#------------------------------------------------------------------------------
#$Date: 2018-08-17 13:49:55 +0300 (Fri, 17 Aug 2018) $
#$Revision: 209873 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/06/25/4062550.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_4062550
loop_
_publ_author_name
'Scholz, Joachim'
'Kahlert, Steffen'
'Görls, Helmar'
_publ_section_title
;
 Synthesis and Structure of the First Homoleptic 1-Aza-1,3-diene Titanium
 Complex: A Tightrope Walk between Ligand Coordination and Ligand Coupling
;
_journal_coden_ASTM              ORGND7
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1594
_journal_page_last               1603
_journal_paper_doi               10.1021/om0341956
_journal_volume                  23
_journal_year                    2004
_chemical_formula_sum            'C48 H63 N3 Zr'
_chemical_formula_weight         773.23
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                107.14(1)
_cell_angle_beta                 92.21(1)
_cell_angle_gamma                98.62(1)
_cell_formula_units_Z            2
_cell_length_a                   9.098(3)
_cell_length_b                   12.335(2)
_cell_length_c                   19.761(4)
_cell_measurement_temperature    183(2)
_cell_volume                     2087.2(9)
_diffrn_ambient_temperature      183(2)
_exptl_crystal_density_diffrn    1.230
_cod_database_code               4062550
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
Zr Zr 0.94187(6) 0.72717(4) 0.72931(3) 0.02088(15) Uani 1 1 d . . .
N1 N 0.9868(5) 0.8796(4) 0.8141(2) 0.0300(10) Uani 1 1 d . . .
N2 N 0.7788(5) 0.7622(3) 0.6627(2) 0.0236(9) Uani 1 1 d . . .
N3 N 0.8946(4) 0.5779(3) 0.7577(2) 0.0218(9) Uani 1 1 d . . .
C1 C 1.1306(6) 0.8575(4) 0.8247(3) 0.0306(12) Uani 1 1 d . . .
H1A H 1.1375 0.8259 0.8657 0.037 Uiso 1 1 calc R . .
C2 C 1.2154(6) 0.8055(4) 0.7721(3) 0.0324(12) Uani 1 1 d . . .
C3 C 1.1724(6) 0.7700(4) 0.6966(3) 0.0289(11) Uani 1 1 d . . .
H3A H 1.2136 0.7008 0.6693 0.035 Uiso 1 1 calc R . .
C4 C 0.9348(7) 0.9561(4) 0.8766(3) 0.0339(12) Uani 1 1 d . . .
H4A H 0.9882 0.9469 0.9193 0.041 Uiso 1 1 calc R . .
C5 C 0.9725(7) 1.0829(4) 0.8810(3) 0.0419(15) Uani 1 1 d . . .
H5A H 1.0815 1.1042 0.8800 0.050 Uiso 1 1 calc R . .
H5B H 0.9224 1.0955 0.8393 0.050 Uiso 1 1 calc R . .
C6 C 0.9224(9) 1.1590(5) 0.9489(4) 0.0523(18) Uani 1 1 d . . .
H6A H 0.9791 1.1513 0.9906 0.063 Uiso 1 1 calc R . .
H6B H 0.9448 1.2404 0.9497 0.063 Uiso 1 1 calc R . .
C7 C 0.7609(8) 1.1274(5) 0.9543(4) 0.0534(18) Uani 1 1 d . . .
H7A H 0.7039 1.1437 0.9157 0.064 Uiso 1 1 calc R . .
H7B H 0.7337 1.1752 1.0002 0.064 Uiso 1 1 calc R . .
C8 C 0.7181(8) 1.0007(5) 0.9488(3) 0.0471(16) Uani 1 1 d . . .
H8A H 0.7638 0.9867 0.9911 0.056 Uiso 1 1 calc R . .
H8B H 0.6084 0.9813 0.9482 0.056 Uiso 1 1 calc R . .
C9 C 0.7697(7) 0.9231(5) 0.8819(3) 0.0418(14) Uani 1 1 d . . .
H9A H 0.7484 0.8423 0.8823 0.050 Uiso 1 1 calc R . .
