#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/44/7004481.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_7004481
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            'C38.5 H58 F3 N5 O4 S Si2 Zr'
_chemical_formula_weight         891.36
_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_hh25
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.1600(10)
_cell_angle_beta                 103.4830(10)
_cell_angle_gamma                110.4440(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9979(6)
_cell_length_b                   13.3201(9)
_cell_length_c                   18.5380(11)
_cell_measurement_temperature    100(2)
_cell_volume                     2230.2(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            52847
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.12
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.402
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2004-2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             934
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.565
_refine_diff_density_min         -0.541
_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   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         13011
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0393
_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)+(0.0510P)²+1.0288P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1052
_reflns_number_gt                10278
_reflns_number_total             13011
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b807808d.txt
_cod_data_source_block           complex_13
_cod_original_formula_sum        'C38.50 H58 F3 N5 O4 S Si2 Zr'
_cod_database_code               7004481
#BEGIN Tags that were not found in dictionaries:
_audit_block_refno               623
#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 0.3323(2) 0.27399(15) 0.39005(10) 0.0148(3) Uani 1 1 d . . .
H1A H 0.2967 0.2075 0.4135 0.018 Uiso 1 1 calc R . .
H1B H 0.4055 0.3311 0.4301 0.018 Uiso 1 1 calc R . .
C2 C 0.41376(19) 0.25208(14) 0.33319(10) 0.0137(3) Uani 1 1 d . . .
C3 C 0.3154(2) 0.15358(15) 0.27316(10) 0.0161(3) Uani 1 1 d . . .
H3A H 0.3719 0.1484 0.2368 0.019 Uiso 1 1 calc R . .
H3B H 0.2978 0.0875 0.2981 0.019 Uiso 1 1 calc R . .
C4 C 0.5382(2) 0.21980(16) 0.37871(11) 0.0180(4) Uani 1 1 d . . .
H4A H 0.5914 0.2016 0.3452 0.027 Uiso 1 1 calc R . .
H4B H 0.4957 0.1570 0.4033 0.027 Uiso 1 1 calc R . .
H4C H 0.6069 0.2803 0.4166 0.027 Uiso 1 1 calc R . .
C5 C 0.4742(2) 0.35105(14) 0.29567(10) 0.0141(3) Uani 1 1 d . . .
C6 C 0.6244(2) 0.40689(16) 0.30413(11) 0.0187(4) Uani 1 1 d . . .
H6 H 0.6950 0.3836 0.3352 0.022 Uiso 1 1 calc R . .
C7 C 0.6715(2) 0.49620(17) 0.26755(11) 0.0213(4) Uani 1 1 d . . .
H7 H 0.7741 0.5347 0.2734 0.026 Uiso 1 1 calc R . .
C8 C 0.5671(2) 0.52844(16) 0.22239(11) 0.0195(4) Uani 1 1 d . . .
H8 H 0.5963 0.5894 0.1965 0.023 Uiso 1 1 calc R . .
C9 C 0.4195(2) 0.47021(15) 0.21568(10) 0.0165(3) Uani 1 1 d . . .
H9 H 0.3477 0.4923 0.1846 0.020 Uiso 1 1 calc R . .
C10 C -0.0269(2) 0.37886(16) 0.38883(11) 0.0197(4) Uani 1 1 d . . .
H10A H -0.0221 0.4135 0.3433 0.030 Uiso 1 1 calc R . .
H10B H -0.0482 0.4230 0.4248 0.030 Uiso 1 1 calc R . .
H10C H -0.1054 0.3070 0.3764 0.030 Uiso 1 1 calc R . .
C11 C 0.2946(2) 0.50284(16) 0.47090(12) 0.0232(4) Uani 1 1 d . . .
H11A H 0.3879 0.4964 0.4971 0.035 Uiso 1 1 calc R . .
H11B H 0.2590 0.5369 0.5062 0.035 Uiso 1 1 calc R . .
H11C H 0.3109 0.5473 0.4305 0.035 Uiso 1 1 calc R . .
C12 C 0.1298(2) 0.28008(16) 0.51030(11) 0.0201(4) Uani 1 1 d . . .
