 128.0(5) . . ?
C64 C65 Ti6 71.8(3) . . ?
C61 C65 Ti6 74.5(2) . . ?
C70 C65 Ti6 122.8(3) . . ?
C75 C71 C72 108.1(4) . . ?
C75 C71 C76 125.3(5) . . ?
C72 C71 C76 126.2(5) . . ?
C75 C71 Ti7 73.4(3) . . ?
C72 C71 Ti7 73.9(3) . . ?
C76 C71 Ti7 123.7(3) . . ?
C71 C72 C73 108.8(5) . . ?
C71 C72 C77 124.0(5) . . ?
C73 C72 C77 126.9(5) . . ?
C71 C72 Ti7 72.7(3) . . ?
C73 C72 Ti7 71.5(3) . . ?
C77 C72 Ti7 127.0(3) . . ?
C74 C73 C72 106.7(4) . . ?
C74 C73 C78 126.1(6) . . ?
C72 C73 C78 127.1(6) . . ?
C74 C73 Ti7 71.3(3) . . ?
C72 C73 Ti7 74.7(3) . . ?
C78 C73 Ti7 122.1(3) . . ?
C75 C74 C73 108.2(5) . . ?
C75 C74 C79 124.5(6) . . ?
C73 C74 C79 127.1(6) . . ?
C75 C74 Ti7 75.5(3) . . ?
C73 C74 Ti7 74.0(3) . . ?
C79 C74 Ti7 121.1(4) . . ?
C71 C75 C74 108.1(4) . . ?
C71 C75 C80 124.4(5) . . ?
C74 C75 C80 127.1(6) . . ?
C71 C75 Ti7 73.2(3) . . ?
C74 C75 Ti7 70.5(3) . . ?
C80 C75 Ti7 128.5(3) . . ?
C85 C81 C82 108.8(5) . . ?
C85 C81 Zr2 74.7(3) . . ?
C82 C81 Zr2 73.5(3) . . ?
C81 C82 C83 108.1(5) . . ?
C81 C82 Zr2 74.4(3) . . ?
C83 C82 Zr2 73.8(3) . . ?
C82 C83 C84 107.4(5) . . ?
C82 C83 Zr2 74.0(3) . . ?
C84 C83 Zr2 74.3(3) . . ?
C83 C84 C85 107.9(5) . . ?
C83 C84 Zr2 73.6(3) . . ?
C85 C84 Zr2 74.4(3) . . ?
C81 C85 C84 107.8(5) . . ?
C81 C85 Zr2 74.0(3) . . ?
C84 C85 Zr2 73.2(3) . . ?
C87 C86 C90 106.9(6) . . ?
C87 C86 Mg2 73.7(3) . . ?
C90 C86 Mg2 73.3(3) . . ?
C86 C87 C88 108.2(6) . . ?
C86 C87 Mg2 72.9(3) . . ?
C88 C87 Mg2 75.2(3) . . ?
C89 C88 C87 107.2(6) . . ?
C89 C88 Mg2 73.2(3) . . ?
C87 C88 Mg2 71.2(3) . . ?
C88 C89 C90 109.0(6) . . ?
C88 C89 Mg2 74.7(4) . . ?
C90 C89 Mg2 71.8(4) . . ?
C89 C90 C86 108.6(6) . . ?
C89 C90 Mg2 75.1(4) . . ?
C86 C90 Mg2 73.2(4) . . ?
Ti6 N2 Ti7 96.26(15) . . ?
Ti6 N2 Ti5 93.34(15) . . ?
Ti7 N2 Ti5 92.12(14) . . ?
Ti6 N56 Ti5 93.44(15) . . ?
Ti6 N56 Zr2 97.95(15) . . ?
Ti5 N56 Zr2 97.82(15) . . ?
Ti7 N57 Ti5 93.54(15) . . ?
Ti7 N57 Mg2 133.15(19) . . ?
Ti5 N57 Mg2 133.3(2) . . ?
Ti7 N57 Zr2 91.66(14) . . ?
Ti5 N57 Zr2 88.15(13) . . ?
Mg2 N57 Zr2 90.89(13) . . ?
Ti6 N67 Ti7 91.26(14) . . ?
Ti6 N67 Zr2 92.74(13) . . ?
Ti7 N67 Zr2 97.48(14) . . ?
N57 Mg2 C90 121.53(19) . . ?
N57 Mg2 C86 144.4(2) . . ?
C90 Mg2 C86 33.5(2) . . ?
N57 Mg2 C87 176.38(19) . . ?
C90 Mg2 C87 55.0(2) . . ?
C86 Mg2 C87 33.4(2) . . ?
N57 Mg2 C89 122.1(2) . . ?
C90 Mg2 C89 33.0(2) . . ?
C86 Mg2 C89 55.1(2) . . ?
C87 Mg2 C89 54.5(2) . . ?
N57 Mg2 C88 144.5(2) . . ?
C90 Mg2 C88 54.5(2) . . ?
C86 Mg2 C88 55.4(2) . . ?
C87 Mg2 C88 33.58(19) . . ?
C89 Mg2 C88 32.1(2) . . ?
N57 Mg2 Cl3 84.28(11) . . ?
C90 Mg2 Cl3 145.77(19) . . ?
C86 Mg2 Cl3 130.60(19) . . ?
C87 Mg2 Cl3 98.48(16) . . ?
C89 Mg2 Cl3 115.7(2) . . ?
C88 Mg2 Cl3 91.35(17) . . ?
N57 Mg2 Cl4 82.94(11) . . ?
C90 Mg2 Cl4 117.0(2) . . ?
C86 Mg2 Cl4 91.62(18) . . ?
C87 Mg2 Cl4 99.55(17) . . ?
C89 Mg2 Cl4 146.72(19) . . ?
C88 Mg2 Cl4 132.0(2) . . ?
Cl3 Mg2 Cl4 85.99(7) . . ?
N57 Mg2 Zr2 49.46(10) . . ?
C90 Mg2 Zr2 162.3(2) . . ?
C86 Mg2 Zr2 142.43(19) . . ?
C87 Mg2 Zr2 134.16(16) . . ?
C89 Mg2 Zr2 161.7(2) . . ?
C88 Mg2 Zr2 142.73(18) . . ?
Cl3 Mg2 Zr2 51.77(4) . . ?
Cl4 Mg2 Zr2 51.36(4) . . ?
Mg2 Cl3 Zr2 80.25(5) . . ?
Mg2 Cl4 Zr2 79.57(5) . . ?
N57 Ti5 N2 86.50(15) . . ?
N57 Ti5 N56 96.26(15) . . ?
N2 Ti5 N56 85.32(15) . . ?
N57 Ti5 C55 105.98(16) . . ?
N2 Ti5 C55 109.78(16) . . ?
N56 Ti5 C55 153.54(15) . . ?
N57 Ti5 C54 135.14(16) . . ?
N2 Ti5 C54 91.29(15) . . ?
N56 Ti5 C54 128.24(16) . . ?
C55 Ti5 C54 34.21(16) . . ?
N57 Ti5 C53 159.60(16) . . ?
N2 Ti5 C53 107.86(16) . . ?
