# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_riv1050
_database_code_depnum_ccdc_archive 'CCDC 1043226'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H64 Cl3 Li N2 O2 Si Zr'
_chemical_formula_sum            'C38 H64 Cl3 Li N2 O2 Si Zr'
_chemical_formula_weight         813.51

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   10.2481(4)
_cell_length_b                   27.2915(11)
_cell_length_c                   15.7628(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.8171(4)
_cell_angle_gamma                90.00
_cell_volume                     4315.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9816
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      27.49

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1720
_exptl_absorpt_coefficient_mu    0.500
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8315
_exptl_absorpt_correction_T_max  0.8640
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38542
_diffrn_reflns_av_R_equivalents  0.0157
_diffrn_reflns_av_sigmaI/netI    0.0126
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.49
_diffrn_reflns_theta_max         27.58
_reflns_number_total             9969
_reflns_number_gt                9002
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0383P)²+3.4942P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9969
_refine_ls_number_parameters     442
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.0989
_refine_ls_wR_factor_gt          0.0961
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_restrained_S_all      1.122
_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
Zr Zr 0.238706(19) 0.131814(7) 0.186323(12) 0.03101(6) Uani 1 1 d . . .
Cl1 Cl 0.08902(8) 0.17394(3) 0.06298(4) 0.06142(19) Uani 1 1 d . . .
Cl2 Cl 0.12628(7) 0.05433(2) 0.12195(4) 0.04917(14) Uani 1 1 d . . .
Cl3 Cl 0.45092(6) 0.12808(3) 0.14580(4) 0.05213(15) Uani 1 1 d . . .
Si Si 0.30673(5) 0.15899(2) 0.36290(3) 0.02832(11) Uani 1 1 d . . .
O1 O 0.11141(19) 0.08567(10) -0.09845(12) 0.0760(7) Uani 1 1 d . . .
O2 O -0.16048(19) 0.09124(9) -0.02987(15) 0.0748(6) Uani 1 1 d D . .
N1 N 0.24471(16) 0.19159(6) 0.26600(10) 0.0296(3) Uani 1 1 d . . .
N2 N 0.26758(16) 0.10265(6) 0.30857(10) 0.0298(3) Uani 1 1 d . . .
C1 C 0.2237(2) 0.17238(9) 0.45666(13) 0.0398(5) Uani 1 1 d . . .
H1 H 0.1254 0.1686 0.4350 0.048 Uiso 1 1 calc R . .
C2 C 0.2485(3) 0.22550(11) 0.48821(19) 0.0604(7) Uani 1 1 d . . .
H2A H 0.1878 0.2338 0.5267 0.072 Uiso 1 1 calc R . .
H2B H 0.2326 0.2477 0.4383 0.072 Uiso 1 1 calc R . .
H2C H 0.3409 0.2289 0.5198 0.072 Uiso 1 1 calc R . .
C3 C 0.2652(3) 0.13638(13) 0.53270(17) 0.0629(8) Uani 1 1 d . . .
H3A H 0.2077 0.1411 0.5747 0.075 Uiso 1 1 calc R . .
H3B H 0.3581 0.1425 0.5610 0.075 Uiso 1 1 calc R . .
H3C H 0.2561 0.1027 0.5108 0.075 Uiso 1 1 calc R . .
C4 C 0.4934(2) 0.16580(9) 0.39514(14) 0.0401(5) Uani 1 1 d . . .
H4 H 0.5278 0.1584 0.3416 0.048 Uiso 1 1 calc R . .
C5 C 0.5417(3) 0.21794(12) 0.4216(2) 0.0637(8) Uani 1 1 d . . .
H5A H 0.6346 0.2216 0.4157 0.076 Uiso 1 1 calc R . .
H5B H 0.5355 0.2238 0.4819 0.076 Uiso 1 1 calc R . .
H5C H 0.4859 0.2417 0.3839 0.076 Uiso 1 1 calc R . .
C6 C 0.5624(3) 0.12900(12) 0.46316(18) 0.0604(8) Uani 1 1 d . . .
H6A H 0.6569 0.1266 0.4606 0.073 Uiso 1 1 calc R . .
H6B H 0.5202 0.0968 0.4514 0.073 Uiso 1 1 calc R . .
H6C H 0.5541 0.1401 0.5210 0.073 Uiso 1 1 calc R . .
C11 C 0.2023(2) 0.24136(7) 0.25059(12) 0.0333(4) Uani 1 1 d . . .
C12 C 0.2852(2) 0.27593(8) 0.22032(14) 0.0401(5) Uani 1 1 d . . .
C13 C 0.2385(3) 0.32371(9) 0.20415(17) 0.0511(6) Uani 1 1 d . . .
H13 H 0.2944 0.3472 0.1849 0.061 Uiso 1 1 calc R . .
C14 C 0.1146(3) 0.33793(9) 0.21512(18) 0.0570(7) Uani 1 1 d . . .
H14 H 0.0857 0.3708 0.2042 0.068 Uiso 1 1 calc R . .
C15 C 0.0329(3) 0.30405(10) 0.24208(17) 0.0529(6) Uani 1 1 d . . .
H15 H -0.0535 0.3138 0.2487 0.063 Uiso 1 1 calc R . .
C16 C 0.0732(2) 0.25572(8) 0.25994(14) 0.0400(5) Uani 1 1 d . . .
C17 C 0.4179(3) 0.26187(10) 0.19922(18) 0.0504(6) Uani 1 1 d . . .
H17 H 0.4445 0.2293 0.2262 0.060 Uiso 1 1 calc R . .
C18 C 0.4044(4) 0.25690(12) 0.1010(2) 0.0708(9) Uani 1 1 d . . .
H18A H 0.3321 0.2340 0.0781 0.085 Uiso 1 1 calc R . .
H18B H 0.4882 0.2445 0.0884 0.085 Uiso 1 1 calc R . .
H18C H 0.3842 0.2890 0.0736 0.085 Uiso 1 1 calc R . .
C19 C 0.5292(3) 0.29875(12) 0.2345(3) 0.0764(10) Uani 1 1 d . . .
H19A H 0.6150 0.2856 0.2268 0.092 Uiso 1 1 calc R . .
H19B H 0.5323 0.3044 0.2963 0.092 Uiso 1 1 calc R . .
H19C H 0.5113 0.3298 0.2029 0.092 Uiso 1 1 calc R . .
C20 C -0.0272(2) 0.22046(10) 0.28428(17) 0.0490(6) Uani 1 1 d . . .
H20 H 0.0197 0.1887 0.3013 0.059 Uiso 1 1 calc R . .
C21 C -0.1413(3) 0.21028(13) 0.2065(2) 0.0694(8) Uani 1 1 d . . .
H21A H -0.1050 0.1958 0.1594 0.083 Uiso 1 1 calc R . .
H21B H -0.1867 0.2411 0.1867 0.083 Uiso 1 1 calc R . .
H21C H -0.2049 0.1875 0.2239 0.083 Uiso 1 1 calc R . .
C22 C -0.0845(3) 0.23822(13) 0.3613(2) 0.0710(9) Uani 1 1 d . . .
H22A H -0.0114 0.2466 0.4096 0.085 Uiso 1 1 calc R . .
H22B H -0.1390 0.2122 0.3793 0.085 Uiso 1 1 calc R . .
H22C H -0.1399 0.2673 0.3442 0.085 Uiso 1 1 calc R . .
C31 C 0.2418(2) 0.05491(7) 0.33906(12) 0.0318(4) Uani 1 1 d . . .
C32 C 0.3377(2) 0.01712(8) 0.34409(13) 0.0353(4) Uani 1 1 d . . .
C33 C 0.3058(3) -0.02947(8) 0.37012(15) 0.0434(5) Uani 1 1 d . . .
H33 H 0.3699 -0.0550 0.3737 0.052 Uiso 1 1 calc R . .
C34 C 0.1850(3) -0.03966(9) 0.39069(16) 0.0475(6) Uani 1 1 d . . .
H34 H 0.1663 -0.0716 0.4087 0.057 Uiso 1 1 calc R . .
C35 C 0.0907(3) -0.00282(9) 0.38489(16) 0.0459(5) Uani 1 1 d . . .
H35 H 0.0070 -0.0099 0.3991 0.055 Uiso 1 1 calc R . .
C36 C 0.1160(2) 0.04433(8) 0.35866(14) 0.0383(4) Uani 1 1 d . . .
C37 C 0.4706(2) 0.02463(8) 0.31815(14) 0.0398(5) Uani 1 1 d . . .
H37 H 0.4863 0.0607 0.3149 0.048 Uiso 1 1 calc R . .
C38 C 0.5883(3) 0.00232(11) 0.38359(18) 0.0532(6) Uani 1 1 d . . .
H38A H 0.5860 0.0141 0.4420 0.064 Uiso 1 1 calc R . .
H38B H 0.6724 0.0122 0.3683 0.064 Uiso 1 1 calc R . .
H38C H 0.5812 -0.0335 0.3820 0.064 Uiso 1 1 calc R . .
C39 C 0.4682(3) 0.00259(10) 0.22839(16) 0.0528(6) Uani 1 1 d . . .
H39A H 0.3960 0.0176 0.1859 0.063 Uiso 1 1 calc R . .
H39B H 0.4534 -0.0328 0.2302 0.063 Uiso 1 1 calc R . .
H39C H 0.5536 0.0089 0.2116 0.063 Uiso 1 1 calc R . .
C40 C 0.0043(2) 0.08207(9) 0.34859(18) 0.0470(5) Uani 1 1 d . . .
H40 H 0.0431 0.1145 0.3378 0.056 Uiso 1 1 calc R . .
C41 C -0.1077(3) 0.07071(12) 0.2704(2) 0.0628(7) Uani 1 1 d . . .
H41A H -0.1760 0.0963 0.2646 0.075 Uiso 1 1 calc R . .
H41B H -0.1475 0.0389 0.2789 0.075 Uiso 1 1 calc R . .
H41C H -0.0709 0.0697 0.2177 0.075 Uiso 1 1 calc R . .
C42 C -0.0547(3) 0.08719(11) 0.4297(2) 0.0628(7) Uani 1 1 d . . .
H42A H -0.1156 0.1152 0.4230 0.075 Uiso 1 1 calc R . .
H42B H 0.0174 0.0923 0.4803 0.075 Uiso 1 1 calc R . .
H42C H -0.1036 0.0573 0.4378 0.075 Uiso 1 1 calc R . .
C51 C 0.0559(3) 0.06796(11) -0.18293(17) 0.0558(6) Uani 1 1 d . B .
H51A H -0.0221 0.0880 -0.2101 0.067 Uiso 1 1 calc R . .
H51B H 0.0268 0.0335 -0.1803 0.067 Uiso 1 1 calc R . .
C52 C 0.1642(4) 0.07175(14) -0.2341(2) 0.0761(9) Uani 1 1 d . . .
H52A H 0.1988 0.0389 -0.2442 0.091 Uiso 1 1 calc R B .
H52B H 0.1302 0.0876 -0.2908 0.091 Uiso 1 1 calc R . .
C53 C 0.2692(3) 0.10172(13) -0.1809(2) 0.0697(8) Uani 1 1 d . B .
H53A H 0.3563 0.0851 -0.1763 0.084 Uiso 1 1 calc R A 1
H53B H 0.2740 0.1338 -0.2095 0.084 Uiso 1 1 calc R A 1
C54A C 0.2437(7) 0.1095(3) -0.0953(4) 0.0634(15) Uiso 0.50 1 d P B 1
H54A H 0.2400 0.1449 -0.0824 0.076 Uiso 0.50 1 calc PR B 1
H54B H 0.3137 0.0940 -0.0507 0.076 Uiso 0.50 1 calc PR B 1
C54B C 0.2551(6) 0.0836(2) -0.0906(4) 0.0537(12) Uiso 0.50 1 d P B 2
H54C H 0.2894 0.0498 -0.0794 0.064 Uiso 0.50 1 calc PR B 2
H54D H 0.3018 0.1056 -0.0441 0.064 Uiso 0.50 1 calc PR B 2
C55 C -0.2350(4) 0.05202(14) -0.0007(3) 0.0990(14) Uani 1 1 d D B .
H55A H -0.1947 0.0430 0.0599 0.119 Uiso 1 1 calc R . .
H55B H -0.2353 0.0227 -0.0377 0.119 Uiso 1 1 calc R . .
C56 C -0.3710(4) 0.07006(17) -0.0064(3) 0.0967(13) Uani 1 1 d D . .
H56A H -0.3892 0.0740 0.0525 0.116 Uiso 1 1 calc R B 1
H56B H -0.4355 0.0461 -0.0382 0.116 Uiso 1 1 calc R B 1
C57A C -0.3869(8) 0.1176(2) -0.0521(5) 0.073(2) Uiso 0.50 1 d PD B 1
H57A H -0.4428 0.1403 -0.0259 0.088 Uiso 0.50 1 calc PR B 1
H57B H -0.4273 0.1133 -0.1143 0.088 Uiso 0.50 1 calc PR B 1
C58A C -0.2416(6) 0.1367(2) -0.0398(5) 0.0673(16) Uiso 0.50 1 d PD B 1
H58A H -0.2287 0.1558 -0.0909 0.081 Uiso 0.50 1 calc PR B 1
H58B H -0.2183 0.1576 0.0125 0.081 Uiso 0.50 1 calc PR B 1
C57B C -0.3570(10) 0.1249(2) -0.0191(6) 0.085(2) Uiso 0.50 1 d PD B 2
H57C H -0.3211 0.1418 0.0362 0.102 Uiso 0.50 1 calc PR B 2
H57D H -0.4426 0.1401 -0.0474 0.102 Uiso 0.50 1 calc PR B 2
C58B C -0.2541(9) 0.1240(3) -0.0804(6) 0.107(3) Uiso 0.50 1 d PD B 2
H58C H -0.2930 0.1105 -0.1384 0.129 Uiso 0.50 1 calc PR B 2
H58D H -0.2152 0.1567 -0.0864 0.129 Uiso 0.50 1 calc PR B 2
Li Li 0.0243(4) 0.0968(2) -0.0058(3) 0.0564(11) Uani 1 1 d . B .


_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
Zr N2 2.0495(16) . ?
Zr N1 2.0521(16) . ?
Zr Cl3 2.3910(6) . ?
Zr Cl1 2.4966(6) . ?
Zr Cl2 2.5199(6) . ?
Zr Si 2.8263(5) . ?
Zr Li 3.491(4) . ?
Cl1 Li 2.399(5) . ?
Cl2 Li 2.372(5) . ?
Si N2 1.7658(17) . ?
Si N1 1.7694(17) . ?
Si C4 1.885(2) . ?
Si C1 1.886(2) . ?
O1 C51 1.421(3) . ?
O1 C54B 1.454(6) . ?
O1 C54A 1.495(7) . ?
O1 Li 1.886(5) . ?
O2 C58B 1.429(5) . ?
O2 C55 1.444(4) . ?
O2 C58A 1.485(5) . ?
O2 Li 1.860(5) . ?
N1 C11 1.432(3) . ?
N2 C31 1.432(3) . ?
C1 C2 1.537(4) . ?
C1 C3 1.541(3) . ?
C4 C6 1.532(4) . ?
C4 C5 1.536(4) . ?
C11 C16 1.416(3) . ?
C11 C12 1.416(3) . ?
C12 C13 1.394(3) . ?
C12 C17 1.513(3) . ?
C13 C14 1.373(4) . ?
C14 C15 1.372(4) . ?
C15 C16 1.394(3) . ?
C16 C20 1.515(3) . ?
C17 C18 1.532(4) . ?
C17 C19 1.538(4) . ?
C20 C22 1.532(4) . ?
C20 C21 1.536(4) . ?
C31 C32 1.415(3) . ?
C31 C36 1.416(3) . ?
C32 C33 1.395(3) . ?
C32 C37 1.514(3) . ?
C33 C34 1.370(4) . ?
C34 C35 1.385(4) . ?
C35 C36 1.392(3) . ?
C36 C40 1.524(3) . ?
C37 C39 1.533(3) . ?
C37 C38 1.543(3) . ?
C40 C42 1.529(4) . ?
C40 C41 1.534(4) . ?
C51 C52 1.503(4) . ?
C52 C53 1.469(4) . ?
C53 C54A 1.441(7) . ?
C53 C54B 1.541(7) . ?
C55 C56 1.463(5) . ?
C56 C57A 1.476(7) . ?
C56 C57B 1.519(7) . ?
C57A C58A 1.552(10) . ?
C57B C58B 1.570(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Zr N1 75.69(6) . . ?
N2 Zr Cl3 105.70(5) . . ?
N1 Zr Cl3 106.41(5) . . ?
N2 Zr Cl1 149.13(5) . . ?
N1 Zr Cl1 92.70(5) . . ?
Cl3 Zr Cl1 105.01(3) . . ?
N2 Zr Cl2 91.08(5) . . ?
N1 Zr Cl2 150.17(5) . . ?
Cl3 Zr Cl2 102.86(2) . . ?
Cl1 Zr Cl2 85.15(2) . . ?
N2 Zr Si 38.47(5) . . ?
N1 Zr Si 38.58(5) . . ?
Cl3 Zr Si 102.70(2) . . ?
Cl1 Zr Si 129.37(2) . . ?
Cl2 Zr Si 128.098(19) . . ?
N2 Zr Li 130.78(10) . . ?
N1 Zr Li 133.10(10) . . ?
Cl3 Zr Li 101.65(7) . . ?
Cl1 Zr Li 43.40(9) . . ?
Cl2 Zr Li 42.79(9) . . ?
Si Zr Li 155.59(7) . . ?
Li Cl1 Zr 90.95(11) . . ?
Li Cl2 Zr 91.01(13) . . ?
N2 Si N1 90.77(8) . . ?
N2 Si C4 109.50(9) . . ?
N1 Si C4 110.39(9) . . ?
N2 Si C1 117.03(9) . . ?
N1 Si C1 116.04(9) . . ?
C4 Si C1 111.44(10) . . ?
N2 Si Zr 46.22(5) . . ?
N1 Si Zr 46.32(5) . . ?
C4 Si Zr 108.87(7) . . ?
C1 Si Zr 139.69(7) . . ?
C51 O1 C54B 105.7(3) . . ?
C51 O1 C54A 111.4(3) . . ?
C51 O1 Li 128.2(2) . . ?
C54B O1 Li 124.9(3) . . ?
C54A O1 Li 118.3(3) . . ?
C58B O2 C55 107.6(5) . . ?
C55 O2 C58A 109.4(3) . . ?
C58B O2 Li 127.0(5) . . ?
C55 O2 Li 125.3(3) . . ?
C58A O2 Li 118.6(4) . . ?
C11 N1 Si 131.80(13) . . ?
C11 N1 Zr 132.87(13) . . ?
Si N1 Zr 95.11(7) . . ?
C31 N2 Si 131.98(13) . . ?
C31 N2 Zr 131.91(13) . . ?
Si N2 Zr 95.31(8) . . ?
C2 C1 C3 110.4(2) . . ?
C2 C1 Si 111.40(17) . . ?
C3 C1 Si 112.89(17) . . ?
C6 C4 C5 109.9(2) . . ?
C6 C4 Si 114.92(18) . . ?
C5 C4 Si 114.68(17) . . ?
C16 C11 C12 119.24(19) . . ?
C16 C11 N1 120.16(18) . . ?
C12 C11 N1 120.47(19) . . ?
C13 C12 C11 118.5(2) . . ?
C13 C12 C17 119.1(2) . . ?
C11 C12 C17 122.2(2) . . ?
C14 C13 C12 122.2(2) . . ?
C15 C14 C13 119.2(2) . . ?
C14 C15 C16 121.7(2) . . ?
C15 C16 C11 119.1(2) . . ?
C15 C16 C20 117.6(2) . . ?
C11 C16 C20 123.3(2) . . ?
C12 C17 C18 110.2(2) . . ?
C12 C17 C19 112.8(2) . . ?
C18 C17 C19 109.3(2) . . ?
C16 C20 C22 113.0(2) . . ?
C16 C20 C21 111.0(2) . . ?
C22 C20 C21 109.7(2) . . ?
C32 C31 C36 119.46(19) . . ?
C32 C31 N2 120.56(18) . . ?
C36 C31 N2 119.83(18) . . ?
C33 C32 C31 118.6(2) . . ?
C33 C32 C37 118.7(2) . . ?
C31 C32 C37 122.58(19) . . ?
C34 C33 C32 122.1(2) . . ?
C33 C34 C35 119.3(2) . . ?
C34 C35 C36 121.4(2) . . ?
C35 C36 C31 119.1(2) . . ?
C35 C36 C40 118.3(2) . . ?
C31 C36 C40 122.53(19) . . ?
C32 C37 C39 110.5(2) . . ?
C32 C37 C38 112.9(2) . . ?
C39 C37 C38 108.96(19) . . ?
C36 C40 C42 113.1(2) . . ?
C36 C40 C41 111.7(2) . . ?
C42 C40 C41 109.4(2) . . ?
O1 C51 C52 106.3(2) . . ?
C53 C52 C51 105.5(2) . . ?
C54A C53 C52 111.4(4) . . ?
C52 C53 C54B 98.8(3) . . ?
C53 C54A O1 104.0(4) . . ?
O1 C54B C53 101.2(4) . . ?
O2 C55 C56 106.8(3) . . ?
C55 C56 C57A 109.5(4) . . ?
C55 C56 C57B 103.0(5) . . ?
C56 C57A C58A 103.2(5) . . ?
O2 C58A C57A 103.5(4) . . ?
C56 C57B C58B 99.2(6) . . ?
O2 C58B C57B 97.2(6) . . ?
O2 Li O1 116.9(2) . . ?
O2 Li Cl2 112.8(2) . . ?
O1 Li Cl2 112.5(2) . . ?
O2 Li Cl1 109.8(2) . . ?
O1 Li Cl1 111.1(2) . . ?
Cl2 Li Cl1 90.70(15) . . ?
O2 Li Zr 129.3(2) . . ?
O1 Li Zr 113.71(18) . . ?
Cl2 Li Zr 46.20(8) . . ?
Cl1 Li Zr 45.65(8) . . ?

