# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_150709c-2_a
_database_code_depnum_ccdc_archive 'CCDC 1444236'
_audit_update_record             
;
2015-12-25 deposited with the CCDC.
2016-04-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H50 N6 Si2 Ti'
_chemical_formula_weight         694.92

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   9.8027(4)
_cell_length_b                   12.2995(4)
_cell_length_c                   17.4058(6)
_cell_angle_alpha                99.9200(10)
_cell_angle_beta                 94.7200(10)
_cell_angle_gamma                109.6330(10)
_cell_volume                     1924.68(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    194(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             740
_exptl_absorpt_coefficient_mu    0.319
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.8912
_exptl_absorpt_correction_T_max  0.9105
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      194(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14852
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         25.05
_reflns_number_total             6666
_reflns_number_gt                5609
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.0487P)²+1.0870P] 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         6666
_refine_ls_number_parameters     430
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.1054
_refine_ls_wR_factor_gt          0.0980
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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
Ti1 Ti 0.72507(4) 0.43219(3) 0.739838(19) 0.02168(10) Uani 1 1 d . . .
Si1 Si 0.40895(6) 0.18434(5) 0.77781(3) 0.03295(15) Uani 1 1 d . . .
Si2 Si 0.86308(7) 0.21304(6) 0.63659(3) 0.03507(16) Uani 1 1 d . . .
N1 N 0.91840(18) 0.55745(15) 0.74931(10) 0.0287(4) Uani 1 1 d . . .
N2 N 0.81673(18) 0.39198(16) 0.83702(9) 0.0308(4) Uani 1 1 d . . .
N3 N 0.58359(18) 0.29004(15) 0.79167(9) 0.0262(4) Uani 1 1 d . . .
N4 N 0.61586(18) 0.53756(15) 0.77023(9) 0.0263(4) Uani 1 1 d . . .
N5 N 0.59097(17) 0.38212(15) 0.63139(9) 0.0245(4) Uani 1 1 d . . .
N6 N 0.75817(17) 0.30120(14) 0.64776(9) 0.0249(4) Uani 1 1 d . . .
C1 C 0.8629(3) 0.6238(3) 0.63095(15) 0.0505(7) Uani 1 1 d . . .
H1 H 0.8195 0.5436 0.6038 0.061 Uiso 1 1 calc R . .
C2 C 0.8633(3) 0.7123(4) 0.5912(2) 0.0756(11) Uani 1 1 d . . .
H2 H 0.8173 0.6919 0.5378 0.091 Uiso 1 1 calc R . .
C3 C 0.9286(4) 0.8281(4) 0.6276(3) 0.0826(12) Uani 1 1 d . . .
H3 H 0.9305 0.8884 0.5998 0.099 Uiso 1 1 calc R . .
C4 C 0.9911(4) 0.8562(3) 0.7043(2) 0.0701(10) Uani 1 1 d . . .
H4 H 1.0362 0.9370 0.7300 0.084 Uiso 1 1 calc R . .
C5 C 0.9907(3) 0.7693(2) 0.74619(16) 0.0469(6) Uani 1 1 d . . .
H5 H 1.0355 0.7914 0.7998 0.056 Uiso 1 1 calc R . .
C6 C 0.9248(2) 0.65006(19) 0.70976(12) 0.0296(4) Uani 1 1 d . . .
C7 C 1.0510(3) 0.5906(3) 0.80890(17) 0.0568(7) Uani 1 1 d . . .
H7A H 1.1379 0.6233 0.7833 0.068 Uiso 1 1 calc R . .
H7B H 1.0494 0.6552 0.8512 0.068 Uiso 1 1 calc R . .
C8 C 1.0716(3) 0.4989(3) 0.84584(18) 0.0660(9) Uani 1 1 d . . .
H8A H 1.1652 0.5341 0.8826 0.079 Uiso 1 1 calc R . .
H8B H 1.0822 0.4377 0.8042 0.079 Uiso 1 1 calc R . .
C9 C 0.9551(2) 0.4392(2) 0.89012(13) 0.0416(6) Uani 1 1 d . . .
H9A H 0.9769 0.3746 0.9091 0.050 Uiso 1 1 calc R . .
H9B H 0.9499 0.4963 0.9364 0.050 Uiso 1 1 calc R . .
C10 C 0.6934(2) 0.31696(18) 0.85009(11) 0.0261(4) Uani 1 1 d . . .
C11 C 0.6766(2) 0.27271(18) 0.92491(11) 0.0289(4) Uani 1 1 d . . .
C12 C 0.7400(3) 0.1934(2) 0.94395(13) 0.0399(5) Uani 1 1 d . . .
H12 H 0.8007 0.1690 0.9104 0.048 Uiso 1 1 calc R . .
C13 C 0.7143(3) 0.1499(2) 1.01211(15) 0.0488(6) Uani 1 1 d . . .
H13 H 0.7569 0.0951 1.0249 0.059 Uiso 1 1 calc R . .
C14 C 0.6273(3) 0.1860(2) 1.06116(13) 0.0476(6) Uani 1 1 d . . .
H14 H 0.6084 0.1549 1.1071 0.057 Uiso 1 1 calc R . .
C15 C 0.5680(3) 0.2665(2) 1.04382(13) 0.0447(6) Uani 1 1 d . . .
H15 H 0.5099 0.2925 1.0784 0.054 Uiso 1 1 calc R . .
C16 C 0.5923(2) 0.3104(2) 0.97576(12) 0.0359(5) Uani 1 1 d . . .
H16 H 0.5509 0.3665 0.9641 0.043 Uiso 1 1 calc R . .
C17 C 0.4053(3) 0.0538(2) 0.82058(15) 0.0513(7) Uani 1 1 d . . .
H17A H 0.4885 0.0308 0.8074 0.077 Uiso 1 1 calc R . .
H17B H 0.3136 -0.0123 0.7987 0.077 Uiso 1 1 calc R . .
H17C H 0.4120 0.0746 0.8781 0.077 Uiso 1 1 calc R . .
C18 C 0.2779(3) 0.2460(3) 0.82300(17) 0.0579(7) Uani 1 1 d . . .
H18A H 0.3018 0.2630 0.8806 0.087 Uiso 1 1 calc R . .
H18B H 0.1780 0.1884 0.8066 0.087 Uiso 1 1 calc R . .
H18C H 0.2848 0.3190 0.8056 0.087 Uiso 1 1 calc R . .
C19 C 0.3497(3) 0.1310(2) 0.66928(14) 0.0502(7) Uani 1 1 d . . .
H19A H 0.3447 0.1967 0.6457 0.075 Uiso 1 1 calc R . .
H19B H 0.2528 0.0683 0.6590 0.075 Uiso 1 1 calc R . .
H19C H 0.4203 0.0999 0.6460 0.075 Uiso 1 1 calc R . .
C20 C 0.6701(3) 0.7524(2) 0.80442(14) 0.0415(5) Uani 1 1 d . . .
H20 H 0.6142 0.7488 0.7562 0.050 Uiso 1 1 calc R . .
C21 C 0.7391(3) 0.8603(2) 0.85662(19) 0.0582(8) Uani 1 1 d . . .
H21 H 0.7289 0.9296 0.8441 0.070 Uiso 1 1 calc R . .
C22 C 0.8218(3) 0.8680(3) 0.9260(2) 0.0716(10) Uani 1 1 d . . .
H22 H 0.8699 0.9425 0.9610 0.086 Uiso 1 1 calc R . .
C23 C 0.8349(3) 0.7677(3) 0.94476(17) 0.0691(9) Uani 1 1 d . . .
H23 H 0.8923 0.7729 0.9929 0.083 Uiso 1 1 calc R . .
C24 C 0.7643(3) 0.6581(2) 0.89354(14) 0.0480(6) Uani 1 1 d . . .
H24 H 0.7726 0.5891 0.9077 0.058 Uiso 1 1 calc R . .
C25 C 0.6820(2) 0.64874(19) 0.82198(12) 0.0317(5) Uani 1 1 d . . .
C26 C 0.4717(2) 0.5187(2) 0.72601(12) 0.0322(5) Uani 1 1 d . . .
H26A H 0.4324 0.5769 0.7530 0.039 Uiso 1 1 calc R . .
H26B H 0.4034 0.4389 0.7272 0.039 Uiso 1 1 calc R . .
C27 C 0.4759(3) 0.5299(2) 0.64007(12) 0.0352(5) Uani 1 1 d . . .
H27A H 0.3864 0.5423 0.6193 0.042 Uiso 1 1 calc R . .
H27B H 0.5616 0.5996 0.6372 0.042 Uiso 1 1 calc R . .
C28 C 0.4858(2) 0.4201(2) 0.58975(12) 0.0328(5) Uani 1 1 d . . .
H28A H 0.3884 0.3562 0.5781 0.039 Uiso 1 1 calc R . .
H28B H 0.5171 0.4371 0.5391 0.039 Uiso 1 1 calc R . .
C29 C 0.6621(2) 0.31809(16) 0.59698(11) 0.0227(4) Uani 1 1 d . . .
C30 C 0.6435(2) 0.27733(18) 0.50926(11) 0.0273(4) Uani 1 1 d . . .
C31 C 0.7616(3) 0.3146(2) 0.46956(13) 0.0375(5) Uani 1 1 d . . .
H31 H 0.8541 0.3666 0.4979 0.045 Uiso 1 1 calc R . .
C32 C 0.7453(3) 0.2763(3) 0.38866(14) 0.0504(7) Uani 1 1 d . . .
H32 H 0.8268 0.3018 0.3616 0.060 Uiso 1 1 calc R . .
C33 C 0.6114(3) 0.2015(2) 0.34735(13) 0.0513(7) Uani 1 1 d . . .
H33 H 0.6009 0.1752 0.2918 0.062 Uiso 1 1 calc R . .
C34 C 0.4935(3) 0.1649(2) 0.38581(14) 0.0499(6) Uani 1 1 d . . .
H34 H 0.4012 0.1131 0.3570 0.060 Uiso 1 1 calc R . .
C35 C 0.5085(3) 0.2034(2) 0.46693(13) 0.0380(5) Uani 1 1 d . . .
H35 H 0.4261 0.1790 0.4935 0.046 Uiso 1 1 calc R . .
C36 C 1.0553(3) 0.3039(3) 0.62978(18) 0.0672(9) Uani 1 1 d . . .
H36A H 1.0572 0.3340 0.5812 0.101 Uiso 1 1 calc R . .
H36B H 1.1163 0.2549 0.6292 0.101 Uiso 1 1 calc R . .
H36C H 1.0934 0.3703 0.6754 0.101 Uiso 1 1 calc R . .
C37 C 0.8576(3) 0.1469(2) 0.72576(14) 0.0506(7) Uani 1 1 d . . .
H37A H 0.9084 0.2093 0.7725 0.076 Uiso 1 1 calc R . .
H37B H 0.9060 0.0886 0.7192 0.076 Uiso 1 1 calc R . .
H37C H 0.7554 0.1080 0.7323 0.076 Uiso 1 1 calc R . .
C38 C 0.7902(4) 0.0887(2) 0.54775(15) 0.0586(8) Uani 1 1 d . . .
H38A H 0.6836 0.0527 0.5439 0.088 Uiso 1 1 calc R . .
H38B H 0.8345 0.0293 0.5526 0.088 Uiso 1 1 calc R . .
H38C H 0.8143 0.1192 0.5002 0.088 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 N1 1.9726(17) . ?
Ti1 N4 1.9735(16) . ?
Ti1 N2 2.0616(16) . ?
Ti1 N5 2.0778(16) . ?
Ti1 N6 2.1947(16) . ?
Ti1 N3 2.2168(17) . ?
Si1 N3 1.7343(17) . ?
Si1 C18 1.860(3) . ?
Si1 C19 1.864(2) . ?
Si1 C17 1.874(2) . ?
Si2 N6 1.7265(16) . ?
Si2 C36 1.866(3) . ?
Si2 C37 1.869(2) . ?
Si2 C38 1.873(3) . ?
N1 C6 1.416(3) . ?
N1 C7 1.486(3) . ?
N2 C10 1.316(3) . ?
N2 C9 1.453(3) . ?
N3 C10 1.329(2) . ?
N4 C25 1.409(3) . ?
N4 C26 1.477(3) . ?
N5 C29 1.320(2) . ?
N5 C28 1.457(2) . ?
N6 C29 1.330(2) . ?
C1 C2 1.387(4) . ?
C1 C6 1.390(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.360(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.356(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.393(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.395(3) . ?
C5 H5 0.9500 . ?
C7 C8 1.452(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.488(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.496(3) . ?
C11 C16 1.385(3) . ?
C11 C12 1.390(3) . ?
C12 C13 1.391(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.378(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.367(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.390(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.387(4) . ?
C20 C25 1.400(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.368(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.372(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.396(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.393(3) . ?
C24 H24 0.9500 . ?
C26 C27 1.529(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.515(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.498(3) . ?
C30 C31 1.383(3) . ?
C30 C35 1.386(3) . ?
C31 C32 1.384(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.375(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.367(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.389(3) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ti1 N4 96.81(7) . . ?
N1 Ti1 N2 84.94(7) . . ?
N4 Ti1 N2 111.63(7) . . ?
N1 Ti1 N5 116.80(7) . . ?
N4 Ti1 N5 85.39(6) . . ?
N2 Ti1 N5 151.40(7) . . ?
N1 Ti1 N6 97.39(7) . . ?
N4 Ti1 N6 147.54(6) . . ?
N2 Ti1 N6 98.59(7) . . ?
N5 Ti1 N6 62.16(6) . . ?
N1 Ti1 N3 146.67(7) . . ?
N4 Ti1 N3 93.03(7) . . ?
N2 Ti1 N3 61.87(6) . . ?
N5 Ti1 N3 95.64(6) . . ?
N6 Ti1 N3 90.92(6) . . ?
N3 Si1 C18 111.68(12) . . ?
N3 Si1 C19 106.99(10) . . ?
C18 Si1 C19 110.23(13) . . ?
N3 Si1 C17 112.31(10) . . ?
C18 Si1 C17 107.87(13) . . ?
C19 Si1 C17 107.70(12) . . ?
N6 Si2 C36 110.08(12) . . ?
