#------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/14/4061479.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_4061479
loop_
_publ_author_name
'Cole, Sarah C.'
'Coles, Martyn P.'
'Hitchcock, Peter B.'
_publ_section_title
;
Boroxide Complexes of the group 4 Metals: A 'Non-Innocent'
Ligand in Olefin Polymerisation
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3279
_journal_page_last               3289
_journal_paper_doi               10.1021/om050202+
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C44 H60 B2 Cl2 Hf1 O4'
_chemical_formula_sum            'C44 H60 B2 Cl2 Hf O4'
_chemical_formula_weight         923.93
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 91.582(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3030(1)
_cell_length_b                   25.2472(3)
_cell_length_c                   16.7087(2)
_cell_measurement_temperature    173(2)
_cell_volume                     4344.64(8)
_diffrn_ambient_temperature      173(2)
_exptl_crystal_density_diffrn    1.413
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C44 H60 B2 Cl2 Hf1 O4'
_cod_database_code               4061479
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Hf Hf 0.408825(18) 0.603559(7) 0.844806(10) 0.02284(6) Uani 1 1 d . . .
Cl1 Cl 0.34152(11) 0.55793(5) 0.96679(6) 0.0337(3) Uani 1 1 d . . .
Cl2 Cl 0.53138(12) 0.64621(5) 0.73985(7) 0.0396(3) Uani 1 1 d . . .
O1 O 0.3068(3) 0.66660(11) 0.86523(17) 0.0296(7) Uani 1 1 d . . .
O2 O 0.2884(3) 0.56554(11) 0.77443(16) 0.0253(6) Uani 1 1 d . . .
O3 O 0.5821(3) 0.62879(12) 0.92361(17) 0.0351(8) Uani 1 1 d . . .
O4 O 0.5411(3) 0.53418(12) 0.82878(18) 0.0330(7) Uani 1 1 d . . .
C1 C 0.1229(5) 0.73138(16) 0.8352(3) 0.0296(10) Uani 1 1 d . . .
C2 C 0.0863(5) 0.71846(17) 0.7547(3) 0.0324(11) Uani 1 1 d . . .
C3 C -0.0371(5) 0.73217(18) 0.7247(3) 0.0387(12) Uani 1 1 d . . .
H3 H -0.0592 0.7235 0.6707 0.046 Uiso 1 1 calc R . .
C4 C -0.1276(5) 0.75749(18) 0.7694(3) 0.0365(12) Uani 1 1 d . . .
C5 C -0.0929(5) 0.76990(17) 0.8485(3) 0.0362(11) Uani 1 1 d . . .
H5 H -0.1543 0.7871 0.8811 0.043 Uiso 1 1 calc R . .
C6 C 0.0297(5) 0.75771(17) 0.8810(3) 0.0306(11) Uani 1 1 d . . .
C7 C 0.1776(5) 0.6902(2) 0.6997(3) 0.0428(13) Uani 1 1 d . . .
H7A H 0.1818 0.6526 0.7139 0.064 Uiso 1 1 calc R . .
H7B H 0.2645 0.7059 0.7053 0.064 Uiso 1 1 calc R . .
H7C H 0.1458 0.6939 0.6441 0.064 Uiso 1 1 calc R . .
C8 C -0.2599(5) 0.7720(2) 0.7350(3) 0.0523(14) Uani 1 1 d . . .
H8A H -0.3102 0.7896 0.7762 0.078 Uiso 0.5 1 calc PR . .
H8B H -0.3053 0.7399 0.7171 0.078 Uiso 0.5 1 calc PR . .
H8C H -0.25 0.796 0.6895 0.078 Uiso 0.5 1 calc PR . .
H8D H -0.2668 0.7607 0.679 0.078 Uiso 0.5 1 calc PR . .
H8E H -0.2717 0.8105 0.7381 0.078 Uiso 0.5 1 calc PR . .
H8F H -0.327 0.7543 0.7657 0.078 Uiso 0.5 1 calc PR . .
C9 C 0.0576(5) 0.77199(19) 0.9681(3) 0.0382(12) Uani 1 1 d . . .
H9A H 0.0749 0.7396 0.999 0.057 Uiso 1 1 calc R . .
H9B H -0.0178 0.7902 0.9897 0.057 Uiso 1 1 calc R . .
H9C H 0.1335 0.7953 0.9719 0.057 Uiso 1 1 calc R . .
