# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_E
_database_code_depnum_ccdc_archive 'CCDC 1418229'
_audit_update_record             
;
2015-12-01 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H24 N2'
_chemical_formula_weight         328.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   16.515(2)
_cell_length_b                   45.244(7)
_cell_length_c                   7.7842(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.294(3)
_cell_angle_gamma                90.00
_cell_volume                     5811.8(14)
_cell_formula_units_Z            12
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4208
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      21.65

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2112
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9883
_exptl_absorpt_correction_T_max  0.9921
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            36565
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       55
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.31
_diffrn_reflns_theta_max         26.06
_reflns_number_total             11472
_reflns_number_gt                6575
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0604P)²+1.2253P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11472
_refine_ls_number_parameters     688
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1350
_refine_ls_R_factor_gt           0.0754
_refine_ls_wR_factor_ref         0.1746
_refine_ls_wR_factor_gt          0.1494
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.63713(15) 0.06112(6) 0.9752(3) 0.0441(6) Uani 1 1 d . . .
C2 C 0.57952(17) 0.06361(6) 1.1017(3) 0.0550(7) Uani 1 1 d . . .
H2 H 0.5249 0.0650 1.0688 0.066 Uiso 1 1 calc R . .
C3 C 0.60201(18) 0.06404(7) 1.2731(3) 0.0616(8) Uani 1 1 d . . .
H3 H 0.5625 0.0658 1.3544 0.074 Uiso 1 1 calc R . .
C4 C 0.68202(19) 0.06195(7) 1.3262(4) 0.0666(9) Uani 1 1 d . . .
H4 H 0.6969 0.0623 1.4427 0.080 Uiso 1 1 calc R . .
C5 C 0.73983(17) 0.05941(6) 1.2054(3) 0.0552(7) Uani 1 1 d . . .
H5 H 0.7940 0.0578 1.2420 0.066 Uiso 1 1 calc R . .
C6 C 0.72009(15) 0.05910(6) 1.0298(3) 0.0430(6) Uani 1 1 d . . .
C7 C 0.78475(15) 0.05651(6) 0.9105(3) 0.0465(7) Uani 1 1 d . . .
H7 H 0.8374 0.0551 0.9570 0.056 Uiso 1 1 calc R . .
C8 C 0.53355(15) 0.05720(7) 0.7408(3) 0.0495(7) Uani 1 1 d . . .
C9 C 0.50233(18) 0.02864(7) 0.7268(4) 0.0607(8) Uani 1 1 d . . .
C10 C 0.4239(2) 0.02514(8) 0.6637(4) 0.0767(10) Uani 1 1 d . . .
H10 H 0.4018 0.0063 0.6542 0.092 Uiso 1 1 calc R . .
C11 C 0.3779(2) 0.04924(9) 0.6145(4) 0.0781(10) Uani 1 1 d . . .
H11 H 0.3251 0.0465 0.5714 0.094 Uiso 1 1 calc R . .
C12 C 0.40863(19) 0.07707(8) 0.6281(4) 0.0712(9) Uani 1 1 d . . .
H12 H 0.3767 0.0931 0.5944 0.085 Uiso 1 1 calc R . .
C13 C 0.48777(18) 0.08164(7) 0.6924(3) 0.0576(8) Uani 1 1 d . . .
C14 C 0.5224(2) 0.11234(8) 0.7096(5) 0.0922(11) Uani 1 1 d . . .
H14A H 0.5451 0.1150 0.8239 0.138 Uiso 1 1 calc R . .
H14B H 0.4802 0.1266 0.6878 0.138 Uiso 1 1 calc R . .
H14C H 0.5639 0.1150 0.6281 0.138 Uiso 1 1 calc R . .
C15 C 0.5531(2) 0.00226(8) 0.7793(5) 0.0915(11) Uani 1 1 d . . .
H15A H 0.6038 0.0031 0.7235 0.137 Uiso 1 1 calc R . .
H15B H 0.5249 -0.0155 0.7463 0.137 Uiso 1 1 calc R . .
H15C H 0.5629 0.0024 0.9017 0.137 Uiso 1 1 calc R . .
C16 C 0.84492(15) 0.05421(6) 0.6444(3) 0.0467(7) Uani 1 1 d . . .
C17 C 0.86297(16) 0.02731(7) 0.5662(3) 0.0534(7) Uani 1 1 d . . .
C18 C 0.92820(18) 0.02644(8) 0.4599(4) 0.0627(8) Uani 1 1 d . . .
H18 H 0.9407 0.0088 0.4058 0.075 Uiso 1 1 calc R . .
C19 C 0.97472(18) 0.05094(9) 0.4326(4) 0.0713(9) Uani 1 1 d . . .
H19 H 1.0194 0.0497 0.3638 0.086 Uiso 1 1 calc R . .
C20 C 0.95509(17) 0.07742(8) 0.5074(4) 0.0665(9) Uani 1 1 d . . .
H20 H 0.9865 0.0940 0.4871 0.080 Uiso 1 1 calc R . .
C21 C 0.88935(16) 0.07987(6) 0.6128(3) 0.0525(7) Uani 1 1 d . . .
C22 C 0.8124(2) 0.00032(7) 0.5937(5) 0.0835(10) Uani 1 1 d . . .
H22A H 0.8303 -0.0154 0.5216 0.125 Uiso 1 1 calc R . .
H22B H 0.7566 0.0047 0.5651 0.125 Uiso 1 1 calc R . .
H22C H 0.8179 -0.0056 0.7119 0.125 Uiso 1 1 calc R . .
C23 C 0.8653(2) 0.10926(7) 0.6846(4) 0.0749(9) Uani 1 1 d . . .
H23A H 0.8734 0.1090 0.8074 0.112 Uiso 1 1 calc R . .
H23B H 0.8092 0.1130 0.6554 0.112 Uiso 1 1 calc R . .
H23C H 0.8979 0.1245 0.6370 0.112 Uiso 1 1 calc R . .
C24 C 0.71541(15) 0.18243(6) -0.0348(3) 0.0432(6) Uani 1 1 d . . .
C25 C 0.77518(16) 0.18054(6) -0.1558(3) 0.0519(7) Uani 1 1 d . . .
H25 H 0.8294 0.1801 -0.1187 0.062 Uiso 1 1 calc R . .
C26 C 0.75561(19) 0.17928(7) -0.3285(4) 0.0615(8) Uani 1 1 d . . .
H26 H 0.7967 0.1779 -0.4065 0.074 Uiso 1 1 calc R . .
C27 C 0.6761(2) 0.17999(7) -0.3881(4) 0.0678(9) Uani 1 1 d . . .
H27 H 0.6632 0.1792 -0.5054 0.081 Uiso 1 1 calc R . .
C28 C 0.61622(17) 0.18192(6) -0.2719(3) 0.0572(8) Uani 1 1 d . . .
H28 H 0.5624 0.1825 -0.3120 0.069 Uiso 1 1 calc R . .
C29 C 0.63342(15) 0.18297(6) -0.0952(3) 0.0448(6) Uani 1 1 d . . .
C30 C 0.56621(15) 0.18468(6) 0.0188(3) 0.0465(7) Uani 1 1 d . . .
H30 H 0.5142 0.1840 -0.0314 0.056 Uiso 1 1 calc R . .
C31 C 0.50095(14) 0.18800(6) 0.2790(3) 0.0453(7) Uani 1 1 d . . .
C32 C 0.48095(16) 0.21449(7) 0.3596(3) 0.0533(7) Uani 1 1 d . . .
C33 C 0.41330(19) 0.21489(8) 0.4577(4) 0.0675(9) Uani 1 1 d . . .
H33 H 0.3986 0.2324 0.5106 0.081 Uiso 1 1 calc R . .
C34 C 0.36716(19) 0.19008(9) 0.4792(4) 0.0730(10) Uani 1 1 d . . .
H34 H 0.3215 0.1909 0.5451 0.088 Uiso 1 1 calc R . .
C35 C 0.38859(17) 0.16403(8) 0.4029(4) 0.0655(8) Uani 1 1 d . . .
H35 H 0.3576 0.1472 0.4192 0.079 Uiso 1 1 calc R . .
C36 C 0.45582(16) 0.16244(7) 0.3019(3) 0.0533(7) Uani 1 1 d . . .
C37 C 0.5330(2) 0.24147(7) 0.3408(4) 0.0804(10) Uani 1 1 d . . .
H37A H 0.5094 0.2578 0.3996 0.121 Uiso 1 1 calc R . .
H37B H 0.5366 0.2462 0.2211 0.121 Uiso 1 1 calc R . .
H37C H 0.5863 0.2376 0.3897 0.121 Uiso 1 1 calc R . .
C38 C 0.4791(2) 0.13337(7) 0.2234(5) 0.0829(10) Uani 1 1 d . . .
H38A H 0.4614 0.1330 0.1044 0.124 Uiso 1 1 calc R . .
H38B H 0.4538 0.1175 0.2832 0.124 Uiso 1 1 calc R . .
H38C H 0.5369 0.1311 0.2325 0.124 Uiso 1 1 calc R . .
C39 C 0.81372(15) 0.18641(7) 0.2126(3) 0.0467(7) Uani 1 1 d . . .
C40 C 0.8436(2) 0.21398(7) 0.2608(4) 0.0663(8) Uani 1 1 d . . .
C41 C 0.9205(2) 0.21544(9) 0.3395(4) 0.0860(11) Uani 1 1 d . . .
H41 H 0.9410 0.2337 0.3744 0.103 Uiso 1 1 calc R . .
C42 C 0.9661(2) 0.19101(11) 0.3667(4) 0.0867(12) Uani 1 1 d . . .
H42 H 1.0177 0.1926 0.4185 0.104 Uiso 1 1 calc R . .
C43 C 0.9371(2) 0.16419(9) 0.3186(4) 0.0738(10) Uani 1 1 d . . .
H43 H 0.9693 0.1475 0.3375 0.089 Uiso 1 1 calc R . .
C44 C 0.85994(18) 0.16089(7) 0.2411(3) 0.0570(8) Uani 1 1 d . . .
C45 C 0.7927(3) 0.24128(9) 0.2297(6) 0.1198(15) Uani 1 1 d . . .
H45A H 0.7674 0.2404 0.1166 0.180 Uiso 1 1 calc R . .
H45B H 0.8265 0.2585 0.2392 0.180 Uiso 1 1 calc R . .
H45C H 0.7517 0.2423 0.3136 0.180 Uiso 1 1 calc R . .
C46 C 0.8273(2) 0.13103(8) 0.1938(5) 0.0939(12) Uani 1 1 d . . .
H46A H 0.7792 0.1273 0.2555 0.141 Uiso 1 1 calc R . .
H46B H 0.8673 0.1163 0.2230 0.141 Uiso 1 1 calc R . .
H46C H 0.8145 0.1304 0.0724 0.141 Uiso 1 1 calc R . .
C47 C 0.18091(13) 0.11329(6) 0.2706(3) 0.0374(6) Uani 1 1 d . . .
C48 C 0.18353(15) 0.09174(6) 0.3991(3) 0.0478(7) Uani 1 1 d . . .
H48 H 0.1876 0.0719 0.3691 0.057 Uiso 1 1 calc R . .
C49 C 0.18012(17) 0.09948(7) 0.5693(3) 0.0581(8) Uani 1 1 d . . .
H49 H 0.1820 0.0848 0.6530 0.070 Uiso 1 1 calc R . .
C50 C 0.17397(18) 0.12874(7) 0.6180(3) 0.0621(8) Uani 1 1 d . . .
H50 H 0.1721 0.1338 0.7335 0.074 Uiso 1 1 calc R . .
C51 C 0.17074(15) 0.15016(6) 0.4935(3) 0.0512(7) Uani 1 1 d . . .
H51 H 0.1661 0.1698 0.5262 0.061 Uiso 1 1 calc R . .
C52 C 0.17427(14) 0.14335(6) 0.3191(3) 0.0382(6) Uani 1 1 d . . .
C53 C 0.17017(14) 0.16759(6) 0.1963(3) 0.0417(6) Uani 1 1 d . . .
H53 H 0.1676 0.1867 0.2404 0.050 Uiso 1 1 calc R . .
C54 C 0.17816(16) 0.07623(6) 0.0376(3) 0.0429(6) Uani 1 1 d . . .
C55 C 0.24725(17) 0.05862(7) 0.0262(3) 0.0545(7) Uani 1 1 d . . .
C56 C 0.2367(2) 0.03027(7) -0.0407(4) 0.0735(9) Uani 1 1 d . . .
H56 H 0.2816 0.0180 -0.0497 0.088 Uiso 1 1 calc R . .
C57 C 0.1623(3) 0.02005(8) -0.0933(4) 0.0834(11) Uani 1 1 d . . .
H57 H 0.1568 0.0010 -0.1374 0.100 Uiso 1 1 calc R . .
C58 C 0.0959(2) 0.03766(8) -0.0815(4) 0.0779(10) Uani 1 1 d . . .
H58 H 0.0454 0.0305 -0.1186 0.093 Uiso 1 1 calc R . .
C59 C 0.10213(17) 0.06600(7) -0.0153(3) 0.0552(7) Uani 1 1 d . . .
C60 C 0.32931(19) 0.06988(9) 0.0818(5) 0.0908(11) Uani 1 1 d . . .
H60A H 0.3370 0.0893 0.0349 0.136 Uiso 1 1 calc R . .
H60B H 0.3701 0.0568 0.0411 0.136 Uiso 1 1 calc R . .
H60C H 0.3335 0.0708 0.2051 0.136 Uiso 1 1 calc R . .
C61 C 0.0289(2) 0.08558(9) -0.0051(5) 0.0939(12) Uani 1 1 d . . .
H61A H 0.0318 0.1011 -0.0886 0.141 Uiso 1 1 calc R . .
H61B H 0.0274 0.0940 0.1079 0.141 Uiso 1 1 calc R . .
H61C H -0.0192 0.0741 -0.0280 0.141 Uiso 1 1 calc R . .
C62 C 0.16638(15) 0.19062(5) -0.0721(3) 0.0392(6) Uani 1 1 d . . .
C63 C 0.23762(16) 0.20552(6) -0.1086(3) 0.0467(7) Uani 1 1 d . . .
C64 C 0.23233(19) 0.22964(6) -0.2187(4) 0.0579(8) Uani 1 1 d . . .
H64 H 0.2792 0.2400 -0.2430 0.069 Uiso 1 1 calc R . .
C65 C 0.1596(2) 0.23862(6) -0.2926(4) 0.0604(8) Uani 1 1 d . . .
