#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:21:20 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179748 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/44/7004480.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_7004480
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            'C32 H55 F3 N6 O3 S Si2 Zr'
_chemical_formula_weight         808.28
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_hh17
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.1230(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4937(5)
_cell_length_b                   19.0633(9)
_cell_length_c                   20.8233(10)
_cell_measurement_temperature    100(2)
_cell_volume                     4072.7(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    'DIRDIF (Beurskens, 1999)'
_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  0.0665
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            98728
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.00
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.432
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2004-2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.089
_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   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         12423
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0436P)²+2.7786P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1063
_reflns_number_gt                8972
_reflns_number_total             12423
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b807808d.txt
_cod_data_source_block           complex_7
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7004480
#BEGIN Tags that were not found in dictionaries:
_audit_block_refno               527
#END Tags that were not found in dictionaries
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'
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 0.2255(2) 0.10686(12) 0.07563(11) 0.0289(5) Uani 1 1 d . . .
H1A H 0.3217 0.1041 0.0882 0.035 Uiso 1 1 calc R . .
H1B H 0.1986 0.0843 0.0321 0.035 Uiso 1 1 calc R . .
C2 C 0.1690(2) 0.06351(11) 0.12559(11) 0.0215(4) Uani 1 1 d . . .
C3 C 0.0184(2) 0.06775(12) 0.11193(12) 0.0279(5) Uani 1 1 d . . .
H3A H -0.0155 0.0534 0.0658 0.034 Uiso 1 1 calc R . .
H3B H -0.0129 0.0329 0.1403 0.034 Uiso 1 1 calc R . .
C4 C 0.2010(2) -0.01347(12) 0.11342(12) 0.0297(5) Uani 1 1 d . . .
H4A H 0.2949 -0.0184 0.1163 0.045 Uiso 1 1 calc R . .
H4B H 0.1539 -0.0277 0.0696 0.045 Uiso 1 1 calc R . .
H4C H 0.1744 -0.0433 0.1466 0.045 Uiso 1 1 calc R . .
C5 C 0.22780(18) 0.08556(11) 0.19543(10) 0.0186(4) Uani 1 1 d . . .
C6 C 0.3044(2) 0.04131(12) 0.24090(12) 0.0266(5) Uani 1 1 d . . .
H6 H 0.3261 -0.0043 0.2282 0.032 Uiso 1 1 calc R . .
C7 C 0.3490(2) 0.06406(13) 0.30485(12) 0.0318(5) Uani 1 1 d . . .
H7 H 0.4010 0.0341 0.3363 0.038 Uiso 1 1 calc R . .
C8 C 0.3177(2) 0.13045(13) 0.32264(11) 0.0290(5) Uani 1 1 d . . .
H8 H 0.3451 0.1465 0.3666 0.035 Uiso 1 1 calc R . .
C9 C 0.2459(2) 0.17283(12) 0.27522(10) 0.0229(4) Uani 1 1 d . . .
H9 H 0.2261 0.2191 0.2871 0.027 Uiso 1 1 calc R . .
C10 C 0.3927(2) 0.18320(15) -0.00938(12) 0.0326(5) Uani 1 1 d . . .
H10A H 0.4572 0.1895 0.0317 0.049 Uiso 1 1 calc R . .
H10B H 0.4223 0.2075 -0.0451 0.049 Uiso 1 1 calc R . .
H10C H 0.3823 0.1331 -0.0196 0.049 Uiso 1 1 calc R . .
C11 C 0.2586(2) 0.31707(12) 0.01151(11) 0.0273(5) Uani 1 1 d . . .
H11A H 0.1768 0.3392 0.0163 0.041 Uiso 1 1 calc R . .
H11B H 0.2864 0.3369 -0.0268 0.041 Uiso 1 1 calc R . .
H11C H 0.3258 0.3258 0.0511 0.041 Uiso 1 1 calc R . .
C12 C 0.1066(2) 0.20327(11) -0.07858(10) 0.0220(4) Uani 1 1 d . . .
C13 C 0.1212(3) 0.12967(14) -0.10609(13) 0.0394(6) Uani 1 1 d . . .
