#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:21:20 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179748 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/44/7004479.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7004479
loop_
_publ_author_name
'Herrmann, Heike'
'Gehrmann, Thorsten'
'Wadepohl, Hubert'
'Gade, Lutz H.'
_publ_section_title
;
 Zirconium and hafnium (1-pyridinio)imido complexes: functionalized
 terminal hydrazinediido analogues
;
_journal_issue                   44
_journal_name_full               'Dalton Transactions'
_journal_page_first              6231
_journal_page_last               6241
_journal_paper_doi               10.1039/b807808d
_journal_year                    2008
_chemical_formula_sum            'C46 H64 N6 Si2 Zr'
_chemical_formula_weight         848.43
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_hh19
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.3620(10)
_cell_angle_beta                 80.6460(10)
_cell_angle_gamma                74.071(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0651(8)
_cell_length_b                   14.2917(11)
_cell_length_c                   15.7951(11)
_cell_measurement_temperature    100(2)
_cell_volume                     2268.3(3)
_computing_cell_refinement       'SAINT (Bruker AXS, 1997-2006)'
_computing_data_collection       'SMART (Bruker AXS, 1997-2003)'
_computing_data_reduction        'SAINT (Bruker AXS, 1997-2006)'
_computing_molecular_graphics    'PLATON (Spek, 1980-2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector (Bruker AXS Smart 1000)'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0772
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            37559
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.92
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.333
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2004-2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.053
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         7996
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0718P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1187
_refine_ls_wR_factor_ref         0.1286
_reflns_number_gt                5613
_reflns_number_total             7996
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b807808d.txt
_cod_data_source_block           complex_5
_cod_database_code               7004479
#BEGIN Tags that were not found in dictionaries:
_audit_block_refno               574
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3618(3) 0.2356(3) 0.0269(2) 0.0231(8) Uani 1 1 d . . .
H1A H 0.3429 0.2996 -0.0224 0.028 Uiso 1 1 calc R . .
H1B H 0.3361 0.1834 0.0099 0.028 Uiso 1 1 calc R . .
C2 C 0.5058(3) 0.2026(3) 0.0319(2) 0.0223(8) Uani 1 1 d . . .
C3 C 0.5469(4) 0.1028(3) 0.1081(2) 0.0250(9) Uani 1 1 d . . .
H3A H 0.5120 0.0503 0.0989 0.030 Uiso 1 1 calc R . .
H3B H 0.6399 0.0800 0.1006 0.030 Uiso 1 1 calc R . .
C4 C 0.5605(4) 0.1745(3) -0.0551(2) 0.0274(9) Uani 1 1 d . . .
H4A H 0.5344 0.2333 -0.1068 0.041 Uiso 1 1 calc R . .
H4B H 0.5291 0.1176 -0.0572 0.041 Uiso 1 1 calc R . .
H4C H 0.6527 0.1548 -0.0567 0.041 Uiso 1 1 calc R . .
C5 C 0.5548(3) 0.2876(3) 0.0403(2) 0.0220(8) Uani 1 1 d . . .
C6 C 0.6378(3) 0.3348(3) -0.0242(2) 0.0233(8) Uani 1 1 d . . .
H6 H 0.6680 0.3122 -0.0759 0.028 Uiso 1 1 calc R . .
C7 C 0.6761(3) 0.4129(3) -0.0141(2) 0.0260(9) Uani 1 1 d . . .
H7 H 0.7320 0.4454 -0.0588 0.031 Uiso 1 1 calc R . .
C8 C 0.6330(3) 0.4449(3) 0.0617(2) 0.0248(9) Uani 1 1 d . . .
H8 H 0.6598 0.4984 0.0709 0.030 Uiso 1 1 calc R . .
C9 C 0.5500(3) 0.3966(3) 0.1234(2) 0.0231(8) Uani 1 1 d . . .
H9 H 0.5186 0.4188 0.1751 0.028 Uiso 1 1 calc R . .
C16 C 0.5212(4) -0.0010(3) 0.3946(2) 0.0255(9) Uani 1 1 d . . .
H16A H 0.5966 0.0171 0.4034 0.038 Uiso 1 1 calc R . .
H16B H 0.5138 -0.0658 0.4388 0.038 Uiso 1 1 calc R . .
H16C H 0.4463 0.0522 0.4024 0.038 Uiso 1 1 calc R . .