H65 H 0.1573 0.2548 -0.3660 0.073 Uiso 1 1 calc R . .
C66 C 0.09069(19) 0.22350(6) -0.2571(3) 0.0581(8) Uani 1 1 d . . .
H66 H 0.0415 0.2297 -0.3068 0.070 Uiso 1 1 calc R . .
C67 C 0.09195(15) 0.19905(6) -0.1489(3) 0.0460(7) Uani 1 1 d . . .
C68 C 0.01548(18) 0.18224(8) -0.1161(4) 0.0829(11) Uani 1 1 d . . .
H68A H -0.0033 0.1874 -0.0049 0.124 Uiso 1 1 calc R . .
H68B H 0.0263 0.1614 -0.1199 0.124 Uiso 1 1 calc R . .
H68C H -0.0253 0.1872 -0.2027 0.124 Uiso 1 1 calc R . .
C69 C 0.31848(17) 0.19564(8) -0.0321(4) 0.0794(10) Uani 1 1 d . . .
H69A H 0.3611 0.2060 -0.0872 0.119 Uiso 1 1 calc R . .
H69B H 0.3246 0.1748 -0.0491 0.119 Uiso 1 1 calc R . .
H69C H 0.3212 0.1999 0.0888 0.119 Uiso 1 1 calc R . .
N1 N 0.77565(12) 0.05599(5) 0.7474(3) 0.0511(6) Uani 1 1 d . . .
N2 N 0.61499(12) 0.06094(5) 0.8044(3) 0.0574(6) Uani 1 1 d . . .
H2A H 0.6522 0.0632 0.7313 0.069 Uiso 1 1 calc R . .
N3 N 0.57237(12) 0.18704(5) 0.1826(3) 0.0493(6) Uani 1 1 d . . .
N4 N 0.73394(13) 0.18398(6) 0.1379(3) 0.0597(7) Uani 1 1 d . . .
H4A H 0.6944 0.1834 0.2064 0.072 Uiso 1 1 calc R . .
N5 N 0.16975(13) 0.16488(4) 0.0333(2) 0.0455(5) Uani 1 1 d . . .
N6 N 0.18556(13) 0.10574(5) 0.1004(2) 0.0504(6) Uani 1 1 d . . .
H6 H 0.1934 0.1196 0.0274 0.060 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.365(3) . ?
C1 C2 1.401(3) . ?
C1 C6 1.421(3) . ?
C2 C3 1.370(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.372(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.372(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.393(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.448(3) . ?
C7 N1 1.272(3) . ?
C7 H7 0.9300 . ?
C8 C13 1.383(4) . ?
C8 C9 1.394(4) . ?
C8 N2 1.425(3) . ?
C9 C10 1.376(4) . ?
C9 C15 1.506(4) . ?
C10 C11 1.374(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.360(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.396(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.506(4) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.398(4) . ?
C16 C21 1.401(4) . ?
C16 N1 1.425(3) . ?
C17 C18 1.385(4) . ?
C17 C22 1.499(4) . ?
C18 C19 1.370(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.377(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.391(4) . ?
C20 H20 0.9300 . ?
C21 C23 1.502(4) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 N4 1.368(3) . ?
C24 C25 1.395(3) . ?
C24 C29 1.416(3) . ?
C25 C26 1.371(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.376(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.369(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.394(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.451(3) . ?
C30 N3 1.280(3) . ?
C30 H30 0.9300 . ?
C31 C36 1.391(4) . ?
C31 C32 1.398(4) . ?
C31 N3 1.424(3) . ?
C32 C33 1.379(4) . ?
C32 C37 1.504(4) . ?
C33 C34 1.370(4) . ?
C33 H33 0.9300 . ?
C34 C35 1.373(4) . ?
C34 H34 0.9300 . ?
C35 C36 1.388(4) . ?
C35 H35 0.9300 . ?
C36 C38 1.506(4) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C40 1.387(4) . ?
C39 C44 1.397(4) . ?
C39 N4 1.423(3) . ?
C40 C41 1.389(5) . ?
C40 C45 1.508(5) . ?
C41 C42 1.350(5) . ?
C41 H41 0.9300 . ?
C42 C43 1.352(5) . ?
C42 H42 0.9300 . ?
C43 C44 1.396(4) . ?
C43 H43 0.9300 . ?
C44 C46 1.495(4) . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 N6 1.374(3) . ?
C47 C48 1.396(3) . ?
C47 C52 1.416(3) . ?
C48 C49 1.373(3) . ?
C48 H48 0.9300 . ?
C49 C50 1.382(4) . ?
C49 H49 0.9300 . ?
C50 C51 1.370(4) . ?
C50 H50 0.9300 . ?
C51 C52 1.396(3) . ?
C51 H51 0.9300 . ?
C52 C53 1.455(3) . ?
C53 N5 1.275(3) . ?
C53 H53 0.9300 . ?
C54 C59 1.385(4) . ?
C54 C55 1.397(4) . ?
C54 N6 1.425(3) . ?
C55 C56 1.393(4) . ?
C55 C60 1.495(4) . ?
C56 C57 1.361(5) . ?
C56 H56 0.9300 . ?
C57 C58 1.361(5) . ?
C57 H57 0.9300 . ?
C58 C59 1.384(4) . ?
C58 H58 0.9300 . ?
C59 C61 1.504(4) . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 0.9600 . ?
C62 C63 1.395(3) . ?
C62 C67 1.398(3) . ?
C62 N5 1.424(3) . ?
C63 C64 1.388(4) . ?
C63 C69 1.508(4) . ?
C64 C65 1.372(4) . ?
C64 H64 0.9300 . ?
C65 C66 1.366(4) . ?
C65 H65 0.9300 . ?
C66 C67 1.390(4) . ?
C66 H66 0.9300 . ?
C67 C68 1.505(4) . ?
C68 H68A 0.9600 . ?
C68 H68B 0.9600 . ?
C68 H68C 0.9600 . ?
C69 H69A 0.9600 . ?
C69 H69B 0.9600 . ?
C69 H69C 0.9600 . ?
N2 H2A 0.8600 . ?
N4 H4A 0.8600 . ?
N6 H6 0.8600 . ?

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
N2 C1 C2 121.5(2) . . ?
N2 C1 C6 120.6(2) . . ?
C2 C1 C6 118.0(2) . . ?
C3 C2 C1 121.3(3) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
C2 C3 C4 120.9(3) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 119.2(3) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C5 C6 122.1(3) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C5 C6 C1 118.5(2) . . ?
C5 C6 C7 118.7(2) . . ?
C1 C6 C7 122.7(2) . . ?
N1 C7 C6 125.5(2) . . ?
N1 C7 H7 117.3 . . ?
C6 C7 H7 117.3 . . ?
C13 C8 C9 121.5(3) . . ?
C13 C8 N2 119.9(3) . . ?
C9 C8 N2 118.6(3) . . ?
C10 C9 C8 118.3(3) . . ?
C10 C9 C15 120.8(3) . . ?
C8 C9 C15 120.9(3) . . ?
C11 C10 C9 120.7(3) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C12 C11 C10 120.8(3) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C13 120.4(3) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C8 C13 C12 118.2(3) . . ?
C8 C13 C14 120.8(3) . . ?
C12 C13 C14 121.0(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C9 C15 H15A 109.5 . . ?
C9 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C9 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C21 121.5(2) . . ?
C17 C16 N1 119.0(3) . . ?
C21 C16 N1 119.3(3) . . ?
C18 C17 C16 118.0(3) . . ?
C18 C17 C22 120.9(3) . . ?
C16 C17 C22 121.1(3) . . ?
C19 C18 C17 121.6(3) . . ?
C19 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
C18 C19 C20 119.7(3) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
C19 C20 C21 121.4(3) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C20 C21 C16 117.7(3) . . ?
C20 C21 C23 121.0(3) . . ?
C16 C21 C23 121.3(3) . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N4 C24 C25 122.0(2) . . ?
N4 C24 C29 119.9(2) . . ?
C25 C24 C29 118.0(2) . . ?
C26 C25 C24 121.3(3) . . ?
C26 C25 H25 119.3 . . ?
C24 C25 H25 119.3 . . ?
C25 C26 C27 120.9(3) . . ?
C25 C26 H26 119.5 . . ?
C27 C26 H26 119.5 . . ?
C28 C27 C26 118.9(3) . . ?
C28 C27 H27 120.5 . . ?
C26 C27 H27 120.5 . . ?
C27 C28 C29 122.0(3) . . ?
C27 C28 H28 119.0 . . ?
C29 C28 H28 119.0 . . ?
C28 C29 C24 118.8(2) . . ?
C28 C29 C30 118.4(2) . . ?
C24 C29 C30 122.8(2) . . ?
N3 C30 C29 125.6(2) . . ?
N3 C30 H30 117.2 . . ?
C29 C30 H30 117.2 . . ?
C36 C31 C32 121.2(2) . . ?
C36 C31 N3 120.1(2) . . ?
C32 C31 N3 118.6(3) . . ?
C33 C32 C31 118.1(3) . . ?
C33 C32 C37 121.5(3) . . ?
C31 C32 C37 120.4(3) . . ?
C34 C33 C32 121.6(3) . . ?
C34 C33 H33 119.2 . . ?
C32 C33 H33 119.2 . . ?
C33 C34 C35 119.8(3) . . ?
C33 C34 H34 120.1 . . ?
C35 C34 H34 120.1 . . ?
C34 C35 C36 121.0(3) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 H35 119.5 . . ?
C35 C36 C31 118.3(3) . . ?
C35 C36 C38 119.9(3) . . ?
C31 C36 C38 121.8(3) . . ?
C32 C37 H37A 109.5 . . ?
C32 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C32 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 C44 120.9(3) . . ?
C40 C39 N4 119.6(3) . . ?
C44 C39 N4 119.5(3) . . ?
C39 C40 C41 118.1(3) . . ?
C39 C40 C45 120.2(3) . . ?
C41 C40 C45 121.7(3) . . ?
C42 C41 C40 121.7(4) . . ?
C42 C41 H41 119.2 . . ?
C40 C41 H41 119.2 . . ?
C41 C42 C43 120.1(4) . . ?
C41 C42 H42 119.9 . . ?
C43 C42 H42 119.9 . . ?
C42 C43 C44 121.5(3) . . ?
C42 C43 H43 119.2 . . ?
C44 C43 H43 119.2 . . ?
C43 C44 C39 117.7(3) . . ?
C43 C44 C46 121.1(3) . . ?
C39 C44 C46 121.2(3) . . ?
C40 C45 H45A 109.5 . . ?
C40 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C40 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N6 C47 C48 121.1(2) . . ?
N6 C47 C52 120.2(2) . . ?
C48 C47 C52 118.7(2) . . ?
C49 C48 C47 120.8(3) . . ?
C49 C48 H48 119.6 . . ?
C47 C48 H48 119.6 . . ?
C48 C49 C50 121.0(2) . . ?
C48 C49 H49 119.5 . . ?
C50 C49 H49 119.5 . . ?
C51 C50 C49 119.0(2) . . ?
C51 C50 H50 120.5 . . ?
C49 C50 H50 120.5 . . ?
C50 C51 C52 122.0(3) . . ?
C50 C51 H51 119.0 . . ?
C52 C51 H51 119.0 . . ?
C51 C52 C47 118.5(2) . . ?
C51 C52 C53 118.0(2) . . ?
C47 C52 C53 123.4(2) . . ?
N5 C53 C52 125.4(2) . . ?
N5 C53 H53 117.3 . . ?
C52 C53 H53 117.3 . . ?
C59 C54 C55 121.6(3) . . ?
C59 C54 N6 118.6(2) . . ?
C55 C54 N6 119.8(2) . . ?
C56 C55 C54 117.3(3) . . ?
C56 C55 C60 121.3(3) . . ?
C54 C55 C60 121.3(3) . . ?
C57 C56 C55 121.5(3) . . ?
C57 C56 H56 119.2 . . ?
C55 C56 H56 119.2 . . ?
C56 C57 C58 120.1(3) . . ?
C56 C57 H57 120.0 . . ?
C58 C57 H57 120.0 . . ?
C57 C58 C59 121.3(3) . . ?
C57 C58 H58 119.3 . . ?
C59 C58 H58 119.3 . . ?
C58 C59 C54 118.2(3) . . ?
C58 C59 C61 121.2(3) . . ?
C54 C59 C61 120.6(3) . . ?
C55 C60 H60A 109.5 . . ?
C55 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C55 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C59 C61 H61A 109.5 . . ?
C59 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C59 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C63 C62 C67 121.0(2) . . ?
C63 C62 N5 119.9(2) . . ?
C67 C62 N5 118.9(2) . . ?
C64 C63 C62 118.2(2) . . ?
C64 C63 C69 120.6(3) . . ?
C62 C63 C69 121.2(2) . . ?
C65 C64 C63 121.6(3) . . ?
C65 C64 H64 119.2 . . ?
C63 C64 H64 119.2 . . ?
C66 C65 C64 119.3(3) . . ?
C66 C65 H65 120.4 . . ?
C64 C65 H65 120.4 . . ?
C65 C66 C67 121.9(3) . . ?
C65 C66 H66 119.0 . . ?
C67 C66 H66 119.0 . . ?
C66 C67 C62 117.9(2) . . ?
C66 C67 C68 120.9(3) . . ?
C62 C67 C68 121.3(2) . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C63 C69 H69A 109.5 . . ?
C63 C69 H69B 109.5 . . ?
H69A C69 H69B 109.5 . . ?
C63 C69 H69C 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C7 N1 C16 119.8(2) . . ?
C1 N2 C8 123.5(2) . . ?
C1 N2 H2A 118.3 . . ?
C8 N2 H2A 118.3 . . ?
C30 N3 C31 119.6(2) . . ?
C24 N4 C39 124.9(2) . . ?
C24 N4 H4A 117.5 . . ?
C39 N4 H4A 117.5 . . ?
C53 N5 C62 119.6(2) . . ?
C47 N6 C54 123.8(2) . . ?
C47 N6 H6 118.1 . . ?
C54 N6 H6 118.1 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.06
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.200
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.037
####################################################################### 
# 
# 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_LH2
_database_code_depnum_ccdc_archive 'CCDC 1418230'
_audit_update_record             
;
2015-12-01 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H50 N4'
_chemical_formula_weight         634.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.2174(10)
_cell_length_b                   10.6434(10)
_cell_length_c                   19.4065(18)
_cell_angle_alpha                77.176(2)
_cell_angle_beta                 80.422(2)
_cell_angle_gamma                66.226(2)
_cell_volume                     1876.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    1727
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      23.17

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             684
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9889
_exptl_absorpt_correction_T_max  0.9922
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      185(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10146
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0733
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         26.04
_reflns_number_total             7216
_reflns_number_gt                4425
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0908P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7216
_refine_ls_number_parameters     449
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.0681
_refine_ls_wR_factor_ref         0.1905
_refine_ls_wR_factor_gt          0.1550
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7895(3) 0.7423(2) 0.38315(13) 0.0319(6) Uani 1 1 d . . .