C13 C 0.0404(3) 0.31876(19) 0.55492(12) 0.0281(5) Uani 1 1 d . . .
H13A H -0.0598 0.3027 0.5233 0.042 Uiso 1 1 calc R . .
H13B H 0.0892 0.3968 0.5705 0.042 Uiso 1 1 calc R . .
H13C H 0.0351 0.2813 0.5992 0.042 Uiso 1 1 calc R . .
C14 C 0.2767(3) 0.29126(19) 0.56514(12) 0.0278(5) Uani 1 1 d . . .
H14A H 0.2569 0.2473 0.6054 0.042 Uiso 1 1 calc R . .
H14B H 0.3313 0.3672 0.5864 0.042 Uiso 1 1 calc R . .
H14C H 0.3358 0.2664 0.5386 0.042 Uiso 1 1 calc R . .
C15 C 0.0421(3) 0.16041(17) 0.47857(13) 0.0285(5) Uani 1 1 d . . .
H15A H 0.0985 0.1343 0.4509 0.043 Uiso 1 1 calc R . .
H15B H -0.0533 0.1529 0.4449 0.043 Uiso 1 1 calc R . .
H15C H 0.0252 0.1177 0.5198 0.043 Uiso 1 1 calc R . .
C16 C -0.0838(2) 0.04133(17) 0.09599(11) 0.0247(4) Uani 1 1 d . . .
H16A H -0.1371 0.0833 0.1125 0.037 Uiso 1 1 calc R . .
H16B H -0.1542 -0.0305 0.0721 0.037 Uiso 1 1 calc R . .
H16C H -0.0323 0.0786 0.0601 0.037 Uiso 1 1 calc R . .
C17 C 0.1695(3) -0.03510(18) 0.14125(13) 0.0271(4) Uani 1 1 d . . .
H17A H 0.2318 0.0168 0.1153 0.041 Uiso 1 1 calc R . .
H17B H 0.1048 -0.1001 0.1062 0.041 Uiso 1 1 calc R . .
H17C H 0.2324 -0.0547 0.1828 0.041 Uiso 1 1 calc R . .
C18 C -0.0498(2) -0.06636(16) 0.23918(11) 0.0224(4) Uani 1 1 d . . .
C19 C -0.1652(3) -0.0277(2) 0.25982(14) 0.0317(5) Uani 1 1 d . . .
H19A H -0.2342 -0.0230 0.2140 0.048 Uiso 1 1 calc R . .
H19B H -0.1154 0.0437 0.2898 0.048 Uiso 1 1 calc R . .
H19C H -0.2200 -0.0791 0.2888 0.048 Uiso 1 1 calc R . .
C20 C 0.0562(3) -0.07090(18) 0.31242(12) 0.0284(5) Uani 1 1 d . . .
H20A H 0.0014 -0.1241 0.3404 0.043 Uiso 1 1 calc R . .
H20B H 0.1004 0.0004 0.3425 0.043 Uiso 1 1 calc R . .
H20C H 0.1345 -0.0919 0.3012 0.043 Uiso 1 1 calc R . .
C21 C -0.1283(3) -0.18140(18) 0.19684(15) 0.0363(6) Uani 1 1 d . . .
H21A H -0.1816 -0.2292 0.2281 0.055 Uiso 1 1 calc R . .
H21B H -0.0548 -0.2078 0.1851 0.055 Uiso 1 1 calc R . .
H21C H -0.1985 -0.1805 0.1503 0.055 Uiso 1 1 calc R . .
C22 C -0.2367(2) 0.19475(17) 0.22040(11) 0.0210(4) Uani 1 1 d . . .
C23 C -0.0104(2) 0.33335(17) 0.07494(11) 0.0216(4) Uani 1 1 d . . .
H23 H -0.0807 0.3429 0.0985 0.026 Uiso 1 1 calc R . .
C24 C -0.0241(2) 0.34918(17) 0.00051(12) 0.0249(4) Uani 1 1 d . . .
H24 H -0.1019 0.3695 -0.0262 0.030 Uiso 1 1 calc R . .