N56 Ti5 C53 99.23(16) . . ?
C55 Ti5 C53 56.05(16) . . ?
C54 Ti5 C53 33.86(16) . . ?
N57 Ti5 C51 104.53(16) . . ?
N2 Ti5 C51 143.07(15) . . ?
N56 Ti5 C51 127.03(16) . . ?
C55 Ti5 C51 33.42(15) . . ?
C54 Ti5 C51 55.92(15) . . ?
C53 Ti5 C51 55.33(15) . . ?
N57 Ti5 C52 130.44(17) . . ?
N2 Ti5 C52 141.51(16) . . ?
N56 Ti5 C52 98.68(16) . . ?
C55 Ti5 C52 55.87(16) . . ?
C54 Ti5 C52 56.26(16) . . ?
C53 Ti5 C52 33.65(16) . . ?
C51 Ti5 C52 33.21(16) . . ?
N57 Ti5 Ti7 43.05(11) . . ?
N2 Ti5 Ti7 43.50(10) . . ?
N56 Ti5 Ti7 89.57(11) . . ?
C55 Ti5 Ti7 116.47(12) . . ?
C54 Ti5 Ti7 121.54(12) . . ?
C53 Ti5 Ti7 149.56(13) . . ?
C51 Ti5 Ti7 137.27(12) . . ?
C52 Ti5 Ti7 170.47(13) . . ?
N57 Ti5 Ti6 93.29(11) . . ?
N2 Ti5 Ti6 42.80(10) . . ?
N56 Ti5 Ti6 42.56(10) . . ?
C55 Ti5 Ti6 146.16(13) . . ?
C54 Ti5 Ti6 114.67(12) . . ?
C53 Ti5 Ti6 107.10(11) . . ?
C51 Ti5 Ti6 161.04(12) . . ?
C52 Ti5 Ti6 128.20(13) . . ?
Ti7 Ti5 Ti6 61.30(3) . . ?
N57 Ti5 Zr2 53.59(10) . . ?
N2 Ti5 Zr2 91.00(10) . . ?
N56 Ti5 Zr2 43.48(10) . . ?
C55 Ti5 Zr2 150.85(12) . . ?
C54 Ti5 Zr2 171.11(13) . . ?
C53 Ti5 Zr2 137.54(13) . . ?
C51 Ti5 Zr2 124.12(11) . . ?
C52 Ti5 Zr2 118.12(12) . . ?
Ti7 Ti5 Zr2 65.24(2) . . ?
Ti6 Ti5 Zr2 62.26(2) . . ?
N56 Ti6 N2 87.82(15) . . ?
N56 Ti6 N67 89.94(14) . . ?
N2 Ti6 N67 86.36(14) . . ?
N56 Ti6 C64 119.98(17) . . ?
N2 Ti6 C64 102.53(16) . . ?
N67 Ti6 C64 148.72(16) . . ?
N56 Ti6 C65 153.28(16) . . ?
N2 Ti6 C65 99.39(15) . . ?
N67 Ti6 C65 116.04(16) . . ?
C64 Ti6 C65 33.37(16) . . ?
N56 Ti6 C63 100.57(17) . . ?
N2 Ti6 C63 133.40(17) . . ?
N67 Ti6 C63 138.70(17) . . ?
C64 Ti6 C63 34.45(17) . . ?
C65 Ti6 C63 56.13(17) . . ?
N56 Ti6 C61 145.96(16) . . ?
N2 Ti6 C61 126.10(16) . . ?
N67 Ti6 C61 94.65(14) . . ?
C64 Ti6 C61 55.78(15) . . ?
C65 Ti6 C61 33.74(15) . . ?
C63 Ti6 C61 55.69(16) . . ?
N56 Ti6 C62 113.67(16) . . ?
N2 Ti6 C62 154.79(15) . . ?
N67 Ti6 C62 105.78(15) . . ?
C64 Ti6 C62 56.04(16) . . ?
C65 Ti6 C62 55.50(15) . . ?
C63 Ti6 C62 33.66(16) . . ?
C61 Ti6 C62 32.96(15) . . ?
N56 Ti6 Ti5 43.99(11) . . ?
N2 Ti6 Ti5 43.87(10) . . ?
N67 Ti6 Ti5 88.91(10) . . ?
C64 Ti6 Ti5 118.38(12) . . ?
C65 Ti6 Ti5 136.15(12) . . ?
C63 Ti6 Ti5 125.88(13) . . ?
C61 Ti6 Ti5 169.20(12) . . ?
C62 Ti6 Ti5 154.30(13) . . ?
N56 Ti6 Ti7 88.62(11) . . ?
N2 Ti6 Ti7 41.97(10) . . ?
N67 Ti6 Ti7 44.39(10) . . ?
C64 Ti6 Ti7 136.31(14) . . ?
C65 Ti6 Ti7 113.92(12) . . ?
C63 Ti6 Ti7 169.90(14) . . ?
C61 Ti6 Ti7 117.68(12) . . ?
C62 Ti6 Ti7 144.61(13) . . ?
Ti5 Ti6 Ti7 58.95(3) . . ?
N56 Ti6 Zr2 44.06(11) . . ?
N2 Ti6 Zr2 92.78(10) . . ?
N67 Ti6 Zr2 46.69(10) . . ?
C64 Ti6 Zr2 157.97(14) . . ?
C65 Ti6 Zr2 158.39(12) . . ?
C63 Ti6 Zr2 124.79(14) . . ?
C61 Ti6 Zr2 125.74(11) . . ?
C62 Ti6 Zr2 111.71(11) . . ?
Ti5 Ti6 Zr2 63.48(2) . . ?
Ti7 Ti6 Zr2 64.96(2) . . ?
N57 Ti7 N2 87.75(15) . . ?
N57 Ti7 N67 95.41(14) . . ?
N2 Ti7 N67 86.11(14) . . ?
N57 Ti7 C74 104.02(17) . . ?
N2 Ti7 C74 115.61(18) . . ?
N67 Ti7 C74 150.98(16) . . ?
N57 Ti7 C73 133.56(19) . . ?
N2 Ti7 C73 94.93(15) . . ?
N67 Ti7 C73 131.02(18) . . ?
C74 Ti7 C73 34.67(18) . . ?
N57 Ti7 C71 130.30(16) . . ?
N2 Ti7 C71 141.50(16) . . ?
N67 Ti7 C71 94.51(16) . . ?
C74 Ti7 C71 56.47(17) . . ?
C73 Ti7 C71 56.46(16) . . ?
N57 Ti7 C75 103.37(16) . . ?
N2 Ti7 C75 149.19(17) . . ?
N67 Ti7 C75 120.55(17) . . ?
C74 Ti7 C75 34.07(17) . . ?
C73 Ti7 C75 56.59(16) . . ?
C71 Ti7 C75 33.42(17) . . ?
N57 Ti7 C72 158.25(16) . . ?
N2 Ti7 C72 108.52(16) . . ?
N67 Ti7 C72 99.90(16) . . ?