C2 C 0.8411(3) 0.6533(3) 0.44564(14) 0.0392(7) Uani 1 1 d . . .
H21 H 0.9394 0.6235 0.4531 0.047 Uiso 1 1 calc R . .
C3 C 0.7514(3) 0.6080(3) 0.49665(15) 0.0465(8) Uani 1 1 d . . .
H31 H 0.7886 0.5471 0.5388 0.056 Uiso 1 1 calc R . .
C4 C 0.6077(3) 0.6503(3) 0.48711(15) 0.0483(8) Uani 1 1 d . . .
H34 H 0.5460 0.6193 0.5226 0.058 Uiso 1 1 calc R . .
C5 C 0.5548(3) 0.7383(3) 0.42542(14) 0.0411(7) Uani 1 1 d . . .
H26 H 0.4564 0.7668 0.4184 0.049 Uiso 1 1 calc R . .
C6 C 0.6435(3) 0.7856(2) 0.37364(14) 0.0334(6) Uani 1 1 d . . .
C7 C 1.0231(3) 0.7423(3) 0.32192(13) 0.0320(6) Uani 1 1 d . . .
C8 C 1.1023(3) 0.5981(3) 0.32802(14) 0.0384(7) Uani 1 1 d . . .
H17 H 1.0532 0.5361 0.3395 0.046 Uiso 1 1 calc R . .
C9 C 1.2497(3) 0.5453(3) 0.31763(15) 0.0439(7) Uani 1 1 d . . .
H38 H 1.3006 0.4473 0.3220 0.053 Uiso 1 1 calc R . .
C10 C 1.3249(3) 0.6323(3) 0.30099(16) 0.0474(8) Uani 1 1 d . . .
H28 H 1.4268 0.5950 0.2941 0.057 Uiso 1 1 calc R . .
C11 C 1.2492(3) 0.7745(3) 0.29453(15) 0.0438(7) Uani 1 1 d . . .
H32 H 1.3005 0.8346 0.2833 0.053 Uiso 1 1 calc R . .
C12 C 1.0996(3) 0.8325(3) 0.30399(13) 0.0336(6) Uani 1 1 d . . .
C13 C 0.4717(3) 0.9872(3) 0.29885(14) 0.0320(6) Uani 1 1 d . . .
C14 C 0.3917(3) 1.0586(3) 0.35438(15) 0.0423(7) Uani 1 1 d . . .
H19 H 0.4218 1.0242 0.4010 0.051 Uiso 1 1 calc R . .
C15 C 0.2707(3) 1.1774(3) 0.34228(16) 0.0466(7) Uani 1 1 d . . .
H29 H 0.2177 1.2228 0.3809 0.056 Uiso 1 1 calc R . .
C16 C 0.2243(3) 1.2325(3) 0.27470(16) 0.0470(8) Uani 1 1 d . . .
H35 H 0.1407 1.3150 0.2668 0.056 Uiso 1 1 calc R . .
C17 C 0.3018(3) 1.1651(3) 0.21934(15) 0.0394(7) Uani 1 1 d . . .
H12 H 0.2713 1.2031 0.1729 0.047 Uiso 1 1 calc R . .
C18 C 0.4244(3) 1.0419(2) 0.22946(14) 0.0320(6) Uani 1 1 d . . .
C19 C 0.4920(3) 0.9742(3) 0.16858(13) 0.0314(6) Uani 1 1 d . . .
H10 H 0.4599 1.0233 0.1234 0.038 Uiso 1 1 calc R . .
C20 C 1.0305(3) 0.9837(3) 0.29674(14) 0.0352(6) Uani 1 1 d . . .
H14 H 1.0903 1.0349 0.2910 0.042 Uiso 1 1 calc R . .
C21 C 0.8426(3) 1.2002(3) 0.29349(14) 0.0346(6) Uani 1 1 d . . .
C22 C 0.7935(3) 1.2855(3) 0.22964(15) 0.0375(7) Uani 1 1 d . . .
C23 C 0.7423(3) 1.4294(3) 0.22615(16) 0.0453(7) Uani 1 1 d . . .
H36 H 0.7105 1.4896 0.1830 0.054 Uiso 1 1 calc R . .
C24 C 0.7375(3) 1.4850(3) 0.28428(16) 0.0442(7) Uani 1 1 d . . .
H37 H 0.7037 1.5832 0.2807 0.053 Uiso 1 1 calc R . .
C25 C 0.7809(3) 1.4000(3) 0.34774(16) 0.0454(7) Uani 1 1 d . . .
H27 H 0.7744 1.4407 0.3877 0.054 Uiso 1 1 calc R . .
C26 C 0.8345(3) 1.2551(3) 0.35431(15) 0.0387(7) Uani 1 1 d . . .
C27 C 0.7966(3) 1.2242(3) 0.16611(16) 0.0477(8) Uani 1 1 d . . .
H39 H 0.8179 1.1227 0.1829 0.057 Uiso 1 1 calc R . .
C28 C 0.9142(6) 1.2359(6) 0.1109(2) 0.124(2) Uani 1 1 d . . .
H47A H 0.8945 1.3343 0.0915 0.186 Uiso 1 1 calc R . .
H47B H 0.9193 1.1869 0.0727 0.186 Uiso 1 1 calc R . .
H47C H 1.0059 1.1939 0.1324 0.186 Uiso 1 1 calc R . .
C29 C 0.6539(5) 1.2866(5) 0.1342(3) 0.125(2) Uani 1 1 d . . .
H48A H 0.5768 1.2881 0.1720 0.188 Uiso 1 1 calc R . .
H48B H 0.6548 1.2302 0.1004 0.188 Uiso 1 1 calc R . .
H48C H 0.6376 1.3819 0.1096 0.188 Uiso 1 1 calc R . .
C30 C 0.8768(4) 1.1596(3) 0.42516(16) 0.0521(8) Uani 1 1 d . . .
H40 H 0.9732 1.0855 0.4162 0.063 Uiso 1 1 calc R . .
C31 C 0.8896(4) 1.2334(4) 0.48147(18) 0.0800(12) Uani 1 1 d . . .
H46A H 0.9565 1.2803 0.4627 0.120 Uiso 1 1 calc R . .
H46B H 0.9253 1.1648 0.5238 0.120 Uiso 1 1 calc R . .
H46C H 0.7950 1.3024 0.4940 0.120 Uiso 1 1 calc R . .
C32 C 0.7711(4) 1.0875(4) 0.45340(18) 0.0686(10) Uani 1 1 d . . .
H45A H 0.6734 1.1579 0.4571 0.103 Uiso 1 1 calc R . .
H45B H 0.7955 1.0316 0.5003 0.103 Uiso 1 1 calc R . .
H45C H 0.7768 1.0267 0.4208 0.103 Uiso 1 1 calc R . .
C33 C 0.6420(3) 0.7880(2) 0.11002(13) 0.0309(6) Uani 1 1 d . . .
C34 C 0.5457(3) 0.7780(3) 0.06928(14) 0.0346(6) Uani 1 1 d . . .
C35 C 0.6051(3) 0.7150(3) 0.00893(15) 0.0424(7) Uani 1 1 d . . .
H23 H 0.5429 0.7079 -0.0201 0.051 Uiso 1 1 calc R . .
C36 C 0.7503(3) 0.6632(3) -0.00937(15) 0.0439(7) Uani 1 1 d . . .
H18 H 0.7870 0.6258 -0.0519 0.053 Uiso 1 1 calc R . .
C37 C 0.8430(3) 0.6657(3) 0.03424(14) 0.0389(7) Uani 1 1 d . . .
H16 H 0.9436 0.6260 0.0224 0.047 Uiso 1 1 calc R . .
C38 C 0.7914(3) 0.7252(2) 0.09512(13) 0.0312(6) Uani 1 1 d . . .
C39 C 0.3861(3) 0.8180(3) 0.08991(15) 0.0393(7) Uani 1 1 d . . .
H24 H 0.3646 0.8506 0.1366 0.047 Uiso 1 1 calc R . .
C40 C 0.2946(3) 0.9376(3) 0.03647(17) 0.0533(8) Uani 1 1 d . . .
H41A H 0.3151 1.0207 0.0345 0.080 Uiso 1 1 calc R . .
H41B H 0.1927 0.9578 0.0513 0.080 Uiso 1 1 calc R . .
H41C H 0.3176 0.9106 -0.0106 0.080 Uiso 1 1 calc R . .
C41 C 0.3458(3) 0.6908(3) 0.1002(2) 0.0602(9) Uani 1 1 d . . .
H44A H 0.3572 0.6617 0.0544 0.090 Uiso 1 1 calc R . .
H44B H 0.2458 0.7150 0.1201 0.090 Uiso 1 1 calc R . .
H44C H 0.4087 0.6144 0.1328 0.090 Uiso 1 1 calc R . .
C42 C 0.8929(3) 0.7252(3) 0.14376(15) 0.0375(6) Uani 1 1 d . . .
H33 H 0.8426 0.7252 0.1926 0.045 Uiso 1 1 calc R . .
C43 C 0.9238(3) 0.8581(3) 0.12339(18) 0.0530(8) Uani 1 1 d . . .
H42A H 0.9754 0.8606 0.0761 0.079 Uiso 1 1 calc R . .
H42B H 0.9827 0.8596 0.1580 0.079 Uiso 1 1 calc R . .
H42C H 0.8331 0.9394 0.1230 0.079 Uiso 1 1 calc R . .
C44 C 1.0307(3) 0.5959(3) 0.14732(17) 0.0472(8) Uani 1 1 d . . .
H43A H 1.0072 0.5125 0.1591 0.071 Uiso 1 1 calc R . .
H43B H 1.0865 0.5954 0.1839 0.071 Uiso 1 1 calc R . .
H43C H 1.0871 0.5964 0.1013 0.071 Uiso 1 1 calc R . .
H100 H 0.641(3) 0.835(3) 0.2699(14) 0.033(7) Uiso 1 1 d . . .
H101 H 0.830(3) 0.891(4) 0.3139(18) 0.077(11) Uiso 1 1 d . . .
N3 N 0.8951(2) 1.0520(2) 0.29755(11) 0.0361(5) Uani 1 1 d . . .
N1 N 0.8752(2) 0.7965(2) 0.33036(12) 0.0371(6) Uani 1 1 d . . .
N2 N 0.5941(2) 0.8706(2) 0.30843(12) 0.0382(6) Uani 1 1 d . . .
N4 N 0.5927(2) 0.8519(2) 0.17124(10) 0.0301(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.395(4) . ?
C1 C6 1.405(3) . ?
C1 N1 1.412(3) . ?
C2 C3 1.376(4) . ?
C2 H21 0.9500 . ?
C3 C4 1.383(4) . ?
C3 H31 0.9500 . ?
C4 C5 1.383(4) . ?
C4 H34 0.9500 . ?
C5 C6 1.387(4) . ?
C5 H26 0.9500 . ?
C6 N2 1.418(3) . ?
C7 N1 1.378(3) . ?
C7 C8 1.405(3) . ?
C7 C12 1.421(4) . ?
C8 C9 1.375(4) . ?
C8 H17 0.9500 . ?
C9 C10 1.383(4) . ?
C9 H38 0.9500 . ?
C10 C11 1.381(4) . ?
C10 H28 0.9500 . ?
C11 C12 1.395(4) . ?
C11 H32 0.9500 . ?
C12 C20 1.457(3) . ?
C13 N2 1.364(3) . ?
C13 C14 1.406(4) . ?
C13 C18 1.424(4) . ?
C14 C15 1.374(4) . ?
C14 H19 0.9500 . ?
C15 C16 1.389(4) . ?
C15 H29 0.9500 . ?
C16 C17 1.377(4) . ?
C16 H35 0.9500 . ?
C17 C18 1.404(3) . ?
C17 H12 0.9500 . ?
C18 C19 1.449(4) . ?
C19 N4 1.290(3) . ?
C19 H10 0.9500 . ?
C20 N3 1.276(3) . ?
C20 H14 0.9500 . ?
C21 C22 1.397(4) . ?
C21 C26 1.406(4) . ?
C21 N3 1.435(3) . ?
C22 C23 1.394(4) . ?
C22 C27 1.508(4) . ?
C23 C24 1.371(4) . ?
C23 H36 0.9500 . ?
C24 C25 1.377(4) . ?
C24 H37 0.9500 . ?
C25 C26 1.397(4) . ?
C25 H27 0.9500 . ?
C26 C30 1.528(4) . ?
C27 C28 1.497(5) . ?
C27 C29 1.512(5) . ?
C27 H39 1.0000 . ?
C28 H47A 0.9800 . ?
C28 H47B 0.9800 . ?
C28 H47C 0.9800 . ?
C29 H48A 0.9800 . ?
C29 H48B 0.9800 . ?
C29 H48C 0.9800 . ?
C30 C31 1.529(4) . ?
C30 C32 1.530(5) . ?
C30 H40 1.0000 . ?
C31 H46A 0.9800 . ?
C31 H46B 0.9800 . ?
C31 H46C 0.9800 . ?
C32 H45A 0.9800 . ?
C32 H45B 0.9800 . ?
C32 H45C 0.9800 . ?
C33 C38 1.406(3) . ?
C33 C34 1.408(3) . ?
C33 N4 1.418(3) . ?
C34 C35 1.405(4) . ?
C34 C39 1.517(4) . ?
C35 C36 1.373(4) . ?
C35 H23 0.9500 . ?
C36 C37 1.382(4) . ?
C36 H18 0.9500 . ?
C37 C38 1.390(4) . ?
C37 H16 0.9500 . ?
C38 C42 1.514(4) . ?
C39 C41 1.530(4) . ?
C39 C40 1.532(4) . ?
C39 H24 1.0000 . ?
C40 H41A 0.9800 . ?
C40 H41B 0.9800 . ?
C40 H41C 0.9800 . ?
C41 H44A 0.9800 . ?
C41 H44B 0.9800 . ?
C41 H44C 0.9800 . ?
C42 C44 1.519(4) . ?
C42 C43 1.525(4) . ?
C42 H33 1.0000 . ?
C43 H42A 0.9800 . ?
C43 H42B 0.9800 . ?
C43 H42C 0.9800 . ?