C25 C 0.0774(3) 0.33485(17) -0.03408(12) 0.0267(4) Uani 1 1 d . . .
H25 H 0.0716 0.3466 -0.0848 0.032 Uiso 1 1 calc R . .
C26 C 0.1877(2) 0.30308(17) 0.00631(11) 0.0245(4) Uani 1 1 d . . .
H26 H 0.2578 0.2914 -0.0165 0.029 Uiso 1 1 calc R . .
C27 C 0.1940(2) 0.28868(16) 0.07999(11) 0.0199(4) Uani 1 1 d . . .
H27 H 0.2693 0.2662 0.1073 0.024 Uiso 1 1 calc R . .
C28 C 0.2267(3) 0.66335(17) 0.28509(13) 0.0284(5) Uani 1 1 d . . .
C51 C 0.4555(3) 0.7940(2) 0.03347(16) 0.0440(7) Uani 1 1 d D . .
C52 C 0.4533(3) 0.7865(2) -0.04349(15) 0.0408(6) Uani 1 1 d D . .
H52 H 0.4735 0.8495 -0.0679 0.049 Uiso 1 1 calc R . .
C53 C 0.4217(3) 0.6871(2) -0.08263(14) 0.0336(5) Uani 1 1 d D . .
H53 H 0.4198 0.6810 -0.1341 0.040 Uiso 1 1 calc R . .
C54 C 0.3928(3) 0.5967(2) -0.04611(15) 0.0402(6) Uani 1 1 d D . .
H54 H 0.3682 0.5278 -0.0730 0.048 Uiso 1 1 calc R . .
C55 C 0.3991(3) 0.6052(3) 0.02898(16) 0.0499(7) Uani 1 1 d D . .
H55 H 0.3816 0.5426 0.0538 0.060 Uiso 1 1 calc R . .
C56 C 0.4300(3) 0.7023(3) 0.06750(16) 0.0447(7) Uani 1 1 d D . .
H56 H 0.4342 0.7070 0.1193 0.054 Uiso 1 1 calc R . .
C57 C 0.4777(4) 0.8995(3) 0.07519(19) 0.0549(8) Uani 1 1 d D . .
H57A H 0.3926 0.9201 0.0551 0.082 Uiso 1 1 calc R . .
H57B H 0.5679 0.9553 0.0694 0.082 Uiso 1 1 calc R . .
H57C H 0.4872 0.8921 0.1284 0.082 Uiso 1 1 calc R . .
C61 C 0.4314(5) 0.0274(3) 0.5480(2) 0.0682(11) Uani 1 1 d D . .
H61 H 0.3824 0.0463 0.5814 0.082 Uiso 0.50 1 d PR . .
C62 C 0.3509(4) -0.0411(3) 0.4831(2) 0.0647(11) Uani 1 1 d D . .
H62 H 0.2460 -0.0694 0.4722 0.078 Uiso 1 1 calc R . .
C63 C 0.5843(5) 0.0687(3) 0.5644(2) 0.0739(13) Uani 1 1 d D . .
H63 H 0.6416 0.1161 0.6092 0.089 Uiso 1 1 calc R . .
C64 C 0.3697(8) 0.0484(5) 0.5994(4) 0.0516(16) Uani 0.50 1 d PD . .
H64A H 0.2704 0.0464 0.5752 0.077 Uiso 0.50 1 calc PR . .
H64B H 0.4303 0.1204 0.6270 0.077 Uiso 0.50 1 calc PR . .
H64C H 0.3627 -0.0058 0.6340 0.077 Uiso 0.50 1 calc PR . .
F1 F 0.1775(2) 0.65902(13) 0.34610(8) 0.0435(4) Uani 1 1 d . . .
F2 F 0.36261(16) 0.66316(12) 0.30457(9) 0.0388(3) Uani 1 1 d . . .
F3 F 0.2334(2) 0.75656(11) 0.25931(9) 0.0479(4) Uani 1 1 d . . .
N1 N 0.20560(17) 0.30718(12) 0.36113(8) 0.0142(3) Uani 1 1 d . . .