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
N2 Zr Cl1 Li -94.80(14) . . . . ?
N1 Zr Cl1 Li -161.02(12) . . . . ?
Cl3 Zr Cl1 Li 91.19(11) . . . . ?
Cl2 Zr Cl1 Li -10.84(11) . . . . ?
Si Zr Cl1 Li -147.85(11) . . . . ?
N2 Zr Cl2 Li 160.28(12) . . . . ?
N1 Zr Cl2 Li 97.94(14) . . . . ?
Cl3 Zr Cl2 Li -93.35(11) . . . . ?
Cl1 Zr Cl2 Li 10.97(11) . . . . ?
Si Zr Cl2 Li 148.91(11) . . . . ?
N1 Zr Si N2 160.19(10) . . . . ?
Cl3 Zr Si N2 -99.33(8) . . . . ?
Cl1 Zr Si N2 138.78(8) . . . . ?
Cl2 Zr Si N2 18.48(8) . . . . ?
Li Zr Si N2 76.6(2) . . . . ?
N2 Zr Si N1 -160.19(10) . . . . ?
Cl3 Zr Si N1 100.48(8) . . . . ?
Cl1 Zr Si N1 -21.42(8) . . . . ?
Cl2 Zr Si N1 -141.71(8) . . . . ?
Li Zr Si N1 -83.6(2) . . . . ?
N2 Zr Si C4 99.27(11) . . . . ?
N1 Zr Si C4 -100.53(11) . . . . ?
Cl3 Zr Si C4 -0.06(8) . . . . ?
Cl1 Zr Si C4 -121.95(8) . . . . ?
Cl2 Zr Si C4 117.76(8) . . . . ?
Li Zr Si C4 175.8(2) . . . . ?
N2 Zr Si C1 -81.00(14) . . . . ?
N1 Zr Si C1 79.19(14) . . . . ?
Cl3 Zr Si C1 179.67(12) . . . . ?
Cl1 Zr Si C1 57.77(13) . . . . ?
Cl2 Zr Si C1 -62.52(12) . . . . ?
Li Zr Si C1 -4.4(3) . . . . ?
N2 Si N1 C11 160.80(18) . . . . ?
C4 Si N1 C11 -88.02(19) . . . . ?
C1 Si N1 C11 40.0(2) . . . . ?
Zr Si N1 C11 175.0(2) . . . . ?
N2 Si N1 Zr -14.16(7) . . . . ?
C4 Si N1 Zr 97.01(9) . . . . ?
C1 Si N1 Zr -134.99(9) . . . . ?
N2 Zr N1 C11 -162.31(19) . . . . ?
Cl3 Zr N1 C11 95.21(17) . . . . ?
Cl1 Zr N1 C11 -11.30(18) . . . . ?
Cl2 Zr N1 C11 -96.26(19) . . . . ?
Si Zr N1 C11 -174.9(2) . . . . ?
Li Zr N1 C11 -29.1(2) . . . . ?
N2 Zr N1 Si 12.56(7) . . . . ?
Cl3 Zr N1 Si -89.91(6) . . . . ?
Cl1 Zr N1 Si 163.58(6) . . . . ?
Cl2 Zr N1 Si 78.62(11) . . . . ?
Li Zr N1 Si 145.76(11) . . . . ?
N1 Si N2 C31 -156.17(18) . . . . ?
C4 Si N2 C31 91.84(19) . . . . ?
C1 Si N2 C31 -36.2(2) . . . . ?
Zr Si N2 C31 -170.4(2) . . . . ?
N1 Si N2 Zr 14.19(7) . . . . ?
C4 Si N2 Zr -97.81(9) . . . . ?
C1 Si N2 Zr 134.17(9) . . . . ?
N1 Zr N2 C31 157.77(18) . . . . ?
Cl3 Zr N2 C31 -98.86(17) . . . . ?
Cl1 Zr N2 C31 87.15(19) . . . . ?
Cl2 Zr N2 C31 4.81(17) . . . . ?
Si Zr N2 C31 170.4(2) . . . . ?
Li Zr N2 C31 22.4(2) . . . . ?
N1 Zr N2 Si -12.59(7) . . . . ?
Cl3 Zr N2 Si 90.77(6) . . . . ?
Cl1 Zr N2 Si -83.22(11) . . . . ?
Cl2 Zr N2 Si -165.55(6) . . . . ?
Li Zr N2 Si -147.93(11) . . . . ?
N2 Si C1 C2 -170.80(17) . . . . ?
N1 Si C1 C2 -65.4(2) . . . . ?
C4 Si C1 C2 62.1(2) . . . . ?
Zr Si C1 C2 -117.61(17) . . . . ?
N2 Si C1 C3 64.3(2) . . . . ?
N1 Si C1 C3 169.75(17) . . . . ?
C4 Si C1 C3 -62.8(2) . . . . ?
Zr Si C1 C3 117.51(18) . . . . ?
N2 Si C4 C6 -66.15(19) . . . . ?
N1 Si C4 C6 -164.60(16) . . . . ?
C1 Si C4 C6 64.9(2) . . . . ?
Zr Si C4 C6 -115.26(16) . . . . ?
N2 Si C4 C5 165.04(18) . . . . ?
N1 Si C4 C5 66.6(2) . . . . ?
C1 Si C4 C5 -63.9(2) . . . . ?
Zr Si C4 C5 115.93(18) . . . . ?
Si N1 C11 C16 -80.4(2) . . . . ?
Zr N1 C11 C16 92.7(2) . . . . ?
Si N1 C11 C12 103.8(2) . . . . ?
Zr N1 C11 C12 -83.0(2) . . . . ?
C16 C11 C12 C13 2.6(3) . . . . ?
N1 C11 C12 C13 178.4(2) . . . . ?
C16 C11 C12 C17 -173.1(2) . . . . ?
N1 C11 C12 C17 2.8(3) . . . . ?
C11 C12 C13 C14 -1.2(4) . . . . ?
C17 C12 C13 C14 174.6(2) . . . . ?
C12 C13 C14 C15 -0.7(4) . . . . ?
C13 C14 C15 C16 1.0(4) . . . . ?
C14 C15 C16 C11 0.5(4) . . . . ?
C14 C15 C16 C20 -176.5(3) . . . . ?
C12 C11 C16 C15 -2.3(3) . . . . ?
N1 C11 C16 C15 -178.1(2) . . . . ?
C12 C11 C16 C20 174.5(2) . . . . ?
N1 C11 C16 C20 -1.3(3) . . . . ?
C13 C12 C17 C18 -73.9(3) . . . . ?
C11 C12 C17 C18 101.7(3) . . . . ?
C13 C12 C17 C19 48.5(3) . . . . ?
C11 C12 C17 C19 -135.8(3) . . . . ?
C15 C16 C20 C22 -55.1(3) . . . . ?
C11 C16 C20 C22 128.0(2) . . . . ?
C15 C16 C20 C21 68.6(3) . . . . ?
C11 C16 C20 C21 -108.3(3) . . . . ?
Si N2 C31 C32 -106.4(2) . . . . ?
Zr N2 C31 C32 86.5(2) . . . . ?
Si N2 C31 C36 78.0(2) . . . . ?
Zr N2 C31 C36 -89.1(2) . . . . ?
C36 C31 C32 C33 -1.3(3) . . . . ?
N2 C31 C32 C33 -176.89(18) . . . . ?
C36 C31 C32 C37 175.62(19) . . . . ?
N2 C31 C32 C37 0.0(3) . . . . ?
C31 C32 C33 C34 0.1(3) . . . . ?
C37 C32 C33 C34 -176.9(2) . . . . ?
C32 C33 C34 C35 0.6(4) . . . . ?
C33 C34 C35 C36 0.0(4) . . . . ?
C34 C35 C36 C31 -1.1(4) . . . . ?
C34 C35 C36 C40 176.3(2) . . . . ?
C32 C31 C36 C35 1.8(3) . . . . ?
N2 C31 C36 C35 177.43(19) . . . . ?
C32 C31 C36 C40 -175.6(2) . . . . ?
N2 C31 C36 C40 0.1(3) . . . . ?
C33 C32 C37 C39 74.8(3) . . . . ?
C31 C32 C37 C39 -102.1(2) . . . . ?
C33 C32 C37 C38 -47.5(3) . . . . ?
C31 C32 C37 C38 135.6(2) . . . . ?
C35 C36 C40 C42 53.7(3) . . . . ?
C31 C36 C40 C42 -128.9(2) . . . . ?
C35 C36 C40 C41 -70.2(3) . . . . ?
C31 C36 C40 C41 107.2(3) . . . . ?
C54B O1 C51 C52 -18.8(4) . . . . ?
C54A O1 C51 C52 10.3(5) . . . . ?
Li O1 C51 C52 173.3(3) . . . . ?
O1 C51 C52 C53 -12.0(4) . . . . ?
C51 C52 C53 C54A 9.9(5) . . . . ?
C51 C52 C53 C54B 35.3(4) . . . . ?
C52 C53 C54A O1 -3.8(6) . . . . ?
C51 O1 C54A C53 -4.3(6) . . . . ?
Li O1 C54A C53 -169.2(3) . . . . ?
C51 O1 C54B C53 40.9(4) . . . . ?
Li O1 C54B C53 -150.7(3) . . . . ?
C52 C53 C54B O1 -46.5(4) . . . . ?
C58B O2 C55 C56 -20.3(6) . . . . ?
C58A O2 C55 C56 9.6(5) . . . . ?
Li O2 C55 C56 160.2(3) . . . . ?
O2 C55 C56 C57A 8.9(6) . . . . ?
O2 C55 C56 C57B -13.4(6) . . . . ?
C55 C56 C57A C58A -22.5(7) . . . . ?
C55 O2 C58A C57A -23.1(6) . . . . ?
Li O2 C58A C57A -175.9(4) . . . . ?
C56 C57A C58A O2 27.1(7) . . . . ?
C55 C56 C57B C58B 38.4(7) . . . . ?
C55 O2 C58B C57B 43.2(7) . . . . ?
Li O2 C58B C57B -137.3(5) . . . . ?
C56 C57B C58B O2 -49.3(8) . . . . ?
C58B O2 Li O1 -70.8(7) . . . . ?
C55 O2 Li O1 108.5(4) . . . . ?
C58A O2 Li O1 -103.3(5) . . . . ?
C58B O2 Li Cl2 156.4(6) . . . . ?
C55 O2 Li Cl2 -24.2(4) . . . . ?
C58A O2 Li Cl2 124.0(4) . . . . ?
C58B O2 Li Cl1 56.9(7) . . . . ?
C55 O2 Li Cl1 -123.7(3) . . . . ?
C58A O2 Li Cl1 24.5(5) . . . . ?
C58B O2 Li Zr 105.2(6) . . . . ?
C55 O2 Li Zr -75.4(4) . . . . ?
C58A O2 Li Zr 72.8(5) . . . . ?
C51 O1 Li O2 -8.0(5) . . . . ?
C54B O1 Li O2 -173.7(4) . . . . ?
C54A O1 Li O2 154.1(4) . . . . ?
C51 O1 Li Cl2 124.8(3) . . . . ?
C54B O1 Li Cl2 -40.9(5) . . . . ?
C54A O1 Li Cl2 -73.1(4) . . . . ?
C51 O1 Li Cl1 -135.1(3) . . . . ?
C54B O1 Li Cl1 59.1(5) . . . . ?
C54A O1 Li Cl1 26.9(4) . . . . ?
C51 O1 Li Zr 175.3(2) . . . . ?
C54B O1 Li Zr 9.6(5) . . . . ?
C54A O1 Li Zr -22.6(5) . . . . ?
Zr Cl2 Li O2 -123.3(2) . . . . ?
Zr Cl2 Li O1 101.9(2) . . . . ?
Zr Cl2 Li Cl1 -11.38(11) . . . . ?
Zr Cl1 Li O2 126.1(2) . . . . ?
Zr Cl1 Li O1 -103.0(2) . . . . ?
Zr Cl1 Li Cl2 11.49(11) . . . . ?
N2 Zr Li O2 58.3(4) . . . . ?
N1 Zr Li O2 -52.8(4) . . . . ?
Cl3 Zr Li O2 -178.9(3) . . . . ?
Cl1 Zr Li O2 -79.3(3) . . . . ?
Cl2 Zr Li O2 84.7(3) . . . . ?
Si Zr Li O2 5.2(5) . . . . ?
N2 Zr Li O1 -125.5(2) . . . . ?
N1 Zr Li O1 123.3(2) . . . . ?
Cl3 Zr Li O1 -2.7(3) . . . . ?
Cl1 Zr Li O1 96.9(3) . . . . ?
Cl2 Zr Li O1 -99.1(3) . . . . ?
Si Zr Li O1 -178.58(10) . . . . ?
N2 Zr Li Cl2 -26.45(15) . . . . ?
N1 Zr Li Cl2 -137.57(9) . . . . ?
Cl3 Zr Li Cl2 96.41(8) . . . . ?
Cl1 Zr Li Cl2 -163.99(16) . . . . ?
Si Zr Li Cl2 -79.5(2) . . . . ?
N2 Zr Li Cl1 137.53(9) . . . . ?
N1 Zr Li Cl1 26.42(16) . . . . ?
Cl3 Zr Li Cl1 -99.60(8) . . . . ?
Cl2 Zr Li Cl1 163.99(16) . . . . ?
Si Zr Li Cl1 84.5(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.58
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.054
####################################################################### 
# 
# 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_riv1113
_database_code_depnum_ccdc_archive 'CCDC 1043227'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H54 Cl2 N3 Si Zr, C16 H32 Li O4'
_chemical_formula_sum            'C48 H86 Cl2 Li N3 O4 Si Zr'
_chemical_formula_weight         966.34

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   15.266(2)
_cell_length_b                   18.419(3)
_cell_length_c                   19.316(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5431.5(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5516
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      18.16

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_F_000             2072
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.235
_exptl_crystal_size_min          0.205
_exptl_absorpt_coefficient_mu    0.363
_shelx_estimated_absorpt_T_min   0.917
_shelx_estimated_absorpt_T_max   0.929
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.7591
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            43340
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.528
_diffrn_reflns_theta_max         26.669
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11293
_reflns_number_gt                9794
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.816
_reflns_Friedel_fraction_max     0.984
_reflns_Friedel_fraction_full    0.999

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'DIRDIF-2008 (Beurskens et al., 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0445P)²+1.9706P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 3887 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.010(19)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         11293
_refine_ls_number_parameters     536
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0485
_refine_ls_wR_factor_ref         0.1135
_refine_ls_wR_factor_gt          0.1088
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.063
_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_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
Zr Zr -0.07291(3) 0.54271(2) 0.50944(2) 0.03066(12) Uani 1 1 d . . . . .
Cl1 Cl -0.15244(10) 0.42617(7) 0.49284(9) 0.0546(4) Uani 1 1 d . . . . .
Cl2 Cl -0.03215(13) 0.50521(10) 0.62782(8) 0.0691(5) Uani 1 1 d . . . . .
Si Si 0.04548(9) 0.60909(7) 0.41082(7) 0.0308(3) Uani 1 1 d . . . . .
N1 N -0.0358(2) 0.5437(2) 0.40403(19) 0.0295(8) Uani 1 1 d . . . . .
N2 N 0.0447(2) 0.60520(18) 0.5002(2) 0.0306(8) Uani 1 1 d . . . . .
N3 N -0.1744(3) 0.6124(2) 0.5244(2) 0.0420(11) Uani 1 1 d . . . . .
C1 C 0.1528(4) 0.5896(3) 0.3652(3) 0.0431(13) Uani 1 1 d . . . . .
H1 H 0.1749 0.5421 0.3832 0.052 Uiso 1 1 calc R U . . .
C2 C 0.1424(4) 0.5815(4) 0.2855(3) 0.0577(16) Uani 1 1 d . . . . .
H2A H 0.1998 0.5716 0.2647 0.069 Uiso 1 1 calc R U . . .
H2B H 0.1186 0.6266 0.2663 0.069 Uiso 1 1 calc R U . . .
H2C H 0.1025 0.5413 0.2754 0.069 Uiso 1 1 calc R U . . .
C3 C 0.2232(4) 0.6469(4) 0.3806(4) 0.0625(18) Uani 1 1 d . . . . .
H3A H 0.2771 0.6345 0.3558 0.075 Uiso 1 1 calc R U . . .
H3B H 0.2348 0.6481 0.4305 0.075 Uiso 1 1 calc R U . . .
H3C H 0.2025 0.6946 0.3653 0.075 Uiso 1 1 calc R U . . .
C4 C 0.0036(4) 0.7002(3) 0.3809(3) 0.0455(13) Uani 1 1 d . . . . .
H4 H -0.0535 0.7068 0.4055 0.055 Uiso 1 1 calc R U . . .
C5 C -0.0187(5) 0.7064(3) 0.3040(3) 0.0592(17) Uani 1 1 d . . . . .
H5A H -0.0396 0.7556 0.2939 0.071 Uiso 1 1 calc R U . . .
H5B H -0.0646 0.6712 0.2923 0.071 Uiso 1 1 calc R U . . .
H5C H 0.0337 0.6964 0.2763 0.071 Uiso 1 1 calc R U . . .
C6 C 0.0599(5) 0.7659(3) 0.4033(4) 0.0660(19) Uani 1 1 d . . . . .
H6A H 0.0336 0.8107 0.3856 0.079 Uiso 1 1 calc R U . . .
H6B H 0.1193 0.7606 0.3846 0.079 Uiso 1 1 calc R U . . .
H6C H 0.0627 0.7679 0.4540 0.079 Uiso 1 1 calc R U . . .
C7 C -0.2047(4) 0.6797(3) 0.4953(4) 0.0531(15) Uani 1 1 d . . . . .
H7A H -0.2643 0.6734 0.4775 0.064 Uiso 1 1 calc R U . . .
H7B H -0.1658 0.6943 0.4574 0.064 Uiso 1 1 calc R U . . .
H7C H -0.2046 0.7174 0.5312 0.064 Uiso 1 1 calc R U . . .
C8 C -0.2348(4) 0.5884(4) 0.5785(4) 0.0674(19) Uani 1 1 d . . . . .
H8A H -0.2946 0.5873 0.5600 0.081 Uiso 1 1 calc R U . . .
H8B H -0.2322 0.6222 0.6177 0.081 Uiso 1 1 calc R U . . .
H8C H -0.2182 0.5397 0.5941 0.081 Uiso 1 1 calc R U . . .
C11 C -0.0595(3) 0.4996(2) 0.3468(2) 0.0289(10) Uani 1 1 d . . . . .
C12 C -0.0105(3) 0.4361(2) 0.3308(3) 0.0374(11) Uani 1 1 d . . . . .
C13 C -0.0347(4) 0.3957(3) 0.2729(3) 0.0494(14) Uani 1 1 d . . . . .
H13 H -0.0011 0.3540 0.2612 0.059 Uiso 1 1 calc R U . . .
C14 C -0.1054(4) 0.4137(3) 0.2318(3) 0.0539(16) Uani 1 1 d . . . . .
H14 H -0.1195 0.3855 0.1921 0.065 Uiso 1 1 calc R U . . .
C15 C -0.1545(4) 0.4725(3) 0.2493(3) 0.0462(14) Uani 1 1 d . . . . .
H15 H -0.2041 0.4843 0.2218 0.055 Uiso 1 1 calc R U . . .
C16 C -0.1346(3) 0.5163(3) 0.3065(3) 0.0357(11) Uani 1 1 d . . . . .
C17 C 0.0638(4) 0.4087(3) 0.3752(3) 0.0479(13) Uani 1 1 d . . . . .
H17 H 0.0770 0.4470 0.4104 0.057 Uiso 1 1 calc R U . . .
C18 C 0.0378(5) 0.3404(4) 0.4139(4) 0.070(2) Uani 1 1 d . . . . .
H18A H -0.0163 0.3494 0.4399 0.084 Uiso 1 1 calc R U . . .
H18B H 0.0847 0.3268 0.4460 0.084 Uiso 1 1 calc R U . . .
H18C H 0.0281 0.3009 0.3808 0.084 Uiso 1 1 calc R U . . .
C19 C 0.1484(4) 0.3934(4) 0.3350(4) 0.068(2) Uani 1 1 d . . . . .
H19A H 0.1661 0.4371 0.3097 0.082 Uiso 1 1 calc R U . . .
H19B H 0.1384 0.3536 0.3023 0.082 Uiso 1 1 calc R U . . .
H19C H 0.1949 0.3797 0.3675 0.082 Uiso 1 1 calc R U . . .
C20 C -0.1954(4) 0.5779(3) 0.3254(3) 0.0436(13) Uani 1 1 d . . . . .
H20 H -0.1629 0.6120 0.3565 0.052 Uiso 1 1 calc R U . . .
C21 C -0.2742(4) 0.5490(4) 0.3650(4) 0.0639(17) Uani 1 1 d . . . . .
H21A H -0.2541 0.5218 0.4055 0.077 Uiso 1 1 calc R U . . .
H21B H -0.3084 0.5170 0.3348 0.077 Uiso 1 1 calc R U . . .
H21C H -0.3109 0.5897 0.3800 0.077 Uiso 1 1 calc R U . . .
C22 C -0.2258(5) 0.6206(4) 0.2616(4) 0.073(2) Uani 1 1 d . . . . .
H22A H -0.1747 0.6389 0.2365 0.087 Uiso 1 1 calc R U . . .
H22B H -0.2624 0.6615 0.2763 0.087 Uiso 1 1 calc R U . . .
H22C H -0.2599 0.5886 0.2313 0.087 Uiso 1 1 calc R U . . .
C31 C 0.1050(3) 0.6310(3) 0.5505(3) 0.0349(11) Uani 1 1 d . . . . .
C32 C 0.1828(4) 0.5918(3) 0.5649(3) 0.0443(13) Uani 1 1 d . . . . .
C33 C 0.2418(4) 0.6189(4) 0.6145(4) 0.0572(16) Uani 1 1 d . . . . .
H33 H 0.2940 0.5927 0.6240 0.069 Uiso 1 1 calc R U . . .
C34 C 0.2257(4) 0.6821(4) 0.6494(4) 0.0582(17) Uani 1 1 d . . . . .
H34 H 0.2671 0.7003 0.6817 0.070 Uiso 1 1 calc R U . . .
C35 C 0.1487(4) 0.7192(3) 0.6373(3) 0.0477(14) Uani 1 1 d . . . . .
H35 H 0.1370 0.7624 0.6625 0.057 Uiso 1 1 calc R U . . .
C36 C 0.0877(3) 0.6950(3) 0.5889(3) 0.0371(11) Uani 1 1 d . . . . .
C37 C 0.2036(4) 0.5188(3) 0.5321(4) 0.0567(17) Uani 1 1 d . . . . .
H37 H 0.1603 0.5108 0.4940 0.068 Uiso 1 1 calc R U . . .
C38 C 0.1923(6) 0.4571(4) 0.5837(5) 0.086(2) Uani 1 1 d . . . . .
H38A H 0.1338 0.4597 0.6044 0.104 Uiso 1 1 calc R U . . .
H38B H 0.2367 0.4613 0.6201 0.104 Uiso 1 1 calc R U . . .
H38C H 0.1992 0.4105 0.5598 0.104 Uiso 1 1 calc R U . . .
C39 C 0.2954(5) 0.5150(4) 0.4997(5) 0.086(2) Uani 1 1 d . . . . .
H39A H 0.3025 0.5549 0.4666 0.104 Uiso 1 1 calc R U . . .
H39B H 0.3025 0.4686 0.4756 0.104 Uiso 1 1 calc R U . . .
H39C H 0.3397 0.5193 0.5361 0.104 Uiso 1 1 calc R U . . .
C40 C 0.0012(3) 0.7357(3) 0.5822(3) 0.0388(11) Uani 1 1 d . . . . .
H40 H -0.0279 0.7194 0.5385 0.047 Uiso 1 1 calc R U . . .
C41 C -0.0589(4) 0.7170(3) 0.6424(3) 0.0530(15) Uani 1 1 d . . . . .
H41A H -0.0664 0.6643 0.6451 0.064 Uiso 1 1 calc R U . . .
H41B H -0.1161 0.7401 0.6354 0.064 Uiso 1 1 calc R U . . .
H41C H -0.0331 0.7348 0.6857 0.064 Uiso 1 1 calc R U . . .
C42 C 0.0126(4) 0.8183(3) 0.5787(4) 0.0580(16) Uani 1 1 d . . . . .
H42A H 0.0515 0.8307 0.5401 0.070 Uiso 1 1 calc R U . . .
H42B H 0.0382 0.8358 0.6221 0.070 Uiso 1 1 calc R U . . .
H42C H -0.0446 0.8412 0.5716 0.070 Uiso 1 1 calc R U . . .
O1 O 0.1487(3) 0.1765(3) 0.6210(3) 0.0642(12) Uani 1 1 d . . . . .
O2 O -0.0363(3) 0.2325(2) 0.5894(3) 0.0619(12) Uani 1 1 d . . . . .
O3 O -0.0178(3) 0.0799(2) 0.6554(3) 0.0739(14) Uani 1 1 d D . . . .
O4 O 0.0346(3) 0.1064(3) 0.5013(3) 0.0830(15) Uani 1 1 d D . . . .
C51 C 0.1875(7) 0.1646(5) 0.6860(5) 0.101(3) Uani 1 1 d . . . . .
H51A H 0.2217 0.1189 0.6858 0.121 Uiso 1 1 calc R U . . .
H51B H 0.1422 0.1614 0.7226 0.121 Uiso 1 1 calc R U . . .
C52 C 0.2460(7) 0.2283(5) 0.6981(6) 0.101(3) Uani 1 1 d . . . . .
H52A H 0.2940 0.2164 0.7306 0.121 Uiso 1 1 calc R U . . .
H52B H 0.2129 0.2706 0.7158 0.121 Uiso 1 1 calc R U . . .
C53 C 0.2798(7) 0.2415(7) 0.6266(7) 0.120(4) Uani 1 1 d . . . . .
H53A H 0.2948 0.2934 0.6202 0.144 Uiso 1 1 calc R U . . .
H53B H 0.3328 0.2119 0.6177 0.144 Uiso 1 1 calc R U . . .
C54 C 0.2076(5) 0.2200(5) 0.5795(5) 0.082(2) Uani 1 1 d . . . . .
H54A H 0.1771 0.2634 0.5612 0.098 Uiso 1 1 calc R U . . .
H54B H 0.2305 0.1914 0.5400 0.098 Uiso 1 1 calc R U . . .
C61 C -0.1280(5) 0.2353(4) 0.5762(5) 0.074(2) Uani 1 1 d . . . . .
H61A H -0.1530 0.1857 0.5760 0.088 Uiso 1 1 calc R U . . .
H61B H -0.1392 0.2578 0.5305 0.088 Uiso 1 1 calc R U . . .
C62 C -0.1686(5) 0.2796(5) 0.6322(5) 0.082(2) Uani 1 1 d . . . . .
H62A H -0.2096 0.3158 0.6126 0.099 Uiso 1 1 calc R U . . .
H62B H -0.2009 0.2482 0.6651 0.099 Uiso 1 1 calc R U . . .
C63 C -0.0942(5) 0.3159(4) 0.6671(4) 0.075(2) Uani 1 1 d . . . . .
H63A H -0.0853 0.2958 0.7141 0.090 Uiso 1 1 calc R U . . .
H63B H -0.1048 0.3688 0.6709 0.090 Uiso 1 1 calc R U . . .
C64 C -0.0157(5) 0.3010(3) 0.6219(4) 0.0670(19) Uani 1 1 d . . . . .
H64A H -0.0080 0.3397 0.5869 0.080 Uiso 1 1 calc R U . . .
H64B H 0.0384 0.2973 0.6499 0.080 Uiso 1 1 calc R U . . .
C71A C -0.0229(7) 0.0037(5) 0.6370(5) 0.060(3) Uiso 0.65 1 d D . P A 1
H71A H 0.0359 -0.0161 0.6265 0.071 Uiso 0.65 1 calc R U P A 1
H71B H -0.0614 -0.0036 0.5963 0.071 Uiso 0.65 1 calc R U P A 1
C72A C -0.0616(8) -0.0318(6) 0.7014(6) 0.064(3) Uiso 0.65 1 d D . P A 1
H72A H -0.0157 -0.0414 0.7365 0.077 Uiso 0.65 1 calc R U P A 1
H72B H -0.0914 -0.0780 0.6898 0.077 Uiso 0.65 1 calc R U P A 1
C73A C -0.1270(7) 0.0252(6) 0.7269(7) 0.071(3) Uiso 0.65 1 d D . P A 1
H73A H -0.1828 0.0224 0.7010 0.085 Uiso 0.65 1 calc R U P A 1
H73B H -0.1390 0.0195 0.7770 0.085 Uiso 0.65 1 calc R U P A 1
C74A C -0.0800(8) 0.0942(6) 0.7125(6) 0.071(3) Uiso 0.65 1 d D . P A 1
H74A H -0.1221 0.1325 0.6989 0.085 Uiso 0.65 1 calc R U P A 1
H74B H -0.0481 0.1106 0.7542 0.085 Uiso 0.65 1 calc R U P A 1
C71B C -0.0017(12) 0.0014(6) 0.6712(11) 0.075(6) Uiso 0.35 1 d D . P A 2
H71C H 0.0490 -0.0054 0.7026 0.090 Uiso 0.35 1 calc R U P A 2
H71D H 0.0070 -0.0277 0.6287 0.090 Uiso 0.35 1 calc R U P A 2
C72B C -0.0896(16) -0.0168(9) 0.7074(14) 0.092(9) Uiso 0.35 1 d D . P A 2
H72C H -0.1341 -0.0323 0.6732 0.111 Uiso 0.35 1 calc R U P A 2
H72D H -0.0817 -0.0558 0.7420 0.111 Uiso 0.35 1 calc R U P A 2
C73B C -0.1163(12) 0.0548(11) 0.7424(10) 0.077(7) Uiso 0.35 1 d D . P A 2
H73C H -0.1737 0.0717 0.7247 0.092 Uiso 0.35 1 calc R U P A 2
H73D H -0.1203 0.0487 0.7932 0.092 Uiso 0.35 1 calc R U P A 2
C74B C -0.0434(15) 0.1088(9) 0.7233(9) 0.078(7) Uiso 0.35 1 d D . P A 2
H74C H -0.0659 0.1591 0.7199 0.093 Uiso 0.35 1 calc R U P A 2
H74D H 0.0056 0.1071 0.7568 0.093 Uiso 0.35 1 calc R U P A 2
C81 C -0.0163(7) 0.1330(5) 0.4444(4) 0.095(3) Uani 1 1 d D . . . .
H81A H -0.0286 0.1855 0.4495 0.114 Uiso 0.5 1 calc R U P B 1
H81B H -0.0724 0.1064 0.4404 0.114 Uiso 0.5 1 calc R U P B 1
H81C H 0.0026 0.1826 0.4312 0.114 Uiso 0.5 1 calc R U P C 2
H81D H -0.0793 0.1342 0.4564 0.114 Uiso 0.5 1 calc R U P C 2
C82A C 0.0411(11) 0.1189(10) 0.3836(8) 0.094(5) Uiso 0.5 1 d D . P D 1
H82A H 0.0073 0.0970 0.3452 0.113 Uiso 0.5 1 calc R U P D 1
H82B H 0.0685 0.1644 0.3670 0.113 Uiso 0.5 1 calc R U P D 1
C83A C 0.1085(11) 0.0675(9) 0.4099(8) 0.092(5) Uiso 0.5 1 d D . P D 1
H83A H 0.1654 0.0927 0.4154 0.111 Uiso 0.5 1 calc R U P D 1
H83B H 0.1163 0.0268 0.3770 0.111 Uiso 0.5 1 calc R U P D 1
C84A C 0.0760(13) 0.0387(7) 0.4807(8) 0.081(5) Uiso 0.5 1 d D . P D 1
H84A H 0.0337 -0.0017 0.4761 0.097 Uiso 0.5 1 calc R U P D 1
H84B H 0.1246 0.0246 0.5119 0.097 Uiso 0.5 1 calc R U P D 1
C82B C 0.0006(13) 0.0801(8) 0.3863(8) 0.088(5) Uiso 0.5 1 d D . P D 2
H82C H -0.0548 0.0646 0.3641 0.105 Uiso 0.5 1 calc R U P D 2
H82D H 0.0396 0.1013 0.3508 0.105 Uiso 0.5 1 calc R U P D 2
C83B C 0.0441(14) 0.0179(9) 0.4229(10) 0.113(7) Uiso 0.5 1 d D . P D 2
H83C H 0.0792 -0.0121 0.3908 0.136 Uiso 0.5 1 calc R U P D 2
H83D H 0.0010 -0.0132 0.4472 0.136 Uiso 0.5 1 calc R U P D 2
C84B C 0.1023(8) 0.0599(8) 0.4741(7) 0.059(4) Uiso 0.5 1 d D . P D 2
H84C H 0.1280 0.0280 0.5100 0.071 Uiso 0.5 1 calc R U P D 2
H84D H 0.1493 0.0875 0.4505 0.071 Uiso 0.5 1 calc R U P D 2
Li Li 0.0340(7) 0.1473(6) 0.5915(6) 0.057(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr N3 2.033(4) . ?
Zr N1 2.113(4) . ?
Zr N2 2.140(4) . ?
Zr Cl2 2.4683(16) . ?
Zr Cl1 2.4868(13) . ?
Si N2 1.728(4) . ?
Si N1 1.735(4) . ?
Si C4 1.887(5) . ?
Si C1 1.895(5) . ?
N1 C11 1.419(6) . ?
N2 C31 1.421(6) . ?
N3 C7 1.438(7) . ?
N3 C8 1.462(8) . ?
C1 C3 1.536(8) . ?
C1 C2 1.553(8) . ?
C4 C5 1.529(8) . ?
C4 C6 1.545(8) . ?
C11 C16 1.419(7) . ?
C11 C12 1.421(6) . ?
C12 C13 1.394(8) . ?
C12 C17 1.509(8) . ?
C13 C14 1.379(8) . ?
C14 C15 1.361(8) . ?
C15 C16 1.401(7) . ?
C16 C20 1.512(7) . ?
C17 C18 1.516(9) . ?
C17 C19 1.534(8) . ?
C20 C21 1.521(9) . ?
C20 C22 1.534(9) . ?
C31 C32 1.417(7) . ?
C31 C36 1.417(7) . ?
C32 C33 1.406(8) . ?
C32 C37 1.521(8) . ?
C33 C34 1.367(9) . ?
C34 C35 1.380(9) . ?
C35 C36 1.392(7) . ?
C36 C40 1.523(7) . ?
C37 C38 1.522(10) . ?
C37 C39 1.536(10) . ?
C40 C41 1.521(8) . ?
C40 C42 1.533(7) . ?
O1 C51 1.405(9) . ?
O1 C54 1.447(9) . ?
O1 Li 1.918(12) . ?
O2 C61 1.424(8) . ?
O2 C64 1.444(8) . ?
O2 Li 1.902(11) . ?
O3 C71A 1.449(8) . ?
O3 C74B 1.469(11) . ?
O3 C74A 1.479(9) . ?
O3 C71B 1.499(11) . ?
O3 Li 1.922(13) . ?
O4 C81 1.432(9) . ?
O4 C84B 1.442(10) . ?
O4 C84A 1.454(11) . ?
O4 Li 1.898(12) . ?
C51 C52 1.493(12) . ?
C52 C53 1.495(15) . ?
C53 C54 1.484(13) . ?
C61 C62 1.491(11) . ?
C62 C63 1.480(12) . ?
C63 C64 1.507(9) . ?
C71A C72A 1.525(10) . ?
C72A C73A 1.531(11) . ?
C73A C74A 1.486(11) . ?
C71B C72B 1.549(12) . ?
C72B C73B 1.537(13) . ?
C73B C74B 1.537(13) . ?
C81 C82A 1.488(11) . ?
C81 C82B 1.509(11) . ?
C82A C83A 1.487(12) . ?
C83A C84A 1.550(12) . ?
C82B C83B 1.500(12) . ?
C83B C84B 1.538(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Zr N1 109.62(16) . . ?
N3 Zr N2 108.15(15) . . ?
N1 Zr N2 71.98(14) . . ?
N3 Zr Cl2 103.71(14) . . ?
N1 Zr Cl2 145.83(11) . . ?
N2 Zr Cl2 90.93(11) . . ?
N3 Zr Cl1 101.03(13) . . ?
N1 Zr Cl1 90.79(11) . . ?
N2 Zr Cl1 149.67(10) . . ?
Cl2 Zr Cl1 90.06(6) . . ?
N2 Si N1 92.39(18) . . ?
N2 Si C4 109.9(2) . . ?
N1 Si C4 110.6(2) . . ?
N2 Si C1 117.6(2) . . ?
N1 Si C1 116.8(2) . . ?
C4 Si C1 108.6(3) . . ?
C11 N1 Si 129.7(3) . . ?
C11 N1 Zr 132.7(3) . . ?
Si N1 Zr 97.17(17) . . ?
C31 N2 Si 131.7(3) . . ?
C31 N2 Zr 131.8(3) . . ?
Si N2 Zr 96.39(17) . . ?
C7 N3 C8 109.7(5) . . ?
C7 N3 Zr 137.2(4) . . ?
C8 N3 Zr 113.1(4) . . ?
C3 C1 C2 109.2(5) . . ?
C3 C1 Si 112.6(4) . . ?
C2 C1 Si 113.0(4) . . ?
C5 C4 C6 109.8(5) . . ?
C5 C4 Si 116.1(4) . . ?
C6 C4 Si 115.0(5) . . ?
C16 C11 N1 120.6(4) . . ?
C16 C11 C12 119.0(4) . . ?
N1 C11 C12 120.4(4) . . ?
C13 C12 C11 118.3(5) . . ?
C13 C12 C17 118.5(5) . . ?
C11 C12 C17 123.2(4) . . ?
C14 C13 C12 122.7(5) . . ?
C15 C14 C13 118.7(5) . . ?
C14 C15 C16 122.3(5) . . ?
C15 C16 C11 118.9(5) . . ?
C15 C16 C20 119.3(5) . . ?
C11 C16 C20 121.8(4) . . ?
C12 C17 C18 111.2(5) . . ?
C12 C17 C19 114.0(5) . . ?
C18 C17 C19 108.5(5) . . ?
C16 C20 C21 110.1(5) . . ?
C16 C20 C22 112.1(5) . . ?
C21 C20 C22 110.1(5) . . ?
C32 C31 C36 118.5(5) . . ?
C32 C31 N2 120.5(4) . . ?
C36 C31 N2 121.0(4) . . ?
C33 C32 C31 119.3(5) . . ?
C33 C32 C37 117.6(5) . . ?
C31 C32 C37 123.0(5) . . ?
C34 C33 C32 121.5(6) . . ?
C33 C34 C35 119.4(6) . . ?
C34 C35 C36 121.6(5) . . ?
C35 C36 C31 119.5(5) . . ?
C35 C36 C40 118.6(5) . . ?
C31 C36 C40 121.8(4) . . ?
C32 C37 C38 111.4(6) . . ?
C32 C37 C39 113.6(6) . . ?
C38 C37 C39 109.7(6) . . ?
C41 C40 C36 110.3(5) . . ?
C41 C40 C42 109.0(5) . . ?
C36 C40 C42 113.2(5) . . ?
C51 O1 C54 108.7(6) . . ?
C51 O1 Li 127.3(6) . . ?
C54 O1 Li 123.9(6) . . ?
C61 O2 C64 105.1(5) . . ?
C61 O2 Li 126.1(6) . . ?
C64 O2 Li 126.1(5) . . ?
C71A O3 C74A 108.7(6) . . ?
C74B O3 C71B 102.2(9) . . ?
C71A O3 Li 119.3(6) . . ?
C74B O3 Li 116.7(8) . . ?
C74A O3 Li 128.9(6) . . ?
C71B O3 Li 133.4(7) . . ?
C81 O4 C84B 108.2(7) . . ?
C81 O4 C84A 108.7(8) . . ?
C81 O4 Li 124.5(5) . . ?
C84B O4 Li 124.9(7) . . ?
C84A O4 Li 126.3(8) . . ?
O1 C51 C52 105.6(7) . . ?
C51 C52 C53 101.0(8) . . ?
C54 C53 C52 105.4(8) . . ?
O1 C54 C53 105.7(8) . . ?
O2 C61 C62 107.3(7) . . ?
C63 C62 C61 105.0(6) . . ?
C62 C63 C64 105.3(6) . . ?
O2 C64 C63 103.7(6) . . ?
O3 C71A C72A 103.7(7) . . ?
C71A C72A C73A 102.8(7) . . ?
C74A C73A C72A 102.2(8) . . ?
O3 C74A C73A 107.3(8) . . ?
O3 C71B C72B 99.1(8) . . ?
C73B C72B C71B 104.1(9) . . ?
C74B C73B C72B 104.9(8) . . ?
O3 C74B C73B 99.9(9) . . ?
O4 C81 C82A 103.1(9) . . ?
O4 C81 C82B 104.9(8) . . ?
C83A C82A C81 104.4(12) . . ?
C82A C83A C84A 107.3(13) . . ?
O4 C84A C83A 94.9(10) . . ?
C83B C82B C81 102.6(12) . . ?
C82B C83B C84B 100.1(13) . . ?
O4 C84B C83B 96.8(11) . . ?
O4 Li O2 108.1(6) . . ?
O4 Li O1 112.4(6) . . ?
O2 Li O1 106.9(5) . . ?
O4 Li O3 109.6(6) . . ?
O2 Li O3 108.3(6) . . ?
O1 Li O3 111.5(6) . . ?