N6 Si2 C37 106.50(10) . . ?
C36 Si2 C37 110.41(13) . . ?
N6 Si2 C38 113.14(11) . . ?
C36 Si2 C38 108.97(15) . . ?
C37 Si2 C38 107.69(13) . . ?
C6 N1 C7 111.19(18) . . ?
C6 N1 Ti1 116.80(13) . . ?
C7 N1 Ti1 129.50(15) . . ?
C10 N2 C9 125.79(17) . . ?
C10 N2 Ti1 95.76(12) . . ?
C9 N2 Ti1 137.19(15) . . ?
C10 N3 Si1 129.04(14) . . ?
C10 N3 Ti1 88.51(12) . . ?
Si1 N3 Ti1 142.43(9) . . ?
C25 N4 C26 114.52(16) . . ?
C25 N4 Ti1 122.40(13) . . ?
C26 N4 Ti1 121.49(13) . . ?
C29 N5 C28 124.69(16) . . ?
C29 N5 Ti1 94.58(11) . . ?
C28 N5 Ti1 138.43(13) . . ?
C29 N6 Si2 131.94(14) . . ?
C29 N6 Ti1 89.13(11) . . ?
Si2 N6 Ti1 138.89(9) . . ?
C2 C1 C6 121.4(3) . . ?
C2 C1 H1 119.3 . . ?
C6 C1 H1 119.3 . . ?
C3 C2 C1 120.7(3) . . ?
C3 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
C4 C3 C2 119.1(3) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 121.5(3) . . ?
C3 C4 H4 119.2 . . ?
C5 C4 H4 119.2 . . ?
C4 C5 C6 120.3(3) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C1 C6 C5 117.0(2) . . ?
C1 C6 N1 119.9(2) . . ?
C5 C6 N1 123.1(2) . . ?
C8 C7 N1 117.7(2) . . ?
C8 C7 H7A 107.9 . . ?
N1 C7 H7A 107.9 . . ?
C8 C7 H7B 107.9 . . ?
N1 C7 H7B 107.9 . . ?
H7A C7 H7B 107.2 . . ?
C7 C8 C9 117.3(3) . . ?
C7 C8 H8A 108.0 . . ?
C9 C8 H8A 108.0 . . ?
C7 C8 H8B 108.0 . . ?
C9 C8 H8B 108.0 . . ?
H8A C8 H8B 107.2 . . ?
N2 C9 C8 107.91(19) . . ?
N2 C9 H9A 110.1 . . ?
C8 C9 H9A 110.1 . . ?
N2 C9 H9B 110.1 . . ?
C8 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
N2 C10 N3 112.79(17) . . ?
N2 C10 C11 123.49(18) . . ?
N3 C10 C11 123.62(18) . . ?
C16 C11 C12 119.26(19) . . ?
C16 C11 C10 118.56(18) . . ?
C12 C11 C10 122.16(19) . . ?
C11 C12 C13 119.9(2) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C14 C13 C12 120.2(2) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C15 C14 C13 120.1(2) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C16 120.3(2) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C11 C16 C15 120.2(2) . . ?
C11 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
Si1 C17 H17A 109.5 . . ?
Si1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si1 C18 H18A 109.5 . . ?
Si1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si1 C19 H19A 109.5 . . ?
Si1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C25 120.8(2) . . ?
C21 C20 H20 119.6 . . ?
C25 C20 H20 119.6 . . ?
C22 C21 C20 120.7(3) . . ?
C22 C21 H21 119.6 . . ?
C20 C21 H21 119.6 . . ?
C21 C22 C23 119.7(3) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
C22 C23 C24 120.4(3) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
C25 C24 C23 120.8(3) . . ?
C25 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
C24 C25 C20 117.6(2) . . ?
C24 C25 N4 119.6(2) . . ?
C20 C25 N4 122.8(2) . . ?
N4 C26 C27 113.96(17) . . ?
N4 C26 H26A 108.8 . . ?
C27 C26 H26A 108.8 . . ?
N4 C26 H26B 108.8 . . ?
C27 C26 H26B 108.8 . . ?
H26A C26 H26B 107.7 . . ?
C28 C27 C26 110.96(17) . . ?
C28 C27 H27A 109.4 . . ?
C26 C27 H27A 109.4 . . ?
C28 C27 H27B 109.4 . . ?
C26 C27 H27B 109.4 . . ?
H27A C27 H27B 108.0 . . ?
N5 C28 C27 109.75(16) . . ?
N5 C28 H28A 109.7 . . ?
C27 C28 H28A 109.7 . . ?
N5 C28 H28B 109.7 . . ?
C27 C28 H28B 109.7 . . ?
H28A C28 H28B 108.2 . . ?
N5 C29 N6 112.90(16) . . ?
N5 C29 C30 122.78(16) . . ?
N6 C29 C30 124.16(17) . . ?
C31 C30 C35 119.28(19) . . ?
C31 C30 C29 119.89(19) . . ?
C35 C30 C29 120.83(19) . . ?
C30 C31 C32 120.1(2) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
C33 C32 C31 120.1(2) . . ?
C33 C32 H32 119.9 . . ?
C31 C32 H32 119.9 . . ?
C34 C33 C32 120.3(2) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C33 C34 C35 120.0(2) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C30 C35 C34 120.1(2) . . ?
C30 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
Si2 C36 H36A 109.5 . . ?
Si2 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
Si2 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
Si2 C37 H37A 109.5 . . ?
Si2 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
Si2 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
Si2 C38 H38A 109.5 . . ?
Si2 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
Si2 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 Ti1 N1 C6 -50.86(15) . . . . ?
N2 Ti1 N1 C6 -162.09(15) . . . . ?
N5 Ti1 N1 C6 37.39(16) . . . . ?
N6 Ti1 N1 C6 99.87(14) . . . . ?
N3 Ti1 N1 C6 -157.03(13) . . . . ?
N4 Ti1 N1 C7 109.4(2) . . . . ?
N2 Ti1 N1 C7 -1.8(2) . . . . ?
N5 Ti1 N1 C7 -162.4(2) . . . . ?
N6 Ti1 N1 C7 -99.9(2) . . . . ?
N3 Ti1 N1 C7 3.2(3) . . . . ?
N1 Ti1 N2 C10 170.50(13) . . . . ?
N4 Ti1 N2 C10 75.16(14) . . . . ?
N5 Ti1 N2 C10 -48.0(2) . . . . ?
N6 Ti1 N2 C10 -92.78(13) . . . . ?
N3 Ti1 N2 C10 -6.35(11) . . . . ?
N1 Ti1 N2 C9 3.6(2) . . . . ?
N4 Ti1 N2 C9 -91.7(2) . . . . ?
N5 Ti1 N2 C9 145.2(2) . . . . ?
N6 Ti1 N2 C9 100.4(2) . . . . ?
N3 Ti1 N2 C9 -173.2(2) . . . . ?
C18 Si1 N3 C10 90.9(2) . . . . ?
C19 Si1 N3 C10 -148.39(19) . . . . ?
C17 Si1 N3 C10 -30.4(2) . . . . ?
C18 Si1 N3 Ti1 -86.58(18) . . . . ?
C19 Si1 N3 Ti1 34.12(19) . . . . ?
C17 Si1 N3 Ti1 152.09(15) . . . . ?
N1 Ti1 N3 C10 0.53(19) . . . . ?
N4 Ti1 N3 C10 -106.72(12) . . . . ?
N2 Ti1 N3 C10 6.26(11) . . . . ?
N5 Ti1 N3 C10 167.62(11) . . . . ?
N6 Ti1 N3 C10 105.51(12) . . . . ?
N1 Ti1 N3 Si1 178.58(12) . . . . ?
N4 Ti1 N3 Si1 71.33(16) . . . . ?
N2 Ti1 N3 Si1 -175.69(18) . . . . ?
N5 Ti1 N3 Si1 -14.33(16) . . . . ?
N6 Ti1 N3 Si1 -76.44(15) . . . . ?
N1 Ti1 N4 C25 -29.58(16) . . . . ?
N2 Ti1 N4 C25 57.66(17) . . . . ?
N5 Ti1 N4 C25 -146.06(16) . . . . ?
N6 Ti1 N4 C25 -144.98(15) . . . . ?
N3 Ti1 N4 C25 118.52(15) . . . . ?
N1 Ti1 N4 C26 135.27(15) . . . . ?
N2 Ti1 N4 C26 -137.49(14) . . . . ?
N5 Ti1 N4 C26 18.79(15) . . . . ?
N6 Ti1 N4 C26 19.9(2) . . . . ?
N3 Ti1 N4 C26 -76.63(15) . . . . ?
N1 Ti1 N5 C29 77.29(13) . . . . ?
N4 Ti1 N5 C29 172.59(12) . . . . ?
N2 Ti1 N5 C29 -58.76(19) . . . . ?
N6 Ti1 N5 C29 -6.75(11) . . . . ?
N3 Ti1 N5 C29 -94.81(12) . . . . ?
N1 Ti1 N5 C28 -84.7(2) . . . . ?
N4 Ti1 N5 C28 10.6(2) . . . . ?
N2 Ti1 N5 C28 139.3(2) . . . . ?
N6 Ti1 N5 C28 -168.7(2) . . . . ?
N3 Ti1 N5 C28 103.2(2) . . . . ?
C36 Si2 N6 C29 101.4(2) . . . . ?
C37 Si2 N6 C29 -138.9(2) . . . . ?
C38 Si2 N6 C29 -20.7(2) . . . . ?
C36 Si2 N6 Ti1 -75.53(17) . . . . ?
C37 Si2 N6 Ti1 44.17(18) . . . . ?
C38 Si2 N6 Ti1 162.29(15) . . . . ?
N1 Ti1 N6 C29 -109.79(12) . . . . ?
N4 Ti1 N6 C29 5.46(19) . . . . ?
N2 Ti1 N6 C29 164.25(11) . . . . ?
N5 Ti1 N6 C29 6.68(10) . . . . ?
N3 Ti1 N6 C29 102.58(11) . . . . ?
N1 Ti1 N6 Si2 67.96(15) . . . . ?
N4 Ti1 N6 Si2 -176.79(12) . . . . ?
N2 Ti1 N6 Si2 -18.01(15) . . . . ?
N5 Ti1 N6 Si2 -175.58(16) . . . . ?
N3 Ti1 N6 Si2 -79.68(14) . . . . ?
C6 C1 C2 C3 2.1(4) . . . . ?
C1 C2 C3 C4 -1.4(5) . . . . ?
C2 C3 C4 C5 0.5(5) . . . . ?
C3 C4 C5 C6 -0.2(4) . . . . ?
C2 C1 C6 C5 -1.7(4) . . . . ?
C2 C1 C6 N1 178.0(2) . . . . ?
C4 C5 C6 C1 0.8(3) . . . . ?
C4 C5 C6 N1 -178.9(2) . . . . ?
C7 N1 C6 C1 146.6(2) . . . . ?
Ti1 N1 C6 C1 -49.6(2) . . . . ?
C7 N1 C6 C5 -33.7(3) . . . . ?
Ti1 N1 C6 C5 130.08(19) . . . . ?
C6 N1 C7 C8 -170.7(2) . . . . ?
Ti1 N1 C7 C8 28.1(4) . . . . ?
N1 C7 C8 C9 -59.4(4) . . . . ?
C10 N2 C9 C8 167.9(2) . . . . ?
Ti1 N2 C9 C8 -28.3(3) . . . . ?
C7 C8 C9 N2 55.4(3) . . . . ?
C9 N2 C10 N3 179.2(2) . . . . ?
Ti1 N2 C10 N3 10.16(18) . . . . ?
C9 N2 C10 C11 2.8(3) . . . . ?
Ti1 N2 C10 C11 -166.24(17) . . . . ?
Si1 N3 C10 N2 172.13(15) . . . . ?
Ti1 N3 C10 N2 -9.40(17) . . . . ?
Si1 N3 C10 C11 -11.5(3) . . . . ?
Ti1 N3 C10 C11 167.00(18) . . . . ?
N2 C10 C11 C16 109.7(2) . . . . ?
N3 C10 C11 C16 -66.3(3) . . . . ?
N2 C10 C11 C12 -71.8(3) . . . . ?
N3 C10 C11 C12 112.2(2) . . . . ?
C16 C11 C12 C13 2.1(4) . . . . ?
C10 C11 C12 C13 -176.4(2) . . . . ?
C11 C12 C13 C14 -0.6(4) . . . . ?
C12 C13 C14 C15 -1.2(4) . . . . ?
C13 C14 C15 C16 1.4(4) . . . . ?
C12 C11 C16 C15 -1.9(3) . . . . ?
C10 C11 C16 C15 176.7(2) . . . . ?
C14 C15 C16 C11 0.1(4) . . . . ?
C25 C20 C21 C22 0.8(4) . . . . ?
C20 C21 C22 C23 -1.0(5) . . . . ?
C21 C22 C23 C24 0.0(5) . . . . ?
C22 C23 C24 C25 1.3(4) . . . . ?
C23 C24 C25 C20 -1.4(4) . . . . ?
C23 C24 C25 N4 177.9(2) . . . . ?
C21 C20 C25 C24 0.4(3) . . . . ?
C21 C20 C25 N4 -178.9(2) . . . . ?
C26 N4 C25 C24 144.6(2) . . . . ?
Ti1 N4 C25 C24 -49.6(2) . . . . ?
C26 N4 C25 C20 -36.1(3) . . . . ?
Ti1 N4 C25 C20 129.69(18) . . . . ?
C25 N4 C26 C27 103.2(2) . . . . ?
Ti1 N4 C26 C27 -62.7(2) . . . . ?
N4 C26 C27 C28 77.3(2) . . . . ?
C29 N5 C28 C27 -155.76(19) . . . . ?
Ti1 N5 C28 C27 2.2(3) . . . . ?
C26 C27 C28 N5 -43.0(2) . . . . ?
C28 N5 C29 N6 176.26(18) . . . . ?
Ti1 N5 C29 N6 10.73(17) . . . . ?
C28 N5 C29 C30 0.6(3) . . . . ?
Ti1 N5 C29 C30 -164.91(16) . . . . ?
Si2 N6 C29 N5 171.87(14) . . . . ?
