#------------------------------------------------------------------------------
#$Date: 2017-02-15 09:24:55 +0200 (Wed, 15 Feb 2017) $
#$Revision: 192113 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/06/22/4062261.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_4062261
loop_
_publ_author_name
'Wang, Haiping'
'Li, Hung-Wing'
'Xie, Zuowei'
_publ_section_title
;
 Multiple Insertion of Unsaturated Molecules into the Zr-N Bonds of
 [η⁵:σ-Me₂A(C₉H₆)(C₂B₁₀H₁₀)]Zr(NMe₂)₂ (A = C, Si)
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              4522
_journal_page_last               4531
_journal_paper_doi               10.1021/om0304255
_journal_volume                  22
_journal_year                    2003
_chemical_formula_sum            'C28 H52 B10 N4 S2 Zr'
_chemical_formula_weight         708.18
_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                98.568(2)
_cell_angle_beta                 97.990(2)
_cell_angle_gamma                107.332(2)
_cell_formula_units_Z            2
_cell_length_a                   11.747(1)
_cell_length_b                   11.956(1)
_cell_length_c                   16.297(1)
_cell_measurement_temperature    293(2)
_cell_volume                     2119.3(3)
_diffrn_ambient_temperature      293(2)
_exptl_crystal_density_diffrn    1.110
_cod_database_code               4062261
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
Zr1 Zr -0.21448(8) 0.79701(8) 0.70068(6) 0.0365(3) Uani 1 1 d . B .
S1 S -0.1825(3) 0.8294(2) 0.86643(16) 0.0531(7) Uani 1 1 d . . .
S2 S -0.1132(2) 0.8044(3) 0.57361(16) 0.0565(8) Uani 1 1 d . B .
N1 N -0.0230(7) 0.9296(7) 0.7229(5) 0.045(2) Uani 1 1 d . B .
N2 N -0.1099(7) 0.6935(7) 0.7657(6) 0.053(2) Uani 1 1 d . . .
N3 N -0.0645(10) 0.6788(9) 0.9099(5) 0.078(3) Uani 1 1 d D . .
N4 N 0.1048(7) 0.9785(9) 0.6199(6) 0.063(3) Uani 1 1 d . B .
C1 C -0.4226(9) 0.9620(9) 0.6947(6) 0.047(3) Uani 1 1 d . B .
C2 C -0.2729(8) 0.9736(8) 0.7197(6) 0.040(2) Uani 1 1 d . . .
C3 C -0.5121(8) 0.8306(10) 0.6633(7) 0.054(3) Uani 1 1 d . . .
C4 C -0.5978(11) 0.8006(12) 0.7290(10) 0.100(5) Uani 1 1 d . B .
H4A H -0.5497 0.8054 0.7829 0.150 Uiso 1 1 calc R . .
H4B H -0.6547 0.7212 0.7094 0.150 Uiso 1 1 calc R . .
H4C H -0.6412 0.8570 0.7347 0.150 Uiso 1 1 calc R . .
C5 C -0.5964(11) 0.8203(11) 0.5792(8) 0.079(4) Uani 1 1 d . B .
H5A H -0.5486 0.8378 0.5366 0.118 Uiso 1 1 calc R . .
H5B H -0.6400 0.8762 0.5868 0.118 Uiso 1 1 calc R . .
H5C H -0.6530 0.7405 0.5619 0.118 Uiso 1 1 calc R . .
C11 C -0.4427(8) 0.7441(9) 0.6545(7) 0.046(3) Uani 1 1 d . B .
C12 C -0.4227(9) 0.6761(10) 0.7169(7) 0.056(3) Uani 1 1 d . . .
H12A H -0.4536 0.6770 0.7698 0.068 Uiso 1 1 calc R B .
C13 C -0.3685(9) 0.5922(9) 0.6818(8) 0.059(3) Uani 1 1 d . B .
H13A H -0.3547 0.5277 0.7083 0.071 Uiso 1 1 calc R . .
C14 C -0.3239(10) 0.5329(11) 0.5351(9) 0.073(3) Uani 1 1 d . . .
H14A H -0.2931 0.4729 0.5477 0.087 Uiso 1 1 calc R . .
C15 C -0.3350(12) 0.5560(13) 0.4533(9) 0.087(5) Uani 1 1 d . . .
H15A H -0.3126 0.5110 0.4107 0.105 Uiso 1 1 calc R . .