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
N2 Si N1 C11 -160.9(4) . . . . ?
C4 Si N1 C11 86.8(4) . . . . ?
C1 Si N1 C11 -38.2(5) . . . . ?
N2 Si N1 Zr 11.90(17) . . . . ?
C4 Si N1 Zr -100.4(2) . . . . ?
C1 Si N1 Zr 134.6(2) . . . . ?
N3 Zr N1 C11 -94.2(4) . . . . ?
N2 Zr N1 C11 162.4(4) . . . . ?
Cl2 Zr N1 C11 99.1(4) . . . . ?
Cl1 Zr N1 C11 7.8(4) . . . . ?
N3 Zr N1 Si 93.32(19) . . . . ?
N2 Zr N1 Si -10.08(15) . . . . ?
Cl2 Zr N1 Si -73.4(3) . . . . ?
Cl1 Zr N1 Si -164.67(14) . . . . ?
N1 Si N2 C31 164.8(4) . . . . ?
C4 Si N2 C31 -82.2(5) . . . . ?
C1 Si N2 C31 42.7(5) . . . . ?
N1 Si N2 Zr -11.73(17) . . . . ?
C4 Si N2 Zr 101.2(2) . . . . ?
C1 Si N2 Zr -133.8(2) . . . . ?
N3 Zr N2 C31 88.2(4) . . . . ?
N1 Zr N2 C31 -166.4(4) . . . . ?
Cl2 Zr N2 C31 -16.5(4) . . . . ?
Cl1 Zr N2 C31 -108.2(4) . . . . ?
N3 Zr N2 Si -95.3(2) . . . . ?
N1 Zr N2 Si 10.10(15) . . . . ?
Cl2 Zr N2 Si 159.98(14) . . . . ?
Cl1 Zr N2 Si 68.3(3) . . . . ?
N1 Zr N3 C7 -31.7(6) . . . . ?
N2 Zr N3 C7 45.1(6) . . . . ?
Cl2 Zr N3 C7 140.7(5) . . . . ?
Cl1 Zr N3 C7 -126.5(5) . . . . ?
N1 Zr N3 C8 147.2(4) . . . . ?
N2 Zr N3 C8 -136.0(4) . . . . ?
Cl2 Zr N3 C8 -40.4(4) . . . . ?
Cl1 Zr N3 C8 52.4(4) . . . . ?
N2 Si C1 C3 -65.6(5) . . . . ?
N1 Si C1 C3 -174.1(4) . . . . ?
C4 Si C1 C3 60.0(5) . . . . ?
N2 Si C1 C2 170.1(4) . . . . ?
N1 Si C1 C2 61.6(5) . . . . ?
C4 Si C1 C2 -64.3(4) . . . . ?
N2 Si C4 C5 -167.0(4) . . . . ?
N1 Si C4 C5 -66.4(5) . . . . ?
C1 Si C4 C5 63.1(5) . . . . ?
N2 Si C4 C6 63.0(5) . . . . ?
N1 Si C4 C6 163.6(4) . . . . ?
C1 Si C4 C6 -66.9(5) . . . . ?
Si N1 C11 C16 -102.6(5) . . . . ?
Zr N1 C11 C16 87.2(5) . . . . ?
Si N1 C11 C12 80.3(5) . . . . ?
Zr N1 C11 C12 -89.9(5) . . . . ?
C16 C11 C12 C13 4.7(7) . . . . ?
N1 C11 C12 C13 -178.2(5) . . . . ?
C16 C11 C12 C17 -172.6(5) . . . . ?
N1 C11 C12 C17 4.5(7) . . . . ?
C11 C12 C13 C14 -1.9(8) . . . . ?
C17 C12 C13 C14 175.6(6) . . . . ?
C12 C13 C14 C15 -1.2(9) . . . . ?
C13 C14 C15 C16 1.5(9) . . . . ?
C14 C15 C16 C11 1.4(8) . . . . ?
C14 C15 C16 C20 -176.1(6) . . . . ?
N1 C11 C16 C15 178.4(5) . . . . ?
C12 C11 C16 C15 -4.5(7) . . . . ?
N1 C11 C16 C20 -4.2(7) . . . . ?
C12 C11 C16 C20 173.0(5) . . . . ?
C13 C12 C17 C18 -69.4(7) . . . . ?
C11 C12 C17 C18 107.9(6) . . . . ?
C13 C12 C17 C19 53.7(7) . . . . ?
C11 C12 C17 C19 -129.0(5) . . . . ?
C15 C16 C20 C21 79.8(6) . . . . ?
C11 C16 C20 C21 -97.7(6) . . . . ?
C15 C16 C20 C22 -43.2(7) . . . . ?
C11 C16 C20 C22 139.4(6) . . . . ?
Si N2 C31 C32 -78.6(6) . . . . ?
Zr N2 C31 C32 96.7(5) . . . . ?
Si N2 C31 C36 103.3(5) . . . . ?
Zr N2 C31 C36 -81.4(6) . . . . ?
C36 C31 C32 C33 -2.4(8) . . . . ?
N2 C31 C32 C33 179.4(5) . . . . ?
C36 C31 C32 C37 173.8(5) . . . . ?
N2 C31 C32 C37 -4.4(8) . . . . ?
C31 C32 C33 C34 0.2(10) . . . . ?
C37 C32 C33 C34 -176.2(6) . . . . ?
C32 C33 C34 C35 1.9(11) . . . . ?
C33 C34 C35 C36 -1.7(10) . . . . ?
C34 C35 C36 C31 -0.6(9) . . . . ?
C34 C35 C36 C40 175.5(6) . . . . ?
C32 C31 C36 C35 2.6(8) . . . . ?
N2 C31 C36 C35 -179.3(5) . . . . ?
C32 C31 C36 C40 -173.3(5) . . . . ?
N2 C31 C36 C40 4.8(7) . . . . ?
C33 C32 C37 C38 70.3(8) . . . . ?
C31 C32 C37 C38 -106.0(7) . . . . ?
C33 C32 C37 C39 -54.2(8) . . . . ?
C31 C32 C37 C39 129.6(7) . . . . ?
C35 C36 C40 C41 -75.7(6) . . . . ?
C31 C36 C40 C41 100.3(6) . . . . ?
C35 C36 C40 C42 46.8(7) . . . . ?
C31 C36 C40 C42 -137.3(5) . . . . ?
C54 O1 C51 C52 27.9(10) . . . . ?
Li O1 C51 C52 -148.1(7) . . . . ?
O1 C51 C52 C53 -36.8(11) . . . . ?
C51 C52 C53 C54 32.1(11) . . . . ?
C51 O1 C54 C53 -7.0(10) . . . . ?
Li O1 C54 C53 169.2(7) . . . . ?
C52 C53 C54 O1 -16.6(11) . . . . ?
C64 O2 C61 C62 -32.1(8) . . . . ?
Li O2 C61 C62 130.0(7) . . . . ?
O2 C61 C62 C63 13.5(9) . . . . ?
C61 C62 C63 C64 9.4(9) . . . . ?
C61 O2 C64 C63 37.4(8) . . . . ?
Li O2 C64 C63 -124.8(7) . . . . ?
C62 C63 C64 O2 -28.6(8) . . . . ?
C74A O3 C71A C72A -21.5(11) . . . . ?
Li O3 C71A C72A 176.4(7) . . . . ?
O3 C71A C72A C73A 36.7(12) . . . . ?
C71A C72A C73A C74A -37.7(12) . . . . ?
C71A O3 C74A C73A -2.5(12) . . . . ?
Li O3 C74A C73A 157.3(8) . . . . ?
C72A C73A C74A O3 25.2(12) . . . . ?
C74B O3 C71B C72B 52.4(17) . . . . ?
Li O3 C71B C72B -160.7(13) . . . . ?
O3 C71B C72B C73B -31(2) . . . . ?
C71B C72B C73B C74B 1(3) . . . . ?
C71B O3 C74B C73B -52.2(15) . . . . ?
Li O3 C74B C73B 154.2(11) . . . . ?
C72B C73B C74B O3 31(2) . . . . ?
C84A O4 C81 C82A -41.3(13) . . . . ?
Li O4 C81 C82A 146.3(10) . . . . ?
C84B O4 C81 C82B 20.9(13) . . . . ?
Li O4 C81 C82B -175.7(10) . . . . ?
O4 C81 C82A C83A 15.0(16) . . . . ?
C81 C82A C83A C84A 13(2) . . . . ?
C81 O4 C84A C83A 46.6(14) . . . . ?
Li O4 C84A C83A -141.2(10) . . . . ?
C82A C83A C84A O4 -34.9(18) . . . . ?
O4 C81 C82B C83B 13.1(16) . . . . ?
C81 C82B C83B C84B -39.4(19) . . . . ?
C81 O4 C84B C83B -44.6(14) . . . . ?
Li O4 C84B C83B 152.1(10) . . . . ?
C82B C83B C84B O4 50.6(17) . . . . ?
C81 O4 Li O2 -5.0(10) . . . . ?
C84B O4 Li O2 155.7(9) . . . . ?
C84A O4 Li O2 -176.1(11) . . . . ?
C81 O4 Li O1 -122.7(8) . . . . ?
C84B O4 Li O1 38.0(12) . . . . ?
C84A O4 Li O1 66.2(12) . . . . ?
C81 O4 Li O3 112.8(7) . . . . ?
C84B O4 Li O3 -86.5(11) . . . . ?
C84A O4 Li O3 -58.3(12) . . . . ?
C61 O2 Li O4 64.6(9) . . . . ?
C64 O2 Li O4 -136.9(6) . . . . ?
C61 O2 Li O1 -174.3(6) . . . . ?
C64 O2 Li O1 -15.8(9) . . . . ?
C61 O2 Li O3 -54.1(9) . . . . ?
C64 O2 Li O3 104.4(7) . . . . ?
C51 O1 Li O4 -135.6(8) . . . . ?
C54 O1 Li O4 48.9(8) . . . . ?
C51 O1 Li O2 106.0(8) . . . . ?
C54 O1 Li O2 -69.5(8) . . . . ?
C51 O1 Li O3 -12.1(10) . . . . ?
C54 O1 Li O3 172.4(6) . . . . ?
C71A O3 Li O4 19.7(9) . . . . ?
C74B O3 Li O4 -165.3(11) . . . . ?
C74A O3 Li O4 -138.3(8) . . . . ?
C71B O3 Li O4 51.5(15) . . . . ?
C71A O3 Li O2 137.4(7) . . . . ?
C74B O3 Li O2 -47.6(13) . . . . ?
C74A O3 Li O2 -20.6(11) . . . . ?
C71B O3 Li O2 169.2(14) . . . . ?
C71A O3 Li O1 -105.3(8) . . . . ?
C74B O3 Li O1 69.7(12) . . . . ?
C74A O3 Li O1 96.7(9) . . . . ?
C71B O3 Li O1 -73.6(15) . . . . ?