Ti1 N6 C29 N5 -10.12(16) . . . . ?
Si2 N6 C29 C30 -12.6(3) . . . . ?
Ti1 N6 C29 C30 165.45(17) . . . . ?
N5 C29 C30 C31 117.7(2) . . . . ?
N6 C29 C30 C31 -57.5(3) . . . . ?
N5 C29 C30 C35 -61.7(3) . . . . ?
N6 C29 C30 C35 123.2(2) . . . . ?
C35 C30 C31 C32 -1.3(3) . . . . ?
C29 C30 C31 C32 179.4(2) . . . . ?
C30 C31 C32 C33 0.3(4) . . . . ?
C31 C32 C33 C34 0.3(4) . . . . ?
C32 C33 C34 C35 0.1(4) . . . . ?
C31 C30 C35 C34 1.7(3) . . . . ?
C29 C30 C35 C34 -179.0(2) . . . . ?
C33 C34 C35 C30 -1.1(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        25.05
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.045
####################################################################### 
# 
# 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_150709a-14_a
_database_code_depnum_ccdc_archive 'CCDC 1444240'
_audit_update_record             
;
2015-12-25 deposited with the CCDC.
2016-04-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H50 N6 Si2 Zr'
_chemical_formula_weight         738.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/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                   10.5821(4)
_cell_length_b                   17.9611(8)
_cell_length_c                   20.3816(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.5500(10)
_cell_angle_gamma                90.00
_cell_volume                     3855.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    194(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.381
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.8781
_exptl_absorpt_correction_T_max  0.8942
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      194(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28637
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.88
_diffrn_reflns_theta_max         25.05
_reflns_number_total             6806
_reflns_number_gt                6128
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.0472P)²+18.2629P] 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         6806
_refine_ls_number_parameters     418
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0618
_refine_ls_wR_factor_ref         0.1442
_refine_ls_wR_factor_gt          0.1384
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.090
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.74322(3) 0.560383(19) 0.260619(18) 0.02360(13) Uani 1 1 d . . .
Si1 Si 0.71172(11) 0.70550(7) 0.12624(6) 0.0342(3) Uani 1 1 d . . .
Si2 Si 0.70181(12) 0.42043(7) 0.12350(6) 0.0381(3) Uani 1 1 d . . .
N1 N 0.8423(3) 0.48265(18) 0.32577(17) 0.0320(8) Uani 1 1 d . . .
N2 N 0.9379(3) 0.56631(18) 0.22627(17) 0.0292(7) Uani 1 1 d . . .
N3 N 0.7894(3) 0.64321(18) 0.18211(16) 0.0273(7) Uani 1 1 d . . .
N4 N 0.6813(3) 0.63181(18) 0.33432(17) 0.0306(7) Uani 1 1 d . . .
N5 N 0.5318(3) 0.5537(2) 0.2383(2) 0.0364(9) Uani 1 1 d . . .
N6 N 0.6531(3) 0.48143(19) 0.18221(17) 0.0300(7) Uani 1 1 d . . .
C1 C 0.6419(5) 0.4363(2) 0.3525(3) 0.0458(12) Uani 1 1 d . . .
H1 H 0.6174 0.4314 0.3067 0.055 Uiso 1 1 calc R . .
C2 C 0.5549(6) 0.4190(3) 0.3974(4) 0.0672(18) Uani 1 1 d . . .
H2 H 0.4710 0.4047 0.3818 0.081 Uiso 1 1 calc R . .
C3 C 0.5893(8) 0.4224(4) 0.4638(4) 0.078(2) Uani 1 1 d . . .
H3 H 0.5298 0.4110 0.4944 0.094 Uiso 1 1 calc R . .
C4 C 0.7116(8) 0.4427(4) 0.4855(3) 0.073(2) Uani 1 1 d . . .
H4 H 0.7369 0.4432 0.5316 0.088 Uiso 1 1 calc R . .
C5 C 0.7990(6) 0.4623(3) 0.4421(3) 0.0509(13) Uani 1 1 d . . .
H5 H 0.8824 0.4769 0.4585 0.061 Uiso 1 1 calc R . .
C6 C 0.7642(4) 0.4607(2) 0.3737(2) 0.0357(10) Uani 1 1 d . . .
C7 C 0.9796(4) 0.4764(3) 0.3451(2) 0.0417(11) Uani 1 1 d . . .
H7A H 0.9953 0.4323 0.3739 0.050 Uiso 1 1 calc R . .
H7B H 1.0081 0.5210 0.3711 0.050 Uiso 1 1 calc R . .
C8 C 1.0576(4) 0.4694(3) 0.2868(3) 0.0454(12) Uani 1 1 d . . .
H8A H 1.1446 0.4534 0.3030 0.055 Uiso 1 1 calc R . .
H8B H 1.0199 0.4301 0.2570 0.055 Uiso 1 1 calc R . .
C9 C 1.0657(4) 0.5406(3) 0.2479(2) 0.0371(10) Uani 1 1 d . . .
H9A H 1.1113 0.5791 0.2758 0.045 Uiso 1 1 calc R . .
H9B H 1.1134 0.5316 0.2092 0.045 Uiso 1 1 calc R . .
C10 C 0.9128(4) 0.6237(2) 0.18792(19) 0.0263(8) Uani 1 1 d . . .
C11 C 1.0139(4) 0.6662(2) 0.1572(2) 0.0318(9) Uani 1 1 d . . .
C12 C 1.0616(5) 0.7308(3) 0.1869(3) 0.0570(15) Uani 1 1 d . . .
H12 H 1.0294 0.7476 0.2262 0.068 Uiso 1 1 calc R . .
C13 C 1.1558(6) 0.7714(4) 0.1604(3) 0.0682(18) Uani 1 1 d . . .
H13 H 1.1878 0.8157 0.1813 0.082 Uiso 1 1 calc R . .
C14 C 1.2022(5) 0.7471(3) 0.1036(3) 0.0587(16) Uani 1 1 d . . .
H14 H 1.2669 0.7745 0.0852 0.070 Uiso 1 1 calc R . .
C15 C 1.1561(6) 0.6840(3) 0.0737(3) 0.0708(19) Uani 1 1 d . . .
H15 H 1.1882 0.6676 0.0342 0.085 Uiso 1 1 calc R . .
C16 C 1.0617(6) 0.6428(3) 0.1006(3) 0.0581(15) Uani 1 1 d . . .
H16 H 1.0305 0.5983 0.0796 0.070 Uiso 1 1 calc R . .
C17 C 0.5411(5) 0.7032(5) 0.1387(5) 0.108(3) Uani 1 1 d . . .
H17A H 0.5083 0.6526 0.1307 0.162 Uiso 1 1 calc R . .
H17B H 0.4947 0.7378 0.1080 0.162 Uiso 1 1 calc R . .
H17C H 0.5299 0.7178 0.1841 0.162 Uiso 1 1 calc R . .
C18 C 0.7328(7) 0.6785(3) 0.0397(3) 0.0723(19) Uani 1 1 d . . .
H18A H 0.8230 0.6813 0.0327 0.109 Uiso 1 1 calc R . .
H18B H 0.6842 0.7125 0.0093 0.109 Uiso 1 1 calc R . .
H18C H 0.7024 0.6274 0.0318 0.109 Uiso 1 1 calc R . .
C19 C 0.7674(6) 0.8032(3) 0.1389(3) 0.0551(14) Uani 1 1 d . . .
H19A H 0.7495 0.8202 0.1827 0.083 Uiso 1 1 calc R . .
H19B H 0.7230 0.8353 0.1052 0.083 Uiso 1 1 calc R . .
H19C H 0.8590 0.8056 0.1353 0.083 Uiso 1 1 calc R . .
C20 C 0.8068(5) 0.6433(3) 0.4440(2) 0.0504(13) Uani 1 1 d . . .
H20 H 0.7376 0.6283 0.4674 0.060 Uiso 1 1 calc R . .
C21 C 0.9234(7) 0.6581(4) 0.4779(3) 0.0664(17) Uani 1 1 d . . .
H21 H 0.9328 0.6537 0.5246 0.080 Uiso 1 1 calc R . .
C22 C 1.0264(6) 0.6792(3) 0.4460(3) 0.0636(16) Uani 1 1 d . . .
H22 H 1.1065 0.6875 0.4701 0.076 Uiso 1 1 calc R . .
C23 C 1.0118(5) 0.6879(3) 0.3792(3) 0.0526(13) Uani 1 1 d . . .
H23 H 1.0824 0.7022 0.3565 0.063 Uiso 1 1 calc R . .
C24 C 0.8951(4) 0.6761(2) 0.3443(2) 0.0350(9) Uani 1 1 d . . .
H24 H 0.8855 0.6856 0.2982 0.042 Uiso 1 1 calc R . .
C25 C 0.7902(4) 0.6504(2) 0.3749(2) 0.0330(9) Uani 1 1 d . . .
C26 C 0.5611(4) 0.6328(3) 0.3646(3) 0.0441(11) Uani 1 1 d . . .
H26A H 0.5624 0.6745 0.3965 0.053 Uiso 1 1 calc R . .
H26B H 0.5528 0.5859 0.3894 0.053 Uiso 1 1 calc R . .
C27 C 0.4479(4) 0.6413(3) 0.3143(3) 0.0514(13) Uani 1 1 d . . .
H27A H 0.4619 0.6851 0.2865 0.062 Uiso 1 1 calc R . .
H27B H 0.3722 0.6517 0.3378 0.062 Uiso 1 1 calc R . .
C28 C 0.4193(4) 0.5747(3) 0.2697(3) 0.0519(14) Uani 1 1 d . . .
H28A H 0.3915 0.5323 0.2958 0.062 Uiso 1 1 calc R . .
H28B H 0.3495 0.5871 0.2355 0.062 Uiso 1 1 calc R . .
C29 C 0.5354(4) 0.4976(2) 0.1972(2) 0.0298(9) Uani 1 1 d . . .
C30 C 0.4206(4) 0.4536(2) 0.1728(2) 0.0321(9) Uani 1 1 d . . .
C31 C 0.4086(5) 0.3807(3) 0.1946(2) 0.0435(11) Uani 1 1 d . . .
H31 H 0.4727 0.3598 0.2249 0.052 Uiso 1 1 calc R . .
C32 C 0.3033(5) 0.3386(3) 0.1720(3) 0.0510(13) Uani 1 1 d . . .
H32 H 0.2951 0.2890 0.1872 0.061 Uiso 1 1 calc R . .
C33 C 0.2109(5) 0.3686(3) 0.1278(3) 0.0511(13) Uani 1 1 d . . .
H33 H 0.1393 0.3396 0.1121 0.061 Uiso 1 1 calc R . .
C34 C 0.2221(5) 0.4409(3) 0.1064(3) 0.0493(13) Uani 1 1 d . . .
H34 H 0.1580 0.4614 0.0758 0.059 Uiso 1 1 calc R . .
C35 C 0.3265(4) 0.4839(3) 0.1292(2) 0.0406(10) Uani 1 1 d . . .
H35 H 0.3331 0.5340 0.1148 0.049 Uiso 1 1 calc R . .
C36 C 0.5857(4) 0.4106(3) 0.0508(2) 0.0381(3) Uani 1 1 d U . .
H36A H 0.5061 0.3907 0.0644 0.057 Uiso 1 1 calc R . .
H36B H 0.6193 0.3765 0.0192 0.057 Uiso 1 1 calc R . .
H36C H 0.5700 0.4594 0.0301 0.057 Uiso 1 1 calc R . .
C37 C 0.7383(4) 0.3298(2) 0.1598(2) 0.0381(3) Uani 1 1 d U . .
H37A H 0.7963 0.3358 0.2000 0.057 Uiso 1 1 calc R . .
H37B H 0.7786 0.2986 0.1283 0.057 Uiso 1 1 calc R . .
H37C H 0.6598 0.3060 0.1708 0.057 Uiso 1 1 calc R . .
C38 C 0.8494(6) 0.4576(4) 0.0941(4) 0.084(2) Uani 1 1 d . . .
H38A H 0.8330 0.5072 0.0750 0.126 Uiso 1 1 calc R . .
H38B H 0.8780 0.4243 0.0604 0.126 Uiso 1 1 calc R . .
H38C H 0.9154 0.4611 0.1311 0.126 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 N4 2.127(3) . ?
Zr1 N1 2.131(3) . ?
Zr1 N2 2.242(3) . ?
Zr1 N5 2.243(3) . ?
Zr1 N3 2.272(3) . ?
Zr1 N6 2.276(3) . ?
Si1 N3 1.744(3) . ?
Si1 C17 1.848(6) . ?
Si1 C19 1.862(5) . ?
Si1 C18 1.862(6) . ?
Si2 N6 1.737(3) . ?
Si2 C37 1.814(5) . ?
Si2 C36 1.840(5) . ?
Si2 C38 1.852(6) . ?
N1 C6 1.397(5) . ?
N1 C7 1.472(6) . ?
N2 C10 1.306(5) . ?
N2 C9 1.456(5) . ?
N3 C10 1.346(5) . ?
N4 C25 1.393(5) . ?
N4 C26 1.466(5) . ?
N5 C29 1.314(5) . ?
N5 C28 1.453(5) . ?
N6 C29 1.343(5) . ?
C1 C2 1.394(7) . ?
C1 C6 1.395(7) . ?
C1 H1 0.9500 . ?
C2 C3 1.368(10) . ?
C2 H2 0.9500 . ?
C3 C4 1.376(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.406(7) . ?
C5 H5 0.9500 . ?
C7 C8 1.516(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.512(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.500(5) . ?
C11 C16 1.370(7) . ?
C11 C12 1.381(7) . ?
C12 C13 1.387(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.372(9) . ?
C13 H13 0.9500 . ?
C14 C15 1.355(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.397(7) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.381(8) . ?
C20 C25 1.408(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.375(9) . ?
C21 H21 0.9500 . ?
C22 C23 1.365(8) . ?
C22 H22 0.9500 . ?
C23 C24 1.381(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.403(6) . ?
C24 H24 0.9500 . ?
C26 C27 1.508(7) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.516(7) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.494(5) . ?
C30 C35 1.381(6) . ?
C30 C31 1.392(6) . ?
C31 C32 1.388(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.374(8) . ?