C10 C 0.3592(4) 0.75843(16) 0.9116(2) 0.0252(10) Uani 1 1 d . . .
C11 C 0.4137(5) 0.79884(17) 0.8645(2) 0.0293(10) Uani 1 1 d . . .
C12 C 0.5058(5) 0.83298(19) 0.8981(3) 0.0367(12) Uani 1 1 d . . .
H12 H 0.5427 0.8594 0.8653 0.044 Uiso 1 1 calc R . .
C13 C 0.5460(5) 0.82976(19) 0.9780(3) 0.0370(12) Uani 1 1 d . . .
C14 C 0.4924(5) 0.79011(19) 1.0239(3) 0.0358(11) Uani 1 1 d . . .
H14 H 0.5184 0.7872 1.0787 0.043 Uiso 1 1 calc R . .
C15 C 0.4017(4) 0.75447(17) 0.9922(2) 0.0283(10) Uani 1 1 d . . .
C16 C 0.3771(5) 0.80357(19) 0.7768(3) 0.0416(12) Uani 1 1 d . . .
H16A H 0.4304 0.831 0.7523 0.062 Uiso 1 1 calc R . .
H16B H 0.2852 0.8132 0.7708 0.062 Uiso 1 1 calc R . .
H16C H 0.392 0.7696 0.7502 0.062 Uiso 1 1 calc R . .
C17 C 0.6474(5) 0.8668(2) 1.0128(3) 0.0532(15) Uani 1 1 d . . .
H17A H 0.6625 0.8587 1.0696 0.08 Uiso 0.5 1 calc PR . .
H17B H 0.6171 0.9035 1.0071 0.08 Uiso 0.5 1 calc PR . .
H17C H 0.7285 0.8624 0.9843 0.08 Uiso 0.5 1 calc PR . .
H17D H 0.6763 0.891 0.971 0.08 Uiso 0.5 1 calc PR . .
H17E H 0.7216 0.8463 1.0336 0.08 Uiso 0.5 1 calc PR . .
H17F H 0.6103 0.8873 1.0564 0.08 Uiso 0.5 1 calc PR . .
C18 C 0.3510(5) 0.71155(19) 1.0461(3) 0.0388(12) Uani 1 1 d . . .
H18A H 0.4167 0.7033 1.0878 0.058 Uiso 1 1 calc R . .
H18B H 0.3319 0.6797 1.0144 0.058 Uiso 1 1 calc R . .
H18C H 0.2715 0.7239 1.0712 0.058 Uiso 1 1 calc R . .
C19 C 0.1824(4) 0.55006(16) 0.6377(2) 0.0254(10) Uani 1 1 d . . .
C20 C 0.0615(4) 0.56542(18) 0.6040(3) 0.0308(10) Uani 1 1 d . . .
C21 C 0.0521(5) 0.57958(18) 0.5239(3) 0.0359(11) Uani 1 1 d . . .
H21 H -0.0299 0.5903 0.502 0.043 Uiso 1 1 calc R . .
C22 C 0.1578(5) 0.57866(19) 0.4746(3) 0.0394(12) Uani 1 1 d . . .
C23 C 0.2752(5) 0.56227(19) 0.5074(3) 0.0372(12) Uani 1 1 d . . .
H23 H 0.3485 0.5606 0.4742 0.045 Uiso 1 1 calc R . .
C24 C 0.2899(4) 0.54806(17) 0.5878(2) 0.0296(10) Uani 1 1 d . . .
C25 C -0.0597(5) 0.5694(2) 0.6526(3) 0.0463(13) Uani 1 1 d . . .
H25A H -0.0584 0.6028 0.6827 0.069 Uiso 1 1 calc R . .
H25B H -0.0628 0.5396 0.69 0.069 Uiso 1 1 calc R . .
H25C H -0.1364 0.5686 0.6167 0.069 Uiso 1 1 calc R . .
C26 C 0.1458(6) 0.5950(2) 0.3874(3) 0.0556(15) Uani 1 1 d . . .
H26A H 0.0559 0.6054 0.3746 0.083 Uiso 0.5 1 calc PR . .
H26B H 0.17 0.5652 0.3533 0.083 Uiso 0.5 1 calc PR . .
H26C H 0.2036 0.625 0.3778 0.083 Uiso 0.5 1 calc PR . .