C16 C -0.3809(11) 0.6487(13) 0.4359(8) 0.076(4) Uani 1 1 d . . .
H16A H -0.3899 0.6619 0.3809 0.092 Uiso 1 1 calc R . .
C17 C -0.4115(9) 0.7177(11) 0.4946(7) 0.061(3) Uani 1 1 d . B .
H17A H -0.4371 0.7801 0.4806 0.073 Uiso 1 1 calc R . .
C18 C -0.4057(8) 0.6971(9) 0.5804(7) 0.047(3) Uani 1 1 d . . .
C19 C -0.3600(9) 0.6014(8) 0.5983(7) 0.053(3) Uani 1 1 d . B .
C20 C -0.1102(10) 0.7263(9) 0.8474(6) 0.053(3) Uani 1 1 d . A .
C21 C -0.036(3) 0.568(2) 0.9013(18) 0.091(9) Uiso 0.50 1 d PD A 1
H21A H -0.0678 0.5234 0.8445 0.136 Uiso 0.50 1 calc PR A 1
H21B H -0.0718 0.5221 0.9401 0.136 Uiso 0.50 1 calc PR A 1
H21C H 0.0507 0.5862 0.9135 0.136 Uiso 0.50 1 calc PR A 1
C22 C -0.017(2) 0.760(2) 0.9937(12) 0.071(8) Uiso 0.50 1 d PD A 1
H22A H -0.0388 0.8309 0.9929 0.106 Uiso 0.50 1 calc PR A 1
H22B H 0.0702 0.7811 1.0064 0.106 Uiso 0.50 1 calc PR A 1
H22C H -0.0505 0.7203 1.0361 0.106 Uiso 0.50 1 calc PR A 1
C21' C -0.111(3) 0.5445(17) 0.9015(18) 0.094(9) Uiso 0.50 1 d PD A 2
H21D H -0.1038 0.5066 0.8470 0.141 Uiso 0.50 1 calc PR A 2
H21E H -0.1945 0.5197 0.9070 0.141 Uiso 0.50 1 calc PR A 2
H21F H -0.0635 0.5219 0.9450 0.141 Uiso 0.50 1 calc PR A 2
C22' C -0.076(2) 0.724(2) 0.9976(11) 0.060(7) Uiso 0.50 1 d PD A 2
H22D H -0.0613 0.8086 1.0062 0.090 Uiso 0.50 1 calc PR A 2
H22E H -0.0183 0.7073 1.0375 0.090 Uiso 0.50 1 calc PR A 2
H22F H -0.1570 0.6847 1.0055 0.090 Uiso 0.50 1 calc PR A 2
C23 C -0.003(2) 0.659(2) 0.7371(14) 0.067(7) Uiso 0.50 1 d PD B 1
H23A H 0.0672 0.7278 0.7637 0.081 Uiso 0.50 1 calc PR B 1
H23B H 0.0027 0.5963 0.7674 0.081 Uiso 0.50 1 calc PR B 1
C24 C 0.022(4) 0.622(3) 0.6595(18) 0.146(14) Uiso 0.50 1 d PD B 1
H24A H 0.0869 0.6873 0.6489 0.175 Uiso 0.50 1 calc PR B 1
H24B H -0.0493 0.6092 0.6167 0.175 Uiso 0.50 1 calc PR B 1
C23' C -0.073(2) 0.594(2) 0.7314(13) 0.061(6) Uiso 0.50 1 d PD B 2
H23C H 0.0067 0.6171 0.7671 0.073 Uiso 0.50 1 calc PR B 2
H23D H -0.1234 0.5331 0.7563 0.073 Uiso 0.50 1 calc PR B 2
C24' C -0.0555(18) 0.523(2) 0.6678(14) 0.075(7) Uiso 0.50 1 d PD B 2
H24C H -0.0959 0.5407 0.6175 0.090 Uiso 0.50 1 calc PR B 2
H24D H -0.1032 0.4433 0.6712 0.090 Uiso 0.50 1 calc PR B 2
C25 C 0.0579(16) 0.5127(17) 0.6475(14) 0.156(8) Uani 1 1 d D . .