C32 H32 0.9500 . ?
C33 C34 1.378(8) . ?
C33 H33 0.9500 . ?
C34 C35 1.392(6) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Zr1 N1 97.00(13) . . ?
N4 Zr1 N2 123.19(13) . . ?
N1 Zr1 N2 79.28(12) . . ?
N4 Zr1 N5 78.78(13) . . ?
N1 Zr1 N5 120.82(14) . . ?
N2 Zr1 N5 150.27(14) . . ?
N4 Zr1 N3 101.79(13) . . ?
N1 Zr1 N3 137.83(12) . . ?
N2 Zr1 N3 58.83(12) . . ?
N5 Zr1 N3 99.82(13) . . ?
N4 Zr1 N6 137.32(12) . . ?
N1 Zr1 N6 100.18(13) . . ?
N2 Zr1 N6 98.36(12) . . ?
N5 Zr1 N6 58.86(12) . . ?
N3 Zr1 N6 91.00(12) . . ?
N3 Si1 C17 107.5(2) . . ?
N3 Si1 C19 113.1(2) . . ?
C17 Si1 C19 107.6(3) . . ?
N3 Si1 C18 111.0(2) . . ?
C17 Si1 C18 109.4(4) . . ?
C19 Si1 C18 108.1(3) . . ?
N6 Si2 C37 110.5(2) . . ?
N6 Si2 C36 113.34(19) . . ?
C37 Si2 C36 110.0(2) . . ?
N6 Si2 C38 108.1(2) . . ?
C37 Si2 C38 107.6(3) . . ?
C36 Si2 C38 107.0(3) . . ?
C6 N1 C7 115.2(4) . . ?
C6 N1 Zr1 109.4(3) . . ?
C7 N1 Zr1 129.0(3) . . ?
C10 N2 C9 124.1(3) . . ?
C10 N2 Zr1 94.8(2) . . ?
C9 N2 Zr1 138.2(3) . . ?
C10 N3 Si1 128.0(3) . . ?
C10 N3 Zr1 92.3(2) . . ?
Si1 N3 Zr1 139.45(17) . . ?
C25 N4 C26 116.6(4) . . ?
C25 N4 Zr1 105.7(2) . . ?
C26 N4 Zr1 130.1(3) . . ?
C29 N5 C28 123.7(4) . . ?
C29 N5 Zr1 94.6(2) . . ?
C28 N5 Zr1 137.8(3) . . ?
C29 N6 Si2 129.6(3) . . ?
C29 N6 Zr1 92.3(2) . . ?
Si2 N6 Zr1 138.16(18) . . ?
C2 C1 C6 121.2(6) . . ?
C2 C1 H1 119.4 . . ?
C6 C1 H1 119.4 . . ?
C3 C2 C1 120.6(6) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 118.8(5) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C3 C4 C5 121.8(6) . . ?
C3 C4 H4 119.1 . . ?
C5 C4 H4 119.1 . . ?
C4 C5 C6 120.1(6) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C1 C6 N1 117.8(4) . . ?
C1 C6 C5 117.3(4) . . ?
N1 C6 C5 124.9(5) . . ?
N1 C7 C8 113.2(4) . . ?
N1 C7 H7A 108.9 . . ?
C8 C7 H7A 108.9 . . ?
N1 C7 H7B 108.9 . . ?
C8 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
C9 C8 C7 113.8(4) . . ?
C9 C8 H8A 108.8 . . ?
C7 C8 H8A 108.8 . . ?
C9 C8 H8B 108.8 . . ?
C7 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
N2 C9 C8 109.2(3) . . ?
N2 C9 H9A 109.8 . . ?
C8 C9 H9A 109.8 . . ?
N2 C9 H9B 109.8 . . ?
C8 C9 H9B 109.8 . . ?
H9A C9 H9B 108.3 . . ?
N2 C10 N3 113.4(3) . . ?
N2 C10 C11 122.7(3) . . ?
N3 C10 C11 123.8(4) . . ?
C16 C11 C12 118.6(4) . . ?
C16 C11 C10 122.1(4) . . ?
C12 C11 C10 119.3(4) . . ?
C11 C12 C13 121.1(5) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C14 C13 C12 119.4(6) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C15 C14 C13 120.2(5) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C16 120.4(5) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C11 C16 C15 120.2(5) . . ?
C11 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
Si1 C17 H17A 109.5 . . ?
Si1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si1 C18 H18A 109.5 . . ?
Si1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si1 C19 H19A 109.5 . . ?
Si1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C25 120.1(5) . . ?
C21 C20 H20 119.9 . . ?
C25 C20 H20 119.9 . . ?
C22 C21 C20 121.8(5) . . ?
C22 C21 H21 119.1 . . ?
C20 C21 H21 119.1 . . ?
C23 C22 C21 119.0(5) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
C22 C23 C24 120.4(5) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
C23 C24 C25 121.9(5) . . ?
C23 C24 H24 119.1 . . ?
C25 C24 H24 119.1 . . ?
N4 C25 C24 117.3(4) . . ?
N4 C25 C20 126.0(4) . . ?
C24 C25 C20 116.6(4) . . ?
N4 C26 C27 112.3(4) . . ?
N4 C26 H26A 109.2 . . ?
C27 C26 H26A 109.2 . . ?
N4 C26 H26B 109.2 . . ?
C27 C26 H26B 109.2 . . ?
H26A C26 H26B 107.9 . . ?
C26 C27 C28 115.3(4) . . ?
C26 C27 H27A 108.4 . . ?
C28 C27 H27A 108.4 . . ?
C26 C27 H27B 108.4 . . ?
C28 C27 H27B 108.4 . . ?
H27A C27 H27B 107.5 . . ?
N5 C28 C27 110.1(4) . . ?
N5 C28 H28A 109.6 . . ?
C27 C28 H28A 109.6 . . ?
N5 C28 H28B 109.6 . . ?
C27 C28 H28B 109.6 . . ?
H28A C28 H28B 108.2 . . ?
N5 C29 N6 113.4(3) . . ?
N5 C29 C30 123.1(4) . . ?
N6 C29 C30 123.5(4) . . ?
C35 C30 C31 119.6(4) . . ?
C35 C30 C29 121.2(4) . . ?
C31 C30 C29 119.2(4) . . ?
C32 C31 C30 120.1(5) . . ?
C32 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
C33 C32 C31 120.1(5) . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C32 C33 C34 120.0(4) . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C33 C34 C35 120.5(5) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 H34 119.8 . . ?
C30 C35 C34 119.7(5) . . ?
C30 C35 H35 120.1 . . ?
C34 C35 H35 120.1 . . ?
Si2 C36 H36A 109.5 . . ?
Si2 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
Si2 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
Si2 C37 H37A 109.5 . . ?
Si2 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
Si2 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
Si2 C38 H38A 109.5 . . ?
Si2 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
Si2 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 Zr1 N1 C6 49.4(3) . . . . ?
N2 Zr1 N1 C6 172.0(3) . . . . ?
N5 Zr1 N1 C6 -31.6(3) . . . . ?
N3 Zr1 N1 C6 165.7(3) . . . . ?
N6 Zr1 N1 C6 -91.3(3) . . . . ?
N4 Zr1 N1 C7 -100.7(4) . . . . ?
N2 Zr1 N1 C7 21.8(4) . . . . ?
N5 Zr1 N1 C7 178.2(3) . . . . ?
N3 Zr1 N1 C7 15.5(5) . . . . ?
N6 Zr1 N1 C7 118.5(4) . . . . ?
N4 Zr1 N2 C10 -79.0(3) . . . . ?
N1 Zr1 N2 C10 -170.4(3) . . . . ?
N5 Zr1 N2 C10 53.5(4) . . . . ?
N3 Zr1 N2 C10 4.6(2) . . . . ?
N6 Zr1 N2 C10 90.7(2) . . . . ?
N4 Zr1 N2 C9 80.7(4) . . . . ?
N1 Zr1 N2 C9 -10.7(4) . . . . ?
N5 Zr1 N2 C9 -146.7(4) . . . . ?
N3 Zr1 N2 C9 164.4(5) . . . . ?
N6 Zr1 N2 C9 -109.5(4) . . . . ?
C17 Si1 N3 C10 175.8(5) . . . . ?
C19 Si1 N3 C10 -65.6(4) . . . . ?
C18 Si1 N3 C10 56.2(4) . . . . ?
C17 Si1 N3 Zr1 2.5(5) . . . . ?
C19 Si1 N3 Zr1 121.1(3) . . . . ?
C18 Si1 N3 Zr1 -117.2(3) . . . . ?
N4 Zr1 N3 C10 117.3(2) . . . . ?
N1 Zr1 N3 C10 2.8(3) . . . . ?
N2 Zr1 N3 C10 -4.5(2) . . . . ?
N5 Zr1 N3 C10 -162.2(2) . . . . ?
N6 Zr1 N3 C10 -103.7(2) . . . . ?
N4 Zr1 N3 Si1 -67.9(3) . . . . ?
N1 Zr1 N3 Si1 177.5(2) . . . . ?
N2 Zr1 N3 Si1 170.2(3) . . . . ?
N5 Zr1 N3 Si1 12.5(3) . . . . ?
N6 Zr1 N3 Si1 71.1(3) . . . . ?
N1 Zr1 N4 C25 53.0(3) . . . . ?
N2 Zr1 N4 C25 -28.7(3) . . . . ?
N5 Zr1 N4 C25 173.1(3) . . . . ?
N3 Zr1 N4 C25 -89.0(3) . . . . ?
N6 Zr1 N4 C25 166.3(2) . . . . ?
N1 Zr1 N4 C26 -94.6(4) . . . . ?
N2 Zr1 N4 C26 -176.4(4) . . . . ?
N5 Zr1 N4 C26 25.5(4) . . . . ?
N3 Zr1 N4 C26 123.3(4) . . . . ?
N6 Zr1 N4 C26 18.7(5) . . . . ?
N4 Zr1 N5 C29 -168.7(3) . . . . ?
N1 Zr1 N5 C29 -77.2(3) . . . . ?
N2 Zr1 N5 C29 50.2(4) . . . . ?
N3 Zr1 N5 C29 91.0(3) . . . . ?
N6 Zr1 N5 C29 5.9(2) . . . . ?
N4 Zr1 N5 C28 -12.4(5) . . . . ?
N1 Zr1 N5 C28 79.1(5) . . . . ?
N2 Zr1 N5 C28 -153.5(4) . . . . ?
N3 Zr1 N5 C28 -112.6(5) . . . . ?
N6 Zr1 N5 C28 162.2(5) . . . . ?
C37 Si2 N6 C29 -93.5(4) . . . . ?
C36 Si2 N6 C29 30.5(4) . . . . ?
C38 Si2 N6 C29 149.0(5) . . . . ?
C37 Si2 N6 Zr1 85.7(3) . . . . ?
C36 Si2 N6 Zr1 -150.3(3) . . . . ?
C38 Si2 N6 Zr1 -31.9(4) . . . . ?
N4 Zr1 N6 C29 2.1(3) . . . . ?
N1 Zr1 N6 C29 114.3(2) . . . . ?
N2 Zr1 N6 C29 -165.2(2) . . . . ?
N5 Zr1 N6 C29 -5.7(2) . . . . ?
N3 Zr1 N6 C29 -106.6(2) . . . . ?
N4 Zr1 N6 Si2 -177.3(2) . . . . ?
N1 Zr1 N6 Si2 -65.1(3) . . . . ?
N2 Zr1 N6 Si2 15.4(3) . . . . ?
N5 Zr1 N6 Si2 174.9(4) . . . . ?
N3 Zr1 N6 Si2 74.0(3) . . . . ?
C6 C1 C2 C3 -2.9(8) . . . . ?
C1 C2 C3 C4 -0.5(9) . . . . ?
C2 C3 C4 C5 2.5(10) . . . . ?
C3 C4 C5 C6 -1.0(9) . . . . ?
C2 C1 C6 N1 -175.0(4) . . . . ?
C2 C1 C6 C5 4.2(7) . . . . ?
C7 N1 C6 C1 -154.5(4) . . . . ?
Zr1 N1 C6 C1 50.8(4) . . . . ?
C7 N1 C6 C5 26.3(6) . . . . ?
Zr1 N1 C6 C5 -128.3(4) . . . . ?
C4 C5 C6 C1 -2.3(7) . . . . ?
C4 C5 C6 N1 176.9(5) . . . . ?
C6 N1 C7 C8 156.3(4) . . . . ?
Zr1 N1 C7 C8 -55.0(5) . . . . ?
N1 C7 C8 C9 72.1(5) . . . . ?
C10 N2 C9 C8 -175.3(4) . . . . ?
Zr1 N2 C9 C8 29.3(6) . . . . ?
C7 C8 C9 N2 -56.1(6) . . . . ?
C9 N2 C10 N3 -171.1(4) . . . . ?
Zr1 N2 C10 N3 -7.3(3) . . . . ?
C9 N2 C10 C11 5.2(6) . . . . ?
Zr1 N2 C10 C11 169.0(3) . . . . ?
Si1 N3 C10 N2 -168.5(3) . . . . ?
Zr1 N3 C10 N2 7.2(3) . . . . ?
Si1 N3 C10 C11 15.3(6) . . . . ?
Zr1 N3 C10 C11 -169.0(3) . . . . ?
N2 C10 C11 C16 82.3(6) . . . . ?
N3 C10 C11 C16 -101.8(6) . . . . ?
N2 C10 C11 C12 -97.2(5) . . . . ?
N3 C10 C11 C12 78.7(6) . . . . ?
C16 C11 C12 C13 0.1(8) . . . . ?
C10 C11 C12 C13 179.6(5) . . . . ?
C11 C12 C13 C14 0.0(9) . . . . ?
C12 C13 C14 C15 0.2(9) . . . . ?
C13 C14 C15 C16 -0.5(10) . . . . ?
C12 C11 C16 C15 -0.4(9) . . . . ?
C10 C11 C16 C15 -179.9(5) . . . . ?
C14 C15 C16 C11 0.6(10) . . . . ?
C25 C20 C21 C22 -0.7(9) . . . . ?
C20 C21 C22 C23 2.1(9) . . . . ?
C21 C22 C23 C24 0.3(8) . . . . ?