H13A H 0.1080 0.0944 -0.0739 0.059 Uiso 1 1 calc R . .
H13B H 0.2088 0.1245 -0.1150 0.059 Uiso 1 1 calc R . .
H13C H 0.0561 0.1232 -0.1469 0.059 Uiso 1 1 calc R . .
C14 C 0.1256(3) 0.25619(15) -0.13142(12) 0.0366(6) Uani 1 1 d . . .
H14A H 0.0616 0.2470 -0.1721 0.055 Uiso 1 1 calc R . .
H14B H 0.2138 0.2514 -0.1396 0.055 Uiso 1 1 calc R . .
H14C H 0.1136 0.3039 -0.1162 0.055 Uiso 1 1 calc R . .
C15 C -0.0317(2) 0.21087(15) -0.06751(12) 0.0354(6) Uani 1 1 d . . .
H15A H -0.0444 0.2586 -0.0526 0.053 Uiso 1 1 calc R . .
H15B H -0.0456 0.1772 -0.0341 0.053 Uiso 1 1 calc R . .
H15C H -0.0942 0.2017 -0.1087 0.053 Uiso 1 1 calc R . .
C16 C -0.2766(2) 0.21992(11) 0.10651(13) 0.0277(5) Uani 1 1 d . . .
H16A H -0.2292 0.2530 0.1390 0.042 Uiso 1 1 calc R . .
H16B H -0.3686 0.2189 0.1095 0.042 Uiso 1 1 calc R . .
H16C H -0.2696 0.2348 0.0624 0.042 Uiso 1 1 calc R . .
C17 C -0.2893(2) 0.07188(13) 0.05494(14) 0.0360(6) Uani 1 1 d . . .
H17A H -0.2779 0.0908 0.0127 0.054 Uiso 1 1 calc R . .
H17B H -0.3824 0.0694 0.0553 0.054 Uiso 1 1 calc R . .
H17C H -0.2514 0.0248 0.0612 0.054 Uiso 1 1 calc R . .
C18 C -0.2351(2) 0.09515(12) 0.20422(13) 0.0291(5) Uani 1 1 d . . .
C19 C -0.1531(6) 0.1332(4) 0.26084(18) 0.137(3) Uani 1 1 d . . .
H19A H -0.1781 0.1188 0.3017 0.205 Uiso 1 1 calc R . .
H19B H -0.1663 0.1839 0.2547 0.205 Uiso 1 1 calc R . .
H19C H -0.0610 0.1220 0.2633 0.205 Uiso 1 1 calc R . .
C20 C -0.2086(7) 0.0185(2) 0.2130(2) 0.123(3) Uani 1 1 d . . .
H20A H -0.1158 0.0096 0.2150 0.185 Uiso 1 1 calc R . .
H20B H -0.2608 -0.0072 0.1759 0.185 Uiso 1 1 calc R . .
H20C H -0.2316 0.0027 0.2539 0.185 Uiso 1 1 calc R . .
C21 C -0.3755(4) 0.1062(3) 0.2088(3) 0.0997(19) Uani 1 1 d . . .
H21A H -0.4331 0.0858 0.1701 0.150 Uiso 1 1 calc R . .
H21B H -0.3931 0.1565 0.2108 0.150 Uiso 1 1 calc R . .
H21C H -0.3914 0.0833 0.2486 0.150 Uiso 1 1 calc R . .
C22 C -0.0783(2) 0.35190(12) 0.04350(11) 0.0245(4) Uani 1 1 d . . .
C23 C -0.2283(2) 0.44913(13) 0.02151(13) 0.0310(5) Uani 1 1 d . . .
C24 C -0.2846(3) 0.48687(15) -0.04247(13) 0.0413(7) Uani 1 1 d . . .
H24A H -0.2137 0.5083 -0.0597 0.062 Uiso 1 1 calc R . .
H24B H -0.3449 0.5235 -0.0344 0.062 Uiso 1 1 calc R . .
H24C H -0.3313 0.4532 -0.0745 0.062 Uiso 1 1 calc R . .
C25 C -0.1519(3) 0.50049(15) 0.07101(14) 0.0467(7) Uani 1 1 d . . .