C17 C 0.4118(4) -0.0821(3) 0.2774(3) 0.0293(9) Uani 1 1 d . . .
H17A H 0.3291 -0.0472 0.2991 0.044 Uiso 1 1 calc R . .
H17B H 0.4341 -0.1522 0.3161 0.044 Uiso 1 1 calc R . .
H17C H 0.4085 -0.0825 0.2159 0.044 Uiso 1 1 calc R . .
C18 C 0.6953(4) -0.1015(3) 0.2643(2) 0.0268(9) Uani 1 1 d . . .
C21 C 0.7975(3) -0.0430(3) 0.2491(3) 0.0302(9) Uani 1 1 d . . .
H21A H 0.7885 -0.0123 0.2978 0.045 Uiso 1 1 calc R . .
H21B H 0.7888 0.0106 0.1917 0.045 Uiso 1 1 calc R . .
H21C H 0.8808 -0.0898 0.2480 0.045 Uiso 1 1 calc R . .
C20 C 0.7190(4) -0.1896(3) 0.3504(3) 0.0338(10) Uani 1 1 d . . .
H20A H 0.8040 -0.2326 0.3446 0.051 Uiso 1 1 calc R . .
H20B H 0.6567 -0.2301 0.3604 0.051 Uiso 1 1 calc R . .
H20C H 0.7115 -0.1626 0.4012 0.051 Uiso 1 1 calc R . .
C19 C 0.7051(4) -0.1484(3) 0.1868(3) 0.0354(10) Uani 1 1 d . . .
H19A H 0.7882 -0.1948 0.1835 0.053 Uiso 1 1 calc R . .
H19B H 0.6937 -0.0941 0.1301 0.053 Uiso 1 1 calc R . .
H19C H 0.6394 -0.1861 0.1979 0.053 Uiso 1 1 calc R . .
C10 C 0.0298(4) 0.3549(3) 0.1741(3) 0.0313(10) Uani 1 1 d . . .
H10A H 0.0461 0.3152 0.2361 0.047 Uiso 1 1 calc R . .
H10B H -0.0604 0.3693 0.1669 0.047 Uiso 1 1 calc R . .
H10C H 0.0553 0.4190 0.1600 0.047 Uiso 1 1 calc R . .
C11 C 0.0876(4) 0.3633(3) -0.0208(2) 0.0300(9) Uani 1 1 d . . .
H11A H 0.1232 0.4228 -0.0351 0.045 Uiso 1 1 calc R . .
H11B H -0.0038 0.3857 -0.0249 0.045 Uiso 1 1 calc R . .
H11C H 0.1257 0.3241 -0.0633 0.045 Uiso 1 1 calc R . .
C12 C 0.0584(3) 0.1634(3) 0.1199(2) 0.0241(8) Uani 1 1 d . . .
C15 C 0.0551(4) 0.1074(3) 0.2209(2) 0.0308(9) Uani 1 1 d . . .
H15A H 0.0185 0.0488 0.2328 0.046 Uiso 1 1 calc R . .
H15B H 0.0035 0.1537 0.2543 0.046 Uiso 1 1 calc R . .
H15C H 0.1410 0.0840 0.2398 0.046 Uiso 1 1 calc R . .
C14 C 0.1380(4) 0.0895(3) 0.0692(3) 0.0343(10) Uani 1 1 d . . .
H14A H 0.2224 0.0627 0.0909 0.051 Uiso 1 1 calc R . .
H14B H 0.1449 0.1252 0.0050 0.051 Uiso 1 1 calc R . .
H14C H 0.0979 0.0333 0.0791 0.051 Uiso 1 1 calc R . .
C13 C -0.0768(4) 0.1957(3) 0.0910(3) 0.0409(11) Uani 1 1 d . . .
H13A H -0.0760 0.2303 0.0265 0.061 Uiso 1 1 calc R . .
H13B H -0.1302 0.2419 0.1238 0.061 Uiso 1 1 calc R . .
H13C H -0.1104 0.1353 0.1043 0.061 Uiso 1 1 calc R . .
C22 C 0.1617(4) 0.0825(3) 0.4533(2) 0.0260(9) Uani 1 1 d . . .
H22 H 0.2123 0.0223 0.4405 0.031 Uiso 1 1 calc R . .