C22 C23 C24 C25 -4.1(7) . . . . ?
C26 N4 C25 C24 -157.4(4) . . . . ?
Zr1 N4 C25 C24 49.8(4) . . . . ?
C26 N4 C25 C20 25.0(6) . . . . ?
Zr1 N4 C25 C20 -127.7(4) . . . . ?
C23 C24 C25 N4 -172.5(4) . . . . ?
C23 C24 C25 C20 5.3(6) . . . . ?
C21 C20 C25 N4 174.7(4) . . . . ?
C21 C20 C25 C24 -2.8(7) . . . . ?
C25 N4 C26 C27 158.1(4) . . . . ?
Zr1 N4 C26 C27 -57.1(5) . . . . ?
N4 C26 C27 C28 69.4(6) . . . . ?
C29 N5 C28 C27 179.6(5) . . . . ?
Zr1 N5 C28 C27 28.4(8) . . . . ?
C26 C27 C28 N5 -53.5(6) . . . . ?
C28 N5 C29 N6 -170.4(4) . . . . ?
Zr1 N5 C29 N6 -9.3(4) . . . . ?
C28 N5 C29 C30 6.3(7) . . . . ?
Zr1 N5 C29 C30 167.4(4) . . . . ?
Si2 N6 C29 N5 -171.4(3) . . . . ?
Zr1 N6 C29 N5 9.1(4) . . . . ?
Si2 N6 C29 C30 11.9(6) . . . . ?
Zr1 N6 C29 C30 -167.6(4) . . . . ?
N5 C29 C30 C35 70.5(6) . . . . ?
N6 C29 C30 C35 -113.1(5) . . . . ?
N5 C29 C30 C31 -109.4(5) . . . . ?
N6 C29 C30 C31 67.0(6) . . . . ?
C35 C30 C31 C32 0.7(7) . . . . ?
C29 C30 C31 C32 -179.4(4) . . . . ?
C30 C31 C32 C33 0.4(8) . . . . ?
C31 C32 C33 C34 -0.7(8) . . . . ?
C32 C33 C34 C35 -0.1(8) . . . . ?
C31 C30 C35 C34 -1.4(7) . . . . ?
C29 C30 C35 C34 178.7(4) . . . . ?
C33 C34 C35 C30 1.1(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.05
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.662
_refine_diff_density_min         -3.474
_refine_diff_density_rms         0.094
####################################################################### 
# 
# 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_151017a-14_a_a
_database_code_depnum_ccdc_archive 'CCDC 1444241'
_audit_update_record             
;
2015-12-25 deposited with the CCDC.
2016-04-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H52 Hf N6 Si2'
_chemical_formula_weight         827.52

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'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.5582(5)
_cell_length_b                   17.9443(8)
_cell_length_c                   20.4584(9)
_cell_angle_alpha                90
_cell_angle_beta                 95.1510(10)
_cell_angle_gamma                90
_cell_volume                     3860.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_F_000             1688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.400
_exptl_absorpt_coefficient_mu    2.798
_shelx_estimated_absorpt_T_min   0.366
_shelx_estimated_absorpt_T_max   0.401
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28442
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.888
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_full        25.048
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             6813
_reflns_number_gt                6213
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²+0.7415P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6813
_refine_ls_number_parameters     430
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0303
_refine_ls_wR_factor_ref         0.1219
_refine_ls_wR_factor_gt          0.1162
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.110
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Hf1 Hf 0.74152(2) 0.44124(2) 0.25930(2) 0.02581(11) Uani 1 1 d . . . . .
Si1 Si 0.70321(12) 0.58081(8) 0.12334(7) 0.0359(3) Uani 1 1 d . U . . .
Si2 Si 0.71182(12) 0.29474(7) 0.12770(7) 0.0382(3) Uani 1 1 d . . . . .
N1 N 0.6825(4) 0.3704(2) 0.33364(19) 0.0343(8) Uani 1 1 d . . . . .
H1 H 0.6670 0.3269 0.3097 0.041 Uiso 1 1 d R U . . .
N2 N 0.5321(4) 0.4481(2) 0.2378(3) 0.0401(11) Uani 1 1 d . . . . .
N3 N 0.6534(3) 0.5198(2) 0.18224(18) 0.0309(8) Uani 1 1 d . . . . .
N4 N 0.8365(3) 0.5185(2) 0.32459(19) 0.0346(8) Uani 1 1 d . . . . .
H4 H 0.8252 0.5636 0.2959 0.042 Uiso 1 1 d R U . . .
N5 N 0.9353(4) 0.43433(18) 0.2264(2) 0.0328(9) Uani 1 1 d . . . . .
N6 N 0.7888(3) 0.3579(2) 0.18270(18) 0.0299(8) Uani 1 1 d . . . . .
C1 C 0.7912(5) 0.3511(2) 0.3753(2) 0.0356(11) Uani 1 1 d . . . . .
C2 C 0.8960(4) 0.3252(3) 0.3459(3) 0.0408(11) Uani 1 1 d . . . . .
H2 H 0.8882 0.3156 0.3001 0.049 Uiso 1 1 calc R U . . .
C3 C 1.0121(6) 0.3129(3) 0.3818(3) 0.0625(17) Uani 1 1 d . . . . .
H3 H 1.0840 0.2981 0.3602 0.075 Uiso 1 1 calc R U . . .
C4 C 1.0224(7) 0.3222(4) 0.4480(4) 0.081(2) Uani 1 1 d . . . . .
H4A H 1.1016 0.3138 0.4728 0.097 Uiso 1 1 calc R U . . .
C5 C 0.9186(7) 0.3437(4) 0.4787(3) 0.077(2) Uani 1 1 d . . . . .
H5 H 0.9252 0.3479 0.5252 0.092 Uiso 1 1 calc R U . . .
C6 C 0.8026(6) 0.3595(3) 0.4427(3) 0.0577(15) Uani 1 1 d . . . . .
H6 H 0.7320 0.3759 0.4645 0.069 Uiso 1 1 calc R U . . .
C7 C 0.5622(5) 0.3681(3) 0.3639(3) 0.0502(13) Uani 1 1 d . . . . .
H7A H 0.5534 0.4143 0.3895 0.060 Uiso 1 1 calc R U . . .
H7B H 0.5635 0.3255 0.3947 0.060 Uiso 1 1 calc R U . . .
C8 C 0.4482(5) 0.3606(3) 0.3137(3) 0.0586(16) Uani 1 1 d . . . . .
H8A H 0.4623 0.3170 0.2856 0.070 Uiso 1 1 calc R U . . .
H8B H 0.3726 0.3498 0.3373 0.070 Uiso 1 1 calc R U . . .
C9 C 0.4188(5) 0.4261(3) 0.2702(4) 0.0574(17) Uani 1 1 d . . . . .
H9A H 0.3487 0.4135 0.2367 0.069 Uiso 1 1 calc R U . . .
H9B H 0.3907 0.4683 0.2966 0.069 Uiso 1 1 calc R U . . .
C10 C 0.5359(4) 0.5042(2) 0.1972(2) 0.0315(9) Uani 1 1 d . . . . .
C11 C 0.4205(4) 0.5471(2) 0.1723(3) 0.0340(10) Uani 1 1 d . . . . .
C12 C 0.3266(4) 0.5160(3) 0.1290(3) 0.0460(12) Uani 1 1 d . . . . .
H12 H 0.3330 0.4656 0.1155 0.055 Uiso 1 1 calc R U . . .
C13 C 0.2230(5) 0.5592(3) 0.1055(3) 0.0527(16) Uani 1 1 d . . . . .
H13 H 0.1597 0.5385 0.0749 0.063 Uiso 1 1 calc R U . . .
C14 C 0.2117(5) 0.6311(3) 0.1262(3) 0.0545(15) Uani 1 1 d . . . . .
H14 H 0.1403 0.6600 0.1099 0.065 Uiso 1 1 calc R U . . .
C15 C 0.3017(5) 0.6618(3) 0.1701(3) 0.0544(14) Uani 1 1 d . . . . .
H15 H 0.2921 0.7115 0.1848 0.065 Uiso 1 1 calc R U . . .
C16 C 0.4076(5) 0.6202(3) 0.1932(3) 0.0473(12) Uani 1 1 d . . . . .
H16 H 0.4710 0.6418 0.2233 0.057 Uiso 1 1 calc R U . . .
C17 C 0.8505(6) 0.5449(4) 0.0940(3) 0.0613(13) Uani 1 1 d . U . . .
H17A H 0.8319 0.4995 0.0683 0.092 Uiso 1 1 calc R U . . .
H17B H 0.9114 0.5334 0.1317 0.092 Uiso 1 1 calc R U . . .
H17C H 0.8869 0.5825 0.0665 0.092 Uiso 1 1 calc R U . . .
C18 C 0.5884(6) 0.5893(4) 0.0509(3) 0.0762(14) Uani 1 1 d . U . . .
H18A H 0.5722 0.5400 0.0314 0.114 Uiso 1 1 calc R U . . .
H18B H 0.6229 0.6223 0.0187 0.114 Uiso 1 1 calc R U . . .
H18C H 0.5086 0.6101 0.0640 0.114 Uiso 1 1 calc R U . . .
C19 C 0.7356(8) 0.6733(4) 0.1584(4) 0.0833(16) Uani 1 1 d . U . . .
H19A H 0.8250 0.6763 0.1758 0.125 Uiso 1 1 calc R U . . .
H19B H 0.6810 0.6819 0.1939 0.125 Uiso 1 1 calc R U . . .
H19C H 0.7182 0.7111 0.1243 0.125 Uiso 1 1 calc R U . . .
C20 C 1.0131(4) 0.3357(2) 0.1575(2) 0.0342(10) Uani 1 1 d . . . . .
C21 C 1.0642(5) 0.2715(4) 0.1882(3) 0.0640(17) Uani 1 1 d . . . . .
H21 H 1.0332 0.2544 0.2277 0.077 Uiso 1 1 calc R U . . .
C22 C 1.1603(6) 0.2327(4) 0.1609(3) 0.074(2) Uani 1 1 d . . . . .
H22 H 1.1963 0.1900 0.1829 0.088 Uiso 1 1 calc R U . . .
C23 C 1.2040(5) 0.2544(4) 0.1033(3) 0.0619(18) Uani 1 1 d . . . . .
H23 H 1.2684 0.2268 0.0845 0.074 Uiso 1 1 calc R U . . .
C24 C 1.1532(7) 0.3164(4) 0.0733(4) 0.080(2) Uani 1 1 d . . . . .
H24 H 1.1824 0.3319 0.0329 0.096 Uiso 1 1 calc R U . . .
C25 C 1.0595(6) 0.3578(3) 0.1003(3) 0.0669(17) Uani 1 1 d . . . . .
H25 H 1.0275 0.4018 0.0789 0.080 Uiso 1 1 calc R U . . .
C26 C 0.9112(4) 0.3768(2) 0.1883(2) 0.0285(9) Uani 1 1 d . . . . .
C27 C 1.0636(5) 0.4614(3) 0.2484(3) 0.0431(11) Uani 1 1 d . . . . .
H27A H 1.1128 0.4695 0.2101 0.052 Uiso 1 1 calc R U . . .
H27B H 1.1089 0.4238 0.2773 0.052 Uiso 1 1 calc R U . . .
C28 C 1.0525(5) 0.5330(3) 0.2851(3) 0.0504(13) Uani 1 1 d . . . . .
H28A H 1.0133 0.5711 0.2545 0.060 Uiso 1 1 calc R U . . .
H28B H 1.1389 0.5506 0.3006 0.060 Uiso 1 1 calc R U . . .
C29 C 0.9742(5) 0.5267(3) 0.3435(3) 0.0486(13) Uani 1 1 d . . . . .
H29A H 1.0042 0.4830 0.3702 0.058 Uiso 1 1 calc R U . . .
H29B H 0.9883 0.5717 0.3712 0.058 Uiso 1 1 calc R U . . .
C30 C 0.7595(5) 0.5413(3) 0.3731(3) 0.0423(12) Uani 1 1 d . . . . .
C31 C 0.7959(7) 0.5411(3) 0.4396(3) 0.0587(16) Uani 1 1 d . . . . .
H31 H 0.8808 0.5279 0.4544 0.070 Uiso 1 1 calc R U . . .
C32 C 0.7121(10) 0.5598(4) 0.4856(4) 0.083(3) Uani 1 1 d . . . . .
H32 H 0.7396 0.5583 0.5311 0.100 Uiso 1 1 calc R U . . .
C33 C 0.5894(9) 0.5805(4) 0.4654(4) 0.088(3) Uani 1 1 d . . . . .
H33 H 0.5317 0.5931 0.4967 0.105 Uiso 1 1 calc R U . . .
C34 C 0.5519(7) 0.5828(4) 0.4008(5) 0.082(2) Uani 1 1 d . . . . .
H34 H 0.4671 0.5966 0.3864 0.098 Uiso 1 1 calc R U . . .
C35 C 0.6374(6) 0.5649(2) 0.3545(4) 0.0529(16) Uani 1 1 d . . . . .
H35 H 0.6104 0.5692 0.3091 0.063 Uiso 1 1 calc R U . . .
C36 C 0.7686(6) 0.1981(3) 0.1417(3) 0.0583(15) Uani 1 1 d . . . . .
H36A H 0.7496 0.1816 0.1854 0.087 Uiso 1 1 calc R U . . .
H36B H 0.8606 0.1961 0.1386 0.087 Uiso 1 1 calc R U . . .
H36C H 0.7257 0.1652 0.1084 0.087 Uiso 1 1 calc R U . . .
C37 C 0.5408(6) 0.2969(5) 0.1410(6) 0.122(4) Uani 1 1 d . . . . .
H37A H 0.5062 0.3465 0.1298 0.183 Uiso 1 1 calc R U . . .
H37B H 0.5303 0.2861 0.1871 0.183 Uiso 1 1 calc R U . . .
H37C H 0.4953 0.2595 0.1130 0.183 Uiso 1 1 calc R U . . .
C38 C 0.7325(8) 0.3210(3) 0.0413(3) 0.081(2) Uani 1 1 d . . . . .
H38A H 0.8228 0.3178 0.0338 0.122 Uiso 1 1 calc R U . . .