H25A H -0.1122 0.4753 0.1113 0.070 Uiso 1 1 calc R . .
H25B H -0.2109 0.5367 0.0812 0.070 Uiso 1 1 calc R . .
H25C H -0.0834 0.5225 0.0524 0.070 Uiso 1 1 calc R . .
C26 C -0.3338(3) 0.41359(18) 0.0491(2) 0.0569(9) Uani 1 1 d . . .
H26A H -0.3806 0.3801 0.0169 0.085 Uiso 1 1 calc R . .
H26B H -0.3950 0.4489 0.0587 0.085 Uiso 1 1 calc R . .
H26C H -0.2944 0.3887 0.0896 0.085 Uiso 1 1 calc R . .
C27 C 0.39268(19) 0.26848(11) 0.18067(10) 0.0212(4) Uani 1 1 d . . .
H27 H 0.4007 0.2191 0.1771 0.025 Uiso 1 1 calc R . .
C28 C 0.5052(2) 0.30814(13) 0.19534(11) 0.0250(4) Uani 1 1 d . . .
H28 H 0.5883 0.2862 0.2026 0.030 Uiso 1 1 calc R . .
C29 C 0.4949(2) 0.38015(13) 0.19936(11) 0.0278(5) Uani 1 1 d . . .
H29 H 0.5705 0.4088 0.2087 0.033 Uiso 1 1 calc R . .
C30 C 0.3716(2) 0.40951(13) 0.18945(11) 0.0276(5) Uani 1 1 d . . .
H30 H 0.3615 0.4589 0.1920 0.033 Uiso 1 1 calc R . .
C31 C 0.2634(2) 0.36644(11) 0.17591(10) 0.0223(4) Uani 1 1 d . . .
H31 H 0.1795 0.3872 0.1697 0.027 Uiso 1 1 calc R . .
C32 C 0.0372(3) 0.33312(13) 0.32716(12) 0.0330(5) Uani 1 1 d . . .
F1 F 0.0142(2) 0.27235(9) 0.35371(8) 0.0628(6) Uani 1 1 d . . .
F3 F -0.00363(18) 0.38482(8) 0.36086(8) 0.0467(4) Uani 1 1 d . . .
F11 F 0.16549(16) 0.33972(8) 0.33400(8) 0.0461(4) Uani 1 1 d . . .
N1 N 0.18853(17) 0.18167(9) 0.06844(8) 0.0199(3) Uani 1 1 d . . .
N2 N -0.03973(16) 0.13628(9) 0.12208(9) 0.0196(3) Uani 1 1 d . . .
N3 N 0.20209(16) 0.15193(9) 0.21264(8) 0.0184(3) Uani 1 1 d . . .
N4 N -0.01454(17) 0.30634(10) 0.07477(9) 0.0223(4) Uani 1 1 d . . .
N5 N -0.1384(2) 0.39557(12) 0.00555(11) 0.0407(6) Uani 1 1 d . . .
N6 N 0.27195(16) 0.29629(9) 0.17115(8) 0.0188(3) Uani 1 1 d . . .
O1 O 0.01791(14) 0.27612(8) 0.21574(7) 0.0209(3) Uani 1 1 d . . .
O2 O -0.00363(17) 0.40317(9) 0.21975(8) 0.0314(4) Uani 1 1 d . . .
O3 O -0.17750(16) 0.32808(11) 0.24019(12) 0.0522(6) Uani 1 1 d . . .
S S -0.04266(5) 0.33707(3) 0.24124(3) 0.02300(11) Uani 1 1 d . . .
Si1 Si 0.23325(5) 0.22050(3) -0.00003(3) 0.01863(11) Uani 1 1 d . . .
Si2 Si -0.20531(5) 0.13060(3) 0.12314(3) 0.02266(13) Uani 1 1 d . . .
Zr1 Zr 0.079328(17) 0.223135(10) 0.129938(9) 0.01583(5) Uani 1 1 d . . .
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'
F F 0.0171 0.0103 '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'
S S 0.1246 0.1234 '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 117.13(17) . . ?
N1 C1 H1A 108.0 . . ?
C2 C1 H1A 108.0 . . ?
N1 C1 H1B 108.0 . . ?