C74 Ti7 C72 56.32(17) . . ?
C73 Ti7 C72 33.82(17) . . ?
C71 Ti7 C72 33.42(15) . . ?
C75 Ti7 C72 55.39(16) . . ?
N57 Ti7 Ti5 43.41(10) . . ?
N2 Ti7 Ti5 44.38(10) . . ?
N67 Ti7 Ti5 89.53(10) . . ?
C74 Ti7 Ti5 119.39(13) . . ?
C73 Ti7 Ti5 124.13(13) . . ?
C71 Ti7 Ti5 173.03(13) . . ?
C75 Ti7 Ti5 139.92(13) . . ?
C72 Ti7 Ti5 151.00(12) . . ?
N57 Ti7 Ti6 92.22(11) . . ?
N2 Ti7 Ti6 41.77(10) . . ?
N67 Ti7 Ti6 44.34(9) . . ?
C74 Ti7 Ti6 152.32(15) . . ?
C73 Ti7 Ti6 119.73(14) . . ?
C71 Ti7 Ti6 126.78(13) . . ?
C75 Ti7 Ti6 160.09(13) . . ?
C72 Ti7 Ti6 109.52(12) . . ?
Ti5 Ti7 Ti6 59.74(3) . . ?
N57 Ti7 Zr2 51.57(10) . . ?
N2 Ti7 Zr2 89.05(11) . . ?
N67 Ti7 Zr2 44.05(10) . . ?
C74 Ti7 Zr2 146.23(15) . . ?
C73 Ti7 Zr2 173.53(14) . . ?
C71 Ti7 Zr2 117.61(11) . . ?
C75 Ti7 Zr2 120.48(12) . . ?
C72 Ti7 Zr2 139.81(12) . . ?
Ti5 Ti7 Zr2 62.10(2) . . ?
Ti6 Ti7 Zr2 60.71(2) . . ?
N56 Zr2 N67 77.89(13) . . ?
N56 Zr2 N57 76.38(12) . . ?
N67 Zr2 N57 75.08(12) . . ?
N56 Zr2 C83 94.86(16) . . ?
N67 Zr2 C83 130.38(16) . . ?
N57 Zr2 C83 151.38(16) . . ?
N56 Zr2 C82 80.67(15) . . ?
N67 Zr2 C82 98.97(16) . . ?
N57 Zr2 C82 157.01(14) . . ?
C83 Zr2 C82 32.15(16) . . ?
N56 Zr2 C84 126.95(17) . . ?
N67 Zr2 C84 127.92(17) . . ?
N57 Zr2 C84 147.07(15) . . ?
C83 Zr2 C84 32.12(17) . . ?
C82 Zr2 C84 52.92(17) . . ?
N56 Zr2 C81 101.68(17) . . ?
N67 Zr2 C81 79.91(16) . . ?
N57 Zr2 C81 154.77(16) . . ?
C83 Zr2 C81 53.24(18) . . ?
C82 Zr2 C81 32.17(17) . . ?
C84 Zr2 C81 52.75(18) . . ?
N56 Zr2 C85 131.68(17) . . ?
N67 Zr2 C85 95.67(19) . . ?
N57 Zr2 C85 148.75(16) . . ?
C83 Zr2 C85 53.39(19) . . ?
C82 Zr2 C85 52.73(18) . . ?
C84 Zr2 C85 32.43(19) . . ?
C81 Zr2 C85 31.23(17) . . ?
N56 Zr2 Cl4 93.67(10) . . ?
N67 Zr2 Cl4 149.12(9) . . ?
N57 Zr2 Cl4 74.07(9) . . ?
C83 Zr2 Cl4 79.47(13) . . ?
C82 Zr2 Cl4 109.00(14) . . ?
C84 Zr2 Cl4 80.86(15) . . ?
C81 Zr2 Cl4 130.96(13) . . ?
C85 Zr2 Cl4 111.45(17) . . ?
N56 Zr2 Cl3 150.23(10) . . ?
N67 Zr2 Cl3 91.30(9) . . ?
N57 Zr2 Cl3 74.04(8) . . ?
C83 Zr2 Cl3 112.82(13) . . ?
C82 Zr2 Cl3 128.77(12) . . ?
C84 Zr2 Cl3 81.50(14) . . ?
C81 Zr2 Cl3 103.60(14) . . ?
C85 Zr2 Cl3 76.46(14) . . ?
Cl4 Zr2 Cl3 81.44(4) . . ?
N56 Zr2 Ti6 37.99(9) . . ?
N67 Zr2 Ti6 40.57(8) . . ?
N57 Zr2 Ti6 77.10(8) . . ?
C83 Zr2 Ti6 112.64(13) . . ?
C82 Zr2 Ti6 84.07(12) . . ?
C84 Zr2 Ti6 135.82(13) . . ?
C81 Zr2 Ti6 86.10(13) . . ?
C85 Zr2 Ti6 115.25(16) . . ?
Cl4 Zr2 Ti6 128.61(3) . . ?
Cl3 Zr2 Ti6 129.08(4) . . ?
N56 Zr2 Ti5 38.70(9) . . ?
N67 Zr2 Ti5 77.82(9) . . ?
N57 Zr2 Ti5 38.25(8) . . ?
C83 Zr2 Ti5 124.82(13) . . ?
C82 Zr2 Ti5 119.07(12) . . ?
C84 Zr2 Ti5 151.89(16) . . ?
C81 Zr2 Ti5 137.88(13) . . ?
C85 Zr2 Ti5 169.05(16) . . ?
Cl4 Zr2 Ti5 77.32(3) . . ?
Cl3 Zr2 Ti5 112.16(4) . . ?
Ti6 Zr2 Ti5 54.26(2) . . ?
C102 C101 C106 118.1 . . ?
C102 C101 C100 120.9 . . ?
C106 C101 C100 120.9 . . ?
C103 C102 C101 121.1 . . ?
C102 C103 C104 120.1 . . ?
C105 C104 C103 119.4 . . ?
C106 C105 C104 120.1 . . ?
C105 C106 C101 121.1 . . ?
C115 C110 C111 117.8(7) . . ?
C115 C110 C116 120.6(7) . . ?
C111 C110 C116 121.5(7) . . ?
C110 C111 C112 121.2(7) . . ?
C113 C112 C111 121.5(7) . . ?
C114 C113 C112 116.8(7) . . ?
C113 C114 C115 122.0(8) . . ?
C110 C115 C114 120.6(7) . . ?
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Toluene'
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_15
_database_code_depnum_ccdc_archive 'CCDC 1415004'
_audit_update_record             
;
2015-08-26 deposited with the CCDC.
2015-09-16 downloaded from the CCDC.
;