H26D H 0.2305 0.5917 0.3625 0.083 Uiso 0.5 1 calc PR . .
H26E H 0.1164 0.6319 0.3838 0.083 Uiso 0.5 1 calc PR . .
H26F H 0.0828 0.572 0.3593 0.083 Uiso 0.5 1 calc PR . .
C27 C 0.4228(5) 0.5296(2) 0.6179(3) 0.0396(12) Uani 1 1 d . . .
H27A H 0.4725 0.5167 0.5727 0.059 Uiso 1 1 calc R . .
H27B H 0.4125 0.501 0.6568 0.059 Uiso 1 1 calc R . .
H27C H 0.469 0.5593 0.6435 0.059 Uiso 1 1 calc R . .
C28 C 0.1173(4) 0.49404(16) 0.7762(2) 0.0225(9) Uani 1 1 d . . .
C29 C 0.0437(4) 0.50676(17) 0.8441(2) 0.0263(10) Uani 1 1 d . . .
C30 C -0.0210(4) 0.46676(18) 0.8842(3) 0.0313(11) Uani 1 1 d . . .
H30 H -0.0692 0.4757 0.9299 0.038 Uiso 1 1 calc R . .
C31 C -0.0174(4) 0.41439(18) 0.8599(3) 0.0317(11) Uani 1 1 d . . .
C32 C 0.0533(4) 0.40250(17) 0.7928(3) 0.0307(10) Uani 1 1 d . . .
H32 H 0.0557 0.3669 0.7747 0.037 Uiso 1 1 calc R . .
C33 C 0.1208(4) 0.44073(17) 0.7512(2) 0.0257(10) Uani 1 1 d . . .
C34 C 0.0267(4) 0.56352(18) 0.8714(3) 0.0340(11) Uani 1 1 d . . .
H34A H 0.0776 0.5871 0.8378 0.051 Uiso 0.5 1 calc PR . .
H34B H 0.0568 0.5669 0.9274 0.051 Uiso 0.5 1 calc PR . .
H34C H -0.0652 0.5733 0.8668 0.051 Uiso 0.5 1 calc PR . .
H34D H -0.0315 0.5644 0.9168 0.051 Uiso 0.5 1 calc PR . .
H34E H -0.0107 0.5846 0.8273 0.051 Uiso 0.5 1 calc PR . .
H34F H 0.1114 0.5782 0.8879 0.051 Uiso 0.5 1 calc PR . .
C35 C -0.0891(5) 0.3716(2) 0.9031(3) 0.0460(13) Uani 1 1 d . . .
H35A H -0.075 0.3375 0.8767 0.069 Uiso 0.5 1 calc PR . .
H35B H -0.1821 0.3797 0.9021 0.069 Uiso 0.5 1 calc PR . .
H35C H -0.0568 0.3696 0.9588 0.069 Uiso 0.5 1 calc PR . .
H35D H -0.1343 0.3871 0.9484 0.069 Uiso 0.5 1 calc PR . .
H35E H -0.0272 0.3448 0.9229 0.069 Uiso 0.5 1 calc PR . .
H35F H -0.1525 0.3549 0.8663 0.069 Uiso 0.5 1 calc PR . .
C36 C 0.1973(5) 0.42343(19) 0.6801(3) 0.0400(12) Uani 1 1 d . . .
H36A H 0.2903 0.4274 0.6925 0.06 Uiso 1 1 calc R . .
H36B H 0.1734 0.4455 0.6337 0.06 Uiso 1 1 calc R . .
H36C H 0.1779 0.3863 0.6679 0.06 Uiso 1 1 calc R . .
C37 C 0.6582(5) 0.67726(19) 0.9135(3) 0.0378(12) Uani 1 1 d . . .
H37A H 0.6005 0.708 0.9034 0.045 Uiso 1 1 calc R . .
H37B H 0.7175 0.6736 0.8682 0.045 Uiso 1 1 calc R . .
C38 C 0.7343(6) 0.6838(2) 0.9917(3) 0.0529(15) Uani 1 1 d . . .
H38A H 0.8211 0.6992 0.9829 0.064 Uiso 1 1 calc R . .
H38B H 0.6872 0.7066 1.0295 0.064 Uiso 1 1 calc R . .
C39 C 0.7448(7) 0.6286(3) 1.0219(4) 0.075(2) Uani 1 1 d . . .