C23 C 0.0773(4) 0.0752(3) 0.5280(3) 0.0336(10) Uani 1 1 d . . .
H23 H 0.0712 0.0100 0.5665 0.040 Uiso 1 1 calc R . .
C24 C 0.0016(4) 0.1606(4) 0.5477(3) 0.0393(11) Uani 1 1 d . . .
H24 H -0.0570 0.1553 0.5992 0.047 Uiso 1 1 calc R . .
C25 C 0.0129(4) 0.2540(4) 0.4910(3) 0.0378(11) Uani 1 1 d . . .
H25 H -0.0382 0.3142 0.5034 0.045 Uiso 1 1 calc R . .
C26 C 0.0975(4) 0.2609(3) 0.4166(3) 0.0296(9) Uani 1 1 d . . .
H26 H 0.1036 0.3260 0.3778 0.035 Uiso 1 1 calc R . .
C32 C 0.2915(4) 0.3989(3) 0.2384(2) 0.0268(9) Uani 1 1 d . . .
C33 C 0.2522(3) 0.4849(3) 0.2453(2) 0.0230(8) Uani 1 1 d . . .
C34 C 0.2146(3) 0.5894(3) 0.2440(2) 0.0213(8) Uani 1 1 d . . .
C39 C 0.2819(4) 0.6278(3) 0.2863(3) 0.0346(10) Uani 1 1 d . . .
H39 H 0.3496 0.5835 0.3203 0.042 Uiso 1 1 calc R . .
C38 C 0.2505(5) 0.7308(4) 0.2791(3) 0.0511(13) Uani 1 1 d . . .
H38 H 0.2968 0.7565 0.3084 0.061 Uiso 1 1 calc R . .
C37 C 0.1546(5) 0.7951(3) 0.2306(3) 0.0503(14) Uani 1 1 d . . .
H37 H 0.1347 0.8655 0.2258 0.060 Uiso 1 1 calc R . .
C36 C 0.0868(4) 0.7595(3) 0.1890(3) 0.0430(12) Uani 1 1 d . . .
H36 H 0.0196 0.8049 0.1551 0.052 Uiso 1 1 calc R . .
C35 C 0.1154(4) 0.6568(3) 0.1959(3) 0.0309(10) Uani 1 1 d . . .
H35 H 0.0667 0.6321 0.1674 0.037 Uiso 1 1 calc R . .
C31 C 0.6442(4) 0.2135(3) 0.3042(3) 0.0264(9) Uani 1 1 d . . .
H31 H 0.6778 0.1931 0.2519 0.032 Uiso 1 1 calc R . .
C30 C 0.7261(4) 0.2160(3) 0.3590(3) 0.0362(10) Uani 1 1 d . . .
H30 H 0.8145 0.1978 0.3445 0.043 Uiso 1 1 calc R . .
C29 C 0.6792(4) 0.2454(3) 0.4361(3) 0.0412(11) Uani 1 1 d . . .
H29 H 0.7343 0.2482 0.4750 0.049 Uiso 1 1 calc R . .
C28 C 0.5512(4) 0.2701(3) 0.4542(3) 0.0357(10) Uani 1 1 d . . .
H28 H 0.5158 0.2892 0.5070 0.043 Uiso 1 1 calc R . .
C27 C 0.4746(4) 0.2672(3) 0.3957(2) 0.0267(9) Uani 1 1 d . . .
H27 H 0.3859 0.2864 0.4086 0.032 Uiso 1 1 calc R . .
N1 N 0.2815(3) 0.2519(2) 0.10740(19) 0.0213(7) Uani 1 1 d . . .
N2 N 0.5116(3) 0.1045(2) 0.20182(18) 0.0196(7) Uani 1 1 d . . .
N3 N 0.5114(3) 0.3202(2) 0.11396(19) 0.0218(7) Uani 1 1 d . . .
N4 N 0.2558(3) 0.1825(2) 0.32500(19) 0.0225(7) Uani 1 1 d . . .
N5 N 0.1736(3) 0.1751(2) 0.3974(2) 0.0239(7) Uani 1 1 d . . .
N6 N 0.5184(3) 0.2386(2) 0.32086(19) 0.0205(7) Uani 1 1 d . . .
Si1 Si 0.12195(10) 0.28093(8) 0.09662(7) 0.0224(2) Uani 1 1 d . . .
