#------------------------------------------------------------------------------
#$Date: 2022-09-15 01:26:15 +0300 (Thu, 15 Sep 2022) $
#$Revision: 277847 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/06/14/4061484.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_4061484
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         'C61 H73 B3 Hf1 O3, 0.5(C5 H12)'
_chemical_formula_sum            'C63.5 H79 B3 Hf O3'
_chemical_formula_weight         1101.19
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                105.180(2)
_cell_angle_beta                 94.640(2)
_cell_angle_gamma                104.603(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2043(4)
_cell_length_b                   15.7658(4)
_cell_length_c                   16.3282(6)
_cell_measurement_temperature    173(2)
_cell_volume                     2897.62(16)
_diffrn_ambient_temperature      173(2)
_exptl_crystal_density_diffrn    1.262
_cod_original_formula_sum        'C63.50 H79 B3 Hf O3'
_cod_database_code               4061484
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
Hf Hf 0.243132(19) 0.325054(16) 0.294133(16) 0.04403(10) Uani 1 1 d . . .
O1 O 0.1687(3) 0.3910(3) 0.2351(3) 0.0476(9) Uani 1 1 d . . .
O2 O 0.1526(4) 0.2670(3) 0.3655(3) 0.0574(11) Uani 1 1 d . . .
O3 O 0.2981(4) 0.2362(3) 0.2173(3) 0.0558(10) Uani 1 1 d . . .
C1 C 0.2170(5) 0.5112(4) 0.1570(4) 0.0472(13) Uani 1 1 d . . .
C2 C 0.2282(5) 0.6055(4) 0.1764(4) 0.0507(14) Uani 1 1 d . . .
C3 C 0.3126(6) 0.6615(5) 0.1465(5) 0.0595(16) Uani 1 1 d . . .
H3 H 0.3201 0.7254 0.1617 0.071 Uiso 1 1 calc R . .
C4 C 0.3861(6) 0.6277(5) 0.0955(5) 0.0611(17) Uani 1 1 d . . .
C5 C 0.3730(6) 0.5349(5) 0.0751(5) 0.0638(18) Uani 1 1 d . . .
H5 H 0.4218 0.5099 0.0395 0.077 Uiso 1 1 calc R . .
C6 C 0.2912(5) 0.4761(4) 0.1047(4) 0.0546(15) Uani 1 1 d . . .
C7 C 0.1505(7) 0.6496(4) 0.2300(5) 0.0668(19) Uani 1 1 d . . .
H7A H 0.1802 0.7164 0.2446 0.1 Uiso 1 1 calc R . .
H7B H 0.1481 0.6312 0.2829 0.1 Uiso 1 1 calc R . .
H7C H 0.073 0.6297 0.1972 0.1 Uiso 1 1 calc R . .
C8 C 0.4750(7) 0.6906(6) 0.0625(6) 0.081(2) Uani 1 1 d . . .
H8A H 0.4704 0.7536 0.084 0.122 Uiso 0.5 1 calc PR . .
H8B H 0.4606 0.6712 -0.0005 0.122 Uiso 0.5 1 calc PR . .
H8C H 0.5515 0.6879 0.0825 0.122 Uiso 0.5 1 calc PR . .
H8D H 0.5179 0.6548 0.0267 0.122 Uiso 0.5 1 calc PR . .
H8E H 0.5278 0.7372 0.1111 0.122 Uiso 0.5 1 calc PR . .
H8F H 0.4368 0.7205 0.0281 0.122 Uiso 0.5 1 calc PR . .
C9 C 0.2831(7) 0.3738(5) 0.0755(5) 0.076(2) Uani 1 1 d . . .
H9A H 0.2969 0.3566 0.0159 0.113 Uiso 1 1 calc R . .
H9B H 0.2065 0.3379 0.0794 0.113 Uiso 1 1 calc R . .
H9C H 0.3408 0.3615 0.1125 0.113 Uiso 1 1 calc R . .
C10 C -0.0018(5) 0.4445(4) 0.1934(4) 0.0478(13) Uani 1 1 d . . .
C11 C -0.0478(5) 0.4686(4) 0.2691(4) 0.0524(15) Uani 1 1 d . . .
C12 C -0.1631(6) 0.4701(4) 0.2632(5) 0.0615(17) Uani 1 1 d . . .
H12 H -0.1932 0.4886 0.3147 0.074 Uiso 1 1 calc R . .
C13 C -0.2336(6) 0.4460(5) 0.1858(5) 0.0664(19) Uani 1 1 d . . .