H9B H 0.7131 0.9287 0.8396 0.050 Uiso 1 1 calc R . .
C10 C 1.1554(6) 0.8518(4) 0.6554(3) 0.0257(11) Uani 1 1 d . . .
C11 C 1.1441(6) 0.8140(5) 0.5810(3) 0.0332(12) Uani 1 1 d . . .
H11A H 1.1463 0.7353 0.5572 0.040 Uiso 1 1 calc R . .
C12 C 1.1301(6) 0.8871(5) 0.5414(3) 0.0389(14) Uani 1 1 d . . .
H12A H 1.1242 0.8587 0.4910 0.047 Uiso 1 1 calc R . .
C13 C 1.1243(7) 1.0022(5) 0.5746(3) 0.0447(16) Uani 1 1 d . . .
H13A H 1.1132 1.0528 0.5473 0.054 Uiso 1 1 calc R . .
C14 C 1.1349(7) 1.0419(5) 0.6478(3) 0.0374(13) Uani 1 1 d . . .
H14A H 1.1314 1.1207 0.6708 0.045 Uiso 1 1 calc R . .
C15 C 1.1507(6) 0.9699(4) 0.6886(3) 0.0326(12) Uani 1 1 d . . .
H15A H 1.1584 0.9995 0.7390 0.039 Uiso 1 1 calc R . .
C16 C 1.3499(6) 0.7658(6) 0.7965(3) 0.0429(15) Uani 1 1 d . . .
H16A H 1.4018 0.7302 0.7553 0.064 Uiso 1 1 calc R . .
H16B H 1.3186 0.7093 0.8214 0.064 Uiso 1 1 calc R . .
H16C H 1.4172 0.8318 0.8289 0.064 Uiso 1 1 calc R . .
C17 C 0.7911(5) 0.6593(4) 0.6113(2) 0.0221(10) Uani 1 1 d . . .
H17A H 0.8440 0.6644 0.5687 0.027 Uiso 1 1 calc R . .
C18 C 0.7648(5) 0.5563(4) 0.6227(2) 0.0215(10) Uani 1 1 d . . .
C19 C 0.6692(5) 0.5354(4) 0.6811(2) 0.0202(10) Uani 1 1 d . . .
H19A H 0.6473 0.6120 0.7095 0.024 Uiso 1 1 calc R . .
C20 C 0.7466(5) 0.8542(4) 0.6349(3) 0.0226(10) Uani 1 1 d . . .
H20A H 0.8227 0.8647 0.6012 0.027 Uiso 1 1 calc R . .
C21 C 0.5933(6) 0.8219(5) 0.5938(3) 0.0339(12) Uani 1 1 d . . .
H21A H 0.5161 0.8086 0.6258 0.041 Uiso 1 1 calc R . .
H21B H 0.5891 0.7496 0.5545 0.041 Uiso 1 1 calc R . .
C22 C 0.5612(7) 0.9175(5) 0.5636(3) 0.0395(14) Uani 1 1 d . . .
H22A H 0.6331 0.9256 0.5283 0.047 Uiso 1 1 calc R . .
H22B H 0.4596 0.8959 0.5387 0.047 Uiso 1 1 calc R . .
C23 C 0.5725(8) 1.0319(5) 0.6213(4) 0.0508(17) Uani 1 1 d . . .
H23A H 0.4935 1.0270 0.6538 0.061 Uiso 1 1 calc R . .
H23B H 0.5584 1.0929 0.5997 0.061 Uiso 1 1 calc R . .
C24 C 0.7262(8) 1.0618(5) 0.6629(4) 0.0466(16) Uani 1 1 d . . .
H24A H 0.8041 1.0749 0.6312 0.056 Uiso 1 1 calc R . .
H24B H 0.7312 1.1339 0.7025 0.056 Uiso 1 1 calc R . .
C25 C 0.7564(7) 0.9666(4) 0.6925(3) 0.0340(13) Uani 1 1 d . . .
H25A H 0.8572 0.9878 0.7181 0.041 Uiso 1 1 calc R . .
H25B H 0.6830 0.9577 0.7270 0.041 Uiso 1 1 calc R . .