Si2 Si 0.53428(10) -0.01351(8) 0.27944(7) 0.0218(2) Uani 1 1 d . . .
Zr Zr 0.36823(3) 0.23396(3) 0.22192(2) 0.01854(12) Uani 1 1 d . . .
C40 C 0.7238(4) 0.5245(3) 0.3322(3) 0.0409(11) Uani 1 1 d . . .
C41 C 0.8453(4) 0.5343(3) 0.3223(3) 0.0469(12) Uani 1 1 d . . .
H41 H 0.8941 0.5343 0.2669 0.056 Uiso 1 1 calc R . .
C42 C 0.8976(5) 0.5442(4) 0.3905(4) 0.0562(14) Uani 1 1 d . . .
H42 H 0.9823 0.5503 0.3827 0.067 Uiso 1 1 calc R . .
C43 C 0.8275(6) 0.5452(4) 0.4705(4) 0.0554(14) Uani 1 1 d . . .
H43 H 0.8635 0.5532 0.5176 0.066 Uiso 1 1 calc R . .
C45 C 0.6564(5) 0.5244(4) 0.4134(3) 0.0495(13) Uani 1 1 d . . .
H45 H 0.5722 0.5170 0.4219 0.059 Uiso 1 1 calc R . .
C46 C 0.6678(6) 0.5139(5) 0.2563(4) 0.0708(17) Uani 1 1 d . . .
H46A H 0.7357 0.4880 0.2154 0.106 Uiso 1 1 calc R . .
H46B H 0.6185 0.5805 0.2237 0.106 Uiso 1 1 calc R . .
H46C H 0.6129 0.4665 0.2801 0.106 Uiso 1 1 calc R . .
C44 C 0.7075(5) 0.5349(3) 0.4825(3) 0.0500(13) Uani 1 1 d . . .
H44 H 0.6592 0.5349 0.5381 0.060 Uiso 1 1 calc R . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 118.3(3) . . ?
N1 C1 H1A 107.7 . . ?
C2 C1 H1A 107.7 . . ?
N1 C1 H1B 107.7 . . ?
C2 C1 H1B 107.7 . . ?
H1A C1 H1B 107.1 . . ?
C5 C2 C4 111.7(3) . . ?
C5 C2 C1 110.5(3) . . ?
C4 C2 C1 105.7(3) . . ?
C5 C2 C3 111.7(3) . . ?
C4 C2 C3 104.7(3) . . ?
C1 C2 C3 112.4(3) . . ?
N2 C3 C2 118.4(3) . . ?
N2 C3 H3A 107.7 . . ?
C2 C3 H3A 107.7 . . ?
N2 C3 H3B 107.7 . . ?
C2 C3 H3B 107.7 . . ?
H3A C3 H3B 107.1 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 C6 119.6(3) . . ?
N3 C5 C2 117.1(3) . . ?
C6 C5 C2 123.3(3) . . ?
C7 C6 C5 120.7(4) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C8 119.5(3) . . ?
C6 C7 H7 120.2 . . ?
C8 C7 H7 120.2 . . ?
C9 C8 C7 117.7(4) . . ?
C9 C8 H8 121.1 . . ?
C7 C8 H8 121.1 . . ?
N3 C9 C8 123.2(3) . . ?
N3 C9 H9 118.4 . . ?
C8 C9 H9 118.4 . . ?
Si2 C16 H16A 109.5 . . ?
Si2 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si2 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si2 C17 H17A 109.5 . . ?
Si2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C21 C18 C20 107.8(3) . . ?
C21 C18 C19 110.6(3) . . ?
C20 C18 C19 107.3(3) . . ?
C21 C18 Si2 109.2(3) . . ?
C20 C18 Si2 109.0(3) . . ?
C19 C18 Si2 112.9(3) . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si1 C10 H10A 109.5 . . ?
Si1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si1 C11 H11A 109.5 . . ?
Si1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C14 C12 C15 108.6(3) . . ?
C14 C12 C13 108.0(3) . . ?
C15 C12 C13 108.5(3) . . ?
C14 C12 Si1 112.4(3) . . ?
C15 C12 Si1 109.9(3) . . ?
C13 C12 Si1 109.4(3) . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N5 C22 C23 120.7(4) . . ?
N5 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C24 C23 C22 121.2(4) . . ?