H25A H 0.1377 0.5410 0.6333 0.187 Uiso 0.50 1 calc PR B 1
H25B H 0.0730 0.4990 0.7047 0.187 Uiso 0.50 1 calc PR B 1
H25C H 0.0959 0.5708 0.6156 0.187 Uiso 0.50 1 d PR B 2
H25D H 0.1181 0.5147 0.6955 0.187 Uiso 0.50 1 d PR B 2
C26 C 0.006(2) 0.391(2) 0.5963(17) 0.137(10) Uiso 0.70 1 d PD B 1
H26A H 0.0708 0.3604 0.5859 0.206 Uiso 0.70 1 calc PR B 1
H26B H -0.0401 0.3928 0.5434 0.206 Uiso 0.70 1 calc PR B 1
H26C H -0.0456 0.3406 0.6261 0.206 Uiso 0.70 1 calc PR B 1
C26' C 0.063(9) 0.392(5) 0.657(7) 0.22(4) Uiso 0.30 1 d PD B 2
H26D H 0.1100 0.3668 0.6182 0.335 Uiso 0.30 1 calc PR B 2
H26E H -0.0175 0.3356 0.6446 0.335 Uiso 0.30 1 calc PR B 2
H26F H 0.1013 0.3955 0.7138 0.335 Uiso 0.30 1 calc PR B 2
C27 C 0.0030(8) 0.9153(9) 0.6476(7) 0.047(3) Uani 1 1 d . . .
C28 C 0.1788(11) 1.1017(12) 0.6574(9) 0.101(5) Uani 1 1 d . . .
H28A H 0.1633 1.1229 0.7129 0.152 Uiso 1 1 calc R B .
H28B H 0.1586 1.1538 0.6226 0.152 Uiso 1 1 calc R . .
H28C H 0.2632 1.1096 0.6612 0.152 Uiso 1 1 calc R . .
C29 C 0.1275(10) 0.9308(13) 0.5390(8) 0.082(4) Uani 1 1 d . . .
H29A H 0.0751 0.8496 0.5194 0.123 Uiso 1 1 calc R B .
H29B H 0.2108 0.9334 0.5452 0.123 Uiso 1 1 calc R . .
H29C H 0.1117 0.9780 0.4987 0.123 Uiso 1 1 calc R . .
C30 C 0.0607(9) 1.0034(10) 0.8012(7) 0.057(3) Uani 1 1 d . . .
H30A H 0.0152 1.0060 0.8464 0.068 Uiso 1 1 calc R B .
H30B H 0.0944 1.0844 0.7928 0.068 Uiso 1 1 calc R . .
C31 C 0.1642(10) 0.9568(12) 0.8281(7) 0.074(4) Uani 1 1 d . B .
H31A H 0.1309 0.8739 0.8329 0.088 Uiso 1 1 calc R . .
H31B H 0.2135 0.9595 0.7849 0.088 Uiso 1 1 calc R . .
C32 C 0.2424(12) 1.0282(14) 0.9105(8) 0.093(5) Uani 1 1 d . . .
H32A H 0.2825 1.1086 0.9031 0.112 Uiso 1 1 calc R B .
H32B H 0.1905 1.0341 0.9513 0.112 Uiso 1 1 calc R . .
C33 C 0.3366(14) 0.9795(18) 0.9463(9) 0.137(7) Uani 1 1 d . B .
H33A H 0.3831 1.0314 0.9987 0.206 Uiso 1 1 calc R . .
H33B H 0.3896 0.9745 0.9071 0.206 Uiso 1 1 calc R . .
H33C H 0.2980 0.9012 0.9564 0.206 Uiso 1 1 calc R . .
B3 B -0.3505(12) 1.0025(11) 0.7976(8) 0.057(3) Uani 1 1 d . B .
H3 H -0.3701 0.9451 0.8442 0.068 Uiso 1 1 calc R . .
B4 B -0.4561(14) 1.0704(14) 0.7564(9) 0.072(4) Uani 1 1 d . . .
H4 H -0.5444 1.0577 0.7758 0.086 Uiso 1 1 calc R B .
B5 B -0.4405(12) 1.0801(12) 0.6530(9) 0.060(4) Uani 1 1 d . B .
H5 H -0.5183 1.0745 0.6046 0.072 Uiso 1 1 calc R . .
B6 B -0.3251(10) 1.0149(11) 0.6308(7) 0.047(3) Uani 1 1 d . B .
H6 H -0.3284 0.9647 0.5677 0.056 Uiso 1 1 calc R . .
B7 B -0.2026(12) 1.0957(10) 0.8007(8) 0.056(3) Uani 1 1 d . B .