C26 C 0.5199(5) 0.4610(4) 0.6477(2) 0.0199(10) Uani 1 1 d . . .
C27 C 0.4931(6) 0.3423(4) 0.6316(3) 0.0305(12) Uani 1 1 d . . .
H27A H 0.5706 0.3033 0.6405 0.037 Uiso 1 1 calc R . .
C28 C 0.3521(6) 0.2795(5) 0.6022(3) 0.0349(13) Uani 1 1 d . . .
H28A H 0.3339 0.1982 0.5924 0.042 Uiso 1 1 calc R . .
C29 C 0.2398(6) 0.3349(5) 0.5875(3) 0.0392(14) Uani 1 1 d . . .
H29A H 0.1437 0.2922 0.5684 0.047 Uiso 1 1 calc R . .
C30 C 0.2670(6) 0.4508(5) 0.6004(3) 0.0407(14) Uani 1 1 d . . .
H30A H 0.1906 0.4889 0.5890 0.049 Uiso 1 1 calc R . .
C31 C 0.4076(6) 0.5146(4) 0.6304(3) 0.0304(12) Uani 1 1 d . . .
H31A H 0.4256 0.5956 0.6390 0.036 Uiso 1 1 calc R . .
C32 C 0.8127(7) 0.4541(4) 0.5715(3) 0.0347(13) Uani 1 1 d . . .
H32A H 0.7854 0.3861 0.5874 0.052 Uiso 1 1 calc R . .
H32B H 0.9211 0.4690 0.5695 0.052 Uiso 1 1 calc R . .
H32C H 0.7630 0.4402 0.5241 0.052 Uiso 1 1 calc R . .
C33 C 0.7574(5) 0.4909(4) 0.7318(3) 0.0202(10) Uani 1 1 d . . .
H33A H 0.7869 0.4168 0.7039 0.024 Uiso 1 1 calc R . .
C34 C 0.6681(5) 0.4691(4) 0.7915(2) 0.0204(10) Uani 1 1 d . . .
C35 C 0.6425(6) 0.3633(4) 0.7969(3) 0.0241(10) Uani 1 1 d . . .
H35A H 0.6820 0.3076 0.7614 0.029 Uiso 1 1 calc R . .
C36 C 1.0150(6) 0.5477(4) 0.7971(3) 0.0249(11) Uani 1 1 d . . .
H36A H 1.1074 0.6010 0.7945 0.030 Uiso 1 1 calc R . .
C37 C 0.9970(7) 0.5697(5) 0.8776(3) 0.0357(13) Uani 1 1 d . . .
H37A H 0.9810 0.6498 0.8993 0.043 Uiso 1 1 calc R . .
H37B H 0.9092 0.5170 0.8841 0.043 Uiso 1 1 calc R . .
C38 C 1.1378(8) 0.5496(6) 0.9137(4) 0.0516(17) Uani 1 1 d . . .
H38A H 1.2236 0.6069 0.9104 0.062 Uiso 1 1 calc R . .
H38B H 1.1247 0.5610 0.9647 0.062 Uiso 1 1 calc R . .
C39 C 1.1712(7) 0.4309(6) 0.8806(4) 0.0492(17) Uani 1 1 d . . .
H39A H 1.0896 0.3736 0.8877 0.059 Uiso 1 1 calc R . .
H39B H 1.2647 0.4226 0.9044 0.059 Uiso 1 1 calc R . .
C40 C 1.1876(7) 0.4071(6) 0.8011(4) 0.0494(17) Uani 1 1 d . . .
H40A H 1.2761 0.4585 0.7940 0.059 Uiso 1 1 calc R . .
H40B H 1.2024 0.3265 0.7801 0.059 Uiso 1 1 calc R . .
C41 C 1.0486(6) 0.4271(5) 0.7643(3) 0.0342(13) Uani 1 1 d . . .
H41A H 1.0629 0.4150 0.7133 0.041 Uiso 1 1 calc R . .
H41B H 0.9622 0.3701 0.7675 0.041 Uiso 1 1 calc R . .
C42 C 0.5628(6) 0.3182(4) 0.8492(3) 0.0254(11) Uani 1 1 d . . .