_refine_diff_density_max         0.664
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.059

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_riv1119
_database_code_depnum_ccdc_archive 'CCDC 1043228'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H52 B Cl2 N2 Si Zr, C16 H32 Li O4'
_chemical_formula_sum            'C46 H84 B Cl2 Li N2 O4 Si Zr'
_chemical_formula_weight         937.11

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   15.4463(17)
_cell_length_b                   18.451(2)
_cell_length_c                   18.574(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5293.6(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9919
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      22.27

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_F_000             2008
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.523
_exptl_crystal_size_mid          0.398
_exptl_crystal_size_min          0.274
_exptl_absorpt_coefficient_mu    0.370
_shelx_estimated_absorpt_T_min   0.830
_shelx_estimated_absorpt_T_max   0.905
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.8016
_exptl_absorpt_correction_T_max  0.9958
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42190
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.556
_diffrn_reflns_theta_max         26.523
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10870
_reflns_number_gt                10278
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_max     0.989
_reflns_Friedel_fraction_full    1.000

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'DIRDIF-2008 (Beurskens et al., 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refined as a 2-component inversion twin. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0711P)²+17.9163P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0036(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.09(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         10870
_refine_ls_number_parameters     537
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0795
_refine_ls_wR_factor_ref         0.2096
_refine_ls_wR_factor_gt          0.2073
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_restrained_S_all      1.145
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Zr Zr 0.06116(5) 0.52607(4) 0.00944(4) 0.0352(2) Uani 1 1 d . . . . .
Cl1 Cl -0.0389(5) 0.6237(3) 0.0452(3) 0.144(3) Uani 1 1 d . . . . .
Cl2 Cl 0.0450(3) 0.5439(2) -0.1231(2) 0.0972(12) Uani 1 1 d . . . . .
Si Si -0.00153(17) 0.39765(12) 0.08104(14) 0.0366(5) Uani 1 1 d . . . . .
N1 N -0.0067(4) 0.4295(3) -0.0079(4) 0.0291(13) Uani 1 1 d . . . . .
N2 N 0.0730(5) 0.4649(3) 0.1044(4) 0.0388(15) Uani 1 1 d . . . . .
C1 C -0.1036(10) 0.4063(7) 0.1388(10) 0.081(4) Uani 1 1 d . . . . .
H1 H -0.0761 0.4152 0.1868 0.097 Uiso 1 1 calc R U . . .
C2 C -0.1550(7) 0.4768(8) 0.1312(7) 0.067(3) Uani 1 1 d . . . . .
H2A H -0.2044 0.4760 0.1643 0.081 Uiso 1 1 calc R U . . .
H2B H -0.1759 0.4814 0.0816 0.081 Uiso 1 1 calc R U . . .
H2C H -0.1175 0.5180 0.1428 0.081 Uiso 1 1 calc R U . . .
C3 C -0.1525(12) 0.3433(9) 0.1557(11) 0.106(6) Uani 1 1 d . . . . .
H3A H -0.2011 0.3566 0.1869 0.127 Uiso 1 1 calc R U . . .
H3B H -0.1155 0.3083 0.1806 0.127 Uiso 1 1 calc R U . . .
H3C H -0.1747 0.3217 0.1112 0.127 Uiso 1 1 calc R U . . .
C4 C 0.0387(8) 0.3021(5) 0.0901(6) 0.052(3) Uani 1 1 d . . . . .
H4 H 0.0962 0.3004 0.0653 0.062 Uiso 1 1 calc R U . . .
C5 C -0.0188(9) 0.2444(5) 0.0527(7) 0.065(3) Uani 1 1 d . . . . .
H5A H 0.0063 0.1962 0.0601 0.078 Uiso 1 1 calc R U . . .
H5B H -0.0219 0.2547 0.0010 0.078 Uiso 1 1 calc R U . . .
H5C H -0.0772 0.2458 0.0733 0.078 Uiso 1 1 calc R U . . .
C6 C 0.0557(11) 0.2804(5) 0.1696(7) 0.073(4) Uani 1 1 d . . . . .
H6A H 0.0772 0.2305 0.1715 0.087 Uiso 1 1 calc R U . . .
H6B H 0.0017 0.2841 0.1971 0.087 Uiso 1 1 calc R U . . .
H6C H 0.0990 0.3131 0.1905 0.087 Uiso 1 1 calc R U . . .
C11 C -0.0306(5) 0.3887(4) -0.0707(5) 0.0337(18) Uani 1 1 d . . . . .
C12 C -0.1124(6) 0.3902(5) -0.0987(4) 0.039(2) Uani 1 1 d . . . . .
C13 C -0.1331(8) 0.3544(6) -0.1605(6) 0.054(3) Uani 1 1 d . . . . .
H13 H -0.1901 0.3580 -0.1795 0.064 Uiso 1 1 calc R U . . .
C14 C -0.0714(9) 0.3123(6) -0.1962(6) 0.061(3) Uani 1 1 d . . . . .
H14 H -0.0864 0.2860 -0.2384 0.074 Uiso 1 1 calc R U . . .
C15 C 0.0117(7) 0.3099(6) -0.1691(6) 0.052(2) Uani 1 1 d . . . . .
H15 H 0.0541 0.2819 -0.1936 0.062 Uiso 1 1 calc R U . . .
C16 C 0.0352(6) 0.3474(4) -0.1069(5) 0.041(2) Uani 1 1 d . . . . .
C17 C -0.1834(7) 0.4372(6) -0.0652(8) 0.063(3) Uani 1 1 d . . . . .
H17 H -0.1616 0.4559 -0.0180 0.076 Uiso 1 1 calc R U . . .
C18 C -0.2065(10) 0.5027(8) -0.1127(13) 0.112(7) Uani 1 1 d . . . . .
H18A H -0.1545 0.5319 -0.1212 0.134 Uiso 1 1 calc R U . . .
H18B H -0.2504 0.5323 -0.0885 0.134 Uiso 1 1 calc R U . . .
H18C H -0.2294 0.4856 -0.1589 0.134 Uiso 1 1 calc R U . . .
C19 C -0.2668(7) 0.3956(7) -0.0514(8) 0.072(3) Uani 1 1 d . . . . .
H19A H -0.2545 0.3534 -0.0210 0.086 Uiso 1 1 calc R U . . .
H19B H -0.2913 0.3794 -0.0973 0.086 Uiso 1 1 calc R U . . .
H19C H -0.3084 0.4272 -0.0268 0.086 Uiso 1 1 calc R U . . .
C20 C 0.1290(6) 0.3464(5) -0.0856(7) 0.056(3) Uani 1 1 d . . . . .
H20 H 0.1341 0.3733 -0.0390 0.067 Uiso 1 1 calc R U . . .
C21 C 0.1915(8) 0.3815(7) -0.1387(9) 0.075(4) Uani 1 1 d . . . . .
H21A H 0.1737 0.4316 -0.1477 0.090 Uiso 1 1 calc R U . . .
H21B H 0.1909 0.3543 -0.1840 0.090 Uiso 1 1 calc R U . . .
H21C H 0.2501 0.3810 -0.1185 0.090 Uiso 1 1 calc R U . . .
C22 C 0.1625(9) 0.2673(6) -0.0721(8) 0.070(3) Uani 1 1 d . . . . .
H22A H 0.2232 0.2689 -0.0570 0.084 Uiso 1 1 calc R U . . .
H22B H 0.1574 0.2391 -0.1166 0.084 Uiso 1 1 calc R U . . .
H22C H 0.1277 0.2445 -0.0343 0.084 Uiso 1 1 calc R U . . .
C31 C 0.1257(7) 0.4643(5) 0.1677(6) 0.054(3) Uani 1 1 d . . . . .
C32 C 0.0989(8) 0.5015(5) 0.2307(6) 0.056(3) Uani 1 1 d . . . . .
C33 C 0.1458(11) 0.4933(6) 0.2940(9) 0.086(5) Uani 1 1 d . . . . .
H33 H 0.1253 0.5146 0.3373 0.103 Uiso 1 1 calc R U . . .
C34 C 0.2238(13) 0.4536(8) 0.2941(11) 0.107(7) Uani 1 1 d . . . . .
H34 H 0.2568 0.4488 0.3370 0.128 Uiso 1 1 calc R U . . .
C35 C 0.2510(11) 0.4224(7) 0.2320(11) 0.106(7) Uani 1 1 d . . . . .
H35 H 0.3034 0.3956 0.2331 0.127 Uiso 1 1 calc R U . . .
C36 C 0.2071(8) 0.4270(6) 0.1665(9) 0.073(4) Uani 1 1 d . . . . .
C37 C 0.0249(8) 0.5532(5) 0.2303(6) 0.055(3) Uani 1 1 d . . . . .
H37 H -0.0069 0.5466 0.1839 0.066 Uiso 1 1 calc R U . . .
C38 C 0.0627(9) 0.6305(5) 0.2308(7) 0.065(3) Uani 1 1 d . . . . .
H38A H 0.1041 0.6357 0.1911 0.079 Uiso 1 1 calc R U . . .
H38B H 0.0922 0.6393 0.2766 0.079 Uiso 1 1 calc R U . . .
H38C H 0.0157 0.6657 0.2248 0.079 Uiso 1 1 calc R U . . .
C39 C -0.0398(9) 0.5450(8) 0.2907(7) 0.079(4) Uani 1 1 d . . . . .
H39A H -0.0639 0.4959 0.2898 0.095 Uiso 1 1 calc R U . . .
H39B H -0.0865 0.5803 0.2845 0.095 Uiso 1 1 calc R U . . .
H39C H -0.0109 0.5533 0.3369 0.095 Uiso 1 1 calc R U . . .
C40 C 0.2489(8) 0.3957(7) 0.0983(10) 0.088(5) Uani 1 1 d . . . . .
H40 H 0.2067 0.3987 0.0576 0.105 Uiso 1 1 calc R U . . .
C41 C 0.3276(9) 0.4376(10) 0.0796(13) 0.122(8) Uani 1 1 d . . . . .
H41A H 0.3118 0.4882 0.0701 0.147 Uiso 1 1 calc R U . . .
H41B H 0.3545 0.4167 0.0365 0.147 Uiso 1 1 calc R U . . .
H41C H 0.3687 0.4357 0.1198 0.147 Uiso 1 1 calc R U . . .
C42 C 0.2756(12) 0.3149(8) 0.1099(12) 0.124(8) Uani 1 1 d . . . . .
H42A H 0.3026 0.2963 0.0659 0.148 Uiso 1 1 calc R U . . .
H42B H 0.2240 0.2861 0.1211 0.148 Uiso 1 1 calc R U . . .
H42C H 0.3168 0.3117 0.1498 0.148 Uiso 1 1 calc R U . . .
B B 0.2022(11) 0.5766(12) 0.0095(12) 0.116(8) Uani 1 1 d D . . . .
H1BA H 0.197(7) 0.519(2) -0.006(6) 0.139 Uiso 1 1 d D U . . .
H1BB H 0.151(5) 0.608(5) -0.018(6) 0.139 Uiso 1 1 d D U . . .
H1BC H 0.194(8) 0.581(7) 0.0679(16) 0.139 Uiso 1 1 d D U . . .
H1BD H 0.266(4) 0.598(6) -0.006(6) 0.139 Uiso 1 1 d D U . . .
O1 O 0.6542(5) 0.6852(4) 0.1253(5) 0.062(2) Uani 1 1 d . . . . .
O2 O 0.5388(5) 0.5452(4) 0.1249(5) 0.063(2) Uani 1 1 d . . . . .
O3 O 0.5473(5) 0.6489(5) -0.0077(5) 0.070(2) Uani 1 1 d . . . . .
O4 O 0.4452(5) 0.6946(4) 0.1337(4) 0.0581(18) Uani 1 1 d . . . . .
C51 C 0.6771(9) 0.7608(8) 0.1219(11) 0.090(5) Uani 1 1 d . . . . .
H51A H 0.6509 0.7880 0.1623 0.108 Uiso 1 1 calc R U . . .
H51B H 0.6576 0.7825 0.0759 0.108 Uiso 1 1 calc R U . . .
C52 C 0.7758(10) 0.7611(10) 0.1272(10) 0.088(5) Uani 1 1 d . . . . .
H52A H 0.8030 0.7554 0.0792 0.106 Uiso 1 1 calc R U . . .
H52B H 0.7972 0.8063 0.1498 0.106 Uiso 1 1 calc R U . . .
C53 C 0.7927(8) 0.6958(10) 0.1746(8) 0.082(4) Uani 1 1 d . . . . .
H53A H 0.8523 0.6773 0.1681 0.099 Uiso 1 1 calc R U . . .
H53B H 0.7833 0.7075 0.2261 0.099 Uiso 1 1 calc R U . . .
C54 C 0.7275(7) 0.6432(7) 0.1480(8) 0.066(3) Uani 1 1 d . . . . .
H54A H 0.7511 0.6149 0.1072 0.080 Uiso 1 1 calc R U . . .
H54B H 0.7107 0.6092 0.1868 0.080 Uiso 1 1 calc R U . . .
C61 C 0.5686(11) 0.4895(6) 0.0799(8) 0.083(4) Uani 1 1 d . . . . .
H61A H 0.6252 0.5028 0.0587 0.099 Uiso 1 1 calc R U . . .
H61B H 0.5270 0.4812 0.0402 0.099 Uiso 1 1 calc R U . . .
C62 C 0.5776(10) 0.4223(7) 0.1243(9) 0.082(4) Uani 1 1 d . . . . .
H62A H 0.5280 0.3892 0.1166 0.098 Uiso 1 1 calc R U . . .
H62B H 0.6319 0.3963 0.1126 0.098 Uiso 1 1 calc R U . . .
C63 C 0.5791(9) 0.4491(8) 0.1984(9) 0.083(4) Uani 1 1 d . . . . .
H63A H 0.6390 0.4604 0.2136 0.100 Uiso 1 1 calc R U . . .
H63B H 0.5544 0.4127 0.2318 0.100 Uiso 1 1 calc R U . . .
C64 C 0.5247(8) 0.5163(7) 0.1972(7) 0.065(3) Uani 1 1 d . . . . .
H64A H 0.4629 0.5047 0.2051 0.078 Uiso 1 1 calc R U . . .
H64B H 0.5439 0.5512 0.2344 0.078 Uiso 1 1 calc R U . . .
C71 C 0.6183(9) 0.6768(11) -0.0496(8) 0.091(5) Uani 1 1 d . . . . .
H71A H 0.6722 0.6501 -0.0385 0.110 Uiso 1 1 calc R U . . .
H71B H 0.6275 0.7289 -0.0391 0.110 Uiso 1 1 calc R U . . .
C72 C 0.5941(9) 0.6667(9) -0.1247(8) 0.081(4) Uani 1 1 d . . . . .
H72A H 0.6165 0.6199 -0.1431 0.097 Uiso 1 1 calc R U . . .
H72B H 0.6175 0.7064 -0.1548 0.097 Uiso 1 1 calc R U . . .
C73 C 0.4966(8) 0.6674(8) -0.1254(8) 0.072(3) Uani 1 1 d . . . . .
H73A H 0.4742 0.7170 -0.1333 0.087 Uiso 1 1 calc R U . . .
H73B H 0.4737 0.6351 -0.1634 0.087 Uiso 1 1 calc R U . . .
C74 C 0.4732(9) 0.6407(12) -0.0534(9) 0.106(6) Uani 1 1 d . . . . .
H74A H 0.4238 0.6688 -0.0341 0.127 Uiso 1 1 calc R U . . .
H74B H 0.4560 0.5890 -0.0560 0.127 Uiso 1 1 calc R U . . .
C81 C 0.3668(7) 0.6591(6) 0.1507(9) 0.067(3) Uani 1 1 d . . . . .
H81A H 0.3721 0.6326 0.1967 0.080 Uiso 1 1 calc R U . . .
H81B H 0.3511 0.6243 0.1123 0.080 Uiso 1 1 calc R U . . .
C82 C 0.2998(10) 0.7175(9) 0.1566(14) 0.112(7) Uani 1 1 d . . . . .
H82A H 0.2522 0.7089 0.1219 0.135 Uiso 1 1 calc R U . . .
H82B H 0.2754 0.7190 0.2058 0.135 Uiso 1 1 calc R U . . .
C83 C 0.3409(11) 0.7796(9) 0.141(2) 0.175(15) Uani 1 1 d . . . . .
H83A H 0.3286 0.8154 0.1798 0.210 Uiso 1 1 calc R U . . .
H83B H 0.3181 0.7994 0.0955 0.210 Uiso 1 1 calc R U . . .
C84 C 0.4319(9) 0.7704(6) 0.1352(9) 0.074(4) Uani 1 1 d . . . . .
H84A H 0.4537 0.7932 0.0905 0.089 Uiso 1 1 calc R U . . .
H84B H 0.4620 0.7924 0.1769 0.089 Uiso 1 1 calc R U . . .
Li Li 0.5459(11) 0.6448(10) 0.0975(11) 0.056(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr N1 2.092(6) . ?
Zr N2 2.101(7) . ?
Zr B 2.370(13) . ?
Zr Cl1 2.465(5) . ?
Zr Cl2 2.497(4) . ?
Zr H1BA 2.12(12) . ?
Zr H1BB 2.12(11) . ?
Si N2 1.748(7) . ?
Si N1 1.755(7) . ?
Si C4 1.878(9) . ?
Si C1 1.913(14) . ?
N1 C11 1.436(10) . ?
N2 C31 1.431(11) . ?
C1 C3 1.422(18) . ?
C1 C2 1.530(19) . ?
C4 C5 1.551(14) . ?
C4 C6 1.552(15) . ?
C11 C12 1.367(12) . ?
C11 C16 1.438(12) . ?
C12 C13 1.362(13) . ?
C12 C17 1.530(15) . ?
C13 C14 1.396(17) . ?
C14 C15 1.379(17) . ?
C15 C16 1.396(14) . ?
C16 C20 1.501(14) . ?
C17 C19 1.522(16) . ?
C17 C18 1.54(2) . ?
C20 C21 1.525(17) . ?
C20 C22 1.568(15) . ?
C31 C32 1.419(16) . ?
C31 C36 1.432(16) . ?
C32 C33 1.388(17) . ?
C32 C37 1.490(16) . ?
C33 C34 1.41(2) . ?
C34 C35 1.36(3) . ?
C35 C36 1.39(2) . ?
C36 C40 1.53(2) . ?
C37 C39 1.510(17) . ?
C37 C38 1.540(14) . ?
C40 C41 1.48(2) . ?
C40 C42 1.561(18) . ?
B H1BA 1.099(13) . ?
B H1BB 1.100(13) . ?
B H1BC 1.095(13) . ?
B H1BD 1.095(13) . ?
O1 C54 1.435(14) . ?
O1 C51 1.439(15) . ?
O1 Li 1.904(19) . ?
O2 C61 1.403(14) . ?
O2 C64 1.461(15) . ?
O2 Li 1.91(2) . ?
O3 C74 1.435(15) . ?
O3 C71 1.439(15) . ?
O3 Li 1.95(2) . ?
O4 C84 1.413(13) . ?
O4 C81 1.414(13) . ?
O4 Li 1.93(2) . ?
C51 C52 1.53(2) . ?
C52 C53 1.51(2) . ?
C53 C54 1.484(17) . ?
C61 C62 1.496(18) . ?
C62 C63 1.46(2) . ?
C63 C64 1.498(17) . ?
C71 C72 1.46(2) . ?
C72 C73 1.506(18) . ?
C73 C74 1.47(2) . ?
C81 C82 1.496(17) . ?
C82 C83 1.34(2) . ?
C83 C84 1.42(2) . ?

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 Zr N2 73.5(3) . . ?
N1 Zr B 142.7(7) . . ?
N2 Zr B 97.5(5) . . ?
N1 Zr Cl1 110.5(3) . . ?
N2 Zr Cl1 102.8(2) . . ?
B Zr Cl1 106.8(7) . . ?
N1 Zr Cl2 84.9(2) . . ?
N2 Zr Cl2 155.1(2) . . ?
B Zr Cl2 92.3(5) . . ?
Cl1 Zr Cl2 96.13(18) . . ?
N1 Zr H1BA 115.1(7) . . ?
N2 Zr H1BA 90(3) . . ?
B Zr H1BA 27.6(4) . . ?
Cl1 Zr H1BA 134.4(7) . . ?
Cl2 Zr H1BA 88(3) . . ?
N1 Zr H1BB 154(3) . . ?
N2 Zr H1BB 121.8(18) . . ?
B Zr H1BB 27.6(4) . . ?
Cl1 Zr H1BB 87(2) . . ?
Cl2 Zr H1BB 75(3) . . ?
H1BA Zr H1BB 50.0(13) . . ?
N2 Si N1 91.5(3) . . ?
N2 Si C4 115.3(4) . . ?
N1 Si C4 114.5(4) . . ?
N2 Si C1 110.1(5) . . ?
N1 Si C1 117.6(6) . . ?
C4 Si C1 107.5(5) . . ?
C11 N1 Si 126.9(5) . . ?
C11 N1 Zr 134.5(5) . . ?
Si N1 Zr 96.7(3) . . ?
C31 N2 Si 124.9(6) . . ?
C31 N2 Zr 138.1(6) . . ?
Si N2 Zr 96.7(3) . . ?
C3 C1 C2 116.0(13) . . ?
C3 C1 Si 119.6(12) . . ?
C2 C1 Si 116.5(8) . . ?
C5 C4 C6 110.3(9) . . ?
C5 C4 Si 114.5(8) . . ?
C6 C4 Si 112.5(7) . . ?
C12 C11 N1 122.5(8) . . ?
C12 C11 C16 119.1(8) . . ?
N1 C11 C16 118.4(7) . . ?
C13 C12 C11 121.9(10) . . ?
C13 C12 C17 116.8(9) . . ?
C11 C12 C17 121.2(8) . . ?
C12 C13 C14 120.7(11) . . ?
C15 C14 C13 118.7(9) . . ?
C14 C15 C16 121.9(10) . . ?
C15 C16 C11 117.8(9) . . ?
C15 C16 C20 117.6(9) . . ?
C11 C16 C20 124.4(8) . . ?
C19 C17 C12 112.9(9) . . ?
C19 C17 C18 107.2(10) . . ?
C12 C17 C18 112.2(12) . . ?
C16 C20 C21 115.8(11) . . ?
C16 C20 C22 111.8(9) . . ?
C21 C20 C22 106.8(9) . . ?
C32 C31 N2 120.5(9) . . ?
C32 C31 C36 120.1(10) . . ?
N2 C31 C36 119.4(11) . . ?
C33 C32 C31 119.6(12) . . ?
C33 C32 C37 118.3(12) . . ?
C31 C32 C37 122.0(9) . . ?
C32 C33 C34 120.2(16) . . ?
C35 C34 C33 118.9(14) . . ?
C34 C35 C36 124.5(15) . . ?
C35 C36 C31 116.2(14) . . ?
C35 C36 C40 119.5(13) . . ?
C31 C36 C40 124.2(11) . . ?
C32 C37 C39 116.1(11) . . ?
C32 C37 C38 107.6(10) . . ?
C39 C37 C38 109.9(10) . . ?
C41 C40 C36 110.0(12) . . ?
C41 C40 C42 108.3(13) . . ?
C36 C40 C42 110.9(16) . . ?
Zr B H1BA 63(6) . . ?
Zr B H1BB 63(6) . . ?
Zr B H1BC 86(6) . . ?
Zr B H1BD 164(6) . . ?
H1BA B H1BB 109.1(15) . . ?
H1BA B H1BC 109.4(15) . . ?
H1BA B H1BD 109.6(16) . . ?
H1BB B H1BC 109.4(16) . . ?
H1BB B H1BD 109.3(15) . . ?
H1BC B H1BD 110.1(16) . . ?
C54 O1 C51 110.1(10) . . ?
C54 O1 Li 124.2(9) . . ?
C51 O1 Li 125.6(10) . . ?
C61 O2 C64 109.1(9) . . ?
C61 O2 Li 121.9(10) . . ?
C64 O2 Li 127.2(9) . . ?
C74 O3 C71 109.0(10) . . ?
C74 O3 Li 125.4(10) . . ?
C71 O3 Li 124.2(10) . . ?
C84 O4 C81 109.2(9) . . ?
C84 O4 Li 126.6(9) . . ?
C81 O4 Li 123.3(8) . . ?
O1 C51 C52 104.2(12) . . ?
C53 C52 C51 101.9(12) . . ?
C54 C53 C52 102.1(11) . . ?
O1 C54 C53 106.2(11) . . ?
O2 C61 C62 108.1(12) . . ?
C63 C62 C61 103.9(12) . . ?
C62 C63 C64 104.9(12) . . ?
O2 C64 C63 103.5(10) . . ?
O3 C71 C72 106.1(11) . . ?
C71 C72 C73 105.2(12) . . ?
C74 C73 C72 103.7(12) . . ?
O3 C74 C73 107.8(11) . . ?
O4 C81 C82 106.0(11) . . ?
C83 C82 C81 105.9(14) . . ?
C82 C83 C84 112.5(13) . . ?
O4 C84 C83 105.4(12) . . ?
O1 Li O2 110.8(9) . . ?
O1 Li O4 115.3(10) . . ?
O2 Li O4 108.6(10) . . ?
O1 Li O3 104.3(10) . . ?
O2 Li O3 107.7(10) . . ?
O4 Li O3 109.8(9) . . ?