_audit_creation_date             2013-11-08T11:24:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

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

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C30 H47 Cl3 N4 Ti3 Zr, C12 H24 K O6, 7(C6 H6)'
_chemical_formula_sum            'C84 H113 Cl3 K N4 O6 Ti3 Zr'
_chemical_formula_weight         1655.15
_chemical_compound_source        'synthesis as described'

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

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_Int_Tables_number      147




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

_cell_length_a                   16.515(2)
_cell_length_b                   16.515(2)
_cell_length_c                   17.886(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4224.7(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    58
_cell_measurement_theta_min      3
_cell_measurement_theta_max      27
_cell_measurement_wavelength     0.71073

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

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1738
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
16 0 -1 0.164
16 -17 -1 0.15
-1 -17 0 0.172
-16 1 1 0.193
-1 1 0 0.195
1 9 0 0.182
-1 0 18 0.054
0 0 -1 0.058

_exptl_special_details           
;
 ?
;

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

_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_T_max  1.005

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

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.1152
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_number            51159
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             6488
_reflns_number_gt                5156
_reflns_threshold_expression     >2sigma(I)
_diffrn_reflns_reduction_process 
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

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

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

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

_refine_special_details          SQUEEZE
_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)+(0.0323P)²+5.8711P] 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_number_reflns         6488
_refine_ls_number_parameters     294
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0658
_refine_ls_wR_factor_ref         0.1284
_refine_ls_wR_factor_gt          0.119
_refine_ls_goodness_of_fit_ref   1.15
_refine_ls_restrained_S_all      1.161
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.1

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

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 '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'