C14 C -0.1880(6) 0.4210(5) 0.1119(5) 0.0679(19) Uani 1 1 d . . .
H14 H -0.2354 0.4039 0.0578 0.082 Uiso 1 1 calc R . .
C15 C -0.0739(5) 0.4199(4) 0.1143(4) 0.0543(15) Uani 1 1 d . . .
C16 C 0.0233(6) 0.4947(5) 0.3566(4) 0.0645(18) Uani 1 1 d . . .
H16A H 0.036 0.4397 0.3682 0.097 Uiso 1 1 calc R . .
H16B H -0.0172 0.5233 0.4004 0.097 Uiso 1 1 calc R . .
H16C H 0.0973 0.5381 0.3582 0.097 Uiso 1 1 calc R . .
C17 C -0.3586(7) 0.4463(7) 0.1820(7) 0.097(3) Uani 1 1 d . . .
H17A H -0.3756 0.4658 0.2405 0.146 Uiso 0.5 1 calc PR . .
H17B H -0.4083 0.3845 0.1523 0.146 Uiso 0.5 1 calc PR . .
H17C H -0.3724 0.4888 0.1508 0.146 Uiso 0.5 1 calc PR . .
H17D H -0.3953 0.4269 0.1219 0.146 Uiso 0.5 1 calc PR . .
H17E H -0.3625 0.5083 0.2101 0.146 Uiso 0.5 1 calc PR . .
H17F H -0.3984 0.4039 0.2116 0.146 Uiso 0.5 1 calc PR . .
C18 C -0.0293(6) 0.3890(6) 0.0302(4) 0.0696(19) Uani 1 1 d . . .
H18A H -0.0117 0.3308 0.026 0.104 Uiso 1 1 calc R . .
H18B H 0.0404 0.4356 0.0288 0.104 Uiso 1 1 calc R . .
H18C H -0.0879 0.3808 -0.0182 0.104 Uiso 1 1 calc R . .
C19 C -0.0162(5) 0.1353(4) 0.3684(4) 0.0471(13) Uani 1 1 d . . .
C20 C -0.1075(5) 0.1574(4) 0.3296(4) 0.0537(15) Uani 1 1 d . . .
C21 C -0.2131(6) 0.0909(5) 0.2968(4) 0.0628(17) Uani 1 1 d . . .
H21 H -0.2746 0.1074 0.2717 0.075 Uiso 1 1 calc R . .
C22 C -0.2301(6) 0.0021(5) 0.3001(4) 0.0603(16) Uani 1 1 d . . .
C23 C -0.1413(6) -0.0201(4) 0.3376(4) 0.0589(16) Uani 1 1 d . . .
H23 H -0.1532 -0.0807 0.3417 0.071 Uiso 1 1 calc R . .
C24 C -0.0329(5) 0.0435(4) 0.3701(4) 0.0480(13) Uani 1 1 d . . .
C25 C -0.0977(6) 0.2538(5) 0.3251(5) 0.0622(17) Uani 1 1 d . . .
H25A H -0.0674 0.2615 0.2729 0.093 Uiso 1 1 calc R . .
H25B H -0.0459 0.2982 0.3756 0.093 Uiso 1 1 calc R . .
H25C H -0.1737 0.2642 0.3239 0.093 Uiso 1 1 calc R . .
C26 C -0.3451(7) -0.0681(6) 0.2638(6) 0.092(3) Uani 1 1 d . . .
H26A H -0.3975 -0.0396 0.2398 0.137 Uiso 0.5 1 calc PR . .
H26B H -0.3771 -0.0911 0.3096 0.137 Uiso 0.5 1 calc PR . .
H26C H -0.3354 -0.1191 0.2184 0.137 Uiso 0.5 1 calc PR . .
H26D H -0.3425 -0.1269 0.2721 0.137 Uiso 0.5 1 calc PR . .
H26E H -0.3629 -0.0754 0.2023 0.137 Uiso 0.5 1 calc PR . .
H26F H -0.4045 -0.0474 0.2934 0.137 Uiso 0.5 1 calc PR . .
C27 C 0.0632(6) 0.0115(5) 0.4055(5) 0.0635(17) Uani 1 1 d . . .
H27A H 0.0314 -0.0492 0.4127 0.095 Uiso 1 1 calc R . .
H27B H 0.1018 0.055 0.4612 0.095 Uiso 1 1 calc R . .