C24 C23 H23 119.4 . . ?
C22 C23 H23 119.4 . . ?
C23 C24 C25 118.2(4) . . ?
C23 C24 H24 120.9 . . ?
C25 C24 H24 120.9 . . ?
C26 C25 C24 120.5(4) . . ?
C26 C25 H25 119.7 . . ?
C24 C25 H25 119.7 . . ?
C25 C26 N5 121.1(4) . . ?
C25 C26 H26 119.5 . . ?
N5 C26 H26 119.5 . . ?
C33 C32 Zr 178.9(3) . . ?
C32 C33 C34 173.4(4) . . ?
C39 C34 C35 118.0(4) . . ?
C39 C34 C33 120.4(4) . . ?
C35 C34 C33 121.5(3) . . ?
C34 C39 C38 120.0(4) . . ?
C34 C39 H39 120.0 . . ?
C38 C39 H39 120.0 . . ?
C37 C38 C39 120.8(4) . . ?
C37 C38 H38 119.6 . . ?
C39 C38 H38 119.6 . . ?
C38 C37 C36 120.4(4) . . ?
C38 C37 H37 119.8 . . ?
C36 C37 H37 119.8 . . ?
C37 C36 C35 120.0(4) . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C36 C35 C34 120.8(4) . . ?
C36 C35 H35 119.6 . . ?
C34 C35 H35 119.6 . . ?
N6 C31 C30 123.1(4) . . ?
N6 C31 H31 118.4 . . ?
C30 C31 H31 118.4 . . ?
C31 C30 C29 119.5(4) . . ?
C31 C30 H30 120.3 . . ?
C29 C30 H30 120.3 . . ?
C28 C29 C30 117.9(4) . . ?
C28 C29 H29 121.0 . . ?
C30 C29 H29 121.0 . . ?
C29 C28 C27 119.5(4) . . ?
C29 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
N6 C27 C28 123.4(4) . . ?
N6 C27 H27 118.3 . . ?
C28 C27 H27 118.3 . . ?
C1 N1 Si1 114.5(2) . . ?
C1 N1 Zr 118.6(2) . . ?
Si1 N1 Zr 126.88(16) . . ?
C3 N2 Si2 114.5(2) . . ?
C3 N2 Zr 116.2(2) . . ?
Si2 N2 Zr 123.01(15) . . ?
C9 N3 C5 119.3(3) . . ?
C9 N3 Zr 123.5(2) . . ?
C5 N3 Zr 117.2(2) . . ?
N5 N4 Zr 163.0(2) . . ?
N4 N5 C22 120.9(3) . . ?
N4 N5 C26 120.7(3) . . ?
C22 N5 C26 118.4(3) . . ?
C31 N6 C27 116.6(3) . . ?
C31 N6 Zr 123.4(2) . . ?
C27 N6 Zr 120.0(2) . . ?
N1 Si1 C10 111.58(17) . . ?
N1 Si1 C11 109.67(16) . . ?
C10 Si1 C11 106.72(18) . . ?
N1 Si1 C12 112.80(15) . . ?
C10 Si1 C12 107.63(18) . . ?
C11 Si1 C12 108.20(17) . . ?
N2 Si2 C16 110.21(16) . . ?
N2 Si2 C17 111.60(16) . . ?
C16 Si2 C17 107.16(17) . . ?
N2 Si2 C18 114.22(16) . . ?
C16 Si2 C18 106.23(17) . . ?
C17 Si2 C18 107.04(17) . . ?
N4 Zr N1 106.51(12) . . ?
N4 Zr N2 106.88(12) . . ?
N1 Zr N2 92.51(11) . . ?
N4 Zr C32 89.99(12) . . ?
N1 Zr C32 100.04(12) . . ?
N2 Zr C32 155.25(12) . . ?
N4 Zr N3 167.46(11) . . ?
N1 Zr N3 82.98(11) . . ?
N2 Zr N3 80.36(10) . . ?
C32 Zr N3 80.11(11) . . ?
N4 Zr N6 91.65(11) . . ?
N1 Zr N6 161.76(10) . . ?
N2 Zr N6 83.70(10) . . ?
C32 Zr N6 77.71(11) . . ?
N3 Zr N6 78.79(10) . . ?
C41 C40 C45 117.8(4) . . ?
C41 C40 C46 120.3(4) . . ?