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
N2 Si N1 C11 155.6(7) . . . . ?
C4 Si N1 C11 36.9(8) . . . . ?
C1 Si N1 C11 -90.7(8) . . . . ?
N2 Si N1 Zr -10.5(3) . . . . ?
C4 Si N1 Zr -129.2(4) . . . . ?
C1 Si N1 Zr 103.2(5) . . . . ?
N2 Zr N1 C11 -155.3(8) . . . . ?
B Zr N1 C11 -74.7(11) . . . . ?
Cl1 Zr N1 C11 107.0(7) . . . . ?
Cl2 Zr N1 C11 12.3(7) . . . . ?
N2 Zr N1 Si 9.1(3) . . . . ?
B Zr N1 Si 89.6(9) . . . . ?
Cl1 Zr N1 Si -88.7(3) . . . . ?
Cl2 Zr N1 Si 176.7(3) . . . . ?
N1 Si N2 C31 -164.0(8) . . . . ?
C4 Si N2 C31 -46.0(9) . . . . ?
C1 Si N2 C31 75.8(9) . . . . ?
N1 Si N2 Zr 10.5(3) . . . . ?
C4 Si N2 Zr 128.5(4) . . . . ?
C1 Si N2 Zr -109.7(6) . . . . ?
N1 Zr N2 C31 164.1(10) . . . . ?
B Zr N2 C31 21.2(12) . . . . ?
Cl1 Zr N2 C31 -88.0(10) . . . . ?
Cl2 Zr N2 C31 133.6(9) . . . . ?
N1 Zr N2 Si -9.1(3) . . . . ?
B Zr N2 Si -152.1(7) . . . . ?
Cl1 Zr N2 Si 98.7(3) . . . . ?
Cl2 Zr N2 Si -39.6(7) . . . . ?
N2 Si C1 C3 -149.9(15) . . . . ?
N1 Si C1 C3 107.2(15) . . . . ?
C4 Si C1 C3 -23.6(18) . . . . ?
N2 Si C1 C2 62.2(14) . . . . ?
N1 Si C1 C2 -40.7(14) . . . . ?
C4 Si C1 C2 -171.5(11) . . . . ?
N2 Si C4 C5 -166.2(8) . . . . ?
N1 Si C4 C5 -61.9(10) . . . . ?
C1 Si C4 C5 70.6(11) . . . . ?
N2 Si C4 C6 66.9(10) . . . . ?
N1 Si C4 C6 171.1(8) . . . . ?
C1 Si C4 C6 -56.3(11) . . . . ?
Si N1 C11 C12 97.3(9) . . . . ?
Zr N1 C11 C12 -102.3(9) . . . . ?
Si N1 C11 C16 -85.6(9) . . . . ?
Zr N1 C11 C16 74.9(10) . . . . ?
N1 C11 C12 C13 176.4(9) . . . . ?
C16 C11 C12 C13 -0.8(14) . . . . ?
N1 C11 C12 C17 1.2(14) . . . . ?
C16 C11 C12 C17 -176.0(9) . . . . ?
C11 C12 C13 C14 2.3(16) . . . . ?
C17 C12 C13 C14 177.7(10) . . . . ?
C12 C13 C14 C15 -2.2(17) . . . . ?
C13 C14 C15 C16 0.8(16) . . . . ?
C14 C15 C16 C11 0.7(15) . . . . ?
C14 C15 C16 C20 -174.8(10) . . . . ?
C12 C11 C16 C15 -0.7(13) . . . . ?
N1 C11 C16 C15 -178.0(8) . . . . ?
C12 C11 C16 C20 174.4(9) . . . . ?
N1 C11 C16 C20 -2.8(14) . . . . ?
C13 C12 C17 C19 54.6(15) . . . . ?
C11 C12 C17 C19 -130.0(11) . . . . ?
C13 C12 C17 C18 -66.7(13) . . . . ?
C11 C12 C17 C18 108.7(11) . . . . ?
C15 C16 C20 C21 63.0(12) . . . . ?
C11 C16 C20 C21 -112.2(11) . . . . ?
C15 C16 C20 C22 -59.6(14) . . . . ?
C11 C16 C20 C22 125.2(11) . . . . ?
Si N2 C31 C32 -95.3(10) . . . . ?
Zr N2 C31 C32 92.9(13) . . . . ?
Si N2 C31 C36 86.2(12) . . . . ?
Zr N2 C31 C36 -85.6(12) . . . . ?
N2 C31 C32 C33 172.6(11) . . . . ?
C36 C31 C32 C33 -8.9(17) . . . . ?
N2 C31 C32 C37 -11.5(15) . . . . ?
C36 C31 C32 C37 167.0(11) . . . . ?
C31 C32 C33 C34 5.6(19) . . . . ?
C37 C32 C33 C34 -170.4(12) . . . . ?
C32 C33 C34 C35 -1(2) . . . . ?
C33 C34 C35 C36 0(3) . . . . ?
C34 C35 C36 C31 -4(2) . . . . ?
C34 C35 C36 C40 174.0(16) . . . . ?
C32 C31 C36 C35 7.7(17) . . . . ?
N2 C31 C36 C35 -173.8(11) . . . . ?
C32 C31 C36 C40 -169.8(11) . . . . ?
N2 C31 C36 C40 8.8(17) . . . . ?
C33 C32 C37 C39 -50.6(15) . . . . ?
C31 C32 C37 C39 133.5(12) . . . . ?
C33 C32 C37 C38 73.0(14) . . . . ?
C31 C32 C37 C38 -102.9(12) . . . . ?
C35 C36 C40 C41 -66.1(18) . . . . ?
C31 C36 C40 C41 111.2(15) . . . . ?
C35 C36 C40 C42 53.6(17) . . . . ?
C31 C36 C40 C42 -129.0(13) . . . . ?
C54 O1 C51 C52 12.8(17) . . . . ?
Li O1 C51 C52 -163.0(12) . . . . ?
O1 C51 C52 C53 -32.0(17) . . . . ?
C51 C52 C53 C54 38.9(16) . . . . ?
C51 O1 C54 C53 12.3(16) . . . . ?
Li O1 C54 C53 -171.9(11) . . . . ?
C52 C53 C54 O1 -32.2(15) . . . . ?
C64 O2 C61 C62 -2.1(16) . . . . ?
Li O2 C61 C62 163.9(11) . . . . ?
O2 C61 C62 C63 -18.0(17) . . . . ?
C61 C62 C63 C64 30.5(16) . . . . ?
C61 O2 C64 C63 20.9(13) . . . . ?
Li O2 C64 C63 -144.2(11) . . . . ?
C62 C63 C64 O2 -31.9(14) . . . . ?
C74 O3 C71 C72 -15.4(19) . . . . ?
Li O3 C71 C72 177.5(12) . . . . ?
O3 C71 C72 C73 26.9(19) . . . . ?
C71 C72 C73 C74 -28.1(19) . . . . ?
C71 O3 C74 C73 -3(2) . . . . ?
Li O3 C74 C73 164.2(12) . . . . ?
C72 C73 C74 O3 19(2) . . . . ?
C84 O4 C81 C82 5.1(18) . . . . ?
Li O4 C81 C82 -164.6(14) . . . . ?
O4 C81 C82 C83 2(3) . . . . ?
C81 C82 C83 C84 -8(3) . . . . ?
C81 O4 C84 C83 -10(2) . . . . ?
Li O4 C84 C83 159.6(18) . . . . ?
C82 C83 C84 O4 11(3) . . . . ?
C54 O1 Li O2 13.6(17) . . . . ?
C51 O1 Li O2 -171.2(12) . . . . ?
C54 O1 Li O4 137.5(12) . . . . ?
C51 O1 Li O4 -47.3(18) . . . . ?
C54 O1 Li O3 -102.0(12) . . . . ?
C51 O1 Li O3 73.2(16) . . . . ?
C61 O2 Li O1 -88.1(14) . . . . ?
C64 O2 Li O1 75.2(14) . . . . ?
C61 O2 Li O4 144.3(12) . . . . ?
C64 O2 Li O4 -52.4(14) . . . . ?
C61 O2 Li O3 25.3(15) . . . . ?
C64 O2 Li O3 -171.3(9) . . . . ?
C84 O4 Li O1 44.3(17) . . . . ?
C81 O4 Li O1 -147.9(12) . . . . ?
C84 O4 Li O2 169.3(11) . . . . ?
C81 O4 Li O2 -22.9(16) . . . . ?
C84 O4 Li O3 -73.2(15) . . . . ?
C81 O4 Li O3 94.7(13) . . . . ?
C74 O3 Li O1 -164.6(13) . . . . ?
C71 O3 Li O1 0.4(16) . . . . ?
C74 O3 Li O2 77.7(16) . . . . ?
C71 O3 Li O2 -117.3(13) . . . . ?
C74 O3 Li O4 -40.5(18) . . . . ?
C71 O3 Li O4 124.6(13) . . . . ?

_refine_diff_density_max         0.760
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.106

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_riv1267
_database_code_depnum_ccdc_archive 'CCDC 1043229'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;

_vrf_CHEMW03_riv1267             
;
RESPONSE: The reported formula and weight contain contributions from the
disordered tetrahydrofuran solvent molecules that were removed by use of the
SQUEEZE routine as implemented in PLATON.  See _platon_squeeze_details in
this CIF for further details.
;

_vrf_PLAT043_riv1267             
;
RESPONSE: see response to CHEMW03
;

_vrf_PLAT041_riv1267             
;
RESPONSE: see response to CHEMW03
;

_vrf_PLAT068_riv1267             
;
RESPONSE: see response to CHEMW03
;

_vrf_FORMU01_riv1267             
;
RESPONSE: see response to CHEMW03
;

_vrf_CELLZ01_riv1267             
;
RESPONSE: see response to CHEMW03
;

_vrf_PLAT605_riv1267             
;
RESPONSE: see response to CHEMW03
;

_vrf_PLAT869_riv1267             
;
RESPONSE: see response to CHEMW03
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H66 B2 N4 Si Zr,0.5(C4 H8 O)'
_chemical_formula_sum            'C39 H70 B2 N4 O0.50 Si Zr'
_chemical_formula_weight         743.92

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   10.8302(4)
_cell_length_b                   16.9778(7)
_cell_length_c                   23.5656(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.9980(10)
_cell_angle_gamma                90.00
_cell_volume                     4330.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9904
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      23.22

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1600
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8671
_exptl_absorpt_correction_T_max  0.9815
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34513
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.73
_diffrn_reflns_theta_max         26.46
_reflns_number_total             8913
_reflns_number_gt                7012
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0459P)²+0.6651P] 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         8913
_refine_ls_number_parameters     441
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_ref         0.0967
_refine_ls_wR_factor_gt          0.0913
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.007
_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
Zr Zr 0.362311(17) 0.308960(11) 0.231738(8) 0.02226(7) Uani 1 1 d . . .
Si Si 0.17807(5) 0.42742(3) 0.24870(2) 0.02568(14) Uani 1 1 d . . .
N1 N 0.26044(15) 0.39762(10) 0.18933(7) 0.0237(4) Uani 1 1 d . . .
N2 N 0.27656(15) 0.37259(9) 0.29445(7) 0.0232(4) Uani 1 1 d . . .
N3 N 0.47117(16) 0.29473(10) 0.14581(7) 0.0265(4) Uani 1 1 d . . .
N4 N 0.6296(2) 0.25850(17) -0.01175(9) 0.0581(7) Uani 1 1 d . . .
C1 C 0.1836(2) 0.53720(13) 0.25962(10) 0.0390(6) Uani 1 1 d . . .
H1 H 0.2731 0.5514 0.2638 0.047 Uiso 1 1 calc R . .
C2 C 0.1310(3) 0.58578(15) 0.20882(12) 0.0523(7) Uani 1 1 d . . .
H2A H 0.1348 0.6420 0.2182 0.063 Uiso 1 1 calc R . .
H2B H 0.0448 0.5706 0.2007 0.063 Uiso 1 1 calc R . .
H2C H 0.1798 0.5756 0.1754 0.063 Uiso 1 1 calc R . .
C3 C 0.1243(3) 0.56380(17) 0.31479(12) 0.0562(8) Uani 1 1 d . . .
H3A H 0.1295 0.6213 0.3180 0.067 Uiso 1 1 calc R . .
H3B H 0.1682 0.5395 0.3474 0.067 Uiso 1 1 calc R . .
H3C H 0.0374 0.5476 0.3141 0.067 Uiso 1 1 calc R . .
C4 C 0.0130(2) 0.39295(14) 0.25875(11) 0.0383(6) Uani 1 1 d . . .
H4 H 0.0064 0.3929 0.3010 0.046 Uiso 1 1 calc R . .
C5 C -0.0222(2) 0.30837(14) 0.24238(11) 0.0433(6) Uani 1 1 d . . .
H5A H -0.1079 0.2983 0.2523 0.052 Uiso 1 1 calc R . .
H5B H 0.0327 0.2715 0.2630 0.052 Uiso 1 1 calc R . .
H5C H -0.0138 0.3012 0.2014 0.052 Uiso 1 1 calc R . .
C6 C -0.0938(2) 0.44654(19) 0.23898(13) 0.0584(8) Uani 1 1 d . . .
H6A H -0.1724 0.4227 0.2492 0.070 Uiso 1 1 calc R . .
H6B H -0.0925 0.4532 0.1977 0.070 Uiso 1 1 calc R . .
H6C H -0.0848 0.4981 0.2574 0.070 Uiso 1 1 calc R . .
C11 C 0.26918(19) 0.43504(11) 0.13545(8) 0.0250(4) Uani 1 1 d . . .
C12 C 0.1760(2) 0.42531(13) 0.09294(9) 0.0329(5) Uani 1 1 d . . .
C13 C 0.1937(2) 0.45546(16) 0.03898(10) 0.0450(6) Uani 1 1 d . . .
H13 H 0.1318 0.4472 0.0101 0.054 Uiso 1 1 calc R . .
C14 C 0.2977(3) 0.49662(17) 0.02627(11) 0.0512(7) Uani 1 1 d . . .
H14 H 0.3081 0.5162 -0.0110 0.061 Uiso 1 1 calc R . .
C15 C 0.3869(2) 0.50931(15) 0.06830(10) 0.0407(6) Uani 1 1 d . . .
H15 H 0.4581 0.5391 0.0598 0.049 Uiso 1 1 calc R . .
C16 C 0.3755(2) 0.47961(12) 0.12298(9) 0.0295(5) Uani 1 1 d . . .
C17 C 0.0571(2) 0.38233(14) 0.10428(10) 0.0371(6) Uani 1 1 d . . .
H17 H 0.0515 0.3777 0.1464 0.045 Uiso 1 1 calc R . .
C18 C 0.0541(3) 0.29950(16) 0.08032(14) 0.0560(8) Uani 1 1 d . . .
H18A H 0.1256 0.2699 0.0955 0.067 Uiso 1 1 calc R . .
H18B H 0.0569 0.3018 0.0388 0.067 Uiso 1 1 calc R . .
H18C H -0.0221 0.2732 0.0911 0.067 Uiso 1 1 calc R . .
C19 C -0.0567(2) 0.42798(18) 0.08259(12) 0.0545(7) Uani 1 1 d . . .
H19A H -0.0571 0.4803 0.1002 0.065 Uiso 1 1 calc R . .
H19B H -0.1315 0.3994 0.0925 0.065 Uiso 1 1 calc R . .
H19C H -0.0544 0.4335 0.0413 0.065 Uiso 1 1 calc R . .
C20 C 0.4773(2) 0.49903(13) 0.16685(10) 0.0366(6) Uani 1 1 d . . .
H20 H 0.4666 0.4639 0.2004 0.044 Uiso 1 1 calc R . .
C21 C 0.4680(3) 0.58404(16) 0.18712(12) 0.0553(8) Uani 1 1 d . . .
H21A H 0.3873 0.5925 0.2036 0.066 Uiso 1 1 calc R . .
H21B H 0.4772 0.6198 0.1549 0.066 Uiso 1 1 calc R . .
H21C H 0.5336 0.5945 0.2159 0.066 Uiso 1 1 calc R . .
C22 C 0.6066(2) 0.48555(17) 0.14548(14) 0.0593(8) Uani 1 1 d . . .
H22A H 0.6132 0.4315 0.1313 0.071 Uiso 1 1 calc R . .
H22B H 0.6675 0.4937 0.1767 0.071 Uiso 1 1 calc R . .
H22C H 0.6223 0.5227 0.1147 0.071 Uiso 1 1 calc R . .
C31 C 0.29080(19) 0.37948(12) 0.35510(8) 0.0258(4) Uani 1 1 d . . .
C32 C 0.3734(2) 0.43622(13) 0.37922(9) 0.0322(5) Uani 1 1 d . . .
C33 C 0.3844(2) 0.44260(15) 0.43806(10) 0.0442(6) Uani 1 1 d . . .
H33 H 0.4388 0.4811 0.4543 0.053 Uiso 1 1 calc R . .
C34 C 0.3194(3) 0.39517(16) 0.47338(10) 0.0480(7) Uani 1 1 d . . .
H34 H 0.3276 0.4013 0.5134 0.058 Uiso 1 1 calc R . .
C35 C 0.2419(2) 0.33853(15) 0.45009(10) 0.0397(6) Uani 1 1 d . . .
H35 H 0.1975 0.3052 0.4745 0.048 Uiso 1 1 calc R . .
C36 C 0.2273(2) 0.32898(13) 0.39148(9) 0.0283(5) Uani 1 1 d . . .
C37 C 0.4556(2) 0.48931(14) 0.34499(10) 0.0421(6) Uani 1 1 d . . .
H37 H 0.4339 0.4810 0.3038 0.051 Uiso 1 1 calc R . .
C38 C 0.5913(2) 0.46865(18) 0.35493(12) 0.0574(8) Uani 1 1 d . . .
H38A H 0.6050 0.4136 0.3442 0.069 Uiso 1 1 calc R . .
H38B H 0.6145 0.4759 0.3952 0.069 Uiso 1 1 calc R . .
H38C H 0.6420 0.5031 0.3318 0.069 Uiso 1 1 calc R . .
C39 C 0.4373(3) 0.57718(16) 0.35847(12) 0.0577(8) Uani 1 1 d . . .
H39A H 0.3519 0.5924 0.3486 0.069 Uiso 1 1 calc R . .
H39B H 0.4940 0.6088 0.3363 0.069 Uiso 1 1 calc R . .
H39C H 0.4542 0.5863 0.3991 0.069 Uiso 1 1 calc R . .
C40 C 0.1469(2) 0.26146(13) 0.36990(10) 0.0316(5) Uani 1 1 d . . .
H40 H 0.1411 0.2650 0.3275 0.038 Uiso 1 1 calc R . .
C41 C 0.2064(3) 0.18220(14) 0.38548(12) 0.0460(6) Uani 1 1 d . . .
H41A H 0.2879 0.1788 0.3688 0.055 Uiso 1 1 calc R . .
H41B H 0.1538 0.1393 0.3708 0.055 Uiso 1 1 calc R . .
H41C H 0.2156 0.1778 0.4269 0.055 Uiso 1 1 calc R . .
C42 C 0.0151(2) 0.26469(17) 0.39166(11) 0.0475(7) Uani 1 1 d . . .
H42A H -0.0242 0.3142 0.3796 0.057 Uiso 1 1 calc R . .
H42B H 0.0181 0.2616 0.4332 0.057 Uiso 1 1 calc R . .
H42C H -0.0328 0.2203 0.3760 0.057 Uiso 1 1 calc R . .
C51 C 0.4044(2) 0.28765(13) 0.09686(9) 0.0307(5) Uani 1 1 d . . .
H51 H 0.3171 0.2913 0.0988 0.037 Uiso 1 1 calc R . .
C52 C 0.4518(2) 0.27575(14) 0.04488(9) 0.0329(5) Uani 1 1 d . . .
H52 H 0.3979 0.2720 0.0123 0.039 Uiso 1 1 calc R . .
C53 C 0.5795(2) 0.26898(15) 0.03915(10) 0.0365(5) Uani 1 1 d . . .
C54 C 0.6492(2) 0.27390(16) 0.09040(10) 0.0420(6) Uani 1 1 d . . .
H54 H 0.7365 0.2685 0.0901 0.050 Uiso 1 1 calc R . .
C55 C 0.5937(2) 0.28629(14) 0.14047(10) 0.0340(5) Uani 1 1 d . . .
H55 H 0.6449 0.2892 0.1740 0.041 Uiso 1 1 calc R . .
C56 C 0.5561(3) 0.2542(2) -0.06369(11) 0.0598(8) Uani 1 1 d . . .
H56A H 0.5036 0.2071 -0.0631 0.072 Uiso 1 1 calc R . .
H56B H 0.6105 0.2511 -0.0960 0.072 Uiso 1 1 calc R . .
H56C H 0.5040 0.3012 -0.0674 0.072 Uiso 1 1 calc R . .
C57 C 0.7617(3) 0.2578(4) -0.01701(16) 0.143(2) Uani 1 1 d . . .
H57A H 0.7959 0.2095 0.0002 0.172 Uiso 1 1 calc R . .
H57B H 0.7978 0.3037 0.0025 0.172 Uiso 1 1 calc R . .
H57C H 0.7814 0.2595 -0.0573 0.172 Uiso 1 1 calc R . .
B1 B 0.2631(3) 0.18474(16) 0.22314(13) 0.0390(7) Uani 1 1 d D . .
H1BA H 0.2157(18) 0.2351(9) 0.2023(8) 0.054(8) Uiso 1 1 d D . .
H1BB H 0.3546(13) 0.1794(12) 0.2034(8) 0.046(7) Uiso 1 1 d D . .
H1BC H 0.2834(19) 0.2042(12) 0.2676(5) 0.046(7) Uiso 1 1 d D . .
H1BD H 0.2120(18) 0.1305(9) 0.2208(9) 0.065(8) Uiso 1 1 d D . .
B2 B 0.5566(3) 0.28985(18) 0.27994(12) 0.0368(6) Uani 1 1 d D . .
H2BA H 0.5337(17) 0.2431(9) 0.2483(7) 0.034(6) Uiso 1 1 d D . .
H2BB H 0.5410(17) 0.3456(8) 0.2558(8) 0.040(6) Uiso 1 1 d D . .
H2BC H 0.4813(15) 0.2885(12) 0.3102(7) 0.040(6) Uiso 1 1 d D . .
H2BD H 0.6487(12) 0.2848(13) 0.2986(9) 0.053(7) Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr N2 2.0758(16) . ?
Zr N1 2.0988(16) . ?
Zr B1 2.372(3) . ?
Zr B2 2.378(3) . ?
Zr N3 2.3907(17) . ?
Si N2 1.7569(17) . ?
Si N1 1.7596(17) . ?
Si C1 1.882(2) . ?
Si C4 1.904(2) . ?
N1 C11 1.426(2) . ?
N2 C31 1.437(3) . ?
N3 C55 1.345(3) . ?
N3 C51 1.345(3) . ?
N4 C53 1.345(3) . ?
N4 C56 1.439(3) . ?
N4 C57 1.441(4) . ?
C1 C3 1.538(3) . ?
C1 C2 1.546(3) . ?
C4 C6 1.531(3) . ?
C4 C5 1.532(3) . ?
C11 C12 1.407(3) . ?
C11 C16 1.417(3) . ?
C12 C13 1.390(3) . ?
C12 C17 1.512(3) . ?
C13 C14 1.367(4) . ?
C14 C15 1.376(3) . ?
C15 C16 1.393(3) . ?
C16 C20 1.521(3) . ?
C17 C18 1.515(3) . ?
C17 C19 1.529(3) . ?
C20 C22 1.521(4) . ?
C20 C21 1.525(3) . ?
C31 C36 1.409(3) . ?
C31 C32 1.420(3) . ?
C32 C33 1.392(3) . ?
C32 C37 1.518(3) . ?
C33 C34 1.370(3) . ?
C34 C35 1.378(4) . ?
C35 C36 1.394(3) . ?
C36 C40 1.516(3) . ?
C37 C38 1.522(4) . ?
C37 C39 1.540(4) . ?
C40 C41 1.531(3) . ?
C40 C42 1.535(3) . ?
C51 C52 1.360(3) . ?
C52 C53 1.399(3) . ?
C53 C54 1.404(3) . ?
C54 C55 1.359(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Zr N1 74.03(6) . . ?
N2 Zr B1 108.12(8) . . ?
N1 Zr B1 111.59(9) . . ?
N2 Zr B2 98.12(8) . . ?
N1 Zr B2 140.08(9) . . ?
B1 Zr B2 108.06(10) . . ?
N2 Zr N3 154.38(6) . . ?
N1 Zr N3 86.31(6) . . ?
B1 Zr N3 94.19(8) . . ?
B2 Zr N3 86.36(8) . . ?
N2 Si N1 91.25(8) . . ?
N2 Si C1 115.15(10) . . ?
N1 Si C1 112.26(10) . . ?
N2 Si C4 108.27(10) . . ?
N1 Si C4 120.99(10) . . ?
C1 Si C4 108.24(11) . . ?
C11 N1 Si 129.14(13) . . ?
C11 N1 Zr 133.90(13) . . ?
Si N1 Zr 95.76(7) . . ?
C31 N2 Si 127.52(13) . . ?
C31 N2 Zr 135.67(13) . . ?
Si N2 Zr 96.66(8) . . ?
C55 N3 C51 114.38(18) . . ?
C55 N3 Zr 127.40(14) . . ?
C51 N3 Zr 117.97(14) . . ?
C53 N4 C56 122.5(2) . . ?
C53 N4 C57 120.7(2) . . ?
C56 N4 C57 116.6(2) . . ?
C3 C1 C2 110.1(2) . . ?
C3 C1 Si 113.21(18) . . ?
C2 C1 Si 114.40(17) . . ?
C6 C4 C5 107.6(2) . . ?
C6 C4 Si 118.82(18) . . ?
C5 C4 Si 118.89(16) . . ?
C12 C11 C16 118.89(19) . . ?
C12 C11 N1 120.90(19) . . ?
C16 C11 N1 120.14(18) . . ?
C13 C12 C11 119.3(2) . . ?
C13 C12 C17 119.0(2) . . ?
C11 C12 C17 121.7(2) . . ?
C14 C13 C12 122.0(2) . . ?
C13 C14 C15 119.0(2) . . ?
C14 C15 C16 121.8(2) . . ?
C15 C16 C11 118.9(2) . . ?
C15 C16 C20 117.7(2) . . ?
C11 C16 C20 123.36(19) . . ?
C12 C17 C18 112.9(2) . . ?
C12 C17 C19 112.2(2) . . ?
C18 C17 C19 109.8(2) . . ?
C22 C20 C16 113.3(2) . . ?
C22 C20 C21 108.5(2) . . ?
C16 C20 C21 111.3(2) . . ?
C36 C31 C32 118.92(19) . . ?
C36 C31 N2 121.19(18) . . ?
C32 C31 N2 119.85(18) . . ?
C33 C32 C31 118.9(2) . . ?
C33 C32 C37 116.8(2) . . ?
C31 C32 C37 124.3(2) . . ?
C34 C33 C32 122.1(2) . . ?
C33 C34 C35 119.1(2) . . ?
C34 C35 C36 121.5(2) . . ?
C35 C36 C31 119.4(2) . . ?
C35 C36 C40 117.7(2) . . ?
C31 C36 C40 122.88(19) . . ?
C32 C37 C38 111.3(2) . . ?
C32 C37 C39 112.6(2) . . ?
C38 C37 C39 108.8(2) . . ?
C36 C40 C41 110.63(19) . . ?
C36 C40 C42 113.00(19) . . ?
C41 C40 C42 109.9(2) . . ?
N3 C51 C52 125.2(2) . . ?
C51 C52 C53 120.3(2) . . ?
N4 C53 C52 121.8(2) . . ?
N4 C53 C54 123.6(2) . . ?
C52 C53 C54 114.6(2) . . ?
C55 C54 C53 121.0(2) . . ?
N3 C55 C54 124.4(2) . . ?