C2 C1 H1B 108.0 . . ?
H1A C1 H1B 107.3 . . ?
C5 C2 C4 111.35(17) . . ?
C5 C2 C1 111.25(18) . . ?
C4 C2 C1 105.79(18) . . ?
C5 C2 C3 110.87(17) . . ?
C4 C2 C3 105.61(18) . . ?
C1 C2 C3 111.73(18) . . ?
N2 C3 C2 117.19(17) . . ?
N2 C3 H3A 108.0 . . ?
C2 C3 H3A 108.0 . . ?
N2 C3 H3B 108.0 . . ?
C2 C3 H3B 108.0 . . ?
H3A C3 H3B 107.2 . . ?
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 120.3(2) . . ?
N3 C5 C2 116.66(17) . . ?
C6 C5 C2 123.08(19) . . ?
C7 C6 C5 119.7(2) . . ?
C7 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
C8 C7 C6 119.6(2) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C9 C8 C7 118.3(2) . . ?
C9 C8 H8 120.9 . . ?
C7 C8 H8 120.9 . . ?
N3 C9 C8 123.1(2) . . ?
N3 C9 H9 118.5 . . ?
C8 C9 H9 118.5 . . ?
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 . . ?
C15 C12 C13 108.4(2) . . ?
C15 C12 C14 108.5(2) . . ?
C13 C12 C14 107.2(2) . . ?
C15 C12 Si1 111.59(15) . . ?
C13 C12 Si1 111.81(15) . . ?
C14 C12 Si1 109.23(16) . . ?
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 . . ?
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 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 . . ?
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 . . ?
C20 C18 C19 108.5(4) . . ?
C20 C18 C21 106.7(3) . . ?
C19 C18 C21 106.9(4) . . ?
C20 C18 Si2 113.3(2) . . ?
C19 C18 Si2 110.6(2) . . ?
C21 C18 Si2 110.5(2) . . ?
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 . . ?
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 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 . . ?
N4 C22 N5 172.7(2) . . ?
N5 C23 C26 109.3(2) . . ?
N5 C23 C24 106.2(2) . . ?
C26 C23 C24 111.4(2) . . ?
N5 C23 C25 109.1(2) . . ?
C26 C23 C25 110.8(3) . . ?
C24 C23 C25 110.0(2) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N6 C27 C28 123.4(2) . . ?
N6 C27 H27 118.3 . . ?
C28 C27 H27 118.3 . . ?
C27 C28 C29 118.9(2) . . ?
C27 C28 H28 120.5 . . ?
C29 C28 H28 120.5 . . ?
C28 C29 C30 118.4(2) . . ?
C28 C29 H29 120.8 . . ?
C30 C29 H29 120.8 . . ?
C31 C30 C29 119.5(2) . . ?
C31 C30 H30 120.3 . . ?
C29 C30 H30 120.3 . . ?
N6 C31 C30 122.8(2) . . ?
N6 C31 H31 118.6 . . ?
C30 C31 H31 118.6 . . ?
F1 C32 F11 107.9(2) . . ?
F1 C32 F3 108.6(2) . . ?
F11 C32 F3 107.72(19) . . ?
F1 C32 S 111.14(17) . . ?
F11 C32 S 110.50(17) . . ?
F3 C32 S 110.87(19) . . ?
C1 N1 Si1 112.34(14) . . ?
C1 N1 Zr1 118.60(14) . . ?
Si1 N1 Zr1 128.70(9) . . ?
C3 N2 Si2 112.93(14) . . ?
C3 N2 Zr1 117.43(13) . . ?
Si2 N2 Zr1 129.61(9) . . ?
C9 N3 C5 118.98(18) . . ?
C9 N3 Zr1 124.07(14) . . ?
C5 N3 Zr1 116.94(13) . . ?
C22 N4 Zr1 174.57(18) . . ?
C22 N5 C23 126.2(2) . . ?
C31 N6 C27 117.04(18) . . ?
C31 N6 Zr1 121.82(13) . . ?
C27 N6 Zr1 120.43(14) . . ?
S O1 Zr1 148.43(10) . . ?
O3 S O2 116.90(12) . . ?