C45 C40 C46 121.9(5) . . ?
C42 C41 C40 121.1(5) . . ?
C42 C41 H41 119.5 . . ?
C40 C41 H41 119.5 . . ?
C41 C42 C43 119.9(5) . . ?
C41 C42 H42 120.1 . . ?
C43 C42 H42 120.1 . . ?
C44 C43 C42 120.4(5) . . ?
C44 C43 H43 119.8 . . ?
C42 C43 H43 119.8 . . ?
C40 C45 C44 121.8(5) . . ?
C40 C45 H45 119.1 . . ?
C44 C45 H45 119.1 . . ?
C40 C46 H46A 109.5 . . ?
C40 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C40 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C43 C44 C45 119.1(5) . . ?
C43 C44 H44 120.5 . . ?
C45 C44 H44 120.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.473(4) . ?
C1 C2 1.540(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C5 1.509(5) . ?
C2 C4 1.538(5) . ?
C2 C3 1.553(5) . ?
C3 N2 1.475(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 N3 1.357(4) . ?
C5 C6 1.390(5) . ?
C6 C7 1.359(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.384(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.378(5) . ?
C8 H8 0.9500 . ?
C9 N3 1.332(4) . ?
C9 H9 0.9500 . ?
C16 Si2 1.863(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 Si2 1.888(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C21 1.529(5) . ?
C18 C20 1.531(5) . ?
C18 C19 1.549(5) . ?
C18 Si2 1.907(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C10 Si1 1.867(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 Si1 1.886(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C14 1.528(5) . ?
C12 C15 1.538(5) . ?
C12 C13 1.539(5) . ?
C12 Si1 1.903(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C22 N5 1.364(5) . ?
C22 C23 1.376(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.373(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.375(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.374(5) . ?
C25 H25 0.9500 . ?
C26 N5 1.376(5) . ?
C26 H26 0.9500 . ?
C32 C33 1.220(5) . ?
C32 Zr 2.359(4) . ?
C33 C34 1.431(5) . ?
C34 C39 1.387(5) . ?
C34 C35 1.389(5) . ?
C39 C38 1.388(6) . ?
C39 H39 0.9500 . ?
C38 C37 1.355(7) . ?
C38 H38 0.9500 . ?
C37 C36 1.356(7) . ?
C37 H37 0.9500 . ?
C36 C35 1.385(6) . ?
C36 H36 0.9500 . ?
C35 H35 0.9500 . ?
C31 N6 1.343(5) . ?
C31 C30 1.365(6) . ?
C31 H31 0.9500 . ?
C30 C29 1.389(6) . ?
C30 H30 0.9500 . ?
C29 C28 1.367(6) . ?
C29 H29 0.9500 . ?
C28 C27 1.368(5) . ?
C28 H28 0.9500 . ?
C27 N6 1.347(4) . ?
C27 H27 0.9500 . ?
N1 Si1 1.723(3) . ?
N1 Zr 2.095(3) . ?
N2 Si2 1.720(3) . ?
N2 Zr 2.154(3) . ?
N3 Zr 2.406(3) . ?
N4 N5 1.335(4) . ?
N4 Zr 1.954(3) . ?
N6 Zr 2.486(3) . ?
C40 C41 1.369(6) . ?
C40 C45 1.373(6) . ?
C40 C46 1.501(6) . ?
C41 C42 1.364(7) . ?
C41 H41 0.9500 . ?
C42 C43 1.373(7) . ?
C42 H42 0.9500 . ?
C43 C44 1.352(7) . ?
C43 H43 0.9500 . ?
C45 C44 1.374(7) . ?
C45 H45 0.9500 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C44 H44 0.9500 . ?
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 C1 C2 C5 -68.4(4) . . . . ?
N1 C1 C2 C4 170.6(3) . . . . ?
N1 C1 C2 C3 57.1(4) . . . . ?
C5 C2 C3 N2 57.5(4) . . . . ?
C4 C2 C3 N2 178.5(3) . . . . ?
C1 C2 C3 N2 -67.3(4) . . . . ?
C4 C2 C5 N3 178.9(3) . . . . ?
C1 C2 C5 N3 61.6(4) . . . . ?
C3 C2 C5 N3 -64.2(4) . . . . ?
C4 C2 C5 C6 0.9(5) . . . . ?
C1 C2 C5 C6 -116.5(4) . . . . ?