N2 N 0.16937(17) 0.15342(12) 0.23066(9) 0.0155(3) Uani 1 1 d . . .
N3 N 0.37275(17) 0.38321(12) 0.25126(8) 0.0142(3) Uani 1 1 d . . .
N4 N -0.11049(18) 0.23258(14) 0.22187(9) 0.0203(3) Uani 1 1 d . . .
N5 N 0.09813(18) 0.30506(13) 0.11527(9) 0.0181(3) Uani 1 1 d . . .
O1 O -0.36411(18) 0.15533(15) 0.21844(10) 0.0374(4) Uani 1 1 d . . .
O2 O 0.12528(15) 0.45843(11) 0.24787(8) 0.0185(3) Uani 1 1 d . . .
O3 O 0.16683(17) 0.57282(12) 0.15038(8) 0.0235(3) Uani 1 1 d . . .
O4 O -0.03881(18) 0.55420(14) 0.20494(10) 0.0326(4) Uani 1 1 d . . .
S S 0.10491(5) 0.55123(4) 0.21296(3) 0.01840(10) Uani 1 1 d . . .
Si1 Si 0.15410(5) 0.36575(4) 0.43070(3) 0.01340(10) Uani 1 1 d . . .
Si2 Si 0.05382(6) 0.02740(4) 0.17847(3) 0.01716(11) Uani 1 1 d . . .
Zr Zr 0.123715(19) 0.288532(14) 0.247501(9) 0.01281(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'
H H 0.0000 0.0000 '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'
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 117.27(14) . . ?
N1 C1 H1A 108.0 . . ?
C2 C1 H1A 108.0 . . ?
N1 C1 H1B 108.0 . . ?
C2 C1 H1B 108.0 . . ?
H1A C1 H1B 107.2 . . ?
C5 C2 C4 111.53(15) . . ?
C5 C2 C1 111.29(14) . . ?
C4 C2 C1 105.51(14) . . ?
C5 C2 C3 109.96(14) . . ?
C4 C2 C3 105.50(14) . . ?
C1 C2 C3 112.85(15) . . ?
N2 C3 C2 116.99(14) . . ?
N2 C3 H3A 108.1 . . ?
C2 C3 H3A 108.1 . . ?
N2 C3 H3B 108.1 . . ?
C2 C3 H3B 108.1 . . ?
H3A C3 H3B 107.3 . . ?
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 120.29(17) . . ?
N3 C5 C2 116.16(15) . . ?
C6 C5 C2 123.55(17) . . ?
C7 C6 C5 120.35(18) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C8 C7 C6 118.93(18) . . ?
C8 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
C9 C8 C7 118.50(18) . . ?
C9 C8 H8 120.7 . . ?
C7 C8 H8 120.7 . . ?
N3 C9 C8 122.90(18) . . ?
N3 C9 H9 118.6 . . ?
C8 C9 H9 118.6 . . ?
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 109.45(18) . . ?
C14 C12 C13 107.42(17) . . ?
C15 C12 C13 108.57(17) . . ?
C14 C12 Si1 113.34(14) . . ?
C15 C12 Si1 110.14(14) . . ?
C13 C12 Si1 107.77(13) . . ?
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 107.42(18) . . ?
C20 C18 C21 108.19(19) . . ?
C19 C18 C21 108.92(19) . . ?
C20 C18 Si2 111.30(14) . . ?
C19 C18 Si2 111.17(15) . . ?
C21 C18 Si2 109.74(15) . . ?
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 O1 179.1(3) . . ?
N5 C23 C24 122.83(19) . . ?
N5 C23 H23 118.6 . . ?
C24 C23 H23 118.6 . . ?
C25 C24 C23 118.8(2) . . ?
C25 C24 H24 120.6 . . ?
C23 C24 H24 120.6 . . ?
C24 C25 C26 118.94(19) . . ?
C24 C25 H25 120.5 . . ?
C26 C25 H25 120.5 . . ?
C27 C26 C25 118.9(2) . . ?
C27 C26 H26 120.6 . . ?
C25 C26 H26 120.6 . . ?