H39A H 0.8226 0.6112 1.0005 0.09 Uiso 1 1 calc R . .
H39B H 0.7521 0.6284 1.0811 0.09 Uiso 1 1 calc R . .
C40 C 0.6297(6) 0.6012(2) 0.9953(3) 0.0572(16) Uani 1 1 d . . .
H40A H 0.5637 0.6021 1.0372 0.069 Uiso 1 1 calc R . .
H40B H 0.6497 0.5638 0.9828 0.069 Uiso 1 1 calc R . .
C41 C 0.6797(5) 0.5336(2) 0.8111(4) 0.0564(16) Uani 1 1 d . . .
H41A H 0.7048 0.5664 0.783 0.068 Uiso 1 1 calc R . .
H41B H 0.7333 0.5302 0.8609 0.068 Uiso 1 1 calc R . .
C42 C 0.6956(6) 0.4876(3) 0.7601(4) 0.0656(18) Uani 1 1 d . . .
H42A H 0.786 0.4744 0.7632 0.079 Uiso 1 1 calc R . .
H42B H 0.6721 0.496 0.7037 0.079 Uiso 1 1 calc R . .
C43 C 0.6019(7) 0.4474(2) 0.7945(4) 0.072(2) Uani 1 1 d . . .
H43A H 0.5619 0.4255 0.7512 0.087 Uiso 1 1 calc R . .
H43B H 0.6479 0.4237 0.8331 0.087 Uiso 1 1 calc R . .
C44 C 0.4993(5) 0.47941(18) 0.8361(3) 0.0436(13) Uani 1 1 d . . .
H44A H 0.413 0.4742 0.8098 0.052 Uiso 1 1 calc R . .
H44B H 0.4945 0.4691 0.8931 0.052 Uiso 1 1 calc R . .
B1 B 0.2628(5) 0.71694(19) 0.8705(3) 0.0268(11) Uani 1 1 d . . .
B2 B 0.1990(5) 0.53778(19) 0.7310(3) 0.0228(11) Uani 1 1 d . . .
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
Hf O2 1.940(3) . ?
Hf O1 1.943(3) . ?
Hf O4 2.240(3) . ?
Hf O3 2.280(3) . ?
Hf Cl2 2.4396(11) . ?
Hf Cl1 2.4577(10) . ?
O1 B1 1.353(6) . ?
O2 B2 1.352(6) . ?
O3 C40 1.458(5) . ?
O3 C37 1.466(5) . ?
O4 C44 1.454(6) . ?
O4 C41 1.466(6) . ?
C1 C6 1.411(6) . ?
C1 C2 1.424(6) . ?
C1 B1 1.585(7) . ?
C2 C3 1.397(7) . ?
C2 C7 1.513(7) . ?
C3 C4 1.369(7) . ?
C4 C5 1.395(7) . ?
C4 C8 1.510(7) . ?
C5 C6 1.396(7) . ?
C6 C9 1.520(6) . ?
C10 C15 1.409(6) . ?
C10 C11 1.414(6) . ?
C10 B1 1.586(7) . ?
C11 C12 1.390(6) . ?
C11 C16 1.507(6) . ?
C12 C13 1.389(7) . ?
C13 C14 1.384(6) . ?
C13 C17 1.508(7) . ?
C14 C15 1.392(6) . ?
C15 C18 1.512(6) . ?
C19 C24 1.406(6) . ?
C19 C20 1.408(6) . ?
C19 B2 1.593(6) . ?
C20 C21 1.387(6) . ?
C20 C25 1.512(6) . ?
C21 C22 1.384(7) . ?
C22 C23 1.378(7) . ?
C22 C26 1.517(6) . ?
C23 C24 1.394(6) . ?
C24 C27 1.518(6) . ?
C28 C33 1.410(6) . ?
C28 C29 1.419(6) . ?
C28 B2 1.592(6) . ?
C29 C30 1.392(6) . ?
C29 C34 1.515(6) . ?
C30 C31 1.384(6) . ?
C31 C32 1.386(6) . ?
C31 C35 1.505(6) . ?
C32 C33 1.387(6) . ?
C33 C36 1.509(6) . ?
C37 C38 1.515(7) . ?
C38 C39 1.484(8) . ?
C39 C40 1.432(8) . ?
C41 C42 1.452(8) . ?
C42 C43 1.524(9) . ?
C43 C44 1.515(7) . ?