C3 C2 C5 C6 117.7(4) . . . . ?
N3 C5 C6 C7 0.2(5) . . . . ?
C2 C5 C6 C7 178.2(3) . . . . ?
C5 C6 C7 C8 0.8(5) . . . . ?
C6 C7 C8 C9 -1.4(5) . . . . ?
C7 C8 C9 N3 1.1(5) . . . . ?
N5 C22 C23 C24 0.8(6) . . . . ?
C22 C23 C24 C25 -0.4(6) . . . . ?
C23 C24 C25 C26 0.3(6) . . . . ?
C24 C25 C26 N5 -0.6(6) . . . . ?
Zr C32 C33 C34 -21(20) . . . . ?
C32 C33 C34 C39 -92(4) . . . . ?
C32 C33 C34 C35 84(4) . . . . ?
C35 C34 C39 C38 -0.8(6) . . . . ?
C33 C34 C39 C38 175.2(4) . . . . ?
C34 C39 C38 C37 -0.2(7) . . . . ?
C39 C38 C37 C36 0.6(7) . . . . ?
C38 C37 C36 C35 0.0(7) . . . . ?
C37 C36 C35 C34 -1.1(6) . . . . ?
C39 C34 C35 C36 1.4(6) . . . . ?
C33 C34 C35 C36 -174.5(4) . . . . ?
N6 C31 C30 C29 0.2(6) . . . . ?
C31 C30 C29 C28 0.5(7) . . . . ?
C30 C29 C28 C27 -1.3(7) . . . . ?
C29 C28 C27 N6 1.6(6) . . . . ?
C2 C1 N1 Si1 -176.2(2) . . . . ?
C2 C1 N1 Zr 1.9(4) . . . . ?
C2 C3 N2 Si2 168.0(3) . . . . ?
C2 C3 N2 Zr 14.9(4) . . . . ?
C8 C9 N3 C5 -0.2(5) . . . . ?
C8 C9 N3 Zr 179.3(3) . . . . ?
C6 C5 N3 C9 -0.5(5) . . . . ?
C2 C5 N3 C9 -178.6(3) . . . . ?
C6 C5 N3 Zr 180.0(2) . . . . ?
C2 C5 N3 Zr 1.8(4) . . . . ?
Zr N4 N5 C22 -161.7(7) . . . . ?
Zr N4 N5 C26 19.3(10) . . . . ?
C23 C22 N5 N4 179.8(3) . . . . ?
C23 C22 N5 C26 -1.1(5) . . . . ?
C25 C26 N5 N4 -179.9(3) . . . . ?
C25 C26 N5 C22 1.0(5) . . . . ?
C30 C31 N6 C27 0.0(5) . . . . ?
C30 C31 N6 Zr -179.8(3) . . . . ?
C28 C27 N6 C31 -1.0(5) . . . . ?
C28 C27 N6 Zr 178.9(3) . . . . ?
C1 N1 Si1 C10 -154.5(2) . . . . ?
Zr N1 Si1 C10 27.6(2) . . . . ?
C1 N1 Si1 C11 -36.5(3) . . . . ?
Zr N1 Si1 C11 145.6(2) . . . . ?
C1 N1 Si1 C12 84.2(3) . . . . ?
Zr N1 Si1 C12 -93.8(2) . . . . ?
C14 C12 Si1 N1 -48.9(3) . . . . ?
C15 C12 Si1 N1 72.1(3) . . . . ?
C13 C12 Si1 N1 -168.9(3) . . . . ?
C14 C12 Si1 C10 -172.4(3) . . . . ?
C15 C12 Si1 C10 -51.4(3) . . . . ?
C13 C12 Si1 C10 67.6(3) . . . . ?
C14 C12 Si1 C11 72.6(3) . . . . ?
C15 C12 Si1 C11 -166.4(3) . . . . ?
C13 C12 Si1 C11 -47.4(3) . . . . ?
C3 N2 Si2 C16 167.3(3) . . . . ?
Zr N2 Si2 C16 -41.7(2) . . . . ?
C3 N2 Si2 C17 -73.8(3) . . . . ?
Zr N2 Si2 C17 77.3(2) . . . . ?
C3 N2 Si2 C18 47.8(3) . . . . ?
Zr N2 Si2 C18 -161.17(17) . . . . ?