H38B H 0.7024 0.3721 0.0332 0.122 Uiso 1 1 calc R U . . .
H38C H 0.6834 0.2869 0.0115 0.122 Uiso 1 1 calc R U . . .


_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
Hf1 N4 2.115(4) . ?
Hf1 N1 2.119(4) . ?
Hf1 N5 2.214(4) . ?
Hf1 N2 2.219(4) . ?
Hf1 N3 2.253(4) . ?
Hf1 N6 2.255(4) . ?
Hf1 C10 2.666(4) . ?
Hf1 C26 2.669(4) . ?
Si1 N3 1.744(4) . ?
Si1 C19 1.827(6) . ?
Si1 C17 1.833(7) . ?
Si1 C18 1.835(6) . ?
Si2 N6 1.745(4) . ?
Si2 C36 1.849(5) . ?
Si2 C37 1.850(7) . ?
Si2 C38 1.860(7) . ?
N1 C1 1.410(6) . ?
N1 C7 1.463(6) . ?
N1 H1 0.9277 . ?
N2 C10 1.307(6) . ?
N2 C9 1.473(7) . ?
N3 C10 1.335(5) . ?
N4 C30 1.399(7) . ?
N4 C29 1.478(6) . ?
N4 H4 1.0000 . ?
N5 C26 1.305(5) . ?
N5 C27 1.471(6) . ?
N6 C26 1.330(5) . ?
C1 C6 1.381(7) . ?
C1 C2 1.387(7) . ?
C2 C3 1.389(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.359(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.367(11) . ?
C4 H4A 0.9500 . ?
C5 C6 1.401(9) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.516(8) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.489(7) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.492(6) . ?
C11 C12 1.385(7) . ?
C11 C16 1.392(6) . ?
C12 C13 1.390(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.367(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.364(8) . ?
C14 H14 0.9500 . ?
C15 C16 1.392(6) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C25 1.366(7) . ?
C20 C21 1.397(7) . ?
C20 C26 1.491(6) . ?
C21 C22 1.388(7) . ?
C21 H21 0.9500 . ?
C22 C23 1.361(10) . ?
C22 H22 0.9500 . ?
C23 C24 1.357(9) . ?
C23 H23 0.9500 . ?
C24 C25 1.391(8) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C27 C28 1.499(7) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.518(8) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C35 1.378(8) . ?
C30 C31 1.381(8) . ?
C31 C32 1.389(10) . ?
C31 H31 0.9500 . ?
C32 C33 1.375(12) . ?
C32 H32 0.9500 . ?
C33 C34 1.346(11) . ?
C33 H33 0.9500 . ?
C34 C35 1.403(9) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Hf1 N1 95.38(15) . . ?
N4 Hf1 N5 80.21(14) . . ?
N1 Hf1 N5 121.60(14) . . ?
N4 Hf1 N2 119.78(15) . . ?
N1 Hf1 N2 79.85(15) . . ?
N5 Hf1 N2 150.96(18) . . ?
N4 Hf1 N3 100.02(17) . . ?
N1 Hf1 N3 138.45(14) . . ?
N5 Hf1 N3 99.04(13) . . ?
N2 Hf1 N3 58.99(14) . . ?
N4 Hf1 N6 138.76(13) . . ?
N1 Hf1 N6 101.45(15) . . ?
N5 Hf1 N6 58.87(13) . . ?
N2 Hf1 N6 100.24(15) . . ?
N3 Hf1 N6 91.85(13) . . ?
N4 Hf1 C10 110.05(14) . . ?
N1 Hf1 C10 108.47(14) . . ?
N5 Hf1 C10 127.89(14) . . ?
N2 Hf1 C10 29.24(14) . . ?
N3 Hf1 C10 30.01(13) . . ?
N6 Hf1 C10 99.88(13) . . ?
N4 Hf1 C26 108.93(13) . . ?
N1 Hf1 C26 112.70(13) . . ?
N5 Hf1 C26 29.13(13) . . ?
N2 Hf1 C26 128.42(16) . . ?
N3 Hf1 C26 98.35(13) . . ?
N6 Hf1 C26 29.87(12) . . ?
C10 Hf1 C26 118.80(13) . . ?
N3 Si1 C19 110.9(3) . . ?
N3 Si1 C17 108.8(2) . . ?
C19 Si1 C17 108.3(4) . . ?
N3 Si1 C18 113.1(3) . . ?
C19 Si1 C18 109.2(4) . . ?
C17 Si1 C18 106.5(3) . . ?
N6 Si2 C36 112.6(2) . . ?
N6 Si2 C37 107.2(3) . . ?
C36 Si2 C37 107.7(4) . . ?
N6 Si2 C38 111.1(3) . . ?
C36 Si2 C38 108.7(3) . . ?
C37 Si2 C38 109.5(5) . . ?
C1 N1 C7 115.4(4) . . ?
C1 N1 Hf1 107.8(3) . . ?
C7 N1 Hf1 130.0(3) . . ?
C1 N1 H1 102.0 . . ?
C7 N1 H1 94.6 . . ?
Hf1 N1 H1 100.1 . . ?
C10 N2 C9 124.4(4) . . ?
C10 N2 Hf1 94.7(3) . . ?
C9 N2 Hf1 136.9(4) . . ?
C10 N3 Si1 129.4(3) . . ?
C10 N3 Hf1 92.4(3) . . ?
Si1 N3 Hf1 138.17(19) . . ?
C30 N4 C29 114.0(4) . . ?
C30 N4 Hf1 111.5(3) . . ?
C29 N4 Hf1 129.0(3) . . ?
C30 N4 H4 97.7 . . ?
C29 N4 H4 97.8 . . ?
Hf1 N4 H4 97.8 . . ?
C26 N5 C27 124.7(4) . . ?
C26 N5 Hf1 95.1(3) . . ?
C27 N5 Hf1 137.7(3) . . ?
C26 N6 Si2 127.9(3) . . ?
C26 N6 Hf1 92.6(3) . . ?
Si2 N6 Hf1 139.40(18) . . ?
C6 C1 C2 117.9(5) . . ?
C6 C1 N1 124.8(5) . . ?
C2 C1 N1 117.3(4) . . ?
C1 C2 C3 121.7(5) . . ?
C1 C2 H2 119.2 . . ?
C3 C2 H2 119.2 . . ?
C4 C3 C2 119.7(7) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 119.8(6) . . ?
C3 C4 H4A 120.1 . . ?
C5 C4 H4A 120.1 . . ?
C4 C5 C6 120.9(6) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C1 C6 C5 119.8(6) . . ?
C1 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
N1 C7 C8 112.5(5) . . ?
N1 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
N1 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.8 . . ?
C9 C8 C7 116.4(5) . . ?
C9 C8 H8A 108.2 . . ?
C7 C8 H8A 108.2 . . ?
C9 C8 H8B 108.2 . . ?
C7 C8 H8B 108.2 . . ?
H8A C8 H8B 107.3 . . ?
N2 C9 C8 110.3(4) . . ?
N2 C9 H9A 109.6 . . ?
C8 C9 H9A 109.6 . . ?
N2 C9 H9B 109.6 . . ?
C8 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
N2 C10 N3 113.0(4) . . ?
N2 C10 C11 122.9(4) . . ?
N3 C10 C11 124.1(4) . . ?
N2 C10 Hf1 56.1(2) . . ?
N3 C10 Hf1 57.6(2) . . ?
C11 C10 Hf1 170.6(3) . . ?
C12 C11 C16 119.5(4) . . ?
C12 C11 C10 121.7(4) . . ?
C16 C11 C10 118.7(4) . . ?
C11 C12 C13 119.4(5) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
C14 C13 C12 120.5(5) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C15 C14 C13 120.7(5) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C14 C15 C16 119.9(5) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C11 C16 C15 119.9(5) . . ?
C11 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
Si1 C17 H17A 109.5 . . ?
Si1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si1 C18 H18A 109.5 . . ?
Si1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si1 C19 H19A 109.5 . . ?
Si1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C25 C20 C21 118.1(5) . . ?
C25 C20 C26 123.1(4) . . ?
C21 C20 C26 118.8(4) . . ?
C22 C21 C20 120.0(6) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C23 C22 C21 121.4(6) . . ?
C23 C22 H22 119.3 . . ?
C21 C22 H22 119.3 . . ?
C24 C23 C22 118.4(5) . . ?
C24 C23 H23 120.8 . . ?
C22 C23 H23 120.8 . . ?
C23 C24 C25 121.7(6) . . ?
C23 C24 H24 119.2 . . ?
C25 C24 H24 119.2 . . ?
C20 C25 C24 120.5(6) . . ?
C20 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
N5 C26 N6 112.9(4) . . ?
N5 C26 C20 122.3(4) . . ?
N6 C26 C20 124.7(4) . . ?
N5 C26 Hf1 55.7(2) . . ?
N6 C26 Hf1 57.6(2) . . ?
C20 C26 Hf1 171.9(3) . . ?
N5 C27 C28 109.0(4) . . ?
N5 C27 H27A 109.9 . . ?
C28 C27 H27A 109.9 . . ?
N5 C27 H27B 109.9 . . ?
C28 C27 H27B 109.9 . . ?
H27A C27 H27B 108.3 . . ?
C27 C28 C29 113.7(5) . . ?
C27 C28 H28A 108.8 . . ?
C29 C28 H28A 108.8 . . ?
C27 C28 H28B 108.8 . . ?
C29 C28 H28B 108.8 . . ?
H28A C28 H28B 107.7 . . ?
N4 C29 C28 113.2(4) . . ?
N4 C29 H29A 108.9 . . ?
C28 C29 H29A 108.9 . . ?
N4 C29 H29B 108.9 . . ?
C28 C29 H29B 108.9 . . ?
H29A C29 H29B 107.8 . . ?
C35 C30 C31 116.3(6) . . ?
C35 C30 N4 118.9(5) . . ?
C31 C30 N4 124.8(5) . . ?
C30 C31 C32 122.0(7) . . ?
C30 C31 H31 119.0 . . ?
C32 C31 H31 119.0 . . ?
C33 C32 C31 120.1(8) . . ?
C33 C32 H32 119.9 . . ?
C31 C32 H32 119.9 . . ?
C34 C33 C32 119.3(7) . . ?
C34 C33 H33 120.3 . . ?
C32 C33 H33 120.3 . . ?
C33 C34 C35 120.4(7) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 H34 119.8 . . ?
C30 C35 C34 121.8(7) . . ?
C30 C35 H35 119.1 . . ?
C34 C35 H35 119.1 . . ?
Si2 C36 H36A 109.5 . . ?
Si2 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
Si2 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
Si2 C37 H37A 109.5 . . ?
Si2 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
Si2 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
Si2 C38 H38A 109.5 . . ?
Si2 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
Si2 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C19 Si1 N3 C10 91.6(5) . . . . ?
C17 Si1 N3 C10 -149.5(4) . . . . ?
C18 Si1 N3 C10 -31.4(5) . . . . ?
C19 Si1 N3 Hf1 -87.9(4) . . . . ?
C17 Si1 N3 Hf1 31.0(4) . . . . ?
C18 Si1 N3 Hf1 149.1(4) . . . . ?
C36 Si2 N6 C26 65.0(5) . . . . ?
C37 Si2 N6 C26 -176.7(5) . . . . ?
C38 Si2 N6 C26 -57.1(5) . . . . ?
C36 Si2 N6 Hf1 -121.4(3) . . . . ?
C37 Si2 N6 Hf1 -3.1(5) . . . . ?
C38 Si2 N6 Hf1 116.5(4) . . . . ?
C7 N1 C1 C6 -27.0(6) . . . . ?
Hf1 N1 C1 C6 127.1(4) . . . . ?
C7 N1 C1 C2 156.3(4) . . . . ?
Hf1 N1 C1 C2 -49.7(4) . . . . ?
C6 C1 C2 C3 -4.5(7) . . . . ?
N1 C1 C2 C3 172.4(4) . . . . ?
C1 C2 C3 C4 3.9(8) . . . . ?
C2 C3 C4 C5 -0.1(9) . . . . ?
C3 C4 C5 C6 -2.8(10) . . . . ?
C2 C1 C6 C5 1.6(8) . . . . ?
N1 C1 C6 C5 -175.2(5) . . . . ?
C4 C5 C6 C1 2.1(10) . . . . ?
C1 N1 C7 C8 -158.6(4) . . . . ?
Hf1 N1 C7 C8 54.4(6) . . . . ?
N1 C7 C8 C9 -68.6(7) . . . . ?
C10 N2 C9 C8 -179.3(5) . . . . ?
Hf1 N2 C9 C8 -28.0(9) . . . . ?
C7 C8 C9 N2 53.6(8) . . . . ?
C9 N2 C10 N3 170.3(5) . . . . ?
Hf1 N2 C10 N3 9.5(4) . . . . ?
C9 N2 C10 C11 -8.0(8) . . . . ?
Hf1 N2 C10 C11 -168.8(4) . . . . ?
C9 N2 C10 Hf1 160.8(7) . . . . ?
Si1 N3 C10 N2 171.0(4) . . . . ?
Hf1 N3 C10 N2 -9.3(4) . . . . ?
Si1 N3 C10 C11 -10.7(7) . . . . ?
Hf1 N3 C10 C11 169.0(4) . . . . ?
Si1 N3 C10 Hf1 -179.7(4) . . . . ?
N2 C10 C11 C12 -69.4(7) . . . . ?
N3 C10 C11 C12 112.5(5) . . . . ?
N2 C10 C11 C16 110.7(6) . . . . ?
N3 C10 C11 C16 -67.4(7) . . . . ?
C16 C11 C12 C13 2.1(8) . . . . ?
C10 C11 C12 C13 -177.9(5) . . . . ?
C11 C12 C13 C14 -1.8(9) . . . . ?
C12 C13 C14 C15 0.1(9) . . . . ?
C13 C14 C15 C16 1.2(9) . . . . ?
C12 C11 C16 C15 -0.8(8) . . . . ?
C10 C11 C16 C15 179.2(5) . . . . ?
C14 C15 C16 C11 -0.9(9) . . . . ?
C25 C20 C21 C22 0.7(9) . . . . ?