C44 H43A 0.9800 . ?
C44 H43B 0.9800 . ?
C44 H43C 0.9800 . ?
N1 H101 0.93(3) . ?
N2 H100 0.89(3) . ?

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
C2 C1 C6 118.4(2) . . ?
C2 C1 N1 123.3(2) . . ?
C6 C1 N1 118.2(2) . . ?
C3 C2 C1 120.9(3) . . ?
C3 C2 H21 119.6 . . ?
C1 C2 H21 119.6 . . ?
C2 C3 C4 120.6(3) . . ?
C2 C3 H31 119.7 . . ?
C4 C3 H31 119.7 . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 H34 120.4 . . ?
C3 C4 H34 120.4 . . ?
C4 C5 C6 120.9(3) . . ?
C4 C5 H26 119.6 . . ?
C6 C5 H26 119.6 . . ?
C5 C6 C1 119.9(2) . . ?
C5 C6 N2 122.2(2) . . ?
C1 C6 N2 117.8(2) . . ?
N1 C7 C8 121.6(2) . . ?
N1 C7 C12 120.3(2) . . ?
C8 C7 C12 118.1(2) . . ?
C9 C8 C7 121.2(3) . . ?
C9 C8 H17 119.4 . . ?
C7 C8 H17 119.4 . . ?
C8 C9 C10 121.1(3) . . ?
C8 C9 H38 119.5 . . ?
C10 C9 H38 119.5 . . ?
C11 C10 C9 118.7(3) . . ?
C11 C10 H28 120.6 . . ?
C9 C10 H28 120.6 . . ?
C10 C11 C12 122.0(3) . . ?
C10 C11 H32 119.0 . . ?
C12 C11 H32 119.0 . . ?
C11 C12 C7 118.9(2) . . ?
C11 C12 C20 117.6(2) . . ?
C7 C12 C20 123.5(2) . . ?
N2 C13 C14 122.8(2) . . ?
N2 C13 C18 119.0(2) . . ?
C14 C13 C18 118.1(2) . . ?
C15 C14 C13 121.1(3) . . ?
C15 C14 H19 119.5 . . ?
C13 C14 H19 119.5 . . ?
C14 C15 C16 121.3(3) . . ?
C14 C15 H29 119.4 . . ?
C16 C15 H29 119.4 . . ?
C17 C16 C15 118.7(3) . . ?
C17 C16 H35 120.7 . . ?
C15 C16 H35 120.7 . . ?
C16 C17 C18 122.0(3) . . ?
C16 C17 H12 119.0 . . ?
C18 C17 H12 119.0 . . ?
C17 C18 C13 118.8(2) . . ?
C17 C18 C19 117.5(2) . . ?
C13 C18 C19 123.6(2) . . ?
N4 C19 C18 124.7(2) . . ?
N4 C19 H10 117.7 . . ?
C18 C19 H10 117.7 . . ?
N3 C20 C12 124.5(2) . . ?
N3 C20 H14 117.7 . . ?
C12 C20 H14 117.7 . . ?
C22 C21 C26 122.1(2) . . ?
C22 C21 N3 118.3(2) . . ?
C26 C21 N3 119.5(2) . . ?
C23 C22 C21 118.0(3) . . ?
C23 C22 C27 120.8(2) . . ?
C21 C22 C27 121.2(2) . . ?
C24 C23 C22 120.8(3) . . ?
C24 C23 H36 119.6 . . ?
C22 C23 H36 119.6 . . ?
C23 C24 C25 120.8(3) . . ?
C23 C24 H37 119.6 . . ?
C25 C24 H37 119.6 . . ?
C24 C25 C26 121.1(3) . . ?
C24 C25 H27 119.5 . . ?
C26 C25 H27 119.5 . . ?
C25 C26 C21 117.2(2) . . ?
C25 C26 C30 121.7(3) . . ?
C21 C26 C30 121.0(2) . . ?
C28 C27 C22 111.7(3) . . ?
C28 C27 C29 110.6(4) . . ?
C22 C27 C29 112.7(3) . . ?
C28 C27 H39 107.2 . . ?
C22 C27 H39 107.2 . . ?
C29 C27 H39 107.2 . . ?
C27 C28 H47A 109.5 . . ?
C27 C28 H47B 109.5 . . ?
H47A C28 H47B 109.5 . . ?
C27 C28 H47C 109.5 . . ?
H47A C28 H47C 109.5 . . ?
H47B C28 H47C 109.5 . . ?
C27 C29 H48A 109.5 . . ?
C27 C29 H48B 109.5 . . ?
H48A C29 H48B 109.5 . . ?
C27 C29 H48C 109.5 . . ?
H48A C29 H48C 109.5 . . ?
H48B C29 H48C 109.5 . . ?
C26 C30 C31 113.9(2) . . ?
C26 C30 C32 110.3(3) . . ?
C31 C30 C32 110.0(3) . . ?
C26 C30 H40 107.5 . . ?
C31 C30 H40 107.5 . . ?
C32 C30 H40 107.5 . . ?
C30 C31 H46A 109.5 . . ?
C30 C31 H46B 109.5 . . ?
H46A C31 H46B 109.5 . . ?
C30 C31 H46C 109.5 . . ?
H46A C31 H46C 109.5 . . ?
H46B C31 H46C 109.5 . . ?
C30 C32 H45A 109.5 . . ?
C30 C32 H45B 109.5 . . ?
H45A C32 H45B 109.5 . . ?
C30 C32 H45C 109.5 . . ?
H45A C32 H45C 109.5 . . ?
H45B C32 H45C 109.5 . . ?
C38 C33 C34 121.4(2) . . ?
C38 C33 N4 117.0(2) . . ?
C34 C33 N4 121.4(2) . . ?
C35 C34 C33 117.0(2) . . ?
C35 C34 C39 118.3(2) . . ?
C33 C34 C39 124.5(2) . . ?
C36 C35 C34 121.9(3) . . ?
C36 C35 H23 119.0 . . ?
C34 C35 H23 119.0 . . ?
C35 C36 C37 119.8(3) . . ?
C35 C36 H18 120.1 . . ?
C37 C36 H18 120.1 . . ?
C36 C37 C38 121.1(3) . . ?
C36 C37 H16 119.5 . . ?
C38 C37 H16 119.5 . . ?
C37 C38 C33 118.4(2) . . ?
C37 C38 C42 121.1(2) . . ?
C33 C38 C42 120.5(2) . . ?
C34 C39 C41 110.5(2) . . ?
C34 C39 C40 112.4(2) . . ?
C41 C39 C40 111.0(2) . . ?
C34 C39 H24 107.6 . . ?
C41 C39 H24 107.6 . . ?
C40 C39 H24 107.6 . . ?
C39 C40 H41A 109.5 . . ?
C39 C40 H41B 109.5 . . ?
H41A C40 H41B 109.5 . . ?
C39 C40 H41C 109.5 . . ?
H41A C40 H41C 109.5 . . ?
H41B C40 H41C 109.5 . . ?
C39 C41 H44A 109.5 . . ?
C39 C41 H44B 109.5 . . ?
H44A C41 H44B 109.5 . . ?
C39 C41 H44C 109.5 . . ?
H44A C41 H44C 109.5 . . ?
H44B C41 H44C 109.5 . . ?
C38 C42 C44 112.9(2) . . ?
C38 C42 C43 110.8(2) . . ?
C44 C42 C43 111.5(2) . . ?
C38 C42 H33 107.1 . . ?
C44 C42 H33 107.1 . . ?
C43 C42 H33 107.1 . . ?
C42 C43 H42A 109.5 . . ?
C42 C43 H42B 109.5 . . ?
H42A C43 H42B 109.5 . . ?
C42 C43 H42C 109.5 . . ?
H42A C43 H42C 109.5 . . ?
H42B C43 H42C 109.5 . . ?
C42 C44 H43A 109.5 . . ?
C42 C44 H43B 109.5 . . ?
H43A C44 H43B 109.5 . . ?
C42 C44 H43C 109.5 . . ?
H43A C44 H43C 109.5 . . ?
H43B C44 H43C 109.5 . . ?
C20 N3 C21 118.0(2) . . ?
C7 N1 C1 125.7(2) . . ?
C7 N1 H101 116(2) . . ?
C1 N1 H101 113(2) . . ?
C13 N2 C6 127.3(2) . . ?
C13 N2 H100 117.0(16) . . ?
C6 N2 H100 114.8(16) . . ?
C19 N4 C33 120.6(2) . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        26.04
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.078
####################################################################### 
# 
# 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_Complex_1a
_database_code_depnum_ccdc_archive 'CCDC 1418231'
_audit_update_record             
;
2015-12-01 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44.50 H49 Cl3 N4 Ti'
_chemical_formula_weight         794.13

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.7714(8)
_cell_length_b                   11.1493(8)
_cell_length_c                   19.3176(14)
_cell_angle_alpha                100.5720(10)
_cell_angle_beta                 101.7320(10)
_cell_angle_gamma                104.8770(10)
_cell_volume                     2126.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    3158
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      25.93

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             834
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8976
_exptl_absorpt_correction_T_max  0.9161
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      185(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11488
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         26.06
_reflns_number_total             8188
_reflns_number_gt                6414
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0771P)²+1.1596P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8188
_refine_ls_number_parameters     486
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0573
_refine_ls_wR_factor_ref         0.1612
_refine_ls_wR_factor_gt          0.1404
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8294(3) 0.3764(3) 0.27200(16) 0.0271(7) Uani 1 1 d . . .
C2 C 0.9527(3) 0.3589(4) 0.26993(18) 0.0380(8) Uani 1 1 d . . .
H2 H 0.9590 0.2971 0.2309 0.046 Uiso 1 1 calc R . .
C3 C 1.0656(4) 0.4319(4) 0.3249(2) 0.0511(11) Uani 1 1 d . . .
H3 H 1.1496 0.4207 0.3233 0.061 Uiso 1 1 calc R . .
C4 C 1.0561(4) 0.5219(5) 0.3826(2) 0.0578(12) Uani 1 1 d . . .
H4 H 1.1345 0.5743 0.4189 0.069 Uiso 1 1 calc R . .
C5 C 0.9353(4) 0.5356(4) 0.38735(18) 0.0444(10) Uani 1 1 d . . .
H5 H 0.9300 0.5968 0.4270 0.053 Uiso 1 1 calc R . .
C6 C 0.8191(3) 0.4590(3) 0.33351(16) 0.0289(7) Uani 1 1 d . . .
C7 C 0.6623(3) 0.5381(3) 0.38707(16) 0.0308(7) Uani 1 1 d . . .
C8 C 0.7032(4) 0.5380(4) 0.46025(17) 0.0447(10) Uani 1 1 d . . .
H8 H 0.7522 0.4823 0.4736 0.054 Uiso 1 1 calc R . .
C9 C 0.6731(4) 0.6184(4) 0.51375(19) 0.0549(11) Uani 1 1 d . . .
H9 H 0.7004 0.6163 0.5634 0.066 Uiso 1 1 calc R . .
C10 C 0.6038(4) 0.7014(4) 0.4957(2) 0.0516(11) Uani 1 1 d . . .
H10 H 0.5830 0.7559 0.5326 0.062 Uiso 1 1 calc R . .
C11 C 0.5651(4) 0.7045(3) 0.42403(19) 0.0408(9) Uani 1 1 d . . .
H11 H 0.5198 0.7634 0.4116 0.049 Uiso 1 1 calc R . .
C12 C 0.5915(3) 0.6218(3) 0.36891(16) 0.0299(7) Uani 1 1 d . . .
C13 C 0.5515(3) 0.6314(3) 0.29426(16) 0.0268(7) Uani 1 1 d . . .
H13 H 0.5329 0.7080 0.2876 0.032 Uiso 1 1 calc R . .
C14 C 0.5075(3) 0.5860(3) 0.16866(15) 0.0235(6) Uani 1 1 d . . .
C15 C 0.6096(3) 0.6254(3) 0.13531(17) 0.0274(7) Uani 1 1 d . . .
C16 C 0.5778(3) 0.6634(3) 0.07109(18) 0.0336(7) Uani 1 1 d . . .
H16 H 0.6449 0.6894 0.0470 0.040 Uiso 1 1 calc R . .
C17 C 0.4494(4) 0.6640(3) 0.04186(18) 0.0366(8) Uani 1 1 d . . .
H17 H 0.4293 0.6912 -0.0017 0.044 Uiso 1 1 calc R . .
C18 C 0.3510(3) 0.6251(3) 0.07575(19) 0.0359(8) Uani 1 1 d . . .
H18 H 0.2638 0.6272 0.0554 0.043 Uiso 1 1 calc R . .
C19 C 0.3759(3) 0.5828(3) 0.13899(17) 0.0283(7) Uani 1 1 d . . .
C20 C 0.7508(3) 0.6270(3) 0.16914(18) 0.0332(7) Uani 1 1 d . . .
H20 H 0.7437 0.5528 0.1920 0.040 Uiso 1 1 calc R . .
C21 C 0.8312(4) 0.6108(4) 0.1137(2) 0.0487(10) Uani 1 1 d . . .
H21A H 0.7833 0.5320 0.0754 0.073 Uiso 1 1 calc R . .
H21B H 0.9182 0.6058 0.1381 0.073 Uiso 1 1 calc R . .
H21C H 0.8439 0.6843 0.0919 0.073 Uiso 1 1 calc R . .
C22 C 0.8254(4) 0.7489(4) 0.2301(2) 0.0582(12) Uani 1 1 d . . .
H22A H 0.8315 0.8240 0.2099 0.087 Uiso 1 1 calc R . .
H22B H 0.9152 0.7466 0.2514 0.087 Uiso 1 1 calc R . .
H22C H 0.7773 0.7540 0.2679 0.087 Uiso 1 1 calc R . .
C23 C 0.2638(3) 0.5325(3) 0.17262(19) 0.0366(8) Uani 1 1 d . . .
H23 H 0.2985 0.4904 0.2105 0.044 Uiso 1 1 calc R . .
C24 C 0.2200(4) 0.6411(5) 0.2110(3) 0.0614(12) Uani 1 1 d . . .
H24A H 0.2957 0.7011 0.2497 0.092 Uiso 1 1 calc R . .
H24B H 0.1480 0.6053 0.2323 0.092 Uiso 1 1 calc R . .
H24C H 0.1883 0.6863 0.1755 0.092 Uiso 1 1 calc R . .
C25 C 0.1455(4) 0.4311(4) 0.1160(2) 0.0563(11) Uani 1 1 d . . .
H25A H 0.1067 0.4704 0.0792 0.085 Uiso 1 1 calc R . .