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
C1 C 0.5445(3) 0.8919(3) -0.0696(2) 0.0397(9) Uani 1 1 d . . .
H1A H 0.5446 0.8878 -0.0144 0.048 Uiso 1 1 calc R . .
H1B H 0.5846 0.9582 -0.0843 0.048 Uiso 1 1 calc R . .
C2 C 0.4143(3) 0.9148(3) -0.0730(2) 0.0397(9) Uani 1 1 d . . .
H2A H 0.4552 0.98 -0.0901 0.048 Uiso 1 1 calc R . .
H2B H 0.4103 0.915 -0.0177 0.048 Uiso 1 1 calc R . .
C3 C 0.5568(3) 0.6807(3) -0.1063(2) 0.0435(9) Uani 1 1 d . . .
H3A H 0.6239 0.7057 -0.0954 0.052 Uiso 1 1 calc R . .
H3B H 0.5484 0.6772 -0.1612 0.052 Uiso 1 1 calc R . .
C4 C 0.5808(3) 0.8336(3) -0.1033(2) 0.0443(9) Uani 1 1 d . . .
H4A H 0.5758 0.8337 -0.1585 0.053 Uiso 1 1 calc R . .
H4B H 0.6475 0.8596 -0.0901 0.053 Uiso 1 1 calc R . .
C11 C 0.4133(3) 0.8876(2) 0.44148(18) 0.0330(8) Uani 1 1 d . . .
C12 C 0.3676(2) 0.9086(2) 0.38432(19) 0.0317(8) Uani 1 1 d . . .
C13 C 0.4257(3) 0.9394(2) 0.32119(19) 0.0324(8) Uani 1 1 d . . .
C14 C 0.5084(3) 0.9376(2) 0.3379(2) 0.0340(8) Uani 1 1 d . . .
C15 C 0.5011(3) 0.9064(2) 0.41302(19) 0.0338(8) Uani 1 1 d . . .
C16 C 0.3799(3) 0.8544(3) 0.5195(2) 0.0521(11) Uani 1 1 d . . .
H16A H 0.4161 0.9052 0.5549 0.078 Uiso 1 1 calc R . .
H16B H 0.3881 0.801 0.531 0.078 Uiso 1 1 calc R . .
H16C H 0.3135 0.8355 0.5234 0.078 Uiso 1 1 calc R . .
C17 C 0.2748(3) 0.9052(3) 0.3903(3) 0.0520(11) Uani 1 1 d . . .
H17A H 0.2848 0.9688 0.3879 0.078 Uiso 1 1 calc R . .
H17B H 0.245 0.8763 0.4379 0.078 Uiso 1 1 calc R . .
H17C H 0.2343 0.8681 0.3489 0.078 Uiso 1 1 calc R . .
C18 C 0.4043(3) 0.9730(3) 0.2493(2) 0.0508(11) Uani 1 1 d . . .
H18A H 0.3421 0.9262 0.2314 0.076 Uiso 1 1 calc R . .
H18B H 0.4512 0.9824 0.2115 0.076 Uiso 1 1 calc R . .
H18C H 0.4057 1.0322 0.2584 0.076 Uiso 1 1 calc R . .
C19 C 0.5900(3) 0.9672(3) 0.2864(3) 0.0546(11) Uani 1 1 d . . .
H19A H 0.6316 1.035 0.2902 0.082 Uiso 1 1 calc R . .
H19B H 0.5675 0.9507 0.2349 0.082 Uiso 1 1 calc R . .
H19C H 0.6243 0.9353 0.3005 0.082 Uiso 1 1 calc R . .
C20 C 0.5742(3) 0.8993(3) 0.4572(3) 0.0588(13) Uani 1 1 d . . .
H20A H 0.5466 0.8374 0.4805 0.088 Uiso 1 1 calc R . .
H20B H 0.5987 0.9475 0.4961 0.088 Uiso 1 1 calc R . .
H20C H 0.6252 0.9084 0.4239 0.088 Uiso 1 1 calc R . .
Cl1 Cl 0.18969(6) 0.60199(7) 0.11490(5) 0.0407(2) Uani 1 1 d . . .
K1 K 0.3333 0.6667 -0.03814(7) 0.0334(3) Uani 1 3 d S . .
N1 N 0.3333 0.6667 0.4007(2) 0.0222(9) Uani 1 3 d S . .
N11 N 0.27129(17) 0.71689(17) 0.27894(13) 0.0225(5) Uani 1 1 d . . .
H11 H 0.2366 0.7449 0.2654 0.027 Uiso 0.67 1 calc PR . .
O1 O 0.45183(17) 0.85774(17) -0.09608(14) 0.0383(6) Uani 1 1 d . . .
O2 O 0.52722(17) 0.74041(17) -0.07564(13) 0.0366(6) Uani 1 1 d . . .
Ti1 Ti 0.38396(4) 0.77990(4) 0.34298(3) 0.02224(14) Uani 1 1 d . . .
Zr1 Zr 0.3333 0.6667 0.19709(3) 0.02567(14) Uani 1 3 d S . .
C103 C 0.8322(3) 0.9408(3) 0.1346(2) 0.0544(11) Uani 1 1 d D . .
H103 H 0.8896 0.9896 0.1538 0.065 Uiso 1 1 calc R . .
C101 C 0.7491(3) 0.8120(3) 0.0515(2) 0.0568(12) Uani 1 1 d D . .
H101 H 0.7493 0.7722 0.0132 0.068 Uiso 1 1 calc R . .
C115 C 0.8613(3) 0.9925(3) 0.6771(2) 0.0631(13) Uani 1 1 d D . .
H115 H 0.9147 1.0474 0.695 0.076 Uiso 1 1 calc R . .
C110 C 0.7875(3) 0.9384(3) 0.7247(2) 0.0588(12) Uani 1 1 d D . .
H110 H 0.7903 0.9564 0.7755 0.071 Uiso 1 1 calc R . .
C104 C 0.7485(3) 0.9273(3) 0.1624(3) 0.0580(12) Uani 1 1 d D . .
H104 H 0.7483 0.9673 0.2005 0.07 Uiso 1 1 calc R . .
C102 C 0.8324(3) 0.8831(3) 0.0787(2) 0.0542(11) Uani 1 1 d D . .
H102 H 0.89 0.8926 0.0591 0.065 Uiso 1 1 calc R . .
C100 C 0.6654(3) 0.7983(3) 0.0796(2) 0.0612(12) Uani 1 1 d D . .
H100 H 0.6079 0.7491 0.0608 0.073 Uiso 1 1 calc R . .
C114 C 0.8564(3) 0.9658(3) 0.6034(2) 0.0651(13) Uani 1 1 d D . .
H114 H 0.9066 1.0023 0.5703 0.078 Uiso 1 1 calc R . .
C111 C 0.7105(3) 0.8589(3) 0.6989(2) 0.0657(13) Uani 1 1 d D . .
H111 H 0.6605 0.822 0.7321 0.079 Uiso 1 1 calc R . .
C113 C 0.7787(3) 0.8862(3) 0.5777(3) 0.0709(15) Uani 1 1 d D . .
H113 H 0.7755 0.8683 0.5269 0.085 Uiso 1 1 calc R . .
C105 C 0.6653(3) 0.8562(3) 0.1351(3) 0.0632(13) Uani 1 1 d D . .
H105 H 0.6078 0.847 0.1546 0.076 Uiso 1 1 calc R . .
C112 C 0.7054(4) 0.8324(4) 0.6254(2) 0.0760(16) Uani 1 1 d D . .
H112 H 0.6519 0.7776 0.6075 0.091 Uiso 1 1 calc R . .