C43 C 0.5772(6) 0.3774(4) 0.9210(3) 0.0299(12) Uani 1 1 d . . .
H43A H 0.6400 0.4504 0.9381 0.036 Uiso 1 1 calc R . .
C44 C 0.5019(7) 0.3319(5) 0.9682(3) 0.0381(13) Uani 1 1 d . . .
H44A H 0.5123 0.3741 1.0173 0.046 Uiso 1 1 calc R . .
C45 C 0.4108(7) 0.2249(6) 0.9445(3) 0.0418(15) Uani 1 1 d . . .
H45A H 0.3586 0.1937 0.9770 0.050 Uiso 1 1 calc R . .
C46 C 0.3974(7) 0.1656(5) 0.8743(4) 0.0450(15) Uani 1 1 d . . .
H46A H 0.3357 0.0921 0.8577 0.054 Uiso 1 1 calc R . .
C47 C 0.4732(6) 0.2111(5) 0.8262(3) 0.0350(13) Uani 1 1 d . . .
H47A H 0.4632 0.1682 0.7772 0.042 Uiso 1 1 calc R . .
C48 C 0.6133(6) 0.5711(4) 0.8408(3) 0.0281(11) Uani 1 1 d . . .
H48A H 0.6455 0.6397 0.8263 0.042 Uiso 1 1 calc R . .
H48B H 0.6547 0.5840 0.8896 0.042 Uiso 1 1 calc R . .
H48C H 0.5041 0.5557 0.8386 0.042 Uiso 1 1 calc R . .
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 2.069(4) . ?
Zr N1 2.091(4) . ?
Zr N2 2.120(4) . ?
Zr C3 2.252(5) . ?
Zr C1 2.495(5) . ?
Zr C17 2.505(5) . ?
Zr C2 2.545(6) . ?
Zr C18 2.753(5) . ?
N1 C1 1.396(7) . ?
N1 C4 1.461(7) . ?
N2 C17 1.395(6) . ?
N2 C20 1.460(6) . ?
N3 C36 1.473(6) . ?
N3 C33 1.482(6) . ?
C1 C2 1.380(8) . ?
C2 C3 1.446(8) . ?
C2 C16 1.498(8) . ?
C3 C10 1.493(7) . ?
C4 C9 1.512(8) . ?
C4 C5 1.526(7) . ?
C5 C6 1.524(8) . ?
C6 C7 1.479(10) . ?
C7 C8 1.524(9) . ?
C8 C9 1.522(8) . ?
C10 C11 1.399(7) . ?
C10 C15 1.418(7) . ?
C11 C12 1.374(8) . ?
C12 C13 1.388(9) . ?
C13 C14 1.378(8) . ?
C14 C15 1.383(8) . ?
C17 C18 1.343(6) . ?
C18 C32 1.500(7) . ?
C18 C19 1.530(7) . ?
C19 C26 1.524(6) . ?
C19 C33 1.531(6) . ?
C20 C25 1.500(7) . ?
C20 C21 1.523(7) . ?
C21 C22 1.529(7) . ?
C22 C23 1.517(9) . ?
C23 C24 1.531(9) . ?
C24 C25 1.512(7) . ?
C26 C27 1.385(6) . ?
C26 C31 1.380(7) . ?
C27 C28 1.401(7) . ?
C28 C29 1.378(8) . ?
C29 C30 1.359(8) . ?
C30 C31 1.404(7) . ?
C33 C34 1.522(7) . ?
C34 C35 1.328(6) . ?
C34 C48 1.512(6) . ?
C35 C42 1.476(7) . ?
C36 C41 1.519(7) . ?
C36 C37 1.552(7) . ?
C37 C38 1.530(8) . ?
C38 C39 1.499(9) . ?
C39 C40 1.527(10) . ?
C40 C41 1.523(8) . ?
C42 C47 1.382(7) . ?
C42 C43 1.382(7) . ?
C43 C44 1.377(8) . ?
C44 C45 1.387(8) . ?
C45 C46 1.355(9) . ?
C46 C47 1.394(8) . ?