C21 C18 Si2 N2 46.2(3) . . . . ?
C20 C18 Si2 N2 163.7(2) . . . . ?
C19 C18 Si2 N2 -77.3(3) . . . . ?
C21 C18 Si2 C16 -75.5(3) . . . . ?
C20 C18 Si2 C16 42.0(3) . . . . ?
C19 C18 Si2 C16 161.0(3) . . . . ?
C21 C18 Si2 C17 170.2(3) . . . . ?
C20 C18 Si2 C17 -72.3(3) . . . . ?
C19 C18 Si2 C17 46.8(3) . . . . ?
N5 N4 Zr N1 -108.9(9) . . . . ?
N5 N4 Zr N2 153.2(8) . . . . ?
N5 N4 Zr C32 -8.4(9) . . . . ?
N5 N4 Zr N3 29.2(12) . . . . ?
N5 N4 Zr N6 69.3(9) . . . . ?
C1 N1 Zr N4 -147.4(2) . . . . ?
Si1 N1 Zr N4 30.4(2) . . . . ?
C1 N1 Zr N2 -39.0(3) . . . . ?
Si1 N1 Zr N2 138.83(19) . . . . ?
C1 N1 Zr C32 119.6(2) . . . . ?
Si1 N1 Zr C32 -62.6(2) . . . . ?
C1 N1 Zr N3 40.9(2) . . . . ?
Si1 N1 Zr N3 -141.2(2) . . . . ?
C1 N1 Zr N6 38.4(5) . . . . ?
Si1 N1 Zr N6 -143.8(3) . . . . ?
C3 N2 Zr N4 138.1(2) . . . . ?
Si2 N2 Zr N4 -12.4(2) . . . . ?
C3 N2 Zr N1 30.0(3) . . . . ?
Si2 N2 Zr N1 -120.54(19) . . . . ?
C3 N2 Zr C32 -90.8(4) . . . . ?
Si2 N2 Zr C32 118.7(3) . . . . ?
C3 N2 Zr N3 -52.4(2) . . . . ?
Si2 N2 Zr N3 157.0(2) . . . . ?
C3 N2 Zr N6 -132.1(3) . . . . ?
Si2 N2 Zr N6 77.36(18) . . . . ?
C33 C32 Zr N4 -152(17) . . . . ?
C33 C32 Zr N1 -45(17) . . . . ?
C33 C32 Zr N2 75(17) . . . . ?
C33 C32 Zr N3 36(17) . . . . ?
C33 C32 Zr N6 117(17) . . . . ?
C9 N3 Zr N4 -5.7(7) . . . . ?
C5 N3 Zr N4 173.8(5) . . . . ?
C9 N3 Zr N1 134.2(3) . . . . ?
C5 N3 Zr N1 -46.3(3) . . . . ?
C9 N3 Zr N2 -132.0(3) . . . . ?
C5 N3 Zr N2 47.5(3) . . . . ?
C9 N3 Zr C32 32.7(3) . . . . ?
C5 N3 Zr C32 -147.8(3) . . . . ?
C9 N3 Zr N6 -46.6(3) . . . . ?
C5 N3 Zr N6 132.9(3) . . . . ?
C31 N6 Zr N4 141.7(3) . . . . ?
C27 N6 Zr N4 -38.2(3) . . . . ?
C31 N6 Zr N1 -43.9(5) . . . . ?
C27 N6 Zr N1 136.2(3) . . . . ?
C31 N6 Zr N2 34.8(3) . . . . ?
C27 N6 Zr N2 -145.0(3) . . . . ?
C31 N6 Zr C32 -128.7(3) . . . . ?
C27 N6 Zr C32 51.4(3) . . . . ?
C31 N6 Zr N3 -46.5(3) . . . . ?
C27 N6 Zr N3 133.6(3) . . . . ?
C45 C40 C41 C42 -0.3(7) . . . . ?
C46 C40 C41 C42 179.9(5) . . . . ?
C40 C41 C42 C43 -0.6(8) . . . . ?
C41 C42 C43 C44 1.1(8) . . . . ?
C41 C40 C45 C44 0.7(7) . . . . ?
C46 C40 C45 C44 -179.5(5) . . . . ?
C42 C43 C44 C45 -0.7(7) . . . . ?
C40 C45 C44 C43 -0.2(7) . . . . ?