H25B H 0.0782 0.3953 0.1402 0.085 Uiso 1 1 calc R . .
H25C H 0.1757 0.3625 0.0923 0.085 Uiso 1 1 calc R . .
C26 C 0.7042(3) 0.2280(3) 0.15707(15) 0.0241(6) Uani 1 1 d . . .
C27 C 0.7856(3) 0.2588(3) 0.11169(16) 0.0300(7) Uani 1 1 d . . .
H27 H 0.8434 0.3437 0.1216 0.036 Uiso 1 1 calc R . .
C28 C 0.7832(3) 0.1670(4) 0.05216(17) 0.0348(8) Uani 1 1 d . . .
H28 H 0.8402 0.1897 0.0219 0.042 Uiso 1 1 calc R . .
C29 C 0.6999(4) 0.0436(4) 0.03590(18) 0.0406(9) Uani 1 1 d . . .
H29 H 0.6995 -0.0187 -0.0050 0.049 Uiso 1 1 calc R . .
C30 C 0.6170(3) 0.0114(3) 0.07986(17) 0.0350(8) Uani 1 1 d . . .
H30 H 0.5600 -0.0740 0.0693 0.042 Uiso 1 1 calc R . .
C31 C 0.6156(3) 0.1032(3) 0.14010(16) 0.0274(7) Uani 1 1 d . . .
C32 C 0.5303(3) 0.0636(3) 0.18622(16) 0.0277(7) Uani 1 1 d . . .
H32 H 0.4954 -0.0259 0.1811 0.033 Uiso 1 1 calc R . .
C33 C 0.4271(3) 0.0730(3) 0.27964(17) 0.0301(7) Uani 1 1 d . . .
C34 C 0.5062(4) 0.0636(3) 0.34483(17) 0.0349(8) Uani 1 1 d . . .
C35 C 0.4401(5) -0.0034(3) 0.38748(19) 0.0466(10) Uani 1 1 d . . .
H35 H 0.4902 -0.0134 0.4314 0.056 Uiso 1 1 calc R . .
C36 C 0.3029(5) -0.0558(4) 0.3674(2) 0.0529(11) Uani 1 1 d . . .
H36 H 0.2602 -0.1028 0.3968 0.064 Uiso 1 1 calc R . .
C37 C 0.2283(4) -0.0399(4) 0.3049(2) 0.0447(9) Uani 1 1 d . . .
H37 H 0.1341 -0.0745 0.2923 0.054 Uiso 1 1 calc R . .
C38 C 0.2877(3) 0.0255(3) 0.25975(18) 0.0330(7) Uani 1 1 d . . .
C39 C 0.2052(3) 0.0435(3) 0.19101(19) 0.0370(8) Uani 1 1 d . . .
H39 H 0.2638 0.1124 0.1751 0.044 Uiso 1 1 calc R . .
C40 C 0.0862(4) 0.0865(4) 0.2037(2) 0.0537(10) Uani 1 1 d . . .
H40A H 0.0252 0.0196 0.2178 0.081 Uiso 1 1 calc R . .
H40B H 0.0396 0.1019 0.1586 0.081 Uiso 1 1 calc R . .
H40C H 0.1175 0.1657 0.2426 0.081 Uiso 1 1 calc R . .
C41 C 0.1578(4) -0.0779(4) 0.1290(2) 0.0491(10) Uani 1 1 d . . .
H41A H 0.2351 -0.1008 0.1183 0.074 Uiso 1 1 calc R . .
H41B H 0.1061 -0.0626 0.0853 0.074 Uiso 1 1 calc R . .
H41C H 0.1019 -0.1481 0.1434 0.074 Uiso 1 1 calc R . .
C42 C 0.6559(4) 0.1216(4) 0.36575(19) 0.0436(9) Uani 1 1 d . . .
H42 H 0.6771 0.1923 0.3407 0.052 Uiso 1 1 calc R . .
C43 C 0.7254(5) 0.0257(5) 0.3409(3) 0.0663(13) Uani 1 1 d . . .
H43A H 0.7111 -0.0421 0.3670 0.100 Uiso 1 1 calc R . .
H43B H 0.8210 0.0693 0.3515 0.100 Uiso 1 1 calc R . .
H43C H 0.6890 -0.0120 0.2883 0.100 Uiso 1 1 calc R . .
C44 C 0.7122(5) 0.1804(5) 0.4486(2) 0.0708(14) Uani 1 1 d . . .
H44A H 0.6663 0.2414 0.4646 0.106 Uiso 1 1 calc R . .
H44B H 0.8077 0.2250 0.4594 0.106 Uiso 1 1 calc R . .
H44C H 0.6984 0.1122 0.4744 0.106 Uiso 1 1 calc R . .
C45 C 0.9280(12) 0.9426(13) 0.5246(7) 0.107(5) Uani 0.50 1 d P . .
H45A H 0.9507 0.8954 0.5616 0.128 Uiso 0.50 1 calc PR . .
H45B H 0.8315 0.9327 0.5142 0.128 Uiso 0.50 1 calc PR . .
Cl1 Cl 0.38272(8) 0.34132(7) 0.30528(4) 0.0310(2) Uani 1 1 d . . .
Cl2 Cl 0.42789(7) 0.28927(7) 0.11837(4) 0.02681(19) Uani 1 1 d . . .
Cl3 Cl 0.9723(2) 0.8860(2) 0.44336(14) 0.1735(12) Uani 1 1 d . . .
N1 N 0.7083(2) 0.3188(2) 0.21984(13) 0.0237(5) Uani 1 1 d . . .
N2 N 0.6868(3) 0.4544(2) 0.33145(12) 0.0262(6) Uani 1 1 d . . .
N3 N 0.5388(2) 0.5463(2) 0.23602(13) 0.0226(5) Uani 1 1 d . . .
N4 N 0.4970(2) 0.1387(2) 0.23384(13) 0.0249(5) Uani 1 1 d . . .
Ti1 Ti 0.54254(5) 0.34897(5) 0.24098(3) 0.02085(15) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.388(4) . ?
C1 C2 1.398(4) . ?
C1 C6 1.406(4) . ?
C2 C3 1.385(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.396(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.368(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.405(5) . ?
C5 H5 0.9500 . ?
C6 N2 1.405(4) . ?
C7 C8 1.393(4) . ?
C7 C12 1.397(4) . ?
C7 N2 1.404(4) . ?
C8 C9 1.387(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.379(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.372(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.401(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.451(4) . ?
C13 N3 1.290(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.400(4) . ?
C14 C19 1.405(4) . ?
C14 N3 1.453(4) . ?
C15 C16 1.390(4) . ?
C15 C20 1.523(4) . ?
C16 C17 1.385(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.375(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.389(4) . ?
C18 H18 0.9500 . ?
C19 C23 1.517(4) . ?
C20 C21 1.522(5) . ?
C20 C22 1.531(5) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C25 1.529(5) . ?
C23 C24 1.531(5) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.387(4) . ?
C26 C31 1.406(4) . ?
C26 N1 1.415(4) . ?
C27 C28 1.383(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.375(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.380(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.407(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.450(4) . ?
C32 N4 1.297(4) . ?
C32 H32 0.9500 . ?
C33 C38 1.402(5) . ?
C33 C34 1.407(4) . ?
C33 N4 1.453(4) . ?
C34 C35 1.391(5) . ?
C34 C42 1.512(5) . ?
C35 C36 1.384(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.376(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.386(5) . ?
C37 H37 0.9500 . ?
C38 C39 1.518(5) . ?
C39 C41 1.526(5) . ?
C39 C40 1.527(5) . ?
C39 H39 1.0000 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.517(5) . ?
C42 C44 1.541(5) . ?
C42 H42 1.0000 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 Cl3 1.785(13) . ?
C45 Cl3 1.852(14) 2_776 ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
Cl1 Ti1 2.3122(9) . ?
Cl2 Ti1 2.3212(8) . ?
Cl3 C45 1.852(14) 2_776 ?
N1 Ti1 2.006(2) . ?
N2 Ti1 2.014(2) . ?
N3 Ti1 2.230(2) . ?
N4 Ti1 2.240(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 127.9(3) . . ?
N1 C1 C6 112.6(3) . . ?
C2 C1 C6 119.4(3) . . ?
C3 C2 C1 119.9(3) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 120.0(3) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.8(3) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 119.9(3) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
N2 C6 C5 127.9(3) . . ?
N2 C6 C1 112.6(3) . . ?
C5 C6 C1 119.4(3) . . ?
C8 C7 C12 118.6(3) . . ?
C8 C7 N2 121.9(3) . . ?
C12 C7 N2 119.5(3) . . ?
C9 C8 C7 120.6(3) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C10 C9 C8 120.7(3) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C11 C10 C9 119.4(3) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C10 C11 C12 120.9(3) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C7 C12 C11 119.8(3) . . ?
C7 C12 C13 121.5(3) . . ?
C11 C12 C13 118.5(3) . . ?
N3 C13 C12 126.4(3) . . ?
N3 C13 H13 116.8 . . ?
C12 C13 H13 116.8 . . ?
C15 C14 C19 122.3(3) . . ?
C15 C14 N3 118.8(3) . . ?
C19 C14 N3 119.0(3) . . ?
C16 C15 C14 117.9(3) . . ?
C16 C15 C20 121.5(3) . . ?
C14 C15 C20 120.6(3) . . ?
C17 C16 C15 120.7(3) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C18 C17 C16 120.2(3) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C17 C18 C19 121.6(3) . . ?
C17 C18 H18 119.2 . . ?
C19 C18 H18 119.2 . . ?
C18 C19 C14 117.2(3) . . ?
C18 C19 C23 120.6(3) . . ?
C14 C19 C23 122.2(3) . . ?
C21 C20 C15 113.4(3) . . ?
C21 C20 C22 110.1(3) . . ?
C15 C20 C22 111.2(3) . . ?
C21 C20 H20 107.3 . . ?
C15 C20 H20 107.3 . . ?
C22 C20 H20 107.3 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C23 C25 111.5(3) . . ?
C19 C23 C24 111.6(3) . . ?
C25 C23 C24 110.9(3) . . ?
C19 C23 H23 107.5 . . ?
C25 C23 H23 107.5 . . ?
C24 C23 H23 107.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C31 119.0(3) . . ?
C27 C26 N1 121.7(3) . . ?
C31 C26 N1 119.4(3) . . ?
C28 C27 C26 120.6(3) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C29 C28 C27 121.3(3) . . ?
C29 C28 H28 119.4 . . ?
C27 C28 H28 119.4 . . ?
C28 C29 C30 119.1(3) . . ?
C28 C29 H29 120.5 . . ?
C30 C29 H29 120.5 . . ?
C29 C30 C31 121.0(3) . . ?
C29 C30 H30 119.5 . . ?
C31 C30 H30 119.5 . . ?
C26 C31 C30 119.1(3) . . ?
C26 C31 C32 121.8(3) . . ?
C30 C31 C32 118.9(3) . . ?
N4 C32 C31 126.2(3) . . ?
N4 C32 H32 116.9 . . ?
C31 C32 H32 116.9 . . ?
C38 C33 C34 122.7(3) . . ?
C38 C33 N4 120.7(3) . . ?
C34 C33 N4 116.6(3) . . ?
C35 C34 C33 116.8(3) . . ?
C35 C34 C42 122.3(3) . . ?
C33 C34 C42 120.9(3) . . ?
C36 C35 C34 121.5(3) . . ?
C36 C35 H35 119.3 . . ?
C34 C35 H35 119.3 . . ?
C37 C36 C35 120.1(3) . . ?
C37 C36 H36 119.9 . . ?
C35 C36 H36 119.9 . . ?
C36 C37 C38 121.4(4) . . ?
C36 C37 H37 119.3 . . ?
C38 C37 H37 119.3 . . ?
C37 C38 C33 117.4(3) . . ?
C37 C38 C39 121.3(3) . . ?
C33 C38 C39 121.3(3) . . ?
C38 C39 C41 111.6(3) . . ?
C38 C39 C40 112.7(3) . . ?
C41 C39 C40 109.9(3) . . ?
C38 C39 H39 107.5 . . ?
C41 C39 H39 107.5 . . ?
C40 C39 H39 107.5 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C34 C42 C43 112.4(3) . . ?
C34 C42 C44 111.8(3) . . ?
C43 C42 C44 109.7(3) . . ?
C34 C42 H42 107.6 . . ?
C43 C42 H42 107.6 . . ?
C44 C42 H42 107.6 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
Cl3 C45 Cl3 104.3(8) . 2_776 ?
Cl3 C45 H45A 110.9 . . ?
Cl3 C45 H45A 110.9 2_776 . ?
Cl3 C45 H45B 110.9 . . ?
Cl3 C45 H45B 110.9 2_776 . ?
H45A C45 H45B 108.9 . . ?
C45 Cl3 C45 75.7(8) . 2_776 ?
C1 N1 C26 118.0(2) . . ?
C1 N1 Ti1 119.54(19) . . ?
C26 N1 Ti1 121.97(19) . . ?
C7 N2 C6 118.8(2) . . ?
C7 N2 Ti1 121.9(2) . . ?
C6 N2 Ti1 118.51(18) . . ?
C13 N3 C14 114.4(2) . . ?
C13 N3 Ti1 121.0(2) . . ?
C14 N3 Ti1 124.22(17) . . ?
C32 N4 C33 113.7(3) . . ?
C32 N4 Ti1 121.7(2) . . ?
C33 N4 Ti1 124.60(18) . . ?
N1 Ti1 N2 76.36(10) . . ?
N1 Ti1 N3 110.89(10) . . ?
N2 Ti1 N3 79.09(9) . . ?
N1 Ti1 N4 79.40(10) . . ?
N2 Ti1 N4 111.82(10) . . ?
N3 Ti1 N4 167.02(9) . . ?
N1 Ti1 Cl1 154.49(8) . . ?
N2 Ti1 Cl1 90.90(7) . . ?
N3 Ti1 Cl1 87.69(7) . . ?
N4 Ti1 Cl1 85.19(7) . . ?
N1 Ti1 Cl2 93.13(7) . . ?
N2 Ti1 Cl2 156.64(8) . . ?
N3 Ti1 Cl2 85.52(6) . . ?
N4 Ti1 Cl2 86.04(7) . . ?
Cl1 Ti1 Cl2 106.04(3) . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        26.06
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.093
####################################################################### 
# 
# 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_Complex_1b
_database_code_depnum_ccdc_archive 'CCDC 1418232'
_audit_update_record             
;
2015-12-01 deposited with the CCDC.