O3 S O1 113.72(10) . . ?
O2 S O1 114.15(9) . . ?
O3 S C32 105.25(14) . . ?
O2 S C32 104.06(11) . . ?
O1 S C32 100.24(11) . . ?
N1 Si1 C10 108.83(10) . . ?
N1 Si1 C11 111.48(9) . . ?
C10 Si1 C11 106.41(12) . . ?
N1 Si1 C12 111.54(9) . . ?
C10 Si1 C12 108.87(10) . . ?
C11 Si1 C12 109.55(10) . . ?
N2 Si2 C16 107.65(10) . . ?
N2 Si2 C17 109.75(10) . . ?
C16 Si2 C17 107.34(11) . . ?
N2 Si2 C18 112.49(10) . . ?
C16 Si2 C18 110.78(11) . . ?
C17 Si2 C18 108.71(12) . . ?
N1 Zr1 N2 92.85(7) . . ?
N1 Zr1 N4 102.19(7) . . ?
N2 Zr1 N4 111.10(7) . . ?
N1 Zr1 O1 163.02(6) . . ?
N2 Zr1 O1 98.80(6) . . ?
N4 Zr1 O1 85.14(6) . . ?
N1 Zr1 N3 86.72(6) . . ?
N2 Zr1 N3 79.87(6) . . ?
N4 Zr1 N3 165.17(6) . . ?
O1 Zr1 N3 83.25(6) . . ?
N1 Zr1 N6 84.85(6) . . ?
N2 Zr1 N6 157.60(6) . . ?
N4 Zr1 N6 91.12(6) . . ?
O1 Zr1 N6 79.66(5) . . ?
N3 Zr1 N6 77.76(6) . . ?
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 1.477(3) . ?
C1 C2 1.541(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C5 1.515(3) . ?
C2 C4 1.538(3) . ?
C2 C3 1.548(3) . ?
C3 N2 1.476(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 N3 1.357(3) . ?
C5 C6 1.391(3) . ?
C6 C7 1.385(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.378(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.372(3) . ?
C8 H8 0.9500 . ?
C9 N3 1.348(3) . ?
C9 H9 0.9500 . ?
C10 Si1 1.865(2) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 Si1 1.868(2) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C15 1.524(3) . ?
C12 C13 1.535(3) . ?
C12 C14 1.536(3) . ?
C12 Si1 1.907(2) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 Si2 1.863(2) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 Si2 1.876(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C20 1.492(4) . ?
C18 C19 1.494(4) . ?
C18 C21 1.511(4) . ?
C18 Si2 1.904(3) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 N4 1.201(3) . ?
C22 N5 1.227(3) . ?
C23 N5 1.475(3) . ?
C23 C26 1.511(4) . ?
C23 C24 1.520(3) . ?
C23 C25 1.522(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 N6 1.349(2) . ?
C27 C28 1.381(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.381(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.384(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.382(3) . ?
C30 H30 0.9500 . ?
C31 N6 1.345(3) . ?
C31 H31 0.9500 . ?
C32 F1 1.328(3) . ?
C32 F11 1.329(3) . ?
C32 F3 1.332(3) . ?
C32 S 1.811(3) . ?
N1 Si1 1.7555(19) . ?
N1 Zr1 2.0480(17) . ?
N2 Si2 1.7456(18) . ?
N2 Zr1 2.0599(18) . ?
N3 Zr1 2.3530(17) . ?
N4 Zr1 2.0810(18) . ?
N6 Zr1 2.4573(17) . ?
O1 S 1.4757(15) . ?
O1 Zr1 2.2608(14) . ?
O2 S 1.4258(18) . ?
O3 S 1.4209(17) . ?
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 -69.5(2) . . . . ?
N1 C1 C2 C4 169.46(19) . . . . ?
N1 C1 C2 C3 55.0(3) . . . . ?
C5 C2 C3 N2 57.3(3) . . . . ?
C4 C2 C3 N2 178.1(2) . . . . ?
C1 C2 C3 N2 -67.4(3) . . . . ?
C4 C2 C5 N3 -177.72(18) . . . . ?
C1 C2 C5 N3 64.5(2) . . . . ?