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
N2 Si N1 C11 -156.48(18) . . . . ?
C1 Si N1 C11 -38.6(2) . . . . ?
C4 Si N1 C11 91.26(19) . . . . ?
N2 Si N1 Zr 12.20(8) . . . . ?
C1 Si N1 Zr 130.12(10) . . . . ?
C4 Si N1 Zr -100.06(10) . . . . ?
N2 Zr N1 C11 157.08(19) . . . . ?
B1 Zr N1 C11 -99.35(19) . . . . ?
B2 Zr N1 C11 73.6(2) . . . . ?
N3 Zr N1 C11 -6.29(18) . . . . ?
N2 Zr N1 Si -10.72(7) . . . . ?
B1 Zr N1 Si 92.85(10) . . . . ?
B2 Zr N1 Si -94.23(13) . . . . ?
N3 Zr N1 Si -174.10(8) . . . . ?
N1 Si N2 C31 163.73(17) . . . . ?
C1 Si N2 C31 48.3(2) . . . . ?
C4 Si N2 C31 -72.94(19) . . . . ?
N1 Si N2 Zr -12.36(8) . . . . ?
C1 Si N2 Zr -127.75(10) . . . . ?
C4 Si N2 Zr 110.98(10) . . . . ?
N1 Zr N2 C31 -164.8(2) . . . . ?
B1 Zr N2 C31 87.2(2) . . . . ?
B2 Zr N2 C31 -24.9(2) . . . . ?
N3 Zr N2 C31 -123.49(19) . . . . ?
N1 Zr N2 Si 10.75(7) . . . . ?
B1 Zr N2 Si -97.25(10) . . . . ?
B2 Zr N2 Si 150.66(9) . . . . ?
N3 Zr N2 Si 52.06(17) . . . . ?
N2 Zr N3 C55 97.0(2) . . . . ?
N1 Zr N3 C55 136.49(18) . . . . ?
B1 Zr N3 C55 -112.11(19) . . . . ?
B2 Zr N3 C55 -4.24(19) . . . . ?
N2 Zr N3 C51 -89.0(2) . . . . ?
N1 Zr N3 C51 -49.53(15) . . . . ?
B1 Zr N3 C51 61.87(17) . . . . ?
B2 Zr N3 C51 169.74(17) . . . . ?
N2 Si C1 C3 -71.2(2) . . . . ?
N1 Si C1 C3 -173.80(17) . . . . ?
C4 Si C1 C3 50.1(2) . . . . ?
N2 Si C1 C2 161.51(18) . . . . ?
N1 Si C1 C2 58.9(2) . . . . ?
C4 Si C1 C2 -77.2(2) . . . . ?
N2 Si C4 C6 160.9(2) . . . . ?
N1 Si C4 C6 -96.1(2) . . . . ?
C1 Si C4 C6 35.5(2) . . . . ?
N2 Si C4 C5 -64.9(2) . . . . ?
N1 Si C4 C5 38.1(2) . . . . ?
C1 Si C4 C5 169.70(18) . . . . ?
Si N1 C11 C12 -81.8(2) . . . . ?
Zr N1 C11 C12 114.0(2) . . . . ?
Si N1 C11 C16 101.4(2) . . . . ?
Zr N1 C11 C16 -62.9(3) . . . . ?
C16 C11 C12 C13 3.9(3) . . . . ?
N1 C11 C12 C13 -173.0(2) . . . . ?
C16 C11 C12 C17 -176.6(2) . . . . ?
N1 C11 C12 C17 6.5(3) . . . . ?
C11 C12 C13 C14 -2.1(4) . . . . ?
C17 C12 C13 C14 178.3(2) . . . . ?
C12 C13 C14 C15 -0.7(4) . . . . ?
C13 C14 C15 C16 1.7(4) . . . . ?
C14 C15 C16 C11 0.1(4) . . . . ?
C14 C15 C16 C20 -178.2(2) . . . . ?
C12 C11 C16 C15 -2.9(3) . . . . ?
N1 C11 C16 C15 174.0(2) . . . . ?
C12 C11 C16 C20 175.3(2) . . . . ?
N1 C11 C16 C20 -7.8(3) . . . . ?
C13 C12 C17 C18 76.6(3) . . . . ?
C11 C12 C17 C18 -102.9(3) . . . . ?
C13 C12 C17 C19 -48.1(3) . . . . ?
C11 C12 C17 C19 132.3(2) . . . . ?
C15 C16 C20 C22 -47.6(3) . . . . ?
C11 C16 C20 C22 134.1(2) . . . . ?
C15 C16 C20 C21 75.0(3) . . . . ?
C11 C16 C20 C21 -103.2(2) . . . . ?
Si N2 C31 C36 96.9(2) . . . . ?
Zr N2 C31 C36 -88.7(2) . . . . ?
Si N2 C31 C32 -85.3(2) . . . . ?
Zr N2 C31 C32 89.1(2) . . . . ?
C36 C31 C32 C33 -3.0(3) . . . . ?
N2 C31 C32 C33 179.1(2) . . . . ?
C36 C31 C32 C37 174.5(2) . . . . ?
N2 C31 C32 C37 -3.3(3) . . . . ?
C31 C32 C33 C34 0.9(4) . . . . ?
C37 C32 C33 C34 -176.9(2) . . . . ?
C32 C33 C34 C35 1.0(4) . . . . ?
C33 C34 C35 C36 -0.7(4) . . . . ?
C34 C35 C36 C31 -1.5(4) . . . . ?
C34 C35 C36 C40 175.9(2) . . . . ?
C32 C31 C36 C35 3.3(3) . . . . ?
N2 C31 C36 C35 -178.9(2) . . . . ?
C32 C31 C36 C40 -173.9(2) . . . . ?
N2 C31 C36 C40 3.9(3) . . . . ?
C33 C32 C37 C38 65.3(3) . . . . ?
C31 C32 C37 C38 -112.4(3) . . . . ?
C33 C32 C37 C39 -57.1(3) . . . . ?
C31 C32 C37 C39 125.2(2) . . . . ?
C35 C36 C40 C41 -66.4(3) . . . . ?
C31 C36 C40 C41 110.8(2) . . . . ?
C35 C36 C40 C42 57.2(3) . . . . ?
C31 C36 C40 C42 -125.5(2) . . . . ?
C55 N3 C51 C52 -2.2(3) . . . . ?
Zr N3 C51 C52 -176.99(18) . . . . ?
N3 C51 C52 C53 0.7(4) . . . . ?
C56 N4 C53 C52 0.5(4) . . . . ?
C57 N4 C53 C52 175.2(4) . . . . ?
C56 N4 C53 C54 -179.6(3) . . . . ?
C57 N4 C53 C54 -4.9(5) . . . . ?
C51 C52 C53 N4 -178.9(2) . . . . ?
C51 C52 C53 C54 1.2(4) . . . . ?
N4 C53 C54 C55 178.5(3) . . . . ?
C52 C53 C54 C55 -1.6(4) . . . . ?
C51 N3 C55 C54 1.9(3) . . . . ?
Zr N3 C55 C54 176.02(19) . . . . ?
C53 C54 C55 N3 0.0(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.46
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.055
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 239 40 ' '
2 0.000 0.500 0.500 239 40 ' '
3 0.050 0.604 0.062 12 1 ' '
4 0.050 0.896 0.562 12 1 ' '
5 0.950 0.104 0.438 12 1 ' '
6 0.950 0.396 0.938 12 1 ' '
_platon_squeeze_details          
;
Attempts to refine peaks of residual electron density as disordered or 
partial-occupancy solvent tetrahydrofuran oxygen or carbon atoms were 
unsuccessful.  The data were corrected for disordered electron density 
through use of the SQUEEZE procedure (Sluis, P. van der; Spek, A. L. 
Acta Crystallogr. 1990, A46, 194201) as implemented in PLATON (Spek, 
A. L. Acta Crystallogr. 1990, A46, C34; Spek, A. L. J. Appl. Cryst. 2003, 
36, 713.  PLATON - a multipurpose crystallographic tool.  Utrecht 
University, Utrecht, The Netherlands).  A total solvent-accessible void 
volume of 525 3 with a total electron count of 83 (consistent with 2 
molecules of solvent tetrahydrofuran, or 0.5 molecules per formula unit 
of the [{iPr2Si(NSiPh3)2}Zr(BH4)2(4-Me2N-pyridine)] molecule) was found 
in the unit cell
;
####################################################################### 
# 
# 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_riv1129
_database_code_depnum_ccdc_archive 'CCDC 1043230'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H62 N2 O Si Zr'
_chemical_formula_sum            'C36 H62 N2 O Si Zr'
_chemical_formula_weight         658.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   11.3162(4)
_cell_length_b                   13.2629(5)
_cell_length_c                   24.9183(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.8730(4)
_cell_angle_gamma                90.00
_cell_volume                     3726.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9193
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      27.43

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1416
_exptl_absorpt_coefficient_mu    0.355
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8883
_exptl_absorpt_correction_T_max  0.9084
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32860
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0153
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         27.55
_reflns_number_total             8605
_reflns_number_gt                7457
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0398P)²+1.3611P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8605
_refine_ls_number_parameters     376
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0272
_refine_ls_wR_factor_ref         0.0767
_refine_ls_wR_factor_gt          0.0726
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr Zr 0.410614(12) 0.232280(10) 0.406968(5) 0.02621(5) Uani 1 1 d . . .
Si Si 0.15910(3) 0.22931(3) 0.397592(14) 0.02180(8) Uani 1 1 d . . .
O O 0.53204(9) 0.11523(8) 0.36947(5) 0.0374(3) Uani 1 1 d . . .
N1 N 0.26592(10) 0.31935(8) 0.42171(4) 0.0238(2) Uani 1 1 d . . .
N2 N 0.26363(10) 0.15173(8) 0.37031(4) 0.0235(2) Uani 1 1 d . . .
C1 C 0.04234(13) 0.28188(11) 0.34674(6) 0.0306(3) Uani 1 1 d . . .
H1 H 0.0849 0.3243 0.3214 0.037 Uiso 1 1 calc R . .
C2 C -0.04383(15) 0.35262(14) 0.37340(8) 0.0433(4) Uani 1 1 d . . .
H2A H -0.0929 0.3889 0.3454 0.052 Uiso 1 1 calc R . .
H2B H 0.0016 0.4012 0.3965 0.052 Uiso 1 1 calc R . .
H2C H -0.0949 0.3127 0.3952 0.052 Uiso 1 1 calc R . .
C3 C -0.02581(15) 0.20097(14) 0.31229(7) 0.0419(4) Uani 1 1 d . . .
H3A H -0.0819 0.2337 0.2857 0.050 Uiso 1 1 calc R . .
H3B H -0.0693 0.1574 0.3356 0.050 Uiso 1 1 calc R . .
H3C H 0.0304 0.1602 0.2937 0.050 Uiso 1 1 calc R . .
C4 C 0.08629(13) 0.17862(11) 0.45813(6) 0.0302(3) Uani 1 1 d . . .
H4 H 0.0718 0.2397 0.4802 0.036 Uiso 1 1 calc R . .
C5 C -0.03529(15) 0.12691(14) 0.44941(7) 0.0429(4) Uani 1 1 d . . .
H5A H -0.0660 0.1140 0.4844 0.051 Uiso 1 1 calc R . .
H5B H -0.0270 0.0629 0.4304 0.051 Uiso 1 1 calc R . .
H5C H -0.0905 0.1708 0.4279 0.051 Uiso 1 1 calc R . .
C6 C 0.16921(16) 0.11232(12) 0.49533(6) 0.0385(4) Uani 1 1 d . . .
H6A H 0.1409 0.1109 0.5314 0.046 Uiso 1 1 calc R . .
H6B H 0.2497 0.1402 0.4974 0.046 Uiso 1 1 calc R . .
H6C H 0.1699 0.0436 0.4809 0.046 Uiso 1 1 calc R . .
C7 C 0.54114(16) 0.34984(13) 0.38111(8) 0.0439(4) Uani 1 1 d . . .
H7A H 0.6223 0.3281 0.3922 0.053 Uiso 1 1 calc R . .
H7B H 0.5257 0.4146 0.3981 0.053 Uiso 1 1 calc R . .
H7C H 0.5316 0.3575 0.3419 0.053 Uiso 1 1 calc R . .
C8 C 0.48828(17) 0.17120(15) 0.48682(7) 0.0471(4) Uani 1 1 d . . .
H8A H 0.5739 0.1839 0.4907 0.057 Uiso 1 1 calc R . .
H8B H 0.4737 0.0985 0.4883 0.057 Uiso 1 1 calc R . .
H8C H 0.4510 0.2047 0.5161 0.057 Uiso 1 1 calc R . .
C11 C 0.24184(13) 0.41855(10) 0.44120(6) 0.0283(3) Uani 1 1 d . . .
C12 C 0.23513(15) 0.43609(12) 0.49686(6) 0.0355(3) Uani 1 1 d . . .
C13 C 0.2103(2) 0.53282(14) 0.51475(8) 0.0524(5) Uani 1 1 d . . .
H13 H 0.2061 0.5443 0.5522 0.063 Uiso 1 1 calc R . .
C14 C 0.1919(2) 0.61210(15) 0.47937(9) 0.0661(6) Uani 1 1 d . . .
H14 H 0.1729 0.6772 0.4921 0.079 Uiso 1 1 calc R . .
C15 C 0.2011(2) 0.59594(13) 0.42534(8) 0.0564(5) Uani 1 1 d . . .
H15 H 0.1898 0.6511 0.4011 0.068 Uiso 1 1 calc R . .
C16 C 0.22669(16) 0.50114(11) 0.40501(7) 0.0368(3) Uani 1 1 d . . .
C17 C 0.25944(17) 0.35472(12) 0.53909(6) 0.0396(4) Uani 1 1 d . . .
H17 H 0.2666 0.2891 0.5199 0.048 Uiso 1 1 calc R . .
C18 C 0.1598(2) 0.34392(18) 0.57662(8) 0.0621(6) Uani 1 1 d . . .
H18A H 0.1807 0.2911 0.6033 0.075 Uiso 1 1 calc R . .
H18B H 0.0859 0.3257 0.5555 0.075 Uiso 1 1 calc R . .
H18C H 0.1491 0.4080 0.5951 0.075 Uiso 1 1 calc R . .
C19 C 0.3768(2) 0.37443(15) 0.57216(8) 0.0560(5) Uani 1 1 d . . .
H19A H 0.3892 0.3231 0.6004 0.067 Uiso 1 1 calc R . .
H19B H 0.3749 0.4413 0.5888 0.067 Uiso 1 1 calc R . .
H19C H 0.4418 0.3715 0.5486 0.067 Uiso 1 1 calc R . .
C20 C 0.24199(16) 0.49405(12) 0.34502(6) 0.0398(4) Uani 1 1 d . . .
H20 H 0.2544 0.4216 0.3359 0.048 Uiso 1 1 calc R . .
C21 C 0.3515(2) 0.55379(17) 0.33070(9) 0.0611(6) Uani 1 1 d . . .
H21A H 0.4212 0.5316 0.3537 0.073 Uiso 1 1 calc R . .
H21B H 0.3383 0.6259 0.3364 0.073 Uiso 1 1 calc R . .
H21C H 0.3648 0.5420 0.2929 0.073 Uiso 1 1 calc R . .
C22 C 0.13395(19) 0.53278(15) 0.30957(8) 0.0529(5) Uani 1 1 d . . .
H22A H 0.0638 0.4935 0.3169 0.064 Uiso 1 1 calc R . .
H22B H 0.1484 0.5255 0.2715 0.064 Uiso 1 1 calc R . .
H22C H 0.1207 0.6040 0.3176 0.064 Uiso 1 1 calc R . .
C31 C 0.25627(12) 0.08970(11) 0.32351(6) 0.0269(3) Uani 1 1 d . . .
C32 C 0.21163(13) -0.01006(11) 0.32491(6) 0.0330(3) Uani 1 1 d . . .
C33 C 0.22404(16) -0.07377(14) 0.28120(8) 0.0460(4) Uani 1 1 d . . .
H33 H 0.1959 -0.1411 0.2825 0.055 Uiso 1 1 calc R . .
C34 C 0.27585(17) -0.04193(16) 0.23623(8) 0.0514(5) Uani 1 1 d . . .
H34 H 0.2867 -0.0875 0.2077 0.062 Uiso 1 1 calc R . .
C35 C 0.31174(17) 0.05680(16) 0.23313(7) 0.0465(4) Uani 1 1 d . . .
H35 H 0.3438 0.0797 0.2013 0.056 Uiso 1 1 calc R . .
C36 C 0.30224(14) 0.12436(13) 0.27563(6) 0.0338(3) Uani 1 1 d . . .
C37 C 0.15218(15) -0.04946(12) 0.37290(7) 0.0392(4) Uani 1 1 d . . .
H37 H 0.1324 0.0102 0.3950 0.047 Uiso 1 1 calc R . .
C38 C 0.03555(19) -0.10372(17) 0.35587(11) 0.0659(6) Uani 1 1 d . . .
H38A H -0.0151 -0.0597 0.3322 0.079 Uiso 1 1 calc R . .
H38B H -0.0052 -0.1203 0.3879 0.079 Uiso 1 1 calc R . .
H38C H 0.0522 -0.1659 0.3366 0.079 Uiso 1 1 calc R . .
C39 C 0.2338(2) -0.11732(16) 0.40888(10) 0.0634(6) Uani 1 1 d . . .
H39A H 0.3084 -0.0819 0.4190 0.076 Uiso 1 1 calc R . .
H39B H 0.2503 -0.1792 0.3893 0.076 Uiso 1 1 calc R . .
H39C H 0.1952 -0.1345 0.4414 0.076 Uiso 1 1 calc R . .
C40 C 0.33593(17) 0.23347(14) 0.26724(7) 0.0421(4) Uani 1 1 d . . .
H40 H 0.3393 0.2677 0.3031 0.051 Uiso 1 1 calc R . .
C41 C 0.4575(2) 0.24668(18) 0.24512(9) 0.0606(6) Uani 1 1 d . . .
H41A H 0.5183 0.2129 0.2691 0.073 Uiso 1 1 calc R . .
H41B H 0.4762 0.3187 0.2431 0.073 Uiso 1 1 calc R . .
H41C H 0.4556 0.2169 0.2091 0.073 Uiso 1 1 calc R . .
C42 C 0.2396(2) 0.28585(17) 0.23027(8) 0.0582(5) Uani 1 1 d . . .
H42A H 0.1627 0.2779 0.2451 0.070 Uiso 1 1 calc R . .
H42B H 0.2362 0.2554 0.1943 0.070 Uiso 1 1 calc R . .
H42C H 0.2584 0.3577 0.2277 0.070 Uiso 1 1 calc R . .
C51 C 0.50692(16) 0.00701(13) 0.37017(10) 0.0511(5) Uani 1 1 d . . .
H51A H 0.4650 -0.0144 0.3355 0.061 Uiso 1 1 calc R . .
H51B H 0.4566 -0.0094 0.3996 0.061 Uiso 1 1 calc R . .
C52 C 0.62312(17) -0.04436(16) 0.37885(9) 0.0546(5) Uani 1 1 d . . .
H52A H 0.6211 -0.1113 0.3612 0.066 Uiso 1 1 calc R . .
H52B H 0.6471 -0.0528 0.4177 0.066 Uiso 1 1 calc R . .
C53 C 0.70509(18) 0.02616(16) 0.35313(11) 0.0613(6) Uani 1 1 d . . .
H53A H 0.7016 0.0153 0.3137 0.074 Uiso 1 1 calc R . .
H53B H 0.7879 0.0172 0.3686 0.074 Uiso 1 1 calc R . .
C54 C 0.65928(15) 0.12877(16) 0.36598(10) 0.0549(5) Uani 1 1 d . . .
H54A H 0.6979 0.1537 0.4006 0.066 Uiso 1 1 calc R . .
H54B H 0.6743 0.1775 0.3372 0.066 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
Zr N1 2.0620(12) . ?
Zr N2 2.1176(11) . ?
Zr C8 2.2562(17) . ?
Zr C7 2.2780(16) . ?
Zr O 2.3215(11) . ?
Zr Si 2.8362(4) . ?
Si N2 1.7484(12) . ?
Si N1 1.7679(12) . ?
Si C1 1.8849(15) . ?
Si C4 1.9019(15) . ?
O C54 1.4610(19) . ?
O C51 1.464(2) . ?
N1 C11 1.4364(17) . ?
N2 C31 1.4238(17) . ?
C1 C3 1.540(2) . ?
C1 C2 1.543(2) . ?
C4 C5 1.536(2) . ?
C4 C6 1.538(2) . ?
C11 C12 1.415(2) . ?
C11 C16 1.420(2) . ?
C12 C13 1.395(2) . ?
C12 C17 1.516(2) . ?
C13 C14 1.377(3) . ?
C14 C15 1.376(3) . ?
C15 C16 1.395(2) . ?
C16 C20 1.522(2) . ?
C17 C19 1.525(3) . ?
C17 C18 1.531(3) . ?
C20 C22 1.535(2) . ?
C20 C21 1.538(3) . ?
C31 C32 1.418(2) . ?
C31 C36 1.418(2) . ?
C32 C33 1.395(2) . ?
C32 C37 1.514(2) . ?
C33 C34 1.374(3) . ?
C34 C35 1.375(3) . ?
C35 C36 1.398(2) . ?
C36 C40 1.516(2) . ?
C37 C39 1.525(3) . ?
C37 C38 1.531(2) . ?
C40 C42 1.533(3) . ?
C40 C41 1.535(3) . ?
C51 C52 1.480(3) . ?
C52 C53 1.499(3) . ?
C53 C54 1.501(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Zr N2 75.69(4) . . ?
N1 Zr C8 107.44(6) . . ?
N2 Zr C8 115.60(6) . . ?
N1 Zr C7 102.17(6) . . ?
N2 Zr C7 136.69(6) . . ?
C8 Zr C7 106.37(7) . . ?
N1 Zr O 162.24(4) . . ?
N2 Zr O 87.65(4) . . ?
C8 Zr O 85.14(6) . . ?
C7 Zr O 85.62(5) . . ?
N1 Zr Si 38.37(3) . . ?
N2 Zr Si 37.95(3) . . ?
C8 Zr Si 112.37(5) . . ?
C7 Zr Si 131.03(5) . . ?
O Zr Si 125.57(3) . . ?
N2 Si N1 93.67(5) . . ?
N2 Si C1 114.52(6) . . ?
N1 Si C1 113.50(6) . . ?
N2 Si C4 116.96(6) . . ?
N1 Si C4 107.39(6) . . ?
C1 Si C4 109.74(7) . . ?
N2 Si Zr 48.15(4) . . ?
N1 Si Zr 46.38(4) . . ?
C1 Si Zr 133.74(5) . . ?
C4 Si Zr 116.03(5) . . ?
C54 O C51 108.34(13) . . ?
C54 O Zr 124.18(10) . . ?
C51 O Zr 121.92(10) . . ?
C11 N1 Si 126.14(10) . . ?
C11 N1 Zr 138.55(9) . . ?
Si N1 Zr 95.25(5) . . ?
C31 N2 Si 131.61(9) . . ?
C31 N2 Zr 129.35(9) . . ?
Si N2 Zr 93.89(5) . . ?
C3 C1 C2 111.02(13) . . ?
C3 C1 Si 113.97(11) . . ?
C2 C1 Si 111.60(11) . . ?
C5 C4 C6 108.86(13) . . ?
C5 C4 Si 119.26(11) . . ?
C6 C4 Si 113.38(11) . . ?
C12 C11 C16 118.82(13) . . ?
C12 C11 N1 120.63(13) . . ?
C16 C11 N1 120.54(13) . . ?
C13 C12 C11 119.59(15) . . ?
C13 C12 C17 117.55(14) . . ?
C11 C12 C17 122.80(14) . . ?
C14 C13 C12 121.44(17) . . ?
C15 C14 C13 119.18(17) . . ?
C14 C15 C16 122.07(17) . . ?
C15 C16 C11 118.84(15) . . ?
C15 C16 C20 117.16(15) . . ?
C11 C16 C20 123.94(14) . . ?
C12 C17 C19 110.58(15) . . ?
C12 C17 C18 113.01(16) . . ?
C19 C17 C18 109.79(16) . . ?
C16 C20 C22 113.15(16) . . ?
C16 C20 C21 110.92(15) . . ?
C22 C20 C21 108.19(15) . . ?
C32 C31 C36 118.70(13) . . ?
C32 C31 N2 121.01(13) . . ?
C36 C31 N2 120.12(13) . . ?
C33 C32 C31 119.10(15) . . ?
C33 C32 C37 119.24(15) . . ?
C31 C32 C37 121.65(13) . . ?
C34 C33 C32 121.91(17) . . ?
C33 C34 C35 119.13(15) . . ?
C34 C35 C36 121.71(17) . . ?
C35 C36 C31 119.13(16) . . ?
C35 C36 C40 118.10(15) . . ?
C31 C36 C40 122.69(13) . . ?
C32 C37 C39 112.36(15) . . ?
C32 C37 C38 111.94(16) . . ?
C39 C37 C38 110.51(17) . . ?
C36 C40 C42 109.96(16) . . ?
C36 C40 C41 113.72(16) . . ?
C42 C40 C41 110.23(16) . . ?
O C51 C52 106.38(15) . . ?
C51 C52 C53 102.98(17) . . ?
C52 C53 C54 103.71(16) . . ?
O C54 C53 105.15(15) . . ?