H27C H 0.1186 0.008 0.3653 0.095 Uiso 1 1 calc R . .
C28 C 0.1616(6) 0.2314(4) 0.5048(5) 0.0581(16) Uani 1 1 d . . .
C29 C 0.1044(7) 0.2581(5) 0.5743(5) 0.0666(18) Uani 1 1 d . . .
C30 C 0.1595(11) 0.2853(5) 0.6585(6) 0.095(3) Uani 1 1 d . . .
H30 H 0.1197 0.3045 0.7044 0.114 Uiso 1 1 calc R . .
C31 C 0.2723(14) 0.2848(6) 0.6763(7) 0.118(5) Uani 1 1 d . . .
C32 C 0.3288(8) 0.2569(7) 0.6091(8) 0.105(4) Uani 1 1 d . . .
H32 H 0.4058 0.2558 0.6213 0.126 Uiso 1 1 calc R . .
C33 C 0.2760(6) 0.2300(6) 0.5231(6) 0.079(2) Uani 1 1 d . . .
C34 C -0.0191(8) 0.2580(6) 0.5598(6) 0.088(3) Uani 1 1 d . . .
H34A H -0.0271 0.2988 0.5251 0.132 Uiso 1 1 calc R . .
H34B H -0.0438 0.2794 0.6153 0.132 Uiso 1 1 calc R . .
H34C H -0.0669 0.1956 0.5297 0.132 Uiso 1 1 calc R . .
C35 C 0.3296(12) 0.3145(10) 0.7695(9) 0.144(5) Uiso 1 1 d . . .
H35A H 0.4086 0.3105 0.7717 0.217 Uiso 0.5 1 calc PR . .
H35B H 0.2871 0.2743 0.8 0.217 Uiso 0.5 1 calc PR . .
H35C H 0.3302 0.3779 0.7968 0.217 Uiso 0.5 1 calc PR . .
H35D H 0.2753 0.3313 0.8073 0.217 Uiso 0.5 1 calc PR . .
H35E H 0.3968 0.3675 0.779 0.217 Uiso 0.5 1 calc PR . .
H35F H 0.3537 0.2639 0.7821 0.217 Uiso 0.5 1 calc PR . .
C36 C 0.3409(7) 0.1989(8) 0.4528(8) 0.114(4) Uani 1 1 d . . .
H36A H 0.3902 0.2525 0.441 0.171 Uiso 1 1 calc R . .
H36B H 0.2869 0.1608 0.4008 0.171 Uiso 1 1 calc R . .
H36C H 0.3884 0.1632 0.4706 0.171 Uiso 1 1 calc R . .
C37 C 0.2127(5) 0.0653(4) 0.1667(4) 0.0491(14) Uani 1 1 d . . .
C38 C 0.0960(5) 0.0572(4) 0.1414(4) 0.0543(15) Uani 1 1 d . . .
C39 C 0.0112(6) -0.0220(5) 0.1380(4) 0.0633(17) Uani 1 1 d . . .
H39 H -0.0666 -0.0262 0.1204 0.076 Uiso 1 1 calc R . .
C40 C 0.0369(6) -0.0949(5) 0.1594(5) 0.0649(18) Uani 1 1 d . . .
C41 C 0.1495(7) -0.0871(5) 0.1859(5) 0.0681(19) Uani 1 1 d . . .
H41 H 0.168 -0.1361 0.202 0.082 Uiso 1 1 calc R . .
C42 C 0.2381(6) -0.0092(4) 0.1898(4) 0.0546(15) Uani 1 1 d . . .
C43 C 0.0585(6) 0.1319(5) 0.1143(5) 0.073(2) Uani 1 1 d . . .
H43A H -0.0089 0.104 0.0694 0.109 Uiso 1 1 calc R . .
H43B H 0.121 0.1672 0.0921 0.109 Uiso 1 1 calc R . .
H43C H 0.0393 0.1727 0.164 0.109 Uiso 1 1 calc R . .
C44 C -0.0572(8) -0.1806(5) 0.1544(6) 0.091(3) Uani 1 1 d . . .
H44A H -0.1316 -0.1737 0.1345 0.136 Uiso 0.5 1 calc PR . .
H44B H -0.0575 -0.1899 0.2115 0.136 Uiso 0.5 1 calc PR . .
H44C H -0.0435 -0.2336 0.1141 0.136 Uiso 0.5 1 calc PR . .
H44D H -0.0235 -0.2244 0.1722 0.136 Uiso 0.5 1 calc PR . .