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

_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
C1 O1 1.422(4) . ?
C1 C4 1.493(5) . ?
C2 O1 1.425(4) . ?
C2 C3 1.491(5) 2_665 ?
C3 O2 1.411(4) . ?
C3 C2 1.491(5) 3_565 ?
C4 O2 1.426(4) . ?
C11 C12 1.414(5) . ?
C11 C15 1.416(5) . ?
C11 C16 1.499(5) . ?
C11 Ti1 2.375(3) . ?
C12 C13 1.402(5) . ?
C12 C17 1.509(5) . ?
C12 Ti1 2.390(3) . ?
C13 C14 1.412(5) . ?
C13 C18 1.511(5) . ?
C13 Ti1 2.397(3) . ?
C14 C15 1.421(5) . ?
C14 C19 1.499(5) . ?
C14 Ti1 2.379(3) . ?
C15 C20 1.495(5) . ?
C15 Ti1 2.374(3) . ?
Cl1 Zr1 2.5290(9) . ?
Cl1 K1 3.4245(14) . ?
K1 O2 2.879(2) 2_665 ?
K1 O2 2.879(2) 3_565 ?
K1 O2 2.879(2) . ?
K1 O1 2.947(3) 2_665 ?
K1 O1 2.947(3) . ?
K1 O1 2.947(3) 3_565 ?
K1 Cl1 3.4245(14) 3_565 ?
K1 Cl1 3.4245(14) 2_665 ?
K1 Zr1 4.2074(15) . ?
N1 Ti1 1.923(2) . ?
N1 Ti1 1.923(2) 2_665 ?
N1 Ti1 1.923(2) 3_565 ?
N11 Ti1 1.980(3) . ?
N11 Ti1 1.981(2) 2_665 ?
N11 Zr1 2.175(2) . ?
Ti1 N11 1.981(2) 3_565 ?
Ti1 Ti1 2.8103(10) 2_665 ?
Ti1 Ti1 2.8103(10) 3_565 ?
Ti1 Zr1 3.0727(8) . ?
Zr1 N11 2.175(3) 3_565 ?
Zr1 N11 2.175(3) 2_665 ?
Zr1 Cl1 2.5290(9) 3_565 ?
Zr1 Cl1 2.5290(9) 2_665 ?
Zr1 Ti1 3.0727(8) 2_665 ?
Zr1 Ti1 3.0727(8) 3_565 ?
C103 C104 1.378(4) . ?
C103 C102 1.382(4) . ?
C101 C102 1.376(4) . ?
C101 C100 1.380(4) . ?
C115 C114 1.379(4) . ?
C115 C110 1.385(4) . ?
C110 C111 1.372(4) . ?
C104 C105 1.375(4) . ?
C100 C105 1.379(4) . ?
C114 C113 1.378(4) . ?
C111 C112 1.375(4) . ?
C113 C112 1.380(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C4 108.0(3) . . ?
O1 C2 C3 108.2(3) . 2_665 ?
O2 C3 C2 109.2(3) . 3_565 ?
O2 C4 C1 108.8(3) . . ?
C12 C11 C15 107.4(3) . . ?
C12 C11 C16 128.1(4) . . ?
C15 C11 C16 124.4(4) . . ?
C12 C11 Ti1 73.33(18) . . ?
C15 C11 Ti1 72.64(18) . . ?
C16 C11 Ti1 121.1(2) . . ?
C13 C12 C11 108.6(3) . . ?
C13 C12 C17 124.7(3) . . ?
C11 C12 C17 126.7(3) . . ?
C13 C12 Ti1 73.26(19) . . ?
C11 C12 Ti1 72.15(18) . . ?
C17 C12 Ti1 123.5(2) . . ?
C12 C13 C14 108.4(3) . . ?
C12 C13 C18 125.1(4) . . ?
C14 C13 C18 126.5(3) . . ?
C12 C13 Ti1 72.68(19) . . ?
C14 C13 Ti1 72.09(19) . . ?
C18 C13 Ti1 123.4(2) . . ?
C13 C14 C15 107.5(3) . . ?
C13 C14 C19 125.7(3) . . ?
C15 C14 C19 126.7(4) . . ?
C13 C14 Ti1 73.52(19) . . ?
C15 C14 Ti1 72.43(19) . . ?
C19 C14 Ti1 121.6(2) . . ?
C11 C15 C14 108.1(3) . . ?
C11 C15 C20 124.8(4) . . ?
C14 C15 C20 127.0(4) . . ?
C11 C15 Ti1 72.65(19) . . ?
C14 C15 Ti1 72.78(19) . . ?
C20 C15 Ti1 123.0(2) . . ?
Zr1 Cl1 K1 88.61(3) . . ?
O2 K1 O2 114.75(4) 2_665 3_565 ?
O2 K1 O2 114.75(4) 2_665 . ?
O2 K1 O2 114.75(4) 3_565 . ?
O2 K1 O1 57.48(7) 2_665 2_665 ?
O2 K1 O1 57.54(7) 3_565 2_665 ?
O2 K1 O1 145.94(8) . 2_665 ?
O2 K1 O1 57.54(7) 2_665 . ?
O2 K1 O1 145.94(8) 3_565 . ?
O2 K1 O1 57.48(7) . . ?