H7 H -0.1253 1.1004 0.8492 0.067 Uiso 1 1 calc R . .
B8 B -0.1877(12) 1.1056(10) 0.6954(8) 0.054(3) Uani 1 1 d . B .
H8 H -0.1004 1.1177 0.6747 0.064 Uiso 1 1 calc R . .
B9 B -0.2905(13) 1.1724(12) 0.6535(9) 0.067(4) Uani 1 1 d . . .
H9 H -0.2711 1.2267 0.6051 0.081 Uiso 1 1 calc R B .
B10 B -0.3702(15) 1.2084(13) 0.7348(9) 0.077(4) Uani 1 1 d . B .
H10 H -0.4012 1.2869 0.7404 0.092 Uiso 1 1 calc R . .
B11 B -0.3162(15) 1.1576(15) 0.8229(10) 0.084(5) Uani 1 1 d . B .
H11 H -0.3133 1.2035 0.8873 0.101 Uiso 1 1 calc R . .
B12 B -0.2137(14) 1.2234(12) 0.7616(9) 0.069(4) Uani 1 1 d . B .
H12 H -0.1438 1.3118 0.7848 0.083 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
Zr1 N2 2.259(8) . ?
Zr1 N1 2.277(8) . ?
Zr1 C2 2.398(9) . ?
Zr1 C12 2.516(9) . ?
Zr1 C13 2.519(10) . ?
Zr1 S2 2.527(3) . ?
Zr1 C11 2.537(10) . ?
Zr1 C18 2.607(9) . ?
Zr1 C19 2.615(9) . ?
Zr1 S1 2.628(3) . ?
Zr1 C27 2.846(9) . ?
S1 C20 1.708(11) . ?
S2 C27 1.750(10) . ?
N1 C27 1.304(12) . ?
N1 C30 1.474(12) . ?
N2 C20 1.331(12) . ?
N2 C23' 1.446(19) . ?
N2 C23 1.54(2) . ?
N3 C20 1.361(12) . ?
N3 C21 1.449(17) . ?
N3 C22 1.478(16) . ?
N3 C22' 1.490(16) . ?
N3 C21' 1.512(17) . ?
N4 C27 1.385(12) . ?
N4 C29 1.449(14) . ?
N4 C28 1.456(14) . ?
C1 C3 1.569(14) . ?
C1 B4 1.694(17) . ?
C1 B3 1.698(15) . ?
C1 B6 1.701(15) . ?
C1 C2 1.707(13) . ?
C1 B5 1.709(14) . ?
C2 B6 1.693(13) . ?
C2 B3 1.715(16) . ?
C2 B7 1.721(15) . ?
C2 B8 1.733(15) . ?
C3 C11 1.499(14) . ?
C3 C5 1.540(14) . ?
C3 C4 1.577(15) . ?
C11 C12 1.430(14) . ?
C11 C18 1.433(14) . ?
C12 C13 1.432(15) . ?
C13 C19 1.397(15) . ?
C14 C15 1.397(18) . ?
C14 C19 1.410(15) . ?
C15 C16 1.416(19) . ?
C16 C17 1.327(16) . ?
C17 C18 1.450(14) . ?
C18 C19 1.450(14) . ?
C23 C24 1.377(18) . ?
C24 C25 1.485(18) . ?
C23' C24' 1.315(16) . ?
C24' C25 1.453(16) . ?
C25 C26 1.466(17) . ?
C25 C26' 1.49(2) . ?
C30 C31 1.519(14) . ?
C31 C32 1.492(15) . ?
C32 C33 1.487(19) . ?
B3 B11 1.75(2) . ?
B3 B7 1.752(19) . ?
B3 B4 1.783(18) . ?
B4 B5 1.737(19) . ?
B4 B11 1.76(2) . ?
B4 B10 1.77(2) . ?
B5 B10 1.77(2) . ?
B5 B9 1.78(2) . ?
B5 B6 1.805(17) . ?
B6 B8 1.742(16) . ?
B6 B9 1.773(17) . ?
B7 B11 1.76(2) . ?
B7 B8 1.766(18) . ?
B7 B12 1.772(18) . ?
B8 B9 1.753(17) . ?
B8 B12 1.771(18) . ?
B9 B12 1.79(2) . ?
B9 B10 1.80(2) . ?
B10 B11 1.75(2) . ?
B10 B12 1.78(2) . ?
B11 B12 1.75(2) . ?