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
N1 Zr Si N2 166.46(7) . . . . ?
C8 Zr Si N2 -103.42(7) . . . . ?
C7 Zr Si N2 116.92(8) . . . . ?
O Zr Si N2 -2.94(6) . . . . ?
N2 Zr Si N1 -166.46(7) . . . . ?
C8 Zr Si N1 90.12(7) . . . . ?
C7 Zr Si N1 -49.54(8) . . . . ?
O Zr Si N1 -169.40(6) . . . . ?
N1 Zr Si C1 81.39(8) . . . . ?
N2 Zr Si C1 -85.07(8) . . . . ?
C8 Zr Si C1 171.51(8) . . . . ?
C7 Zr Si C1 31.85(9) . . . . ?
O Zr Si C1 -88.01(8) . . . . ?
N1 Zr Si C4 -89.66(7) . . . . ?
N2 Zr Si C4 103.88(7) . . . . ?
C8 Zr Si C4 0.46(8) . . . . ?
C7 Zr Si C4 -139.20(8) . . . . ?
O Zr Si C4 100.94(6) . . . . ?
N1 Zr O C54 145.64(16) . . . . ?
N2 Zr O C54 165.81(14) . . . . ?
C8 Zr O C54 -78.25(15) . . . . ?
C7 Zr O C54 28.62(15) . . . . ?
Si Zr O C54 167.62(13) . . . . ?
N1 Zr O C51 -63.8(2) . . . . ?
N2 Zr O C51 -43.59(13) . . . . ?
C8 Zr O C51 72.35(14) . . . . ?
C7 Zr O C51 179.22(14) . . . . ?
Si Zr O C51 -41.78(14) . . . . ?
N2 Si N1 C11 167.46(11) . . . . ?
C1 Si N1 C11 48.68(13) . . . . ?
C4 Si N1 C11 -72.79(12) . . . . ?
Zr Si N1 C11 177.52(14) . . . . ?
N2 Si N1 Zr -10.06(5) . . . . ?
C1 Si N1 Zr -128.84(6) . . . . ?
C4 Si N1 Zr 109.68(6) . . . . ?
N2 Zr N1 C11 -168.43(14) . . . . ?
C8 Zr N1 C11 78.78(15) . . . . ?
C7 Zr N1 C11 -32.93(15) . . . . ?
O Zr N1 C11 -147.61(14) . . . . ?
Si Zr N1 C11 -176.98(16) . . . . ?
N2 Zr N1 Si 8.55(5) . . . . ?
C8 Zr N1 Si -104.24(7) . . . . ?
C7 Zr N1 Si 144.05(6) . . . . ?
O Zr N1 Si 29.37(16) . . . . ?
N1 Si N2 C31 -145.78(13) . . . . ?
C1 Si N2 C31 -27.85(15) . . . . ?
C4 Si N2 C31 102.58(13) . . . . ?
Zr Si N2 C31 -155.56(15) . . . . ?
N1 Si N2 Zr 9.78(5) . . . . ?
C1 Si N2 Zr 127.71(6) . . . . ?
C4 Si N2 Zr -101.86(6) . . . . ?
N1 Zr N2 C31 147.80(12) . . . . ?
C8 Zr N2 C31 -109.45(12) . . . . ?
C7 Zr N2 C31 55.12(15) . . . . ?
O Zr N2 C31 -25.97(12) . . . . ?
Si Zr N2 C31 156.42(14) . . . . ?
N1 Zr N2 Si -8.63(5) . . . . ?
C8 Zr N2 Si 94.13(7) . . . . ?
C7 Zr N2 Si -101.30(8) . . . . ?
O Zr N2 Si 177.60(5) . . . . ?
N2 Si C1 C3 55.39(14) . . . . ?
N1 Si C1 C3 161.36(11) . . . . ?
C4 Si C1 C3 -78.49(13) . . . . ?
Zr Si C1 C3 110.05(12) . . . . ?
N2 Si C1 C2 -177.87(11) . . . . ?
N1 Si C1 C2 -71.90(13) . . . . ?
C4 Si C1 C2 48.25(13) . . . . ?
Zr Si C1 C2 -123.21(11) . . . . ?
N2 Si C4 C5 -96.50(13) . . . . ?
N1 Si C4 C5 159.93(12) . . . . ?
C1 Si C4 C5 36.13(14) . . . . ?
Zr Si C4 C5 -150.73(11) . . . . ?
N2 Si C4 C6 33.73(13) . . . . ?
N1 Si C4 C6 -69.84(12) . . . . ?
C1 Si C4 C6 166.36(10) . . . . ?
Zr Si C4 C6 -20.50(12) . . . . ?
Si N1 C11 C12 94.28(16) . . . . ?
Zr N1 C11 C12 -89.45(18) . . . . ?
Si N1 C11 C16 -86.98(16) . . . . ?
Zr N1 C11 C16 89.29(18) . . . . ?
C16 C11 C12 C13 2.0(3) . . . . ?
N1 C11 C12 C13 -179.28(16) . . . . ?
C16 C11 C12 C17 -175.14(16) . . . . ?
N1 C11 C12 C17 3.6(2) . . . . ?
C11 C12 C13 C14 0.1(3) . . . . ?
C17 C12 C13 C14 177.4(2) . . . . ?
C12 C13 C14 C15 -1.7(4) . . . . ?
C13 C14 C15 C16 1.2(4) . . . . ?
C14 C15 C16 C11 0.9(3) . . . . ?
C14 C15 C16 C20 -176.4(2) . . . . ?
C12 C11 C16 C15 -2.5(3) . . . . ?
N1 C11 C16 C15 178.77(17) . . . . ?
C12 C11 C16 C20 174.70(16) . . . . ?
N1 C11 C16 C20 -4.1(2) . . . . ?
C13 C12 C17 C19 -68.6(2) . . . . ?
C11 C12 C17 C19 108.57(18) . . . . ?
C13 C12 C17 C18 55.0(2) . . . . ?
C11 C12 C17 C18 -127.90(17) . . . . ?
C15 C16 C20 C22 -56.5(2) . . . . ?
C11 C16 C20 C22 126.30(18) . . . . ?
C15 C16 C20 C21 65.3(2) . . . . ?
C11 C16 C20 C21 -111.91(19) . . . . ?
Si N2 C31 C32 -84.92(17) . . . . ?
Zr N2 C31 C32 127.34(12) . . . . ?
Si N2 C31 C36 99.96(15) . . . . ?
Zr N2 C31 C36 -47.78(18) . . . . ?
C36 C31 C32 C33 5.8(2) . . . . ?
N2 C31 C32 C33 -169.42(14) . . . . ?
C36 C31 C32 C37 -174.97(14) . . . . ?
N2 C31 C32 C37 9.8(2) . . . . ?
C31 C32 C33 C34 -1.5(3) . . . . ?
C37 C32 C33 C34 179.17(17) . . . . ?
C32 C33 C34 C35 -3.0(3) . . . . ?
C33 C34 C35 C36 3.2(3) . . . . ?
C34 C35 C36 C31 1.1(3) . . . . ?
C34 C35 C36 C40 -175.80(17) . . . . ?
C32 C31 C36 C35 -5.5(2) . . . . ?
N2 C31 C36 C35 169.69(14) . . . . ?
C32 C31 C36 C40 171.20(15) . . . . ?
N2 C31 C36 C40 -13.6(2) . . . . ?
C33 C32 C37 C39 77.1(2) . . . . ?
C31 C32 C37 C39 -102.19(18) . . . . ?
C33 C32 C37 C38 -48.0(2) . . . . ?
C31 C32 C37 C38 132.77(16) . . . . ?
C35 C36 C40 C42 74.0(2) . . . . ?
C31 C36 C40 C42 -102.80(17) . . . . ?
C35 C36 C40 C41 -50.2(2) . . . . ?
C31 C36 C40 C41 133.05(17) . . . . ?
C54 O C51 C52 11.9(2) . . . . ?
Zr O C51 C52 -142.79(13) . . . . ?
O C51 C52 C53 -30.2(2) . . . . ?
C51 C52 C53 C54 36.8(2) . . . . ?
C51 O C54 C53 11.4(2) . . . . ?
Zr O C54 C53 165.36(14) . . . . ?
C52 C53 C54 O -29.9(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.55
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.046
####################################################################### 
# 
# 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_riv1301
_database_code_depnum_ccdc_archive 'CCDC 1043231'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H84 Cl Li N4 O3 Si Zr, 0.5(C4 H8 O)'
_chemical_formula_sum            'C48 H88 Cl Li N4 O3.50 Si Zr'
_chemical_formula_weight         938.92

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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   25.9179(11)
_cell_length_b                   10.9638(5)
_cell_length_c                   36.5714(15)
_cell_angle_alpha                90
_cell_angle_beta                 90.0434(6)
_cell_angle_gamma                90
_cell_volume                     10392.1(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9253
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      21.90

_exptl_crystal_description       fragment
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_F_000             4048
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.364
_exptl_crystal_size_mid          0.318
_exptl_crystal_size_min          0.175
_exptl_absorpt_coefficient_mu    0.328
_shelx_estimated_absorpt_T_min   0.890
_shelx_estimated_absorpt_T_max   0.945
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.9045
_exptl_absorpt_correction_T_max  0.9805
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41191
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         1.114
_diffrn_reflns_theta_max         26.459
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10729
_reflns_number_gt                7893
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0598P)²+13.9890P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10729
_refine_ls_number_parameters     525
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0461
_refine_ls_wR_factor_ref         0.1288
_refine_ls_wR_factor_gt          0.1145
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.040
_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_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
Zr Zr 0.06634(2) 0.22579(2) 0.37190(2) 0.02358(9) Uani 1 1 d . . . . .
Cl Cl -0.01765(3) 0.30791(7) 0.40190(2) 0.03647(18) Uani 1 1 d . . . . .
Si Si 0.16568(3) 0.26110(7) 0.40567(2) 0.02415(17) Uani 1 1 d . . . . .
O1 O -0.12222(10) 0.4803(2) 0.36167(6) 0.0540(6) Uani 1 1 d . . . . .
O2A O -0.14446(17) 0.2864(4) 0.41959(13) 0.0479(12) Uiso 0.65 1 d . . P A 1
O2B O -0.1464(3) 0.2461(9) 0.4140(3) 0.054(3) Uiso 0.35 1 d . . P A 2
O3 O -0.11246(10) 0.2021(2) 0.33861(7) 0.0554(7) Uani 1 1 d . . . . .
N1 N 0.14747(9) 0.2267(2) 0.36080(6) 0.0244(5) Uani 1 1 d . . . . .
N2 N 0.10360(9) 0.29764(19) 0.41986(6) 0.0242(5) Uani 1 1 d . . . . .
N3 N 0.04376(9) 0.0462(2) 0.37772(7) 0.0325(6) Uani 1 1 d . . . . .
N4 N 0.03783(10) 0.2846(2) 0.32211(7) 0.0335(6) Uani 1 1 d . . . . .
C1 C 0.19740(12) 0.1190(3) 0.42569(8) 0.0346(7) Uani 1 1 d . . . . .
H1 H 0.2235 0.0945 0.4069 0.041 Uiso 1 1 calc R U . . .
C2 C 0.16199(12) 0.0082(3) 0.42905(8) 0.0371(7) Uani 1 1 d . . . . .
H2A H 0.1813 -0.0601 0.4397 0.045 Uiso 1 1 calc R U . . .
H2B H 0.1493 -0.0149 0.4048 0.045 Uiso 1 1 calc R U . . .
H2C H 0.1327 0.0284 0.4449 0.045 Uiso 1 1 calc R U . . .
C3 C 0.22840(14) 0.1316(3) 0.46095(9) 0.0493(9) Uani 1 1 d . . . . .
H3A H 0.2424 0.0518 0.4679 0.059 Uiso 1 1 calc R U . . .
H3B H 0.2059 0.1618 0.4805 0.059 Uiso 1 1 calc R U . . .
H3C H 0.2568 0.1891 0.4571 0.059 Uiso 1 1 calc R U . . .
C4 C 0.21387(11) 0.3900(3) 0.40998(8) 0.0328(7) Uani 1 1 d . . . . .
H4 H 0.2008 0.4575 0.3941 0.039 Uiso 1 1 calc R U . . .
C5 C 0.26726(12) 0.3551(3) 0.39493(10) 0.0447(8) Uani 1 1 d . . . . .
H5A H 0.2907 0.4249 0.3971 0.054 Uiso 1 1 calc R U . . .
H5B H 0.2641 0.3319 0.3691 0.054 Uiso 1 1 calc R U . . .
H5C H 0.2811 0.2862 0.4089 0.054 Uiso 1 1 calc R U . . .
C6 C 0.21896(13) 0.4435(3) 0.44878(9) 0.0439(8) Uani 1 1 d . . . . .
H6A H 0.2440 0.5105 0.4485 0.053 Uiso 1 1 calc R U . . .
H6B H 0.2308 0.3798 0.4656 0.053 Uiso 1 1 calc R U . . .
H6C H 0.1853 0.4742 0.4569 0.053 Uiso 1 1 calc R U . . .
C7 C 0.03740(14) -0.0500(3) 0.35134(10) 0.0462(8) Uani 1 1 d . . . . .
H7A H 0.0019 -0.0808 0.3524 0.055 Uiso 1 1 calc R U . . .
H7B H 0.0615 -0.1164 0.3569 0.055 Uiso 1 1 calc R U . . .
H7C H 0.0445 -0.0184 0.3268 0.055 Uiso 1 1 calc R U . . .
C8 C 0.02839(14) 0.0034(3) 0.41363(9) 0.0478(9) Uani 1 1 d . . . . .
H8A H -0.0083 -0.0177 0.4133 0.057 Uiso 1 1 calc R U . . .
H8B H 0.0344 0.0679 0.4317 0.057 Uiso 1 1 calc R U . . .
H8C H 0.0487 -0.0688 0.4201 0.057 Uiso 1 1 calc R U . . .
C9 C 0.05626(14) 0.2085(3) 0.29260(9) 0.0440(8) Uani 1 1 d . . . . .
H9A H 0.0721 0.2598 0.2737 0.053 Uiso 1 1 calc R U . . .
H9B H 0.0273 0.1633 0.2820 0.053 Uiso 1 1 calc R U . . .
H9C H 0.0820 0.1510 0.3020 0.053 Uiso 1 1 calc R U . . .
C10 C 0.00075(13) 0.3735(3) 0.30927(9) 0.0467(8) Uani 1 1 d . . . . .
H10A H 0.0172 0.4274 0.2914 0.056 Uiso 1 1 calc R U . . .
H10B H -0.0117 0.4219 0.3300 0.056 Uiso 1 1 calc R U . . .
H10C H -0.0284 0.3313 0.2978 0.056 Uiso 1 1 calc R U . . .
C11 C 0.18008(10) 0.2199(2) 0.32983(7) 0.0256(6) Uani 1 1 d . . . . .
C12 C 0.19902(11) 0.1066(3) 0.31655(7) 0.0288(6) Uani 1 1 d . . . . .
C13 C 0.23311(12) 0.1046(3) 0.28739(8) 0.0381(7) Uani 1 1 d . . . . .
H13 H 0.2462 0.0283 0.2793 0.046 Uiso 1 1 calc R U . . .
C14 C 0.24870(13) 0.2094(3) 0.26966(9) 0.0440(8) Uani 1 1 d . . . . .
H14 H 0.2727 0.2061 0.2501 0.053 Uiso 1 1 calc R U . . .
C15 C 0.22845(13) 0.3185(3) 0.28123(9) 0.0418(8) Uani 1 1 d . . . . .
H15 H 0.2380 0.3910 0.2687 0.050 Uiso 1 1 calc R U . . .
C16 C 0.19452(12) 0.3269(3) 0.31049(8) 0.0324(7) Uani 1 1 d . . . . .
C17 C 0.18194(12) -0.0148(3) 0.33227(8) 0.0345(7) Uani 1 1 d . . . . .
H17 H 0.1569 0.0020 0.3524 0.041 Uiso 1 1 calc R U . . .
C18 C 0.15448(13) -0.0925(3) 0.30338(9) 0.0431(8) Uani 1 1 d . . . . .
H18A H 0.1251 -0.0470 0.2934 0.052 Uiso 1 1 calc R U . . .
H18B H 0.1421 -0.1682 0.3146 0.052 Uiso 1 1 calc R U . . .
H18C H 0.1786 -0.1121 0.2836 0.052 Uiso 1 1 calc R U . . .
C19 C 0.22679(14) -0.0879(3) 0.34828(10) 0.0459(8) Uani 1 1 d . . . . .
H19A H 0.2445 -0.0388 0.3668 0.055 Uiso 1 1 calc R U . . .
H19B H 0.2511 -0.1091 0.3288 0.055 Uiso 1 1 calc R U . . .
H19C H 0.2135 -0.1627 0.3595 0.055 Uiso 1 1 calc R U . . .
C20 C 0.17306(13) 0.4522(3) 0.31945(9) 0.0408(8) Uani 1 1 d . . . . .
H20 H 0.1540 0.4460 0.3431 0.049 Uiso 1 1 calc R U . . .
C21 C 0.13515(15) 0.4946(3) 0.29043(12) 0.0611(11) Uani 1 1 d . . . . .
H21A H 0.1079 0.4335 0.2875 0.073 Uiso 1 1 calc R U . . .
H21B H 0.1533 0.5054 0.2672 0.073 Uiso 1 1 calc R U . . .
H21C H 0.1198 0.5724 0.2979 0.073 Uiso 1 1 calc R U . . .
C22 C 0.21547(15) 0.5483(3) 0.32405(10) 0.0503(9) Uani 1 1 d . . . . .
H22A H 0.2400 0.5211 0.3427 0.060 Uiso 1 1 calc R U . . .
H22B H 0.2000 0.6258 0.3316 0.060 Uiso 1 1 calc R U . . .
H22C H 0.2335 0.5594 0.3008 0.060 Uiso 1 1 calc R U . . .
C31 C 0.09005(10) 0.3820(2) 0.44792(7) 0.0249(6) Uani 1 1 d . . . . .
C32 C 0.08203(11) 0.3421(3) 0.48442(8) 0.0302(6) Uani 1 1 d . . . . .
C33 C 0.06863(12) 0.4272(3) 0.51107(8) 0.0387(7) Uani 1 1 d . . . . .
H33 H 0.0635 0.3999 0.5354 0.046 Uiso 1 1 calc R U . . .
C34 C 0.06262(13) 0.5485(3) 0.50345(9) 0.0452(8) Uani 1 1 d . . . . .
H34 H 0.0535 0.6045 0.5222 0.054 Uiso 1 1 calc R U . . .
C35 C 0.07006(12) 0.5878(3) 0.46823(9) 0.0398(8) Uani 1 1 d . . . . .
H35 H 0.0663 0.6721 0.4628 0.048 Uiso 1 1 calc R U . . .
C36 C 0.08301(11) 0.5076(3) 0.44015(8) 0.0296(6) Uani 1 1 d . . . . .
C37 C 0.08535(12) 0.2101(3) 0.49505(8) 0.0366(7) Uani 1 1 d . . . . .
H37 H 0.1001 0.1638 0.4739 0.044 Uiso 1 1 calc R U . . .
C38 C 0.03174(15) 0.1590(3) 0.50307(10) 0.0557(10) Uani 1 1 d . . . . .
H38A H 0.0088 0.1762 0.4824 0.067 Uiso 1 1 calc R U . . .
H38B H 0.0180 0.1974 0.5252 0.067 Uiso 1 1 calc R U . . .
H38C H 0.0341 0.0706 0.5068 0.067 Uiso 1 1 calc R U . . .
C39 C 0.12031(17) 0.1892(4) 0.52828(10) 0.0633(11) Uani 1 1 d . . . . .
H39A H 0.1540 0.2269 0.5239 0.076 Uiso 1 1 calc R U . . .
H39B H 0.1248 0.1014 0.5322 0.076 Uiso 1 1 calc R U . . .
H39C H 0.1045 0.2260 0.5500 0.076 Uiso 1 1 calc R U . . .
C40 C 0.08826(13) 0.5608(3) 0.40217(9) 0.0410(8) Uani 1 1 d . . . . .
H40 H 0.0998 0.4941 0.3854 0.049 Uiso 1 1 calc R U . . .
C41 C 0.03647(15) 0.6088(3) 0.38814(10) 0.0525(9) Uani 1 1 d . . . . .
H41A H 0.0412 0.6450 0.3639 0.063 Uiso 1 1 calc R U . . .
H41B H 0.0233 0.6708 0.4050 0.063 Uiso 1 1 calc R U . . .
H41C H 0.0118 0.5413 0.3865 0.063 Uiso 1 1 calc R U . . .
C42 C 0.12824(14) 0.6631(3) 0.40046(11) 0.0562(10) Uani 1 1 d . . . . .
H42A H 0.1295 0.6963 0.3756 0.067 Uiso 1 1 calc R U . . .
H42B H 0.1622 0.6306 0.4071 0.067 Uiso 1 1 calc R U . . .
H42C H 0.1187 0.7278 0.4176 0.067 Uiso 1 1 calc R U . . .
C51 C -0.13110(15) 0.5268(3) 0.32546(10) 0.0531(9) Uani 1 1 d . . . . .
H51A H -0.1624 0.4893 0.3147 0.064 Uiso 1 1 calc R U . . .
H51B H -0.1013 0.5088 0.3094 0.064 Uiso 1 1 calc R U . . .
C52 C -0.13812(19) 0.6625(4) 0.32965(12) 0.0720(12) Uani 1 1 d . . . . .
H52A H -0.1248 0.7067 0.3080 0.086 Uiso 1 1 calc R U . . .
H52B H -0.1749 0.6835 0.3332 0.086 Uiso 1 1 calc R U . . .
C53 C -0.10730(18) 0.6918(4) 0.36287(13) 0.0718(12) Uani 1 1 d . . . . .
H53A H -0.1198 0.7673 0.3748 0.086 Uiso 1 1 calc R U . . .
H53B H -0.0702 0.7009 0.3570 0.086 Uiso 1 1 calc R U . . .
C54 C -0.11672(19) 0.5826(4) 0.38625(11) 0.0713(12) Uani 1 1 d . . . . .
H54A H -0.0874 0.5693 0.4031 0.086 Uiso 1 1 calc R U . . .
H54B H -0.1485 0.5935 0.4009 0.086 Uiso 1 1 calc R U . . .
C61A C -0.1391(3) 0.1670(7) 0.4365(2) 0.070(2) Uiso 0.65 1 d . . P A 1
H61A H -0.1025 0.1406 0.4369 0.084 Uiso 0.65 1 calc R U P A 1
H61B H -0.1598 0.1050 0.4234 0.084 Uiso 0.65 1 calc R U P A 1
C62A C -0.1587(3) 0.1863(8) 0.4742(2) 0.065(3) Uiso 0.65 1 d . . P A 1
H62A H -0.1301 0.2019 0.4915 0.079 Uiso 0.65 1 calc R U P A 1
H62B H -0.1788 0.1150 0.4827 0.079 Uiso 0.65 1 calc R U P A 1
C63A C -0.1933(4) 0.2992(8) 0.4700(3) 0.080(3) Uiso 0.65 1 d . . P A 1
H63A H -0.2298 0.2737 0.4679 0.096 Uiso 0.65 1 calc R U P A 1
H63B H -0.1898 0.3520 0.4918 0.096 Uiso 0.65 1 calc R U P A 1
C64A C -0.1785(2) 0.3651(6) 0.43809(17) 0.0607(16) Uiso 0.65 1 d . . P A 1
H64A H -0.2090 0.3839 0.4227 0.073 Uiso 0.65 1 calc R U P A 1
H64B H -0.1611 0.4423 0.4447 0.073 Uiso 0.65 1 calc R U P A 1
C61B C -0.1283(4) 0.1833(11) 0.4492(3) 0.044(3) Uiso 0.35 1 d . . P A 2
H61C H -0.0942 0.2154 0.4568 0.053 Uiso 0.35 1 calc R U P A 2
H61D H -0.1253 0.0942 0.4455 0.053 Uiso 0.35 1 calc R U P A 2
C62B C -0.1698(5) 0.2123(13) 0.4785(4) 0.045(3) Uiso 0.35 1 d . . P A 2
H62C H -0.1841 0.1355 0.4886 0.054 Uiso 0.35 1 calc R U P A 2
H62D H -0.1543 0.2593 0.4988 0.054 Uiso 0.35 1 calc R U P A 2
C63B C -0.2104(5) 0.2828(12) 0.4614(4) 0.053(3) Uiso 0.35 1 d . . P A 2
H63C H -0.2442 0.2412 0.4637 0.063 Uiso 0.35 1 calc R U P A 2
H63D H -0.2129 0.3651 0.4723 0.063 Uiso 0.35 1 calc R U P A 2
C64B C -0.1949(5) 0.2891(12) 0.4252(4) 0.069(3) Uiso 0.35 1 d . . P A 2
H64C H -0.1969 0.3758 0.4179 0.083 Uiso 0.35 1 calc R U P A 2
H64D H -0.2210 0.2448 0.4106 0.083 Uiso 0.35 1 calc R U P A 2
C71A C -0.0760(3) 0.1014(7) 0.3333(2) 0.0470(19) Uiso 0.5 1 d . . P B 1
H71A H -0.0406 0.1336 0.3302 0.056 Uiso 0.5 1 calc R U P B 1
H71B H -0.0763 0.0468 0.3549 0.056 Uiso 0.5 1 calc R U P B 1
C72A C -0.0914(3) 0.0356(7) 0.3013(2) 0.0476(17) Uiso 0.5 1 d . . P B 1
H72A H -0.0808 -0.0510 0.3027 0.057 Uiso 0.5 1 calc R U P B 1
H72B H -0.0768 0.0726 0.2789 0.057 Uiso 0.5 1 calc R U P B 1
C73A C -0.1508(3) 0.0483(8) 0.3022(3) 0.062(2) Uiso 0.5 1 d . . P B 1
H73A H -0.1668 -0.0171 0.3170 0.075 Uiso 0.5 1 calc R U P B 1
H73B H -0.1656 0.0466 0.2772 0.075 Uiso 0.5 1 calc R U P B 1
C74A C -0.1579(4) 0.1747(9) 0.3203(3) 0.065(2) Uiso 0.5 1 d . . P B 1
H74A H -0.1650 0.2373 0.3014 0.078 Uiso 0.5 1 calc R U P B 1
H74B H -0.1872 0.1727 0.3376 0.078 Uiso 0.5 1 calc R U P B 1
C71B C -0.0899(4) 0.0844(9) 0.3447(3) 0.067(3) Uiso 0.5 1 d . . P B 2
H71C H -0.0520 0.0886 0.3416 0.080 Uiso 0.5 1 calc R U P B 2
H71D H -0.0974 0.0561 0.3698 0.080 Uiso 0.5 1 calc R U P B 2
C72B C -0.1117(4) 0.0028(10) 0.3186(3) 0.084(3) Uiso 0.5 1 d . . P B 2
H72C H -0.1379 -0.0499 0.3303 0.101 Uiso 0.5 1 calc R U P B 2
H72D H -0.0846 -0.0498 0.3079 0.101 Uiso 0.5 1 calc R U P B 2
C73B C -0.1371(3) 0.0846(7) 0.2882(2) 0.055(2) Uiso 0.5 1 d . . P B 2
H73C H -0.1138 0.0939 0.2669 0.066 Uiso 0.5 1 calc R U P B 2
H73D H -0.1702 0.0491 0.2798 0.066 Uiso 0.5 1 calc R U P B 2
C74B C -0.1454(3) 0.2008(7) 0.3064(2) 0.0432(17) Uiso 0.5 1 d . . P B 2
H74C H -0.1363 0.2690 0.2899 0.052 Uiso 0.5 1 calc R U P B 2
H74D H -0.1820 0.2095 0.3136 0.052 Uiso 0.5 1 calc R U P B 2
Li Li -0.1017(2) 0.3189(5) 0.37662(16) 0.0452(13) Uani 1 1 d . . . . .
O1S O 0.0218(4) 0.7246(10) 0.2806(3) 0.136(2) Uiso 0.5 1 d D U P C -1
C1S C -0.0295(5) 0.7776(14) 0.2788(4) 0.136(2) Uiso 0.5 1 d D U P C -1
H1SA H -0.0339 0.8436 0.2970 0.164 Uiso 0.5 1 calc R U P C -1
H1SB H -0.0566 0.7152 0.2825 0.164 Uiso 0.5 1 calc R U P C -1
C2S C -0.0299(5) 0.8255(13) 0.2411(4) 0.136(2) Uiso 0.5 1 d D U P C -1
H2SA H -0.0145 0.9081 0.2401 0.164 Uiso 0.5 1 calc R U P C -1
H2SB H -0.0655 0.8293 0.2313 0.164 Uiso 0.5 1 calc R U P C -1
C3S C 0.0031(6) 0.7331(15) 0.2192(4) 0.136(2) Uiso 0.5 1 d D U P C -1
H3SA H -0.0182 0.6643 0.2104 0.164 Uiso 0.5 1 calc R U P C -1
H3SB H 0.0199 0.7728 0.1981 0.164 Uiso 0.5 1 calc R U P C -1
C4S C 0.0419(5) 0.6909(14) 0.2460(4) 0.136(2) Uiso 0.5 1 d D U P C -1
H4SA H 0.0464 0.6014 0.2445 0.164 Uiso 0.5 1 calc R U P C -1
H4SB H 0.0756 0.7307 0.2416 0.164 Uiso 0.5 1 calc R U P C -1