C26 C20 C21 C22 -179.3(5) . . . . ?
C20 C21 C22 C23 -2.1(10) . . . . ?
C21 C22 C23 C24 1.4(10) . . . . ?
C22 C23 C24 C25 0.5(11) . . . . ?
C21 C20 C25 C24 1.1(9) . . . . ?
C26 C20 C25 C24 -178.9(6) . . . . ?
C23 C24 C25 C20 -1.8(11) . . . . ?
C27 N5 C26 N6 171.5(4) . . . . ?
Hf1 N5 C26 N6 6.7(4) . . . . ?
C27 N5 C26 C20 -5.8(7) . . . . ?
Hf1 N5 C26 C20 -170.6(4) . . . . ?
C27 N5 C26 Hf1 164.8(5) . . . . ?
Si2 N6 C26 N5 169.2(3) . . . . ?
Hf1 N6 C26 N5 -6.6(4) . . . . ?
Si2 N6 C26 C20 -13.5(6) . . . . ?
Hf1 N6 C26 C20 170.6(4) . . . . ?
Si2 N6 C26 Hf1 175.8(4) . . . . ?
C25 C20 C26 N5 -83.9(6) . . . . ?
C21 C20 C26 N5 96.1(6) . . . . ?
C25 C20 C26 N6 99.1(6) . . . . ?
C21 C20 C26 N6 -80.9(6) . . . . ?
C26 N5 C27 C28 173.7(5) . . . . ?
Hf1 N5 C27 C28 -29.1(7) . . . . ?
N5 C27 C28 C29 57.4(6) . . . . ?
C30 N4 C29 C28 -156.3(4) . . . . ?
Hf1 N4 C29 C28 52.5(6) . . . . ?
C27 C28 C29 N4 -72.4(6) . . . . ?
C29 N4 C30 C35 154.1(5) . . . . ?
Hf1 N4 C30 C35 -49.6(5) . . . . ?
C29 N4 C30 C31 -26.7(7) . . . . ?
Hf1 N4 C30 C31 129.6(5) . . . . ?
C35 C30 C31 C32 3.4(8) . . . . ?
N4 C30 C31 C32 -175.7(5) . . . . ?
C30 C31 C32 C33 -1.2(10) . . . . ?
C31 C32 C33 C34 -0.3(11) . . . . ?
C32 C33 C34 C35 -0.6(11) . . . . ?
C31 C30 C35 C34 -4.4(8) . . . . ?
N4 C30 C35 C34 174.8(5) . . . . ?
C33 C34 C35 C30 3.1(10) . . . . ?

_refine_diff_density_max         0.695
_refine_diff_density_min         -1.452
_refine_diff_density_rms         0.087

####################################################################### 
# 
# 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_150709b-2_a
_database_code_depnum_ccdc_archive 'CCDC 1444243'
_audit_update_record             
;
2015-12-25 deposited with the CCDC.
2016-04-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H69 Li4 N6 O2 Si2'
_chemical_formula_weight         822.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   12.2130(5)
_cell_length_b                   13.3811(5)
_cell_length_c                   16.3014(7)
_cell_angle_alpha                84.4800(10)
_cell_angle_beta                 72.5300(10)
_cell_angle_gamma                83.8350(10)
_cell_volume                     2520.70(18)
_cell_formula_units_Z            33
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    17.870
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             14619
_exptl_absorpt_coefficient_mu    1.812
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25182
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.89
_diffrn_reflns_theta_max         28.25
_reflns_number_total             12118
_reflns_number_gt                8776
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.0000P)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         12118
_refine_ls_number_parameters     559
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0830
_refine_ls_wR_factor_ref         0.1895
_refine_ls_wR_factor_gt          0.1857
_refine_ls_goodness_of_fit_ref   4.002
_refine_ls_restrained_S_all      4.002
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Li1 Li 0.6632(4) 0.4851(4) 0.2330(3) 0.0407(12) Uani 1 1 d . . .
Li2 Li 0.6090(4) 0.2666(4) 0.2814(3) 0.0425(12) Uani 1 1 d . . .
Li3 Li 0.7716(5) 0.1263(4) 0.2780(3) 0.0469(13) Uani 1 1 d . . .
Li4 Li 0.8236(4) 0.3079(4) 0.2523(3) 0.0409(12) Uani 1 1 d . . .
Si1 Si 0.50871(7) 0.09539(6) 0.21092(5) 0.0423(2) Uani 1 1 d . . .
Si2 Si 1.01690(7) 0.20487(8) 0.34017(5) 0.0526(3) Uani 1 1 d . . .
O1 O 0.63554(17) 0.61709(14) 0.17529(12) 0.0430(5) Uani 1 1 d . . .
O2 O 0.8187(2) -0.01785(18) 0.28942(19) 0.0789(8) Uani 1 1 d . . .
N1 N 0.52805(18) 0.40009(16) 0.30221(13) 0.0303(5) Uani 1 1 d . . .
N2 N 0.68021(19) 0.23631(17) 0.38112(13) 0.0343(5) Uani 1 1 d . . .
N3 N 0.87540(19) 0.21113(18) 0.33838(13) 0.0381(6) Uani 1 1 d . . .
N4 N 0.83652(18) 0.44558(17) 0.20019(13) 0.0348(6) Uani 1 1 d . . .
N5 N 0.79644(19) 0.22915(17) 0.15942(13) 0.0347(6) Uani 1 1 d . . .
N6 N 0.63134(18) 0.14920(16) 0.20944(13) 0.0322(5) Uani 1 1 d . . .
C1 C 0.5155(3) 0.4086(2) 0.15825(17) 0.0375(7) Uani 1 1 d . . .
C2 C 0.4549(3) 0.4318(2) 0.09842(19) 0.0501(8) Uani 1 1 d . . .
H2 H 0.4926 0.4208 0.0395 0.060 Uiso 1 1 calc R . .
C3 C 0.3408(3) 0.4706(3) 0.1224(2) 0.0586(9) Uani 1 1 d . . .
H3 H 0.3003 0.4867 0.0807 0.070 Uiso 1 1 calc R . .
C4 C 0.2878(3) 0.4851(2) 0.2080(2) 0.0544(9) Uani 1 1 d . . .
H4 H 0.2095 0.5113 0.2253 0.065 Uiso 1 1 calc R . .
C5 C 0.3450(2) 0.4629(2) 0.26931(19) 0.0437(7) Uani 1 1 d . . .
H5 H 0.3053 0.4739 0.3279 0.052 Uiso 1 1 calc R . .
C6 C 0.4625(2) 0.42389(19) 0.24656(16) 0.0301(6) Uani 1 1 d . . .
C7 C 0.4594(2) 0.4069(2) 0.39427(15) 0.0358(7) Uani 1 1 d . . .
C8 C 0.5263(2) 0.3657(2) 0.45761(16) 0.0395(7) Uani 1 1 d . . .
C9 C 0.5711(2) 0.2529(2) 0.45061(17) 0.0390(7) Uani 1 1 d . . .
C10 C 0.7786(2) 0.22540(19) 0.40130(16) 0.0306(6) Uani 1 1 d . . .
C11 C 0.7813(2) 0.2267(2) 0.49275(15) 0.0294(6) Uani 1 1 d . . .
C12 C 0.8020(2) 0.3129(2) 0.52256(17) 0.0395(7) Uani 1 1 d . . .
H12 H 0.8080 0.3733 0.4863 0.047 Uiso 1 1 calc R . .
C13 C 0.8144(3) 0.3143(3) 0.60508(19) 0.0504(8) Uani 1 1 d . . .
C14 C 0.8046(3) 0.2257(3) 0.65730(18) 0.0543(9) Uani 1 1 d . . .
H14 H 0.8139 0.2250 0.7131 0.065 Uiso 1 1 calc R . .
C15 C 0.7814(3) 0.1391(3) 0.62944(19) 0.0597(10) Uani 1 1 d . . .
H15 H 0.7728 0.0791 0.6662 0.072 Uiso 1 1 calc R . .
C16 C 0.7708(3) 0.1397(2) 0.54722(18) 0.0499(8) Uani 1 1 d . . .
H16 H 0.7561 0.0793 0.5277 0.060 Uiso 1 1 calc R . .
C17 C 1.0599(4) 0.3299(4) 0.3524(4) 0.166(3) Uani 1 1 d . . .
H17A H 1.0538 0.3760 0.3032 0.248 Uiso 1 1 calc R . .
H17B H 1.1397 0.3230 0.3547 0.248 Uiso 1 1 calc R . .
H17C H 1.0091 0.3567 0.4058 0.248 Uiso 1 1 calc R . .
C18 C 1.0505(3) 0.1238(3) 0.4289(3) 0.0910(15) Uani 1 1 d . . .
H18A H 1.0011 0.1471 0.4842 0.137 Uiso 1 1 calc R . .
H18B H 1.1314 0.1271 0.4257 0.137 Uiso 1 1 calc R . .
H18C H 1.0366 0.0541 0.4241 0.137 Uiso 1 1 calc R . .
C19 C 1.1037(4) 0.1625(7) 0.2365(3) 0.238(5) Uani 1 1 d . . .
H19A H 1.0586 0.1737 0.1954 0.358 Uiso 1 1 calc R . .
H19B H 1.1273 0.0905 0.2427 0.358 Uiso 1 1 calc R . .
H19C H 1.1723 0.2003 0.2154 0.358 Uiso 1 1 calc R . .
C20 C 0.9546(2) 0.5757(2) 0.22255(19) 0.0427(7) Uani 1 1 d . . .
H20 H 1.0031 0.5755 0.1648 0.051 Uiso 1 1 calc R . .
C21 C 0.9736(3) 0.6385(2) 0.2778(2) 0.0540(9) Uani 1 1 d . . .
H21 H 1.0346 0.6814 0.2572 0.065 Uiso 1 1 calc R . .
C22 C 0.9069(3) 0.6407(2) 0.3620(2) 0.0584(9) Uani 1 1 d . . .
H22 H 0.9229 0.6839 0.3992 0.070 Uiso 1 1 calc R . .
C23 C 0.8150(3) 0.5792(2) 0.3933(2) 0.0522(8) Uani 1 1 d . . .
C24 C 0.7950(2) 0.5153(2) 0.33776(18) 0.0433(7) Uani 1 1 d . . .
C25 C 0.8640(2) 0.5113(2) 0.25007(17) 0.0340(6) Uani 1 1 d . . .
C26 C 0.9118(2) 0.4455(2) 0.11172(16) 0.0418(7) Uani 1 1 d . . .
H26A H 0.9923 0.4278 0.1127 0.050 Uiso 1 1 calc R . .
H26B H 0.9077 0.5143 0.0838 0.050 Uiso 1 1 calc R . .
C27 C 0.8806(3) 0.3722(2) 0.05851(17) 0.0472(8) Uani 1 1 d . . .
H27A H 0.9284 0.3827 -0.0021 0.057 Uiso 1 1 calc R . .
H27B H 0.7992 0.3891 0.0598 0.057 Uiso 1 1 calc R . .
C28 C 0.8956(2) 0.2594(2) 0.08714(17) 0.0443(8) Uani 1 1 d . . .
C29 C 0.7178(2) 0.17909(19) 0.14305(16) 0.0290(6) Uani 1 1 d . . .
C30 C 0.7257(2) 0.1535(2) 0.05320(16) 0.0345(7) Uani 1 1 d . . .
C31 C 0.7016(3) 0.2270(2) -0.00686(17) 0.0453(8) Uani 1 1 d . . .
H31 H 0.6852 0.2953 0.0073 0.054 Uiso 1 1 calc R . .
C32 C 0.7014(3) 0.2011(3) -0.08692(19) 0.0591(9) Uani 1 1 d . . .
H32 H 0.6841 0.2517 -0.1273 0.071 Uiso 1 1 calc R . .
C33 C 0.7263(3) 0.1025(3) -0.1085(2) 0.0688(11) Uani 1 1 d . . .
H33 H 0.7257 0.0848 -0.1635 0.083 Uiso 1 1 calc R . .
C34 C 0.7523(3) 0.0291(3) -0.0495(2) 0.0680(11) Uani 1 1 d . . .
H34 H 0.7708 -0.0390 -0.0641 0.082 Uiso 1 1 calc R . .
C35 C 0.7513(3) 0.0556(2) 0.03061(18) 0.0491(8) Uani 1 1 d . . .
H35 H 0.7687 0.0050 0.0709 0.059 Uiso 1 1 calc R . .
C36 C 0.4428(3) 0.1424(3) 0.1239(2) 0.0677(11) Uani 1 1 d . . .
H36A H 0.4339 0.2162 0.1208 0.102 Uiso 1 1 calc R . .
H36B H 0.3671 0.1163 0.1364 0.102 Uiso 1 1 calc R . .
H36C H 0.4927 0.1194 0.0686 0.102 Uiso 1 1 calc R . .
C37 C 0.5311(3) -0.0444(3) 0.2092(3) 0.0803(12) Uani 1 1 d . . .
H37A H 0.5813 -0.0628 0.1525 0.121 Uiso 1 1 calc R . .
H37B H 0.4566 -0.0724 0.2204 0.121 Uiso 1 1 calc R . .
H37C H 0.5672 -0.0717 0.2537 0.121 Uiso 1 1 calc R . .
C38 C 0.4024(3) 0.1285(3) 0.3142(2) 0.0739(12) Uani 1 1 d . . .
H38A H 0.4360 0.1091 0.3616 0.111 Uiso 1 1 calc R . .
H38B H 0.3334 0.0926 0.3234 0.111 Uiso 1 1 calc R . .
H38C H 0.3814 0.2013 0.3124 0.111 Uiso 1 1 calc R . .
C39 C 0.6706(4) 0.6298(3) 0.0839(2) 0.0749(12) Uani 1 1 d . . .
H39A H 0.6013 0.6398 0.0636 0.090 Uiso 1 1 calc R . .
H39B H 0.7154 0.5675 0.0603 0.090 Uiso 1 1 calc R . .
C40 C 0.5318(3) 0.6788(2) 0.2131(2) 0.0595(9) Uani 1 1 d . . .
H40A H 0.4641 0.6485 0.2076 0.071 Uiso 1 1 calc R . .