N5 C27 C26 122.98(19) . . ?
N5 C27 H27 118.5 . . ?
C26 C27 H27 118.5 . . ?
F2 C28 F1 108.16(19) . . ?
F2 C28 F3 108.0(2) . . ?
F1 C28 F3 108.31(18) . . ?
F2 C28 S 111.39(14) . . ?
F1 C28 S 111.29(17) . . ?
F3 C28 S 109.56(16) . . ?
C56 C51 C52 118.8(2) . . ?
C56 C51 C57 120.8(3) . . ?
C52 C51 C57 120.3(3) . . ?
C53 C52 C51 119.6(3) . . ?
C53 C52 H52 120.2 . . ?
C51 C52 H52 120.2 . . ?
C54 C53 C52 119.2(2) . . ?
C54 C53 H53 120.4 . . ?
C52 C53 H53 120.4 . . ?
C55 C54 C53 120.7(3) . . ?
C55 C54 H54 119.6 . . ?
C53 C54 H54 119.6 . . ?
C56 C55 C54 120.3(3) . . ?
C56 C55 H55 119.9 . . ?
C54 C55 H55 119.9 . . ?
C55 C56 C51 121.4(3) . . ?
C55 C56 H56 119.3 . . ?
C51 C56 H56 119.3 . . ?
C51 C57 H57A 109.5 . . ?
C51 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C51 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C64 C61 C62 122.5(5) . . ?
C64 C61 C63 117.6(5) . . ?
C62 C61 C63 119.6(4) . . ?
C64 C61 H61 5.9 . . ?
C62 C61 H61 120.2 . . ?
C63 C61 H61 120.3 . . ?
C63 C62 C61 121.5(4) 2_656 . ?
C63 C62 H62 119.2 2_656 . ?
C61 C62 H62 119.2 . . ?
C62 C63 C61 118.9(4) 2_656 . ?
C62 C63 H63 120.6 2_656 . ?
C61 C63 H63 120.6 . . ?
C61 C64 H61 14.6 . . ?
C61 C64 H64A 109.5 . . ?
H61 C64 H64A 97.4 . . ?
C61 C64 H64B 109.5 . . ?
H61 C64 H64B 107.4 . . ?
H64A C64 H64B 109.5 . . ?
C61 C64 H64C 109.5 . . ?
H61 C64 H64C 122.7 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C1 N1 Si1 113.82(11) . . ?
C1 N1 Zr 117.16(11) . . ?
Si1 N1 Zr 128.89(8) . . ?
C3 N2 Si2 112.57(12) . . ?
C3 N2 Zr 117.75(11) . . ?
Si2 N2 Zr 129.40(9) . . ?
C9 N3 C5 119.03(16) . . ?
C9 N3 Zr 123.97(12) . . ?
C5 N3 Zr 116.88(12) . . ?
C22 N4 Zr 167.54(16) . . ?
C23 N5 C27 117.50(17) . . ?
C23 N5 Zr 121.07(13) . . ?
C27 N5 Zr 121.42(13) . . ?
S O2 Zr 154.70(9) . . ?
O4 S O3 117.26(9) . . ?
O4 S O2 113.79(9) . . ?
O3 S O2 113.31(8) . . ?
O4 S C28 104.73(11) . . ?
O3 S C28 103.89(10) . . ?
O2 S C28 101.51(9) . . ?
N1 Si1 C11 110.93(9) . . ?
N1 Si1 C10 108.91(8) . . ?
C11 Si1 C10 108.70(9) . . ?
N1 Si1 C12 112.24(8) . . ?
C11 Si1 C12 108.36(10) . . ?
C10 Si1 C12 107.59(9) . . ?
N2 Si2 C16 111.70(9) . . ?
N2 Si2 C17 109.01(9) . . ?
C16 Si2 C17 106.92(10) . . ?
N2 Si2 C18 110.74(8) . . ?
C16 Si2 C18 108.81(10) . . ?
C17 Si2 C18 109.58(10) . . ?
N2 Zr N1 93.78(6) . . ?
N2 Zr N4 104.67(6) . . ?