C3 C2 C5 N3 -60.5(2) . . . . ?
C4 C2 C5 C6 2.1(3) . . . . ?
C1 C2 C5 C6 -115.6(2) . . . . ?
C3 C2 C5 C6 119.4(2) . . . . ?
N3 C5 C6 C7 3.2(3) . . . . ?
C2 C5 C6 C7 -176.6(2) . . . . ?
C5 C6 C7 C8 -0.4(3) . . . . ?
C6 C7 C8 C9 -2.0(4) . . . . ?
C7 C8 C9 N3 1.7(3) . . . . ?
N6 C27 C28 C29 -1.3(3) . . . . ?
C27 C28 C29 C30 1.0(3) . . . . ?
C28 C29 C30 C31 -0.1(3) . . . . ?
C29 C30 C31 N6 -0.7(3) . . . . ?
C2 C1 N1 Si1 -168.71(16) . . . . ?
C2 C1 N1 Zr1 5.0(3) . . . . ?
C2 C3 N2 Si2 -166.59(16) . . . . ?
C2 C3 N2 Zr1 15.2(3) . . . . ?
C8 C9 N3 C5 1.1(3) . . . . ?
C8 C9 N3 Zr1 -179.81(16) . . . . ?
C6 C5 N3 C9 -3.6(3) . . . . ?
C2 C5 N3 C9 176.28(18) . . . . ?
C6 C5 N3 Zr1 177.29(15) . . . . ?
C2 C5 N3 Zr1 -2.9(2) . . . . ?
N5 C22 N4 Zr1 -113(2) . . . . ?
N4 C22 N5 C23 177(2) . . . . ?
C26 C23 N5 C22 -56.0(4) . . . . ?
C24 C23 N5 C22 -176.3(3) . . . . ?
C25 C23 N5 C22 65.3(4) . . . . ?
C30 C31 N6 C27 0.4(3) . . . . ?
C30 C31 N6 Zr1 -170.06(17) . . . . ?
C28 C27 N6 C31 0.6(3) . . . . ?
C28 C27 N6 Zr1 171.21(16) . . . . ?
Zr1 O1 S O3 94.7(2) . . . . ?
Zr1 O1 S O2 -42.9(2) . . . . ?
Zr1 O1 S C32 -153.47(17) . . . . ?
F1 C32 S O3 59.1(2) . . . . ?
F11 C32 S O3 178.85(17) . . . . ?
F3 C32 S O3 -61.8(2) . . . . ?
F1 C32 S O2 -177.38(19) . . . . ?
F11 C32 S O2 -57.66(19) . . . . ?
F3 C32 S O2 61.7(2) . . . . ?
F1 C32 S O1 -59.1(2) . . . . ?
F11 C32 S O1 60.63(18) . . . . ?
F3 C32 S O1 179.99(17) . . . . ?
C1 N1 Si1 C10 -36.68(18) . . . . ?
Zr1 N1 Si1 C10 150.44(13) . . . . ?
C1 N1 Si1 C11 -153.74(16) . . . . ?
Zr1 N1 Si1 C11 33.38(15) . . . . ?
C1 N1 Si1 C12 83.44(17) . . . . ?
Zr1 N1 Si1 C12 -89.44(13) . . . . ?
C15 C12 Si1 N1 41.91(19) . . . . ?
C13 C12 Si1 N1 -79.71(19) . . . . ?
C14 C12 Si1 N1 161.86(16) . . . . ?
C15 C12 Si1 C10 162.01(18) . . . . ?
C13 C12 Si1 C10 40.4(2) . . . . ?
C14 C12 Si1 C10 -78.04(19) . . . . ?
C15 C12 Si1 C11 -82.00(19) . . . . ?
C13 C12 Si1 C11 156.38(18) . . . . ?
C14 C12 Si1 C11 37.95(19) . . . . ?
C3 N2 Si2 C16 -160.33(16) . . . . ?
Zr1 N2 Si2 C16 17.60(16) . . . . ?
C3 N2 Si2 C17 -43.80(19) . . . . ?
Zr1 N2 Si2 C17 134.12(14) . . . . ?
C3 N2 Si2 C18 77.35(17) . . . . ?