2015-12-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44.50 H49 Cl3 N4 Zr'
_chemical_formula_weight         837.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.8808(13)
_cell_length_b                   11.2260(13)
_cell_length_c                   19.417(2)
_cell_angle_alpha                100.183(2)
_cell_angle_beta                 103.090(2)
_cell_angle_gamma                104.971(2)
_cell_volume                     2160.8(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    1549
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      21.33

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             870
_exptl_absorpt_coefficient_mu    0.474
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8826
_exptl_absorpt_correction_T_max  0.8947
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      185(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11353
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.1158
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         26.01
_reflns_number_total             8262
_reflns_number_gt                5494
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1246P)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_extinction_coef       ?
_refine_ls_number_reflns         8262
_refine_ls_number_parameters     476
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1317
_refine_ls_R_factor_gt           0.0844
_refine_ls_wR_factor_ref         0.2403
_refine_ls_wR_factor_gt          0.2013
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8358(7) 0.9723(7) 0.8342(4) 0.0322(16) Uani 1 1 d . . .
C2 C 0.9545(8) 1.0548(8) 0.8842(4) 0.0414(19) Uani 1 1 d . . .
H2 H 0.9520 1.1216 0.9209 0.050 Uiso 1 1 calc R . .
C3 C 1.0753(8) 1.0397(8) 0.8804(5) 0.048(2) Uani 1 1 d . . .
H3 H 1.1555 1.0959 0.9144 0.058 Uiso 1 1 calc R . .
C4 C 1.0786(7) 0.9427(8) 0.8272(4) 0.044(2) Uani 1 1 d . . .
H4 H 1.1612 0.9304 0.8256 0.053 Uiso 1 1 calc R . .
C5 C 0.9638(7) 0.8635(8) 0.7764(4) 0.0373(18) Uani 1 1 d . . .
H5 H 0.9676 0.7956 0.7409 0.045 Uiso 1 1 calc R . .
C6 C 0.8417(7) 0.8815(7) 0.7762(4) 0.0290(15) Uani 1 1 d . . .
C7 C 0.7106(6) 0.7242(6) 0.6625(4) 0.0236(14) Uani 1 1 d . . .
C8 C 0.7938(7) 0.7547(7) 0.6188(4) 0.0302(16) Uani 1 1 d . . .
H8 H 0.8550 0.8380 0.6310 0.036 Uiso 1 1 calc R . .
C9 C 0.7891(8) 0.6661(8) 0.5582(4) 0.0400(19) Uani 1 1 d . . .
H9 H 0.8461 0.6892 0.5290 0.048 Uiso 1 1 calc R . .
C10 C 0.7016(8) 0.5438(8) 0.5399(4) 0.042(2) Uani 1 1 d . . .
H10 H 0.6994 0.4823 0.4988 0.051 Uiso 1 1 calc R . .
C11 C 0.6177(7) 0.5122(7) 0.5820(4) 0.0358(18) Uani 1 1 d . . .
H11 H 0.5577 0.4282 0.5691 0.043 Uiso 1 1 calc R . .
C12 C 0.6182(7) 0.6004(6) 0.6432(4) 0.0291(15) Uani 1 1 d . . .
C13 C 0.5311(7) 0.5582(6) 0.6855(4) 0.0301(16) Uani 1 1 d . . .
H13 H 0.4961 0.4689 0.6792 0.036 Uiso 1 1 calc R . .
C14 C 0.6831(7) 1.0568(7) 0.8881(4) 0.0311(16) Uani 1 1 d . . .
C15 C 0.7370(9) 1.0641(8) 0.9615(4) 0.047(2) Uani 1 1 d . . .
H15 H 0.7942 1.0156 0.9748 0.056 Uiso 1 1 calc R . .
C16 C 0.7087(9) 1.1400(9) 1.0144(4) 0.054(2) Uani 1 1 d . . .
H16 H 0.7471 1.1446 1.0642 0.064 Uiso 1 1 calc R . .
C17 C 0.6245(10) 1.2110(9) 0.9967(5) 0.062(3) Uani 1 1 d . . .
H17 H 0.6027 1.2609 1.0342 0.074 Uiso 1 1 calc R . .
C18 C 0.5736(9) 1.2091(8) 0.9260(4) 0.043(2) Uani 1 1 d . . .
H18 H 0.5198 1.2613 0.9143 0.052 Uiso 1 1 calc R . .
C19 C 0.5994(7) 1.1312(6) 0.8700(4) 0.0290(15) Uani 1 1 d . . .
C20 C 0.5492(7) 1.1373(7) 0.7956(4) 0.0326(17) Uani 1 1 d . . .
H20 H 0.5259 1.2113 0.7892 0.039 Uiso 1 1 calc R . .
C21 C 0.4244(7) 0.5660(6) 0.7764(4) 0.0300(16) Uani 1 1 d . . .
C22 C 0.2853(8) 0.5204(7) 0.7542(4) 0.0352(17) Uani 1 1 d . . .
C23 C 0.2264(9) 0.4566(7) 0.7992(5) 0.048(2) Uani 1 1 d . . .
H23 H 0.1324 0.4226 0.7854 0.058 Uiso 1 1 calc R . .
C24 C 0.2981(10) 0.4407(8) 0.8624(5) 0.056(2) Uani 1 1 d . . .
H24 H 0.2542 0.3950 0.8913 0.067 Uiso 1 1 calc R . .
C25 C 0.4347(10) 0.4913(7) 0.8841(4) 0.046(2) Uani 1 1 d . . .
H25 H 0.4840 0.4806 0.9284 0.055 Uiso 1 1 calc R . .
C26 C 0.5015(8) 0.5574(7) 0.8428(4) 0.0382(18) Uani 1 1 d . . .
C27 C 0.2035(7) 0.5390(7) 0.6857(4) 0.0380(18) Uani 1 1 d . . .
H27 H 0.2637 0.6063 0.6704 0.046 Uiso 1 1 calc R . .
C28 C 0.1529(10) 0.4177(9) 0.6222(5) 0.061(3) Uani 1 1 d . . .
H28A H 0.2283 0.3904 0.6144 0.091 Uiso 1 1 calc R . .
H28B H 0.1072 0.4360 0.5776 0.091 Uiso 1 1 calc R . .
H28C H 0.0911 0.3498 0.6344 0.091 Uiso 1 1 calc R . .
C29 C 0.0892(9) 0.5863(9) 0.6967(6) 0.065(3) Uani 1 1 d . . .
H29A H 0.0200 0.5173 0.7032 0.098 Uiso 1 1 calc R . .
H29B H 0.0525 0.6145 0.6538 0.098 Uiso 1 1 calc R . .
H29C H 0.1212 0.6578 0.7401 0.098 Uiso 1 1 calc R . .
C30 C 0.6498(9) 0.6182(8) 0.8675(4) 0.048(2) Uani 1 1 d . . .
H30 H 0.6708 0.6836 0.8394 0.057 Uiso 1 1 calc R . .
C31 C 0.6996(11) 0.6877(11) 0.9476(5) 0.083(4) Uani 1 1 d . . .
H31A H 0.6485 0.7455 0.9576 0.124 Uiso 1 1 calc R . .
H31B H 0.7937 0.7368 0.9597 0.124 Uiso 1 1 calc R . .
H31C H 0.6890 0.6258 0.9773 0.124 Uiso 1 1 calc R . .
C32 C 0.7219(11) 0.5240(11) 0.8499(7) 0.088(4) Uani 1 1 d . . .
H32A H 0.7068 0.4601 0.8782 0.132 Uiso 1 1 calc R . .
H32B H 0.8172 0.5687 0.8625 0.132 Uiso 1 1 calc R . .
H32C H 0.6884 0.4818 0.7977 0.132 Uiso 1 1 calc R . .
C33 C 0.4971(7) 1.0928(6) 0.6700(4) 0.0276(15) Uani 1 1 d . . .
C34 C 0.3651(7) 1.0861(6) 0.6390(4) 0.0322(16) Uani 1 1 d . . .
C35 C 0.3376(8) 1.1258(7) 0.5746(4) 0.0368(18) Uani 1 1 d . . .
H35 H 0.2501 1.1261 0.5533 0.044 Uiso 1 1 calc R . .
C36 C 0.4369(7) 1.1655(7) 0.5407(4) 0.0381(18) Uani 1 1 d . . .
H36 H 0.4160 1.1901 0.4962 0.046 Uiso 1 1 calc R . .
C37 C 0.5648(7) 1.1685(7) 0.5724(4) 0.0351(17) Uani 1 1 d . . .
H37 H 0.6317 1.1962 0.5495 0.042 Uiso 1 1 calc R . .
C38 C 0.5983(7) 1.1323(6) 0.6369(4) 0.0284(15) Uani 1 1 d . . .
C39 C 0.2565(7) 1.0325(8) 0.6709(5) 0.0401(19) Uani 1 1 d . . .
H39 H 0.2938 0.9935 0.7100 0.048 Uiso 1 1 calc R . .
C40 C 0.2083(9) 1.1365(9) 0.7061(6) 0.061(3) Uani 1 1 d . . .
H40A H 0.2826 1.2000 0.7446 0.092 Uiso 1 1 calc R . .
H40B H 0.1386 1.0992 0.7274 0.092 Uiso 1 1 calc R . .
H40C H 0.1726 1.1773 0.6691 0.092 Uiso 1 1 calc R . .
C41 C 0.1402(8) 0.9282(9) 0.6142(6) 0.066(3) Uani 1 1 d . . .
H41A H 0.0886 0.9670 0.5819 0.099 Uiso 1 1 calc R . .
H41B H 0.0831 0.8803 0.6389 0.099 Uiso 1 1 calc R . .
H41C H 0.1740 0.8705 0.5852 0.099 Uiso 1 1 calc R . .
C42 C 0.7388(7) 1.1339(7) 0.6711(4) 0.0376(18) Uani 1 1 d . . .
H42 H 0.7318 1.0619 0.6952 0.045 Uiso 1 1 calc R . .
C43 C 0.8157(8) 1.1128(9) 0.6158(5) 0.057(2) Uani 1 1 d . . .
H43A H 0.7638 1.0353 0.5773 0.085 Uiso 1 1 calc R . .
H43B H 0.9007 1.1036 0.6405 0.085 Uiso 1 1 calc R . .
H43C H 0.8322 1.1859 0.5943 0.085 Uiso 1 1 calc R . .
C44 C 0.8179(8) 1.2544(9) 0.7297(6) 0.065(3) Uani 1 1 d . . .
H44A H 0.8286 1.3274 0.7078 0.098 Uiso 1 1 calc R . .
H44B H 0.9054 1.2485 0.7525 0.098 Uiso 1 1 calc R . .
H44C H 0.7709 1.2656 0.7667 0.098 Uiso 1 1 calc R . .
Cl1 Cl 0.39222(19) 0.83967(17) 0.81669(11) 0.0391(5) Uani 1 1 d . . .
Cl2 Cl 0.42776(17) 0.79217(16) 0.61199(9) 0.0319(4) Uani 1 1 d . . .
N1 N 0.7055(6) 0.9749(5) 0.8317(3) 0.0297(13) Uani 1 1 d . . .
N2 N 0.7166(5) 0.8146(5) 0.7256(3) 0.0262(12) Uani 1 1 d . . .
N3 N 0.4960(5) 0.6316(5) 0.7317(3) 0.0246(12) Uani 1 1 d . . .
N4 N 0.5329(5) 1.0545(5) 0.7380(3) 0.0256(12) Uani 1 1 d . . .
Zr1 Zr 0.54295(6) 0.85123(6) 0.74193(3) 0.0214(2) Uani 1 1 d . . .
Cl3 Cl -0.0069(6) 0.4051(6) 0.9388(3) 0.183(2) Uiso 1 1 d D . .
C45 C 0.071(3) 0.5692(18) 0.9793(16) 0.120(10) Uiso 0.50 1 d PD . .
H45A H 0.0451 0.6211 0.9458 0.144 Uiso 0.50 1 calc PR . .
H45B H 0.1690 0.5901 0.9941 0.144 Uiso 0.50 1 calc PR . .


_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 C2 1.401(10) . ?
C1 C6 1.404(9) . ?
C1 N1 1.417(9) . ?
C2 C3 1.384(11) . ?
C2 H2 0.9500 . ?
C3 C4 1.377(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.371(10) . ?
C4 H4 0.9500 . ?
C5 C6 1.394(9) . ?
C5 H5 0.9500 . ?
C6 N2 1.410(8) . ?
C7 C8 1.395(9) . ?
C7 C12 1.417(9) . ?
C7 N2 1.423(8) . ?
C8 C9 1.382(10) . ?
C8 H8 0.9500 . ?
C9 C10 1.385(11) . ?
C9 H9 0.9500 . ?
C10 C11 1.379(11) . ?
C10 H10 0.9500 . ?
C11 C12 1.404(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.434(10) . ?
C13 N3 1.299(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.391(10) . ?
C14 N1 1.409(8) . ?
C14 C19 1.416(10) . ?
C15 C16 1.359(10) . ?
C15 H15 0.9500 . ?
C16 C17 1.386(12) . ?
C16 H16 0.9500 . ?
C17 C18 1.353(12) . ?
C17 H17 0.9500 . ?
C18 C19 1.398(10) . ?
C18 H18 0.9500 . ?
C19 C20 1.444(9) . ?
C20 N4 1.265(8) . ?
C20 H20 0.9500 . ?
C21 C22 1.402(10) . ?
C21 C26 1.404(10) . ?
C21 N3 1.461(9) . ?
C22 C23 1.387(10) . ?
C22 C27 1.504(11) . ?
C23 C24 1.366(12) . ?
C23 H23 0.9500 . ?
C24 C25 1.380(12) . ?
C24 H24 0.9500 . ?
C25 C26 1.386(11) . ?
C25 H25 0.9500 . ?
C26 C30 1.505(11) . ?
C27 C29 1.515(11) . ?
C27 C28 1.545(12) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C32 1.507(12) . ?
C30 C31 1.513(12) . ?
C30 H30 1.0000 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.402(10) . ?
C33 C38 1.411(9) . ?
C33 N4 1.462(8) . ?
C34 C35 1.396(10) . ?
C34 C39 1.496(10) . ?
C35 C36 1.407(11) . ?
C35 H35 0.9500 . ?
C36 C37 1.377(10) . ?
C36 H36 0.9500 . ?
C37 C38 1.384(10) . ?
C37 H37 0.9500 . ?
C38 C42 1.516(10) . ?
C39 C40 1.517(11) . ?
C39 C41 1.528(11) . ?
C39 H39 1.0000 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C44 1.508(11) . ?
C42 C43 1.525(11) . ?