N1 Zr N4 108.58(6) . . ?
N2 Zr O2 162.89(6) . . ?
N1 Zr O2 93.08(5) . . ?
N4 Zr O2 87.91(6) . . ?
N2 Zr N3 85.17(6) . . ?
N1 Zr N3 83.00(6) . . ?
N4 Zr N3 163.89(6) . . ?
O2 Zr N3 80.14(5) . . ?
N2 Zr N5 88.43(6) . . ?
N1 Zr N5 163.19(6) . . ?
N4 Zr N5 86.87(6) . . ?
O2 Zr N5 80.59(5) . . ?
N3 Zr N5 80.58(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 1.477(2) . ?
C1 C2 1.550(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C5 1.515(3) . ?
C2 C4 1.535(2) . ?
C2 C3 1.551(2) . ?
C3 N2 1.488(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 N3 1.353(2) . ?
C5 C6 1.390(3) . ?
C6 C7 1.384(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.381(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.379(3) . ?
C8 H8 0.9500 . ?
C9 N3 1.349(2) . ?
C9 H9 0.9500 . ?
C10 Si1 1.8663(19) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 Si1 1.866(2) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C14 1.534(3) . ?
C12 C15 1.539(3) . ?
C12 C13 1.544(3) . ?
C12 Si1 1.908(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 1.867(2) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 Si2 1.873(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C20 1.533(3) . ?
C18 C19 1.533(3) . ?
C18 C21 1.537(3) . ?
C18 Si2 1.909(2) . ?
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 1.177(3) . ?
C22 O1 1.187(3) . ?
C23 N5 1.344(2) . ?
C23 C24 1.386(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.380(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.387(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.376(3) . ?
C26 H26 0.9500 . ?
C27 N5 1.350(3) . ?
C27 H27 0.9500 . ?
C28 F2 1.323(3) . ?
C28 F1 1.330(3) . ?
C28 F3 1.333(2) . ?
C28 S 1.822(2) . ?
C51 C56 1.368(4) . ?
C51 C52 1.421(4) . ?
C51 C57 1.497(4) . ?
C52 C53 1.382(3) . ?
C52 H52 0.9500 . ?
C53 C54 1.378(4) . ?
C53 H53 0.9500 . ?
C54 C55 1.377(4) . ?
C54 H54 0.9500 . ?
C55 C56 1.351(4) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C61 C64 1.319(7) . ?
C61 C62 1.370(5) . ?
C61 C63 1.384(5) . ?
C61 H61 0.9500 . ?
C62 C63 1.320(6) 2_656 ?
C62 H62 0.9500 . ?
C63 C62 1.320(6) 2_656 ?
C63 H63 0.9500 . ?
C64 H61 0.3870 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
N1 Si1 1.7469(16) . ?
N1 Zr 2.0453(15) . ?
N2 Si2 1.7579(16) . ?
N2 Zr 2.0353(16) . ?
N3 Zr 2.3480(15) . ?
N4 Zr 2.1212(16) . ?
N5 Zr 2.4312(16) . ?
O2 S 1.4707(14) . ?
O2 Zr 2.2573(13) . ?
O3 S 1.4309(15) . ?
O4 S 1.4244(16) . ?
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 58.8(2) . . . . ?
N1 C1 C2 C4 179.93(15) . . . . ?
N1 C1 C2 C3 -65.4(2) . . . . ?
C5 C2 C3 N2 -71.54(19) . . . . ?
C4 C2 C3 N2 168.07(15) . . . . ?
C1 C2 C3 N2 53.4(2) . . . . ?
C4 C2 C5 N3 177.05(15) . . . . ?
C1 C2 C5 N3 -65.42(19) . . . . ?
C3 C2 C5 N3 60.38(19) . . . . ?
C4 C2 C5 C6 -2.1(2) . . . . ?
C1 C2 C5 C6 115.46(19) . . . . ?
C3 C2 C5 C6 -118.75(19) . . . . ?
N3 C5 C6 C7 0.3(3) . . . . ?
C2 C5 C6 C7 179.41(17) . . . . ?