H40B H 0.5350 0.7469 0.1832 0.071 Uiso 1 1 calc R . .
C41 C 0.7415(4) 0.7164(3) 0.0500(3) 0.1085(17) Uani 1 1 d . . .
H41A H 0.6918 0.7794 0.0588 0.163 Uiso 1 1 calc R . .
H41B H 0.7800 0.7112 -0.0116 0.163 Uiso 1 1 calc R . .
H41C H 0.7994 0.7159 0.0807 0.163 Uiso 1 1 calc R . .
C42 C 0.5222(3) 0.6853(3) 0.3061(2) 0.0735(11) Uani 1 1 d . . .
H42A H 0.5171 0.6177 0.3354 0.110 Uiso 1 1 calc R . .
H42B H 0.4529 0.7283 0.3331 0.110 Uiso 1 1 calc R . .
H42C H 0.5903 0.7143 0.3108 0.110 Uiso 1 1 calc R . .
C43 C 0.9324(9) -0.0382(10) 0.2177(13) 0.201(10) Uani 0.50 1 d P . .
C44 C 0.8335(9) -0.0982(8) 0.2288(6) 0.094(3) Uani 0.50 1 d P . .
C45 C 0.8041(8) -0.0700(4) 0.3674(4) 0.194(4) Uani 1 1 d . . .
H45A H 0.8476 -0.0393 0.3994 0.233 Uiso 1 1 calc R . .
H45B H 0.8384 -0.1399 0.3575 0.233 Uiso 1 1 calc R . .
C46 C 0.9367(6) -0.0996(7) 0.1695(4) 0.185(4) Uani 1 1 d . . .
H46 H 0.9840 -0.1308 0.1196 0.222 Uiso 1 1 calc R . .
C47 C 0.6900(7) -0.0738(7) 0.4194(4) 0.273(7) Uani 1 1 d . . .
H47A H 0.6586 -0.0063 0.4376 0.409 Uiso 1 1 calc R . .
H47B H 0.6877 -0.1199 0.4702 0.409 Uiso 1 1 calc R . .
H47C H 0.6438 -0.0979 0.3866 0.409 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Li1 O1 1.965(5) . ?
Li1 N4 2.044(5) . ?
Li1 N1 2.081(5) . ?
Li2 N1 1.954(5) . ?
Li2 N6 1.997(5) . ?
Li2 N2 2.052(5) . ?
Li2 N5 2.580(5) . ?
Li3 O2 1.960(6) . ?
Li3 N5 2.224(5) . ?
Li3 N3 2.267(5) . ?
Li3 N2 2.289(6) . ?
Li3 N6 2.290(5) . ?
Li4 N4 1.954(5) . ?
Li4 N3 2.014(5) . ?
Li4 N5 2.048(5) . ?
Li4 N2 2.483(5) . ?
Si1 N6 1.723(2) . ?
Si1 C38 1.851(3) . ?
Si1 C36 1.861(3) . ?
Si1 C37 1.863(4) . ?
Si2 N3 1.730(2) . ?
Si2 C19 1.811(4) . ?
Si2 C18 1.843(3) . ?
Si2 C17 1.852(5) . ?
O1 C39 1.419(3) . ?
O1 C40 1.439(4) . ?
O2 C45 1.362(5) . ?
O2 C44 1.490(10) . ?
O2 C43 1.541(14) . ?
N1 C6 1.376(3) . ?
N1 C7 1.489(3) . ?
N2 C10 1.328(3) . ?
N2 C9 1.479(3) . ?
N3 C10 1.322(3) . ?
N4 C25 1.383(3) . ?
N4 C26 1.459(3) . ?
N5 C29 1.330(3) . ?
N5 C28 1.475(3) . ?
N6 C29 1.329(3) . ?
C1 C2 1.386(4) . ?
C1 C6 1.415(3) . ?
C2 C3 1.387(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.373(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.376(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.424(4) . ?
C5 H5 0.9500 . ?
C8 C9 1.552(4) . ?
C10 C11 1.503(3) . ?
C11 C12 1.369(4) . ?
C11 C16 1.387(4) . ?
C12 C13 1.401(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.385(4) . ?
C14 C15 1.371(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.384(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.373(4) . ?
C20 C25 1.414(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.371(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.405(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.391(4) . ?
C24 C25 1.428(4) . ?
C26 C27 1.518(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.545(4) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C29 C30 1.509(3) . ?
C30 C35 1.373(4) . ?
C30 C31 1.393(4) . ?
C31 C32 1.383(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.378(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.388(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.382(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C41 1.485(5) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C42 1.496(4) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C46 1.177(12) . ?
C43 C44 1.478(15) . ?
C44 C46 1.338(10) . ?
C45 C47 1.400(9) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46 0.9500 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Li1 N4 109.1(2) . . ?
O1 Li1 N1 121.5(3) . . ?
N4 Li1 N1 129.0(3) . . ?
N1 Li2 N6 143.4(3) . . ?
N1 Li2 N2 103.7(2) . . ?
N6 Li2 N2 112.4(2) . . ?
N1 Li2 N5 124.8(2) . . ?
N6 Li2 N5 57.99(14) . . ?
N2 Li2 N5 96.35(19) . . ?
O2 Li3 N5 129.1(3) . . ?
O2 Li3 N3 108.2(2) . . ?
N5 Li3 N3 95.2(2) . . ?
O2 Li3 N2 130.3(3) . . ?
N5 Li3 N2 100.5(2) . . ?
N3 Li3 N2 59.79(15) . . ?
O2 Li3 N6 109.4(2) . . ?
N5 Li3 N6 60.55(14) . . ?
N3 Li3 N6 142.4(3) . . ?
N2 Li3 N6 94.6(2) . . ?
N4 Li4 N3 142.3(3) . . ?
N4 Li4 N5 103.9(2) . . ?
N3 Li4 N5 109.5(2) . . ?
N4 Li4 N2 131.1(3) . . ?
N3 Li4 N2 59.59(14) . . ?
N5 Li4 N2 99.53(19) . . ?
N6 Si1 C38 104.79(13) . . ?
N6 Si1 C36 116.13(12) . . ?
C38 Si1 C36 106.95(17) . . ?
N6 Si1 C37 112.51(14) . . ?
C38 Si1 C37 108.81(18) . . ?
C36 Si1 C37 107.32(17) . . ?
N3 Si2 C19 105.94(17) . . ?
N3 Si2 C18 115.57(14) . . ?
C19 Si2 C18 111.0(3) . . ?
N3 Si2 C17 111.82(17) . . ?
C19 Si2 C17 108.4(3) . . ?
C18 Si2 C17 104.1(2) . . ?
C39 O1 C40 112.1(3) . . ?
C39 O1 Li1 120.0(2) . . ?
C40 O1 Li1 118.8(2) . . ?
C45 O2 C44 103.5(5) . . ?
C45 O2 C43 118.6(8) . . ?
C44 O2 C43 58.3(5) . . ?
C45 O2 Li3 122.5(3) . . ?
C44 O2 Li3 130.4(4) . . ?
C43 O2 Li3 107.1(7) . . ?
C6 N1 C7 112.7(2) . . ?
C6 N1 Li2 109.7(2) . . ?
C7 N1 Li2 111.4(2) . . ?
C6 N1 Li1 95.80(19) . . ?
C7 N1 Li1 127.3(2) . . ?
Li2 N1 Li1 97.9(2) . . ?
C10 N2 C9 118.7(2) . . ?
C10 N2 Li2 144.2(2) . . ?
C9 N2 Li2 95.8(2) . . ?
C10 N2 Li3 84.8(2) . . ?
C9 N2 Li3 140.9(2) . . ?
Li2 N2 Li3 72.51(19) . . ?
C10 N2 Li4 75.16(18) . . ?
C9 N2 Li4 147.6(2) . . ?
Li2 N2 Li4 70.17(18) . . ?
Li3 N2 Li4 64.25(17) . . ?
C10 N3 Si2 129.98(18) . . ?
C10 N3 Li4 94.7(2) . . ?
Si2 N3 Li4 119.49(18) . . ?
C10 N3 Li3 85.8(2) . . ?
Si2 N3 Li3 136.42(19) . . ?
Li4 N3 Li3 72.59(19) . . ?
C25 N4 C26 114.0(2) . . ?
C25 N4 Li4 113.8(2) . . ?
C26 N4 Li4 110.4(2) . . ?
C25 N4 Li1 97.5(2) . . ?
C26 N4 Li1 124.1(2) . . ?
Li4 N4 Li1 95.7(2) . . ?
C29 N5 C28 118.7(2) . . ?
C29 N5 Li4 142.1(2) . . ?
C28 N5 Li4 98.2(2) . . ?
C29 N5 Li3 85.3(2) . . ?
C28 N5 Li3 135.8(2) . . ?
Li4 N5 Li3 72.91(19) . . ?
C29 N5 Li2 74.53(18) . . ?
C28 N5 Li2 153.1(2) . . ?
Li4 N5 Li2 68.13(18) . . ?
Li3 N5 Li2 64.29(19) . . ?
C29 N6 Si1 129.95(18) . . ?
C29 N6 Li2 99.1(2) . . ?
Si1 N6 Li2 116.44(19) . . ?
C29 N6 Li3 82.69(19) . . ?
Si1 N6 Li3 138.78(17) . . ?
Li2 N6 Li3 73.4(2) . . ?
C2 C1 C6 120.8(3) . . ?
C1 C2 C3 121.6(3) . . ?
C1 C2 H2 119.2 . . ?
C3 C2 H2 119.2 . . ?
C4 C3 C2 118.2(3) . . ?
C4 C3 H3 120.9 . . ?
C2 C3 H3 120.9 . . ?
C3 C4 C5 121.9(3) . . ?
C3 C4 H4 119.1 . . ?
C5 C4 H4 119.1 . . ?
C4 C5 C6 121.2(3) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
N1 C6 C1 117.7(2) . . ?
N1 C6 C5 126.1(2) . . ?
C1 C6 C5 116.2(2) . . ?
N2 C9 C8 113.1(2) . . ?
N3 C10 N2 118.0(2) . . ?
N3 C10 C11 120.3(2) . . ?
N2 C10 C11 121.7(2) . . ?
C12 C11 C16 118.2(2) . . ?
C12 C11 C10 120.4(2) . . ?
C16 C11 C10 121.2(2) . . ?
C11 C12 C13 121.7(3) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 H12 119.2 . . ?
C14 C13 C12 118.4(3) . . ?
C15 C14 C13 120.9(3) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C16 119.4(3) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C15 C16 C11 121.4(3) . . ?
C15 C16 H16 119.3 . . ?
C11 C16 H16 119.3 . . ?
Si2 C17 H17A 109.5 . . ?
Si2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si2 C18 H18A 109.5 . . ?
Si2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si2 C19 H19A 109.5 . . ?
Si2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C25 121.2(3) . . ?
C21 C20 H20 119.4 . . ?
C25 C20 H20 119.4 . . ?
C22 C21 C20 121.7(3) . . ?
C22 C21 H21 119.2 . . ?
C20 C21 H21 119.2 . . ?
C21 C22 C23 120.0(3) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C22 118.7(3) . . ?
C23 C24 C25 122.2(3) . . ?
N4 C25 C20 126.2(2) . . ?
N4 C25 C24 117.6(2) . . ?
C20 C25 C24 116.3(2) . . ?
N4 C26 C27 113.0(2) . . ?
N4 C26 H26A 109.0 . . ?
C27 C26 H26A 109.0 . . ?
N4 C26 H26B 109.0 . . ?
C27 C26 H26B 109.0 . . ?
H26A C26 H26B 107.8 . . ?
C26 C27 C28 116.0(2) . . ?
C26 C27 H27A 108.3 . . ?
C28 C27 H27A 108.3 . . ?
C26 C27 H27B 108.3 . . ?
C28 C27 H27B 108.3 . . ?
H27A C27 H27B 107.4 . . ?
N5 C28 C27 111.4(2) . . ?
N6 C29 N5 117.8(2) . . ?
N6 C29 C30 119.9(2) . . ?
N5 C29 C30 122.3(2) . . ?
C35 C30 C31 118.6(3) . . ?
C35 C30 C29 120.2(3) . . ?
C31 C30 C29 121.1(3) . . ?
C32 C31 C30 120.4(3) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C33 C32 C31 120.4(3) . . ?
C33 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C32 C33 C34 119.5(3) . . ?
C32 C33 H33 120.3 . . ?
C34 C33 H33 120.3 . . ?
C35 C34 C33 119.7(3) . . ?
C35 C34 H34 120.2 . . ?
C33 C34 H34 120.2 . . ?
C30 C35 C34 121.4(3) . . ?
C30 C35 H35 119.3 . . ?
C34 C35 H35 119.3 . . ?
Si1 C36 H36A 109.5 . . ?
Si1 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
Si1 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
Si1 C37 H37A 109.5 . . ?
Si1 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
Si1 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
Si1 C38 H38A 109.5 . . ?
Si1 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
Si1 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O1 C39 C41 113.1(3) . . ?
O1 C39 H39A 109.0 . . ?
C41 C39 H39A 109.0 . . ?
O1 C39 H39B 109.0 . . ?
C41 C39 H39B 109.0 . . ?
H39A C39 H39B 107.8 . . ?
O1 C40 C42 107.9(3) . . ?
O1 C40 H40A 110.1 . . ?
C42 C40 H40A 110.1 . . ?
O1 C40 H40B 110.1 . . ?
C42 C40 H40B 110.1 . . ?
H40A C40 H40B 108.4 . . ?
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 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C46 C43 C44 59.2(7) . . ?
C46 C43 O2 118.3(11) . . ?
C44 C43 O2 59.1(7) . . ?
C46 C44 C43 49.1(6) . . ?
C46 C44 O2 111.5(9) . . ?
C43 C44 O2 62.5(7) . . ?
O2 C45 C47 115.7(7) . . ?
O2 C45 H45A 108.4 . . ?
C47 C45 H45A 108.4 . . ?
O2 C45 H45B 108.3 . . ?
C47 C45 H45B 108.4 . . ?
H45A C45 H45B 107.4 . . ?
C43 C46 C44 71.7(8) . . ?
C43 C46 H46 144.2 . . ?
C44 C46 H46 144.2 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        28.25
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.068