O1 K1 O1 108.33(5) 2_665 . ?
O2 K1 O1 145.94(8) 2_665 3_565 ?
O2 K1 O1 57.48(7) 3_565 3_565 ?
O2 K1 O1 57.54(7) . 3_565 ?
O1 K1 O1 108.33(5) 2_665 3_565 ?
O1 K1 O1 108.33(5) . 3_565 ?
O2 K1 Cl1 81.63(5) 2_665 3_565 ?
O2 K1 Cl1 140.24(6) 3_565 3_565 ?
O2 K1 Cl1 86.30(5) . 3_565 ?
O1 K1 Cl1 121.48(6) 2_665 3_565 ?
O1 K1 Cl1 73.76(5) . 3_565 ?
O1 K1 Cl1 126.91(5) 3_565 3_565 ?
O2 K1 Cl1 86.30(5) 2_665 . ?
O2 K1 Cl1 81.63(5) 3_565 . ?
O2 K1 Cl1 140.24(6) . . ?
O1 K1 Cl1 73.76(5) 2_665 . ?
O1 K1 Cl1 126.91(5) . . ?
O1 K1 Cl1 121.48(6) 3_565 . ?
Cl1 K1 Cl1 62.72(3) 3_565 . ?
O2 K1 Cl1 140.24(6) 2_665 2_665 ?
O2 K1 Cl1 86.30(5) 3_565 2_665 ?
O2 K1 Cl1 81.63(5) . 2_665 ?
O1 K1 Cl1 126.91(5) 2_665 2_665 ?
O1 K1 Cl1 121.48(6) . 2_665 ?
O1 K1 Cl1 73.76(5) 3_565 2_665 ?
Cl1 K1 Cl1 62.72(3) 3_565 2_665 ?
Cl1 K1 Cl1 62.72(3) . 2_665 ?
O2 K1 Zr1 103.47(5) 2_665 . ?
O2 K1 Zr1 103.47(5) 3_565 . ?
O2 K1 Zr1 103.47(5) . . ?
O1 K1 Zr1 110.59(5) 2_665 . ?
O1 K1 Zr1 110.59(5) . . ?
O1 K1 Zr1 110.59(5) 3_565 . ?
Cl1 K1 Zr1 36.94(2) 3_565 . ?
Cl1 K1 Zr1 36.94(2) . . ?
Cl1 K1 Zr1 36.94(2) 2_665 . ?
Ti1 N1 Ti1 93.89(14) . 2_665 ?
Ti1 N1 Ti1 93.89(14) . 3_565 ?
Ti1 N1 Ti1 93.89(14) 2_665 3_565 ?
Ti1 N11 Ti1 90.39(10) . 2_665 ?
Ti1 N11 Zr1 95.26(10) . . ?
Ti1 N11 Zr1 95.24(10) 2_665 . ?
C1 O1 C2 112.3(3) . . ?
C1 O1 K1 108.3(2) . . ?
C2 O1 K1 109.3(2) . . ?
C3 O2 C4 112.0(3) . . ?
C3 O2 K1 119.7(2) . . ?
C4 O2 K1 119.7(2) . . ?
N1 Ti1 N11 87.82(10) . . ?
N1 Ti1 N11 87.80(10) . 3_565 ?
N11 Ti1 N11 89.41(15) . 3_565 ?
N1 Ti1 C15 109.85(13) . . ?
N11 Ti1 C15 154.95(12) . . ?
N11 Ti1 C15 108.31(12) 3_565 . ?
N1 Ti1 C11 99.01(13) . . ?
N11 Ti1 C11 127.53(12) . . ?
N11 Ti1 C11 142.41(12) 3_565 . ?
C15 Ti1 C11 34.71(12) . . ?
N1 Ti1 C14 143.36(12) . . ?
N11 Ti1 C14 128.58(12) . . ?
N11 Ti1 C14 95.65(11) 3_565 . ?
C15 Ti1 C14 34.80(12) . . ?
C11 Ti1 C14 57.80(12) . . ?
N1 Ti1 C12 120.75(12) . . ?
N11 Ti1 C12 98.75(11) . . ?
N11 Ti1 C12 150.37(11) 3_565 . ?
C15 Ti1 C12 57.22(12) . . ?
C11 Ti1 C12 34.52(12) . . ?
C14 Ti1 C12 57.17(12) . . ?
N1 Ti1 C13 154.42(12) . . ?
N11 Ti1 C13 99.32(11) . . ?
N11 Ti1 C13 116.61(11) 3_565 . ?
C15 Ti1 C13 57.22(12) . . ?
C11 Ti1 C13 57.26(12) . . ?
C14 Ti1 C13 34.39(12) . . ?
C12 Ti1 C13 34.07(12) . . ?
N1 Ti1 Ti1 43.05(7) . 2_665 ?
N11 Ti1 Ti1 44.81(7) . 2_665 ?
N11 Ti1 Ti1 89.65(7) 3_565 2_665 ?
C15 Ti1 Ti1 148.15(9) . 2_665 ?
C11 Ti1 Ti1 120.29(9) . 2_665 ?
C14 Ti1 Ti1 171.66(10) . 2_665 ?
C12 Ti1 Ti1 116.13(9) . 2_665 ?
C13 Ti1 Ti1 137.28(9) . 2_665 ?
N1 Ti1 Ti1 43.05(7) . 3_565 ?
N11 Ti1 Ti1 89.66(7) . 3_565 ?
N11 Ti1 Ti1 44.80(7) 3_565 3_565 ?
C15 Ti1 Ti1 115.39(9) . 3_565 ?
C11 Ti1 Ti1 129.39(9) . 3_565 ?
C14 Ti1 Ti1 128.02(10) . 3_565 ?
C12 Ti1 Ti1 161.82(9) . 3_565 ?