C5 C6 C7 C8 -0.3(3) . . . . ?
C6 C7 C8 C9 0.1(3) . . . . ?
C7 C8 C9 N3 0.0(3) . . . . ?
N5 C23 C24 C25 0.3(3) . . . . ?
C23 C24 C25 C26 1.2(3) . . . . ?
C24 C25 C26 C27 -1.1(3) . . . . ?
C25 C26 C27 N5 -0.6(3) . . . . ?
C56 C51 C52 C53 1.8(4) . . . . ?
C57 C51 C52 C53 -175.2(3) . . . . ?
C51 C52 C53 C54 0.0(4) . . . . ?
C52 C53 C54 C55 -1.8(4) . . . . ?
C53 C54 C55 C56 1.7(5) . . . . ?
C54 C55 C56 C51 0.1(5) . . . . ?
C52 C51 C56 C55 -1.9(4) . . . . ?
C57 C51 C56 C55 175.1(3) . . . . ?
C64 C61 C62 C63 -173.9(4) . . . 2_656 ?
C63 C61 C62 C63 -0.2(6) . . . 2_656 ?
C64 C61 C63 C62 174.2(4) . . . 2_656 ?
C62 C61 C63 C62 0.2(5) . . . 2_656 ?
C2 C1 N1 Si1 -163.05(12) . . . . ?
C2 C1 N1 Zr 13.1(2) . . . . ?
C2 C3 N2 Si2 -168.02(13) . . . . ?
C2 C3 N2 Zr 6.4(2) . . . . ?
C8 C9 N3 C5 0.0(3) . . . . ?
C8 C9 N3 Zr 175.95(14) . . . . ?
C6 C5 N3 C9 -0.2(3) . . . . ?
C2 C5 N3 C9 -179.36(15) . . . . ?
C6 C5 N3 Zr -176.40(13) . . . . ?
C2 C5 N3 Zr 4.45(19) . . . . ?
O1 C22 N4 Zr -91(18) . . . . ?
C24 C23 N5 C27 -2.0(3) . . . . ?
C24 C23 N5 Zr 176.51(15) . . . . ?
C26 C27 N5 C23 2.2(3) . . . . ?
C26 C27 N5 Zr -176.35(15) . . . . ?
Zr O2 S O4 92.0(2) . . . . ?
Zr O2 S O3 -45.3(2) . . . . ?
Zr O2 S C28 -156.0(2) . . . . ?
F2 C28 S O4 172.90(15) . . . . ?
F1 C28 S O4 52.11(18) . . . . ?
F3 C28 S O4 -67.65(18) . . . . ?
F2 C28 S O3 -63.53(17) . . . . ?
F1 C28 S O3 175.68(15) . . . . ?
F3 C28 S O3 55.92(18) . . . . ?
F2 C28 S O2 54.27(17) . . . . ?
F1 C28 S O2 -66.52(17) . . . . ?
F3 C28 S O2 173.72(16) . . . . ?
C1 N1 Si1 C11 71.21(15) . . . . ?
Zr N1 Si1 C11 -104.39(12) . . . . ?
C1 N1 Si1 C10 -169.20(13) . . . . ?
Zr N1 Si1 C10 15.20(14) . . . . ?
C1 N1 Si1 C12 -50.18(15) . . . . ?
Zr N1 Si1 C12 134.23(11) . . . . ?
C14 C12 Si1 N1 78.32(16) . . . . ?
C15 C12 Si1 N1 -44.67(17) . . . . ?
C13 C12 Si1 N1 -162.95(14) . . . . ?
C14 C12 Si1 C11 -44.53(16) . . . . ?
C15 C12 Si1 C11 -167.52(14) . . . . ?
C13 C12 Si1 C11 74.21(17) . . . . ?
C14 C12 Si1 C10 -161.88(14) . . . . ?
C15 C12 Si1 C10 75.12(16) . . . . ?
C13 C12 Si1 C10 -43.15(17) . . . . ?
C3 N2 Si2 C16 -154.17(13) . . . . ?
Zr N2 Si2 C16 32.17(14) . . . . ?