C42 H42 1.0000 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
Cl1 Zr1 2.4184(18) . ?
Cl2 Zr1 2.4338(19) . ?
N1 Zr1 2.138(6) . ?
N2 Zr1 2.113(5) . ?
N3 Zr1 2.348(5) . ?
N4 Zr1 2.327(5) . ?
Cl3 C45 1.763(17) . ?
Cl3 C45 1.88(3) 2_567 ?
C45 Cl3 1.88(3) 2_567 ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?

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
C2 C1 C6 119.1(7) . . ?
C2 C1 N1 126.9(7) . . ?
C6 C1 N1 113.9(6) . . ?
C3 C2 C1 120.5(7) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C4 C3 C2 119.6(8) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C5 C4 C3 120.7(7) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 120.9(7) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 118.7(6) . . ?
C5 C6 N2 128.1(6) . . ?
C1 C6 N2 113.2(6) . . ?
C8 C7 C12 118.9(6) . . ?
C8 C7 N2 121.5(6) . . ?
C12 C7 N2 119.6(6) . . ?
C9 C8 C7 121.4(7) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C8 C9 C10 120.2(7) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C11 C10 C9 119.3(7) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C10 C11 C12 122.0(7) . . ?
C10 C11 H11 119.0 . . ?
C12 C11 H11 119.0 . . ?
C11 C12 C7 118.2(7) . . ?
C11 C12 C13 118.3(6) . . ?
C7 C12 C13 123.3(6) . . ?
N3 C13 C12 125.6(6) . . ?
N3 C13 H13 117.2 . . ?
C12 C13 H13 117.2 . . ?
C15 C14 N1 122.2(6) . . ?
C15 C14 C19 118.5(6) . . ?
N1 C14 C19 119.2(6) . . ?
C16 C15 C14 120.6(8) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C15 C16 C17 121.0(8) . . ?
C15 C16 H16 119.5 . . ?
C17 C16 H16 119.5 . . ?
C18 C17 C16 119.9(8) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C17 C18 C19 120.8(7) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 H18 119.6 . . ?
C18 C19 C14 119.1(6) . . ?
C18 C19 C20 119.0(6) . . ?
C14 C19 C20 121.7(6) . . ?
N4 C20 C19 127.0(6) . . ?
N4 C20 H20 116.5 . . ?
C19 C20 H20 116.5 . . ?
C22 C21 C26 122.9(7) . . ?
C22 C21 N3 120.3(6) . . ?
C26 C21 N3 116.7(6) . . ?
C23 C22 C21 116.1(8) . . ?
C23 C22 C27 121.5(7) . . ?
C21 C22 C27 122.4(7) . . ?
C24 C23 C22 122.7(8) . . ?
C24 C23 H23 118.7 . . ?
C22 C23 H23 118.7 . . ?
C23 C24 C25 119.6(8) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
C24 C25 C26 121.5(8) . . ?
C24 C25 H25 119.3 . . ?
C26 C25 H25 119.3 . . ?
C25 C26 C21 116.9(8) . . ?
C25 C26 C30 122.0(8) . . ?
C21 C26 C30 121.1(7) . . ?
C22 C27 C29 113.5(7) . . ?
C22 C27 C28 112.0(6) . . ?
C29 C27 C28 110.4(7) . . ?
C22 C27 H27 106.8 . . ?
C29 C27 H27 106.8 . . ?
C28 C27 H27 106.8 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C26 C30 C32 112.0(7) . . ?
C26 C30 C31 112.0(8) . . ?
C32 C30 C31 111.5(8) . . ?
C26 C30 H30 107.0 . . ?
C32 C30 H30 107.0 . . ?
C31 C30 H30 107.0 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C38 122.6(6) . . ?
C34 C33 N4 119.8(6) . . ?
C38 C33 N4 117.6(6) . . ?
C35 C34 C33 117.0(7) . . ?
C35 C34 C39 121.0(7) . . ?
C33 C34 C39 121.9(7) . . ?
C34 C35 C36 121.4(7) . . ?
C34 C35 H35 119.3 . . ?
C36 C35 H35 119.3 . . ?
C37 C36 C35 119.5(7) . . ?
C37 C36 H36 120.2 . . ?
C35 C36 H36 120.2 . . ?
C36 C37 C38 121.6(7) . . ?
C36 C37 H37 119.2 . . ?
C38 C37 H37 119.2 . . ?
C37 C38 C33 117.8(6) . . ?
C37 C38 C42 121.4(7) . . ?
C33 C38 C42 120.7(6) . . ?
C34 C39 C40 111.1(7) . . ?
C34 C39 C41 112.0(7) . . ?
C40 C39 C41 110.1(7) . . ?
C34 C39 H39 107.8 . . ?
C40 C39 H39 107.8 . . ?
C41 C39 H39 107.8 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C44 C42 C38 112.4(7) . . ?
C44 C42 C43 109.4(7) . . ?
C38 C42 C43 113.7(7) . . ?
C44 C42 H42 107.0 . . ?
C38 C42 H42 107.0 . . ?
C43 C42 H42 107.0 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C14 N1 C1 120.4(6) . . ?
C14 N1 Zr1 120.5(5) . . ?
C1 N1 Zr1 119.1(4) . . ?
C6 N2 C7 118.4(5) . . ?
C6 N2 Zr1 120.7(4) . . ?
C7 N2 Zr1 120.9(4) . . ?
C13 N3 C21 114.5(5) . . ?
C13 N3 Zr1 122.6(5) . . ?
C21 N3 Zr1 123.0(4) . . ?
C20 N4 C33 115.3(5) . . ?
C20 N4 Zr1 121.3(4) . . ?
C33 N4 Zr1 123.3(4) . . ?
N2 Zr1 N1 73.1(2) . . ?
N2 Zr1 N4 115.3(2) . . ?
N1 Zr1 N4 75.7(2) . . ?
N2 Zr1 N3 76.5(2) . . ?
N1 Zr1 N3 116.92(19) . . ?
N4 Zr1 N3 165.67(18) . . ?
N2 Zr1 Cl1 146.39(16) . . ?
N1 Zr1 Cl1 91.69(17) . . ?
N4 Zr1 Cl1 88.40(14) . . ?
N3 Zr1 Cl1 84.63(14) . . ?
N2 Zr1 Cl2 93.75(16) . . ?
N1 Zr1 Cl2 148.85(17) . . ?
N4 Zr1 Cl2 85.33(14) . . ?
N3 Zr1 Cl2 85.80(14) . . ?
Cl1 Zr1 Cl2 112.55(7) . . ?
C45 Cl3 C45 77.5(14) . 2_567 ?
Cl3 C45 Cl3 102.5(14) . 2_567 ?
Cl3 C45 H45A 111.3 . . ?
Cl3 C45 H45A 111.3 2_567 . ?
Cl3 C45 H45B 111.3 . . ?
Cl3 C45 H45B 111.3 2_567 . ?
H45A C45 H45B 109.2 . . ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        26.01
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         1.517
_refine_diff_density_min         -1.564
_refine_diff_density_rms         0.144
####################################################################### 
# 
# 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_Complex_1c
_database_code_depnum_ccdc_archive 'CCDC 1418233'
_audit_update_record             
;
2015-12-01 deposited with the CCDC.
2015-12-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C47.50 H53 Cl2 Hf N4'
_chemical_formula_weight         929.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.9945(7)
_cell_length_b                   11.1586(7)
_cell_length_c                   19.4967(13)
_cell_angle_alpha                98.0360(10)
_cell_angle_beta                 104.9630(10)
_cell_angle_gamma                105.1930(10)
_cell_volume                     2174.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    6906
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      26.02

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             944
_exptl_absorpt_coefficient_mu    2.559
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6412
_exptl_absorpt_correction_T_max  0.6785
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      185(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11180
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         26.03
_reflns_number_total             8296
_reflns_number_gt                7519
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0532P)²+2.3178P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8296
_refine_ls_number_parameters     485
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.0981
_refine_ls_wR_factor_gt          0.0860
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.112
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8230(5) 0.8712(5) 0.7792(3) 0.0377(11) Uani 1 1 d . . .
C2 C 0.9491(5) 0.8636(6) 0.7818(3) 0.0508(13) Uani 1 1 d . . .
H2 H 0.9584 0.8020 0.7462 0.061 Uiso 1 1 calc R . .
C3 C 1.0616(6) 0.9462(7) 0.8363(4) 0.0697(19) Uani 1 1 d . . .
H3 H 1.1468 0.9399 0.8380 0.084 Uiso 1 1 calc R . .
C4 C 1.0490(6) 1.0369(7) 0.8877(4) 0.0703(19) Uani 1 1 d . . .
H4 H 1.1262 1.0964 0.9225 0.084 Uiso 1 1 calc R . .
C5 C 0.9259(6) 1.0420(6) 0.8890(3) 0.0586(16) Uani 1 1 d . . .
H5 H 0.9186 1.1034 0.9254 0.070 Uiso 1 1 calc R . .
C6 C 0.8103(5) 0.9562(5) 0.8363(3) 0.0413(12) Uani 1 1 d . . .
C7 C 0.6511(5) 1.0265(5) 0.8841(3) 0.0412(11) Uani 1 1 d . . .
C8 C 0.7003(7) 1.0288(6) 0.9588(3) 0.0608(17) Uani 1 1 d . . .
H8 H 0.7573 0.9803 0.9741 0.073 Uiso 1 1 calc R . .
C9 C 0.6665(8) 1.1005(7) 1.0095(3) 0.0688(19) Uani 1 1 d . . .
H9 H 0.6973 1.0974 1.0592 0.083 Uiso 1 1 calc R . .
C10 C 0.5895(8) 1.1766(7) 0.9904(3) 0.0665(18) Uani 1 1 d . . .
H10 H 0.5706 1.2284 1.0266 0.080 Uiso 1 1 calc R . .
C11 C 0.5396(6) 1.1771(5) 0.9174(3) 0.0508(14) Uani 1 1 d . . .
H11 H 0.4843 1.2280 0.9035 0.061 Uiso 1 1 calc R . .
C12 C 0.5703(5) 1.1024(5) 0.8635(3) 0.0410(11) Uani 1 1 d . . .
C13 C 0.5246(5) 1.1132(4) 0.7905(3) 0.0348(10) Uani 1 1 d . . .
H13 H 0.5020 1.1882 0.7836 0.042 Uiso 1 1 calc R . .
C14 C 0.4792(4) 1.0742(4) 0.6641(3) 0.0291(9) Uani 1 1 d . . .
C15 C 0.5835(4) 1.1229(4) 0.6364(3) 0.0328(10) Uani 1 1 d . . .
C16 C 0.5545(5) 1.1626(4) 0.5730(3) 0.0404(11) Uani 1 1 d . . .
H16 H 0.6239 1.1960 0.5536 0.048 Uiso 1 1 calc R . .
C17 C 0.4255(5) 1.1555(5) 0.5358(3) 0.0440(12) Uani 1 1 d . . .
H17 H 0.4078 1.1849 0.4919 0.053 Uiso 1 1 calc R . .
C18 C 0.3243(5) 1.1064(5) 0.5624(3) 0.0437(12) Uani 1 1 d . . .
H18 H 0.2366 1.1019 0.5367 0.052 Uiso 1 1 calc R . .
C19 C 0.3479(5) 1.0621(4) 0.6275(3) 0.0344(10) Uani 1 1 d . . .
C20 C 0.7251(5) 1.1319(5) 0.6787(3) 0.0406(11) Uani 1 1 d . . .
H20 H 0.7190 1.0600 0.7044 0.049 Uiso 1 1 calc R . .
C21 C 0.7935(6) 1.2542(7) 0.7362(4) 0.077(2) Uani 1 1 d . . .
H21A H 0.8002 1.3269 0.7129 0.116 Uiso 1 1 calc R . .
H21B H 0.8825 1.2549 0.7629 0.116 Uiso 1 1 calc R . .
H21C H 0.7421 1.2600 0.7702 0.116 Uiso 1 1 calc R . .
C22 C 0.8103(6) 1.1172(7) 0.6296(4) 0.0656(18) Uani 1 1 d . . .
H22A H 0.7629 1.0412 0.5902 0.098 Uiso 1 1 calc R . .
H22B H 0.8938 1.1085 0.6582 0.098 Uiso 1 1 calc R . .
H22C H 0.8290 1.1926 0.6089 0.098 Uiso 1 1 calc R . .
C23 C 0.2341(5) 0.9999(5) 0.6536(3) 0.0483(13) Uani 1 1 d . . .
H23 H 0.2685 0.9554 0.6918 0.058 Uiso 1 1 calc R . .
C24 C 0.1818(8) 1.0974(8) 0.6885(5) 0.086(2) Uani 1 1 d . . .
H24A H 0.2426 1.1398 0.7375 0.129 Uiso 1 1 calc R . .
H24B H 0.0941 1.0547 0.6918 0.129 Uiso 1 1 calc R . .
H24C H 0.1750 1.1608 0.6588 0.129 Uiso 1 1 calc R . .
C25 C 0.1216(6) 0.9020(8) 0.5946(5) 0.086(2) Uani 1 1 d . . .
H25A H 0.0696 0.9448 0.5638 0.129 Uiso 1 1 calc R . .
H25B H 0.0649 0.8469 0.6165 0.129 Uiso 1 1 calc R . .
H25C H 0.1570 0.8503 0.5648 0.129 Uiso 1 1 calc R . .
C26 C 0.7000(4) 0.7161(4) 0.6663(2) 0.0308(9) Uani 1 1 d . . .
C27 C 0.7855(5) 0.7506(5) 0.6261(3) 0.0361(10) Uani 1 1 d . . .
H27 H 0.8485 0.8333 0.6403 0.043 Uiso 1 1 calc R . .
C28 C 0.7795(5) 0.6644(5) 0.5646(3) 0.0433(12) Uani 1 1 d . . .
H28 H 0.8349 0.6909 0.5357 0.052 Uiso 1 1 calc R . .
C29 C 0.6942(5) 0.5416(5) 0.5456(3) 0.0447(12) Uani 1 1 d . . .
H29 H 0.6938 0.4822 0.5055 0.054 Uiso 1 1 calc R . .
C30 C 0.6100(5) 0.5062(5) 0.5853(3) 0.0427(12) Uani 1 1 d . . .
H30 H 0.5508 0.4217 0.5720 0.051 Uiso 1 1 calc R . .
C31 C 0.6086(5) 0.5916(4) 0.6453(2) 0.0324(10) Uani 1 1 d . . .
C32 C 0.5166(5) 0.5451(4) 0.6835(3) 0.0366(10) Uani 1 1 d . . .