C13 Ti1 Ti1 159.68(9) . 3_565 ?
Ti1 Ti1 Ti1 60 2_665 3_565 ?
N1 Ti1 Zr1 90.59(10) . . ?
N11 Ti1 Zr1 44.82(7) . . ?
N11 Ti1 Zr1 44.82(7) 3_565 . ?
C15 Ti1 Zr1 146.90(9) . . ?
C11 Ti1 Zr1 167.79(9) . . ?
C14 Ti1 Zr1 117.21(9) . . ?
C12 Ti1 Zr1 133.37(9) . . ?
C13 Ti1 Zr1 111.83(8) . . ?
Ti1 Ti1 Zr1 62.787(10) 2_665 . ?
Ti1 Ti1 Zr1 62.787(10) 3_565 . ?
N11 Zr1 N11 79.65(10) . 3_565 ?
N11 Zr1 N11 79.65(10) . 2_665 ?
N11 Zr1 N11 79.65(10) 3_565 2_665 ?
N11 Zr1 Cl1 91.78(7) . . ?
N11 Zr1 Cl1 171.43(7) 3_565 . ?
N11 Zr1 Cl1 98.85(7) 2_665 . ?
N11 Zr1 Cl1 98.85(7) . 3_565 ?
N11 Zr1 Cl1 91.78(7) 3_565 3_565 ?
N11 Zr1 Cl1 171.43(7) 2_665 3_565 ?
Cl1 Zr1 Cl1 89.61(3) . 3_565 ?
N11 Zr1 Cl1 171.43(7) . 2_665 ?
N11 Zr1 Cl1 98.85(7) 3_565 2_665 ?
N11 Zr1 Cl1 91.78(7) 2_665 2_665 ?
Cl1 Zr1 Cl1 89.61(3) . 2_665 ?
Cl1 Zr1 Cl1 89.61(3) 3_565 2_665 ?
N11 Zr1 Ti1 39.92(7) . . ?
N11 Zr1 Ti1 39.93(7) 3_565 . ?
N11 Zr1 Ti1 79.57(7) 2_665 . ?
Cl1 Zr1 Ti1 131.53(3) . . ?
Cl1 Zr1 Ti1 93.84(3) 3_565 . ?
Cl1 Zr1 Ti1 138.67(3) 2_665 . ?
N11 Zr1 Ti1 39.93(7) . 2_665 ?
N11 Zr1 Ti1 79.57(7) 3_565 2_665 ?
N11 Zr1 Ti1 39.92(7) 2_665 2_665 ?
Cl1 Zr1 Ti1 93.84(3) . 2_665 ?
Cl1 Zr1 Ti1 138.67(3) 3_565 2_665 ?
Cl1 Zr1 Ti1 131.53(3) 2_665 2_665 ?
Ti1 Zr1 Ti1 54.43(2) . 2_665 ?
N11 Zr1 Ti1 79.57(7) . 3_565 ?
N11 Zr1 Ti1 39.92(7) 3_565 3_565 ?
N11 Zr1 Ti1 39.93(7) 2_665 3_565 ?
Cl1 Zr1 Ti1 138.67(3) . 3_565 ?
Cl1 Zr1 Ti1 131.53(3) 3_565 3_565 ?
Cl1 Zr1 Ti1 93.84(3) 2_665 3_565 ?
Ti1 Zr1 Ti1 54.43(2) . 3_565 ?
Ti1 Zr1 Ti1 54.43(2) 2_665 3_565 ?
N11 Zr1 K1 132.31(6) . . ?
N11 Zr1 K1 132.31(6) 3_565 . ?
N11 Zr1 K1 132.31(6) 2_665 . ?
Cl1 Zr1 K1 54.46(2) . . ?
Cl1 Zr1 K1 54.46(2) 3_565 . ?
Cl1 Zr1 K1 54.46(2) 2_665 . ?
Ti1 Zr1 K1 148.127(12) . . ?
Ti1 Zr1 K1 148.127(12) 2_665 . ?
Ti1 Zr1 K1 148.127(12) 3_565 . ?
C104 C103 C102 119.8(4) . . ?
C102 C101 C100 120.2(4) . . ?
C114 C115 C110 119.2(4) . . ?
C111 C110 C115 120.4(4) . . ?
C105 C104 C103 120.2(4) . . ?
C101 C102 C103 119.9(4) . . ?
C105 C100 C101 119.8(4) . . ?
C113 C114 C115 120.1(4) . . ?
C110 C111 C112 120.4(4) . . ?
C114 C113 C112 120.5(4) . . ?
C104 C105 C100 120.0(4) . . ?
C111 C112 C113 119.4(4) . . ?

# 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 0.333 0.667 0.691 175 27 ' '
2 0.667 0.333 0.309 176 27 ' '
_platon_squeeze_details          
;
Compound 10 crystallized with seven molecules of benzene, which were found in the difference Fourier map 
(two and 1/3 of benzene molecules per asymmetric unit), but it was not possible to get a chemically 
sensible model for one of them, so the Squeeze procedure was employed to its contribution to 
the structure factors.
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Benzene'
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