C3 N2 Si2 C17 -36.24(15) . . . . ?
Zr N2 Si2 C17 150.09(12) . . . . ?
C3 N2 Si2 C18 84.38(14) . . . . ?
Zr N2 Si2 C18 -89.28(13) . . . . ?
C20 C18 Si2 N2 -50.37(17) . . . . ?
C19 C18 Si2 N2 69.34(17) . . . . ?
C21 C18 Si2 N2 -170.10(15) . . . . ?
C20 C18 Si2 C16 -173.50(15) . . . . ?
C19 C18 Si2 C16 -53.79(17) . . . . ?
C21 C18 Si2 C16 66.77(18) . . . . ?
C20 C18 Si2 C17 69.91(17) . . . . ?
C19 C18 Si2 C17 -170.37(15) . . . . ?
C21 C18 Si2 C17 -49.82(19) . . . . ?
C3 N2 Zr N1 -43.57(13) . . . . ?
Si2 N2 Zr N1 129.81(11) . . . . ?
C3 N2 Zr N4 -153.90(13) . . . . ?
Si2 N2 Zr N4 19.49(12) . . . . ?
C3 N2 Zr O2 69.9(2) . . . . ?
Si2 N2 Zr O2 -116.74(18) . . . . ?
C3 N2 Zr N3 39.07(13) . . . . ?
Si2 N2 Zr N3 -147.55(11) . . . . ?
C3 N2 Zr N5 119.74(13) . . . . ?
Si2 N2 Zr N5 -66.87(11) . . . . ?
C1 N1 Zr N2 33.30(13) . . . . ?
Si1 N1 Zr N2 -151.23(11) . . . . ?
C1 N1 Zr N4 140.15(12) . . . . ?
Si1 N1 Zr N4 -44.38(12) . . . . ?
C1 N1 Zr O2 -131.02(12) . . . . ?
Si1 N1 Zr O2 44.45(11) . . . . ?
C1 N1 Zr N3 -51.36(12) . . . . ?
Si1 N1 Zr N3 124.11(11) . . . . ?
C1 N1 Zr N5 -63.8(2) . . . . ?
Si1 N1 Zr N5 111.63(19) . . . . ?
C22 N4 Zr N2 75.9(8) . . . . ?
C22 N4 Zr N1 -23.3(8) . . . . ?
C22 N4 Zr O2 -115.9(8) . . . . ?
C22 N4 Zr N3 -157.8(7) . . . . ?
C22 N4 Zr N5 163.4(8) . . . . ?
S O2 Zr N2 63.0(3) . . . . ?
S O2 Zr N1 176.6(2) . . . . ?
S O2 Zr N4 -74.9(2) . . . . ?
S O2 Zr N3 94.2(2) . . . . ?
S O2 Zr N5 12.2(2) . . . . ?
C9 N3 Zr N2 135.30(14) . . . . ?
C5 N3 Zr N2 -48.71(13) . . . . ?
C9 N3 Zr N1 -130.28(14) . . . . ?
C5 N3 Zr N1 45.71(12) . . . . ?
C9 N3 Zr N4 6.8(3) . . . . ?
C5 N3 Zr N4 -177.25(19) . . . . ?
C9 N3 Zr O2 -35.90(14) . . . . ?
C5 N3 Zr O2 140.08(13) . . . . ?
C9 N3 Zr N5 46.09(14) . . . . ?
C5 N3 Zr N5 -137.92(13) . . . . ?
C23 N5 Zr N2 138.94(15) . . . . ?
C27 N5 Zr N2 -42.59(15) . . . . ?
C23 N5 Zr N1 -123.1(2) . . . . ?
C27 N5 Zr N1 55.3(3) . . . . ?
C23 N5 Zr N4 34.16(15) . . . . ?
C27 N5 Zr N4 -147.38(15) . . . . ?
C23 N5 Zr O2 -54.24(15) . . . . ?
C27 N5 Zr O2 124.23(15) . . . . ?
C23 N5 Zr N3 -135.70(15) . . . . ?
C27 N5 Zr N3 42.77(14) . . . . ?