Zr1 N2 Si2 C18 -104.72(14) . . . . ?
C20 C18 Si2 N2 -72.9(3) . . . . ?
C19 C18 Si2 N2 49.2(4) . . . . ?
C21 C18 Si2 N2 167.4(3) . . . . ?
C20 C18 Si2 C16 166.6(3) . . . . ?
C19 C18 Si2 C16 -71.3(4) . . . . ?
C21 C18 Si2 C16 46.8(3) . . . . ?
C20 C18 Si2 C17 48.9(4) . . . . ?
C19 C18 Si2 C17 170.9(3) . . . . ?
C21 C18 Si2 C17 -70.9(3) . . . . ?
C1 N1 Zr1 N2 -42.17(16) . . . . ?
Si1 N1 Zr1 N2 130.32(12) . . . . ?
C1 N1 Zr1 N4 -154.47(16) . . . . ?
Si1 N1 Zr1 N4 18.02(13) . . . . ?
C1 N1 Zr1 O1 91.3(3) . . . . ?
Si1 N1 Zr1 O1 -96.2(2) . . . . ?
C1 N1 Zr1 N3 37.50(16) . . . . ?
Si1 N1 Zr1 N3 -150.00(12) . . . . ?
C1 N1 Zr1 N6 115.49(16) . . . . ?
Si1 N1 Zr1 N6 -72.01(12) . . . . ?
C3 N2 Zr1 N1 31.39(16) . . . . ?
Si2 N2 Zr1 N1 -146.46(13) . . . . ?
C3 N2 Zr1 N4 135.62(15) . . . . ?
Si2 N2 Zr1 N4 -42.23(14) . . . . ?
C3 N2 Zr1 O1 -136.22(15) . . . . ?
Si2 N2 Zr1 O1 45.93(13) . . . . ?
C3 N2 Zr1 N3 -54.76(15) . . . . ?
Si2 N2 Zr1 N3 127.39(13) . . . . ?
C3 N2 Zr1 N6 -52.0(3) . . . . ?
Si2 N2 Zr1 N6 130.15(14) . . . . ?
C22 N4 Zr1 N1 123.4(18) . . . . ?
C22 N4 Zr1 N2 25.5(19) . . . . ?
C22 N4 Zr1 O1 -72.1(18) . . . . ?
C22 N4 Zr1 N3 -110.6(18) . . . . ?
C22 N4 Zr1 N6 -151.6(18) . . . . ?
S O1 Zr1 N1 110.7(2) . . . . ?
S O1 Zr1 N2 -116.54(17) . . . . ?
S O1 Zr1 N4 -5.90(17) . . . . ?
S O1 Zr1 N3 164.86(18) . . . . ?
S O1 Zr1 N6 86.13(17) . . . . ?
C9 N3 Zr1 N1 139.48(17) . . . . ?
C5 N3 Zr1 N1 -41.43(14) . . . . ?
C9 N3 Zr1 N2 -127.03(17) . . . . ?
C5 N3 Zr1 N2 52.06(14) . . . . ?
C9 N3 Zr1 N4 11.9(4) . . . . ?
C5 N3 Zr1 N4 -169.0(2) . . . . ?
C9 N3 Zr1 O1 -26.79(16) . . . . ?
C5 N3 Zr1 O1 152.30(14) . . . . ?
C9 N3 Zr1 N6 54.05(16) . . . . ?
C5 N3 Zr1 N6 -126.86(15) . . . . ?
C31 N6 Zr1 N1 128.92(16) . . . . ?
C27 N6 Zr1 N1 -41.22(15) . . . . ?
C31 N6 Zr1 N2 -146.11(18) . . . . ?
C27 N6 Zr1 N2 43.7(2) . . . . ?
C31 N6 Zr1 N4 26.78(16) . . . . ?
C27 N6 Zr1 N4 -143.36(16) . . . . ?
C31 N6 Zr1 O1 -58.07(16) . . . . ?
C27 N6 Zr1 O1 131.79(16) . . . . ?
C31 N6 Zr1 N3 -143.33(17) . . . . ?
C27 N6 Zr1 N3 46.53(15) . . . . ?