H32 H 0.4784 0.4553 0.6742 0.044 Uiso 1 1 calc R . .
C33 C 0.4081(5) 0.5418(4) 0.7704(3) 0.0365(11) Uani 1 1 d . . .
C34 C 0.4779(6) 0.5311(5) 0.8386(3) 0.0448(12) Uani 1 1 d . . .
C35 C 0.4044(7) 0.4576(6) 0.8753(3) 0.0571(16) Uani 1 1 d . . .
H35 H 0.4497 0.4475 0.9217 0.069 Uiso 1 1 calc R . .
C36 C 0.2739(8) 0.4008(6) 0.8484(4) 0.070(2) Uani 1 1 d . . .
H36 H 0.2285 0.3500 0.8749 0.084 Uiso 1 1 calc R . .
C37 C 0.2050(7) 0.4163(6) 0.7821(4) 0.0637(17) Uani 1 1 d . . .
H37 H 0.1118 0.3767 0.7641 0.076 Uiso 1 1 calc R . .
C38 C 0.2672(6) 0.4884(5) 0.7399(4) 0.0502(14) Uani 1 1 d . . .
C39 C 0.1894(6) 0.5099(6) 0.6694(3) 0.0547(15) Uani 1 1 d . . .
H39 H 0.2505 0.5802 0.6563 0.066 Uiso 1 1 calc R . .
C40 C 0.1430(7) 0.3933(7) 0.6062(4) 0.0714(19) Uani 1 1 d . . .
H40A H 0.2199 0.3702 0.5996 0.107 Uiso 1 1 calc R . .
H40B H 0.0961 0.4133 0.5615 0.107 Uiso 1 1 calc R . .
H40C H 0.0832 0.3217 0.6172 0.107 Uiso 1 1 calc R . .
C41 C 0.0713(7) 0.5539(7) 0.6763(5) 0.078(2) Uani 1 1 d . . .
H41A H 0.0314 0.5774 0.6312 0.117 Uiso 1 1 calc R . .
H41B H 0.1017 0.6279 0.7171 0.117 Uiso 1 1 calc R . .
H41C H 0.0053 0.4846 0.6850 0.117 Uiso 1 1 calc R . .
C42 C 0.6230(7) 0.5942(6) 0.8675(3) 0.0536(14) Uani 1 1 d . . .
H42 H 0.6442 0.6672 0.8436 0.064 Uiso 1 1 calc R . .
C43 C 0.6956(8) 0.5039(8) 0.8463(4) 0.086(2) Uani 1 1 d . . .
H43A H 0.6790 0.4320 0.8700 0.129 Uiso 1 1 calc R . .
H43B H 0.7909 0.5491 0.8618 0.129 Uiso 1 1 calc R . .
H43C H 0.6637 0.4722 0.7933 0.129 Uiso 1 1 calc R . .
C44 C 0.6732(8) 0.6488(8) 0.9498(4) 0.083(2) Uani 1 1 d . . .
H44A H 0.6281 0.7100 0.9619 0.124 Uiso 1 1 calc R . .
H44B H 0.7690 0.6918 0.9650 0.124 Uiso 1 1 calc R . .
H44C H 0.6547 0.5795 0.9752 0.124 Uiso 1 1 calc R . .
C45 C 0.9464(19) 0.372(2) -0.0063(11) 0.211(8) Uiso 1 1 d D . .
H45 H 0.9121 0.2817 -0.0160 0.253 Uiso 1 1 calc R . .
C46 C 0.913(2) 0.3873(18) 0.1184(9) 0.109(6) Uiso 0.50 1 d PD . .
H46A H 0.9891 0.4251 0.1623 0.163 Uiso 1 1 calc R . .
H46B H 0.8942 0.2947 0.1066 0.163 Uiso 1 1 calc R . .
H46C H 0.8351 0.4068 0.1269 0.163 Uiso 1 1 calc R . .
C47 C 0.9433(17) 0.4435(18) 0.0534(10) 0.174(6) Uiso 1 1 d D . .
C48 C 1.0013(17) 0.4322(18) -0.0548(10) 0.183(6) Uiso 1 1 d . . .
H48 H 0.9991 0.3751 -0.0964 0.219 Uiso 1 1 calc R . .
Cl1 Cl 0.41696(12) 0.77946(10) 0.60824(6) 0.0357(2) Uani 1 1 d . . .
Cl2 Cl 0.36407(14) 0.80928(11) 0.80384(7) 0.0453(3) Uani 1 1 d . . .
Hf1 Hf 0.524224(18) 0.830561(16) 0.738390(10) 0.02856(8) Uani 1 1 d . . .
N1 N 0.7019(4) 0.8012(3) 0.7279(2) 0.0306(8) Uani 1 1 d . . .
N2 N 0.6803(4) 0.9503(4) 0.8305(2) 0.0381(9) Uani 1 1 d . . .
N3 N 0.5098(4) 1.0315(3) 0.7312(2) 0.0283(8) Uani 1 1 d . . .
N4 N 0.4802(4) 0.6136(4) 0.7295(2) 0.0353(9) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.390(6) . ?
C1 C2 1.400(7) . ?
C1 C6 1.418(7) . ?
C2 C3 1.400(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.382(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.376(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.415(8) . ?
C5 H5 0.9500 . ?
C6 N2 1.387(7) . ?
C7 C12 1.405(7) . ?
C7 N2 1.409(6) . ?
C7 C8 1.410(7) . ?
C8 C9 1.370(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.371(9) . ?
C9 H9 0.9500 . ?
C10 C11 1.388(9) . ?
C10 H10 0.9500 . ?
C11 C12 1.414(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.414(7) . ?
C13 N3 1.314(6) . ?
C13 H13 0.9500 . ?
C14 C19 1.396(6) . ?
C14 C15 1.406(6) . ?
C14 N3 1.443(6) . ?
C15 C16 1.362(7) . ?
C15 C20 1.532(6) . ?
C16 C17 1.392(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.365(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.412(7) . ?
C18 H18 0.9500 . ?
C19 C23 1.511(7) . ?
C20 C21 1.511(8) . ?
C20 C22 1.524(8) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C25 1.501(9) . ?
C23 C24 1.516(9) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.386(7) . ?
C26 N1 1.414(6) . ?
C26 C31 1.415(6) . ?
C27 C28 1.405(7) . ?
C27 H27 0.9500 . ?
C28 C29 1.378(8) . ?
C28 H28 0.9500 . ?
C29 C30 1.370(8) . ?
C29 H29 0.9500 . ?
C30 C31 1.408(7) . ?
C30 H30 0.9500 . ?
C31 C32 1.438(7) . ?
C32 N4 1.306(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.392(7) . ?
C33 C38 1.432(8) . ?
C33 N4 1.440(6) . ?
C34 C35 1.398(8) . ?
C34 C42 1.482(9) . ?
C35 C36 1.333(10) . ?
C35 H35 0.9500 . ?
C36 C37 1.379(10) . ?
C36 H36 0.9500 . ?
C37 C38 1.406(7) . ?
C37 H37 0.9500 . ?
C38 C39 1.508(9) . ?
C39 C40 1.533(9) . ?
C39 C41 1.534(9) . ?
C39 H39 1.0000 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.516(9) . ?
C42 C44 1.530(9) . ?
C42 H42 1.0000 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C47 1.33(2) . ?
C45 C48 1.40(2) . ?
C45 H45 0.9500 . ?
C46 C47 1.563(15) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C48 1.35(2) 2_765 ?
C48 C47 1.35(2) 2_765 ?
C48 H48 0.9500 . ?
Cl1 Hf1 2.4193(11) . ?
Cl2 Hf1 2.4106(12) . ?
Hf1 N1 2.119(4) . ?
Hf1 N2 2.120(4) . ?
Hf1 N3 2.310(3) . ?
Hf1 N4 2.313(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
N1 C1 C2 128.3(5) . . ?
N1 C1 C6 112.9(4) . . ?
C2 C1 C6 118.8(5) . . ?
C1 C2 C3 120.4(6) . . ?
C1 C2 H2 119.8 . . ?
C3 C2 H2 119.8 . . ?
C4 C3 C2 120.1(6) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C5 C4 C3 120.7(6) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 120.2(6) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
N2 C6 C5 126.7(5) . . ?
N2 C6 C1 113.9(4) . . ?
C5 C6 C1 119.2(5) . . ?
C12 C7 N2 119.8(4) . . ?
C12 C7 C8 118.3(5) . . ?
N2 C7 C8 121.9(5) . . ?
C9 C8 C7 120.6(6) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C8 C9 C10 121.8(6) . . ?
C8 C9 H9 119.1 . . ?
C10 C9 H9 119.1 . . ?
C9 C10 C11 119.2(6) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
C10 C11 C12 120.4(5) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C7 C12 C13 122.2(4) . . ?
C7 C12 C11 119.6(5) . . ?
C13 C12 C11 118.2(5) . . ?
N3 C13 C12 127.5(4) . . ?
N3 C13 H13 116.3 . . ?
C12 C13 H13 116.3 . . ?
C19 C14 C15 122.1(4) . . ?
C19 C14 N3 119.7(4) . . ?
C15 C14 N3 118.2(4) . . ?
C16 C15 C14 118.2(4) . . ?
C16 C15 C20 122.3(4) . . ?
C14 C15 C20 119.5(4) . . ?
C15 C16 C17 121.5(5) . . ?
C15 C16 H16 119.3 . . ?
C17 C16 H16 119.3 . . ?
C18 C17 C16 120.0(4) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 121.1(4) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 H18 119.5 . . ?
C14 C19 C18 117.1(4) . . ?
C14 C19 C23 122.4(4) . . ?
C18 C19 C23 120.5(4) . . ?
C21 C20 C22 109.6(5) . . ?
C21 C20 C15 112.1(5) . . ?
C22 C20 C15 113.0(5) . . ?
C21 C20 H20 107.3 . . ?
C22 C20 H20 107.3 . . ?
C15 C20 H20 107.3 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C25 C23 C19 113.2(5) . . ?
C25 C23 C24 109.2(6) . . ?
C19 C23 C24 111.7(5) . . ?
C25 C23 H23 107.5 . . ?
C19 C23 H23 107.5 . . ?
C24 C23 H23 107.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 N1 122.0(4) . . ?
C27 C26 C31 118.9(4) . . ?
N1 C26 C31 119.1(4) . . ?
C26 C27 C28 120.6(5) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
C29 C28 C27 120.6(5) . . ?
C29 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
C30 C29 C28 119.2(5) . . ?
C30 C29 H29 120.4 . . ?
C28 C29 H29 120.4 . . ?
C29 C30 C31 121.8(5) . . ?
C29 C30 H30 119.1 . . ?
C31 C30 H30 119.1 . . ?
C30 C31 C26 118.8(4) . . ?
C30 C31 C32 117.5(4) . . ?
C26 C31 C32 123.6(4) . . ?
N4 C32 C31 126.7(4) . . ?
N4 C32 H32 116.7 . . ?
C31 C32 H32 116.7 . . ?
C34 C33 C38 123.0(5) . . ?
C34 C33 N4 118.6(5) . . ?
C38 C33 N4 118.4(4) . . ?
C33 C34 C35 116.6(6) . . ?
C33 C34 C42 119.6(5) . . ?
C35 C34 C42 123.9(5) . . ?
C36 C35 C34 123.2(6) . . ?
C36 C35 H35 118.4 . . ?
C34 C35 H35 118.4 . . ?
C35 C36 C37 119.7(6) . . ?
C35 C36 H36 120.2 . . ?
C37 C36 H36 120.2 . . ?
C36 C37 C38 122.6(6) . . ?
C36 C37 H37 118.7 . . ?
C38 C37 H37 118.7 . . ?
C37 C38 C33 114.8(6) . . ?
C37 C38 C39 121.8(6) . . ?
C33 C38 C39 123.3(5) . . ?
C38 C39 C40 112.8(5) . . ?
C38 C39 C41 112.8(6) . . ?
C40 C39 C41 110.1(6) . . ?
C38 C39 H39 107.0 . . ?
C40 C39 H39 107.0 . . ?
C41 C39 H39 107.0 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C34 C42 C43 110.3(5) . . ?
C34 C42 C44 113.7(6) . . ?
C43 C42 C44 111.0(6) . . ?
C34 C42 H42 107.2 . . ?
C43 C42 H42 107.2 . . ?
C44 C42 H42 107.2 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C47 C45 C48 118.8(19) . . ?
C47 C45 H45 120.6 . . ?
C48 C45 H45 120.6 . . ?
C47 C46 H46A 109.5 . . ?
C47 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C47 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 C48 109.1(17) . 2_765 ?
C45 C47 C46 122.7(19) . . ?
C48 C47 C46 126.5(19) 2_765 . ?
C47 C48 C45 132.1(19) 2_765 . ?
C47 C48 H48 114.0 2_765 . ?
C45 C48 H48 114.0 . . ?
N1 Hf1 N2 72.96(15) . . ?
N1 Hf1 N3 114.87(14) . . ?
N2 Hf1 N3 76.81(14) . . ?
N1 Hf1 N4 77.44(14) . . ?
N2 Hf1 N4 116.34(15) . . ?
N3 Hf1 N4 165.02(14) . . ?
N1 Hf1 Cl2 148.13(11) . . ?
N2 Hf1 Cl2 92.82(12) . . ?
N3 Hf1 Cl2 88.18(9) . . ?
N4 Hf1 Cl2 84.16(10) . . ?
N1 Hf1 Cl1 93.60(10) . . ?
N2 Hf1 Cl1 148.81(12) . . ?
N3 Hf1 Cl1 84.14(9) . . ?
N4 Hf1 Cl1 86.65(11) . . ?
Cl2 Hf1 Cl1 111.21(5) . . ?
C1 N1 C26 119.0(4) . . ?
C1 N1 Hf1 120.3(3) . . ?
C26 N1 Hf1 120.6(3) . . ?
C6 N2 C7 120.7(4) . . ?
C6 N2 Hf1 119.8(3) . . ?
C7 N2 Hf1 119.5(3) . . ?
C13 N3 C14 115.9(4) . . ?
C13 N3 Hf1 119.8(3) . . ?
C14 N3 Hf1 124.2(3) . . ?
C32 N4 C33 114.4(4) . . ?
C32 N4 Hf1 120.9(3) . . ?
C33 N4 Hf1 124.7(3) . . ?

_diffrn_measured_fraction_theta_max 0.965
_diffrn_reflns_theta_full        26.03
_diffrn_measured_fraction_theta_full 0.965
_refine_diff_density_max         1.521
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.122


#===END