_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
Zr N3 2.065(2) . ?
Zr N4 2.067(2) . ?
Zr N1 2.142(2) . ?
Zr N2 2.151(2) . ?
Zr Cl 2.5993(8) . ?
Cl Li 2.370(6) . ?
Si N2 1.738(2) . ?
Si N1 1.748(2) . ?
Si C4 1.892(3) . ?
Si C1 1.907(3) . ?
O1 C51 1.437(4) . ?
O1 C54 1.444(4) . ?
O1 Li 1.926(6) . ?
O2A C64A 1.408(7) . ?
O2A C61A 1.455(9) . ?
O2A Li 1.956(7) . ?
O2B C64B 1.404(15) . ?
O2B C61B 1.533(14) . ?
O2B Li 1.960(11) . ?
O3 C74A 1.387(9) . ?
O3 C71B 1.434(10) . ?
O3 C74B 1.454(8) . ?
O3 C71A 1.466(8) . ?
O3 Li 1.910(6) . ?
N1 C11 1.416(3) . ?
N2 C31 1.426(3) . ?
N3 C7 1.439(4) . ?
N3 C8 1.451(4) . ?
N4 C9 1.445(4) . ?
N4 C10 1.447(4) . ?
C1 C3 1.525(4) . ?
C1 C2 1.528(4) . ?
C4 C5 1.538(4) . ?
C4 C6 1.541(4) . ?
C11 C16 1.420(4) . ?
C11 C12 1.422(4) . ?
C12 C13 1.385(4) . ?
C12 C17 1.516(4) . ?
C13 C14 1.379(4) . ?
C14 C15 1.374(4) . ?
C15 C16 1.389(4) . ?
C16 C20 1.519(4) . ?
C17 C19 1.528(4) . ?
C17 C18 1.533(4) . ?
C20 C21 1.519(5) . ?
C20 C22 1.532(5) . ?
C31 C36 1.418(4) . ?
C31 C32 1.421(4) . ?
C32 C33 1.393(4) . ?
C32 C37 1.501(4) . ?
C33 C34 1.368(5) . ?
C34 C35 1.372(5) . ?
C35 C36 1.393(4) . ?
C36 C40 1.512(4) . ?
C37 C38 1.526(5) . ?
C37 C39 1.532(5) . ?
C40 C42 1.528(5) . ?
C40 C41 1.530(5) . ?
C51 C52 1.507(5) . ?
C52 C53 1.489(6) . ?
C53 C54 1.492(6) . ?
C61A C62A 1.483(11) . ?
C62A C63A 1.535(12) . ?
C63A C64A 1.425(10) . ?
C61B C62B 1.553(17) . ?
C62B C63B 1.448(18) . ?
C63B C64B 1.386(17) . ?
C71A C72A 1.431(10) . ?
C72A C73A 1.545(11) . ?
C73A C74A 1.547(12) . ?
C71B C72B 1.423(13) . ?
C72B C73B 1.574(13) . ?
C73B C74B 1.454(10) . ?
O1S C4S 1.418(9) . ?
O1S C1S 1.452(9) . ?
C1S C2S 1.477(9) . ?
C2S C3S 1.548(9) . ?
C3S C4S 1.476(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Zr N4 106.67(10) . . ?
N3 Zr N1 107.61(9) . . ?
N4 Zr N1 100.48(9) . . ?
N3 Zr N2 113.09(9) . . ?
N4 Zr N2 139.82(9) . . ?
N1 Zr N2 73.30(8) . . ?
N3 Zr Cl 92.82(7) . . ?
N4 Zr Cl 87.99(7) . . ?
N1 Zr Cl 154.28(6) . . ?
N2 Zr Cl 84.52(6) . . ?
Li Cl Zr 128.55(14) . . ?
N2 Si N1 94.62(11) . . ?
N2 Si C4 114.47(12) . . ?
N1 Si C4 114.63(12) . . ?
N2 Si C1 118.21(13) . . ?
N1 Si C1 107.47(12) . . ?
C4 Si C1 107.07(14) . . ?
C51 O1 C54 108.3(3) . . ?
C51 O1 Li 129.1(3) . . ?
C54 O1 Li 120.6(3) . . ?
C64A O2A C61A 114.0(5) . . ?
C64A O2A Li 129.0(4) . . ?
C61A O2A Li 116.8(4) . . ?
C64B O2B C61B 100.3(9) . . ?
C64B O2B Li 126.6(8) . . ?
C61B O2B Li 126.0(7) . . ?
C71B O3 C74B 110.8(5) . . ?
C74A O3 C71A 108.6(5) . . ?
C74A O3 Li 128.3(5) . . ?
C71B O3 Li 115.6(5) . . ?
C74B O3 Li 132.9(4) . . ?
C71A O3 Li 120.5(4) . . ?
C11 N1 Si 126.98(19) . . ?
C11 N1 Zr 137.57(18) . . ?
Si N1 Zr 95.02(10) . . ?
C31 N2 Si 126.37(18) . . ?
C31 N2 Zr 135.55(18) . . ?
Si N2 Zr 95.01(10) . . ?
C7 N3 C8 109.8(3) . . ?
C7 N3 Zr 131.5(2) . . ?
C8 N3 Zr 118.7(2) . . ?
C9 N4 C10 111.5(3) . . ?
C9 N4 Zr 111.1(2) . . ?
C10 N4 Zr 137.1(2) . . ?
C3 C1 C2 108.6(3) . . ?
C3 C1 Si 118.5(2) . . ?
C2 C1 Si 114.9(2) . . ?
C5 C4 C6 110.4(3) . . ?
C5 C4 Si 112.2(2) . . ?
C6 C4 Si 114.7(2) . . ?
N1 C11 C16 120.8(2) . . ?
N1 C11 C12 121.7(2) . . ?
C16 C11 C12 117.4(2) . . ?
C13 C12 C11 119.8(3) . . ?
C13 C12 C17 117.7(3) . . ?
C11 C12 C17 122.4(2) . . ?
C14 C13 C12 122.4(3) . . ?
C15 C14 C13 117.9(3) . . ?
C14 C15 C16 122.5(3) . . ?
C15 C16 C11 119.8(3) . . ?
C15 C16 C20 117.3(3) . . ?
C11 C16 C20 122.9(3) . . ?
C12 C17 C19 112.6(3) . . ?
C12 C17 C18 111.2(3) . . ?
C19 C17 C18 109.0(2) . . ?
C16 C20 C21 111.3(3) . . ?
C16 C20 C22 112.5(3) . . ?
C21 C20 C22 109.3(3) . . ?
C36 C31 C32 118.0(2) . . ?
C36 C31 N2 121.2(2) . . ?
C32 C31 N2 120.8(2) . . ?
C33 C32 C31 119.2(3) . . ?
C33 C32 C37 118.6(3) . . ?
C31 C32 C37 122.2(2) . . ?
C34 C33 C32 122.5(3) . . ?
C33 C34 C35 118.7(3) . . ?
C34 C35 C36 121.8(3) . . ?
C35 C36 C31 119.8(3) . . ?
C35 C36 C40 117.1(3) . . ?
C31 C36 C40 123.2(2) . . ?
C32 C37 C38 110.6(3) . . ?
C32 C37 C39 112.5(3) . . ?
C38 C37 C39 109.3(3) . . ?
C36 C40 C42 112.4(3) . . ?
C36 C40 C41 111.2(3) . . ?
C42 C40 C41 109.2(3) . . ?
O1 C51 C52 106.0(3) . . ?
C53 C52 C51 103.4(3) . . ?
C52 C53 C54 101.9(4) . . ?
O1 C54 C53 106.4(3) . . ?
O2A C61A C62A 103.5(6) . . ?
C61A C62A C63A 102.9(7) . . ?
C64A C63A C62A 109.5(7) . . ?
O2A C64A C63A 104.5(6) . . ?
O2B C61B C62B 106.1(9) . . ?
C63B C62B C61B 108.3(10) . . ?
C64B C63B C62B 103.2(11) . . ?
C63B C64B O2B 121.6(12) . . ?
C72A C71A O3 107.9(6) . . ?
C71A C72A C73A 102.5(6) . . ?
C72A C73A C74A 102.0(7) . . ?
O3 C74A C73A 107.5(7) . . ?
C72B C71B O3 107.5(8) . . ?
C71B C72B C73B 106.3(8) . . ?
C74B C73B C72B 103.7(7) . . ?
O3 C74B C73B 107.1(6) . . ?
O3 Li O1 111.7(3) . . ?
O3 Li O2A 112.4(3) . . ?
O1 Li O2A 103.9(3) . . ?
O3 Li O2B 98.5(4) . . ?
O1 Li O2B 114.2(4) . . ?
O3 Li Cl 112.5(3) . . ?
O1 Li Cl 114.2(3) . . ?
O2A Li Cl 101.4(3) . . ?
O2B Li Cl 104.5(4) . . ?
C4S O1S C1S 113.6(10) . . ?
O1S C1S C2S 100.9(11) . . ?
C1S C2S C3S 104.2(11) . . ?
C4S C3S C2S 103.8(11) . . ?
O1S C4S C3S 105.1(10) . . ?

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
N3 Zr Cl Li -75.0(2) . . . . ?
N4 Zr Cl Li 31.6(2) . . . . ?
N1 Zr Cl Li 141.9(2) . . . . ?
N2 Zr Cl Li 172.1(2) . . . . ?
N2 Si N1 C11 161.7(2) . . . . ?
C4 Si N1 C11 42.1(3) . . . . ?
C1 Si N1 C11 -76.8(2) . . . . ?
N2 Si N1 Zr -11.82(10) . . . . ?
C4 Si N1 Zr -131.45(12) . . . . ?
C1 Si N1 Zr 109.68(12) . . . . ?
N3 Zr N1 C11 88.1(3) . . . . ?
N4 Zr N1 C11 -23.3(3) . . . . ?
N2 Zr N1 C11 -162.4(3) . . . . ?
Cl Zr N1 C11 -130.9(2) . . . . ?
N3 Zr N1 Si -99.61(11) . . . . ?
N4 Zr N1 Si 149.00(10) . . . . ?
N2 Zr N1 Si 9.92(9) . . . . ?
Cl Zr N1 Si 41.44(19) . . . . ?
N1 Si N2 C31 -150.9(2) . . . . ?
C4 Si N2 C31 -31.1(3) . . . . ?
C1 Si N2 C31 96.5(2) . . . . ?
N1 Si N2 Zr 11.77(10) . . . . ?
C4 Si N2 Zr 131.52(12) . . . . ?
C1 Si N2 Zr -100.88(13) . . . . ?
N3 Zr N2 C31 -107.6(2) . . . . ?
N4 Zr N2 C31 63.5(3) . . . . ?
N1 Zr N2 C31 150.0(3) . . . . ?
Cl Zr N2 C31 -16.9(2) . . . . ?
N3 Zr N2 Si 92.46(11) . . . . ?
N4 Zr N2 Si -96.48(15) . . . . ?
N1 Zr N2 Si -9.98(9) . . . . ?
Cl Zr N2 Si -176.80(9) . . . . ?
N4 Zr N3 C7 34.4(3) . . . . ?
N1 Zr N3 C7 -72.7(3) . . . . ?
N2 Zr N3 C7 -151.6(3) . . . . ?
Cl Zr N3 C7 123.1(3) . . . . ?
N4 Zr N3 C8 -142.0(2) . . . . ?
N1 Zr N3 C8 110.9(2) . . . . ?
N2 Zr N3 C8 32.0(3) . . . . ?
Cl Zr N3 C8 -53.2(2) . . . . ?
N3 Zr N4 C9 -57.4(2) . . . . ?
N1 Zr N4 C9 54.8(2) . . . . ?
N2 Zr N4 C9 131.2(2) . . . . ?
Cl Zr N4 C9 -149.7(2) . . . . ?
N3 Zr N4 C10 115.2(3) . . . . ?
N1 Zr N4 C10 -132.7(3) . . . . ?
N2 Zr N4 C10 -56.2(4) . . . . ?
Cl Zr N4 C10 22.8(3) . . . . ?
N2 Si C1 C3 -89.1(3) . . . . ?
N1 Si C1 C3 165.5(2) . . . . ?
C4 Si C1 C3 41.9(3) . . . . ?
N2 Si C1 C2 41.7(3) . . . . ?
N1 Si C1 C2 -63.6(2) . . . . ?
C4 Si C1 C2 172.8(2) . . . . ?
N2 Si C4 C5 -176.6(2) . . . . ?
N1 Si C4 C5 -68.7(3) . . . . ?
C1 Si C4 C5 50.3(3) . . . . ?
N2 Si C4 C6 56.5(3) . . . . ?
N1 Si C4 C6 164.3(2) . . . . ?
C1 Si C4 C6 -76.6(2) . . . . ?
Si N1 C11 C16 -82.5(3) . . . . ?
Zr N1 C11 C16 87.9(3) . . . . ?
Si N1 C11 C12 98.4(3) . . . . ?
Zr N1 C11 C12 -91.2(3) . . . . ?
N1 C11 C12 C13 -176.5(3) . . . . ?
C16 C11 C12 C13 4.4(4) . . . . ?
N1 C11 C12 C17 5.7(4) . . . . ?
C16 C11 C12 C17 -173.4(3) . . . . ?
C11 C12 C13 C14 -1.9(5) . . . . ?
C17 C12 C13 C14 176.1(3) . . . . ?
C12 C13 C14 C15 -1.4(5) . . . . ?
C13 C14 C15 C16 2.0(5) . . . . ?
C14 C15 C16 C11 0.7(5) . . . . ?
C14 C15 C16 C20 -177.3(3) . . . . ?
N1 C11 C16 C15 177.0(3) . . . . ?
C12 C11 C16 C15 -3.8(4) . . . . ?
N1 C11 C16 C20 -5.1(4) . . . . ?
C12 C11 C16 C20 174.0(3) . . . . ?
C13 C12 C17 C19 62.6(4) . . . . ?
C11 C12 C17 C19 -119.6(3) . . . . ?
C13 C12 C17 C18 -60.1(4) . . . . ?
C11 C12 C17 C18 117.8(3) . . . . ?
C15 C16 C20 C21 70.6(4) . . . . ?
C11 C16 C20 C21 -107.3(3) . . . . ?
C15 C16 C20 C22 -52.4(4) . . . . ?
C11 C16 C20 C22 129.6(3) . . . . ?
Si N2 C31 C36 88.0(3) . . . . ?
Zr N2 C31 C36 -66.9(3) . . . . ?
Si N2 C31 C32 -93.5(3) . . . . ?
Zr N2 C31 C32 111.6(3) . . . . ?
C36 C31 C32 C33 -1.2(4) . . . . ?
N2 C31 C32 C33 -179.7(3) . . . . ?
C36 C31 C32 C37 176.2(3) . . . . ?
N2 C31 C32 C37 -2.3(4) . . . . ?
C31 C32 C33 C34 0.3(5) . . . . ?
C37 C32 C33 C34 -177.2(3) . . . . ?
C32 C33 C34 C35 0.0(5) . . . . ?
C33 C34 C35 C36 0.6(5) . . . . ?
C34 C35 C36 C31 -1.5(5) . . . . ?
C34 C35 C36 C40 177.8(3) . . . . ?
C32 C31 C36 C35 1.8(4) . . . . ?
N2 C31 C36 C35 -179.7(3) . . . . ?
C32 C31 C36 C40 -177.5(3) . . . . ?
N2 C31 C36 C40 1.1(4) . . . . ?
C33 C32 C37 C38 69.8(4) . . . . ?
C31 C32 C37 C38 -107.7(3) . . . . ?
C33 C32 C37 C39 -52.8(4) . . . . ?
C31 C32 C37 C39 129.8(3) . . . . ?
C35 C36 C40 C42 57.4(4) . . . . ?
C31 C36 C40 C42 -123.3(3) . . . . ?
C35 C36 C40 C41 -65.4(4) . . . . ?
C31 C36 C40 C41 113.9(3) . . . . ?
C54 O1 C51 C52 -7.6(4) . . . . ?
Li O1 C51 C52 -171.5(3) . . . . ?
O1 C51 C52 C53 28.1(4) . . . . ?
C51 C52 C53 C54 -36.8(5) . . . . ?
C51 O1 C54 C53 -16.0(4) . . . . ?
Li O1 C54 C53 149.5(3) . . . . ?
C52 C53 C54 O1 33.0(5) . . . . ?
C64A O2A C61A C62A -18.1(8) . . . . ?
Li O2A C61A C62A 158.9(5) . . . . ?
O2A C61A C62A C63A 22.5(9) . . . . ?
C61A C62A C63A C64A -21.6(10) . . . . ?
C61A O2A C64A C63A 4.5(8) . . . . ?
Li O2A C64A C63A -172.0(6) . . . . ?
C62A C63A C64A O2A 10.9(9) . . . . ?
C64B O2B C61B C62B -5.6(12) . . . . ?
Li O2B C61B C62B 146.1(8) . . . . ?
O2B C61B C62B C63B 2.1(14) . . . . ?
C61B C62B C63B C64B 2.4(15) . . . . ?
C62B C63B C64B O2B -7.4(18) . . . . ?
C61B O2B C64B C63B 8.5(16) . . . . ?
Li O2B C64B C63B -143.0(11) . . . . ?
C74A O3 C71A C72A 21.4(8) . . . . ?
Li O3 C71A C72A -175.2(5) . . . . ?
O3 C71A C72A C73A -33.1(8) . . . . ?
C71A C72A C73A C74A 31.7(9) . . . . ?
C71A O3 C74A C73A 0.5(9) . . . . ?
Li O3 C74A C73A -161.2(5) . . . . ?
C72A C73A C74A O3 -19.9(10) . . . . ?
C74B O3 C71B C72B -5.4(10) . . . . ?
Li O3 C71B C72B 166.4(7) . . . . ?
O3 C71B C72B C73B 16.6(11) . . . . ?
C71B C72B C73B C74B -21.8(11) . . . . ?
C71B O3 C74B C73B -9.1(8) . . . . ?
Li O3 C74B C73B -178.9(5) . . . . ?
C72B C73B C74B O3 18.2(9) . . . . ?
C74A O3 Li O1 -56.7(7) . . . . ?
C71B O3 Li O1 169.2(5) . . . . ?
C74B O3 Li O1 -21.4(7) . . . . ?
C71A O3 Li O1 143.6(5) . . . . ?
C74A O3 Li O2A 59.6(7) . . . . ?
C71A O3 Li O2A -100.2(5) . . . . ?
C71B O3 Li O2B -70.5(6) . . . . ?
C74B O3 Li O2B 99.0(6) . . . . ?
C74A O3 Li Cl 173.3(6) . . . . ?
C71B O3 Li Cl 39.2(6) . . . . ?
C74B O3 Li Cl -151.4(5) . . . . ?
C71A O3 Li Cl 13.5(6) . . . . ?
C51 O1 Li O3 -17.1(5) . . . . ?
C54 O1 Li O3 -179.2(3) . . . . ?
C51 O1 Li O2A -138.4(3) . . . . ?
C54 O1 Li O2A 59.4(4) . . . . ?
C51 O1 Li O2B -127.8(5) . . . . ?
C54 O1 Li O2B 70.0(5) . . . . ?
C51 O1 Li Cl 112.0(4) . . . . ?
C54 O1 Li Cl -50.1(4) . . . . ?
C64A O2A Li O3 -126.8(5) . . . . ?
C61A O2A Li O3 56.8(6) . . . . ?
C64A O2A Li O1 -5.9(6) . . . . ?
C61A O2A Li O1 177.7(5) . . . . ?
C64A O2A Li Cl 112.9(5) . . . . ?
C61A O2A Li Cl -63.6(6) . . . . ?
C64B O2B Li O3 -106.0(10) . . . . ?
C61B O2B Li O3 109.5(9) . . . . ?
C64B O2B Li O1 12.4(12) . . . . ?
C61B O2B Li O1 -132.0(9) . . . . ?
C64B O2B Li Cl 137.9(10) . . . . ?
C61B O2B Li Cl -6.5(10) . . . . ?
Zr Cl Li O3 24.6(4) . . . . ?
Zr Cl Li O1 -104.0(3) . . . . ?
Zr Cl Li O2A 144.91(19) . . . . ?
Zr Cl Li O2B 130.5(3) . . . . ?
C4S O1S C1S C2S -25.0(17) . . . . ?
O1S C1S C2S C3S 33.8(16) . . . . ?
C1S C2S C3S C4S -32.5(16) . . . . ?
C1S O1S C4S C3S 4.7(17) . . . . ?
C2S C3S C4S O1S 17.0(16) . . . . ?

_refine_diff_density_max         0.773
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.070

_shelxl_version_number           2013-4