H44E H -0.0975 -0.2083 0.0953 0.136 Uiso 0.5 1 calc PR . .
H44F H -0.1115 -0.1645 0.1926 0.136 Uiso 0.5 1 calc PR . .
C45 C 0.3602(7) -0.0066(5) 0.2203(6) 0.075(2) Uani 1 1 d . . .
H45A H 0.3922 0.0448 0.2725 0.112 Uiso 1 1 calc R . .
H45B H 0.407 0.0011 0.1754 0.112 Uiso 1 1 calc R . .
H45C H 0.3602 -0.0642 0.2328 0.112 Uiso 1 1 calc R . .
C46 C 0.4229(5) 0.1550(4) 0.1303(4) 0.0494(14) Uani 1 1 d . . .
C47 C 0.5323(6) 0.1975(4) 0.1798(4) 0.0560(15) Uani 1 1 d . . .
C48 C 0.6303(5) 0.1978(5) 0.1414(5) 0.0585(16) Uani 1 1 d . . .
H48 H 0.7036 0.2257 0.176 0.07 Uiso 1 1 calc R . .
C49 C 0.6234(6) 0.1584(4) 0.0540(5) 0.0582(16) Uani 1 1 d . . .
C50 C 0.5168(6) 0.1170(4) 0.0061(4) 0.0567(15) Uani 1 1 d . . .
H50 H 0.5108 0.0883 -0.0536 0.068 Uiso 1 1 calc R . .
C51 C 0.4163(5) 0.1152(4) 0.0417(4) 0.0508(14) Uani 1 1 d . . .
C52 C 0.5472(6) 0.2397(6) 0.2770(4) 0.073(2) Uani 1 1 d . . .
H52A H 0.6165 0.2311 0.3043 0.109 Uiso 1 1 calc R . .
H52B H 0.4804 0.2097 0.299 0.109 Uiso 1 1 calc R . .
H52C H 0.5545 0.3054 0.2901 0.109 Uiso 1 1 calc R . .
C53 C 0.7319(7) 0.1642(6) 0.0137(6) 0.081(2) Uani 1 1 d . . .
H53A H 0.799 0.1964 0.0584 0.122 Uiso 0.5 1 calc PR . .
H53B H 0.7308 0.1977 -0.0291 0.122 Uiso 0.5 1 calc PR . .
H53C H 0.7359 0.1022 -0.0144 0.122 Uiso 0.5 1 calc PR . .
H53D H 0.7115 0.1344 -0.0484 0.122 Uiso 0.5 1 calc PR . .
H53E H 0.7796 0.1332 0.039 0.122 Uiso 0.5 1 calc PR . .
H53F H 0.7745 0.2287 0.0243 0.122 Uiso 0.5 1 calc PR . .
C54 C 0.3026(6) 0.0748(5) -0.0183(4) 0.0658(18) Uani 1 1 d . . .
H54A H 0.2446 0.0442 0.0107 0.099 Uiso 1 1 calc R . .
H54B H 0.3112 0.0302 -0.0701 0.099 Uiso 1 1 calc R . .
H54C H 0.2787 0.1239 -0.0343 0.099 Uiso 1 1 calc R . .
C55 C 0.3987(6) 0.4247(5) 0.3781(5) 0.073(2) Uani 1 1 d . . .
H55A H 0.4276 0.3991 0.4218 0.087 Uiso 1 1 calc R . .
H55B H 0.46 0.4403 0.3437 0.087 Uiso 1 1 calc R . .
C56 C 0.3632(5) 0.5079(5) 0.4201(4) 0.0615(17) Uani 1 1 d . . .
C57 C 0.3786(7) 0.5822(5) 0.3862(5) 0.076(2) Uani 1 1 d . . .
H57 H 0.4129 0.5798 0.3358 0.091 Uiso 1 1 calc R . .
C58 C 0.3455(7) 0.6586(5) 0.4237(5) 0.074(2) Uani 1 1 d . . .
H58 H 0.3596 0.7087 0.4001 0.089 Uiso 1 1 calc R . .
C59 C 0.2920(6) 0.6633(5) 0.4955(5) 0.072(2) Uani 1 1 d . . .
H59 H 0.2688 0.7159 0.5215 0.086 Uiso 1 1 calc R . .
C60 C 0.2733(7) 0.5904(6) 0.5284(5) 0.077(2) Uani 1 1 d . . .
H60 H 0.2357 0.5925 0.5773 0.093 Uiso 1 1 calc R . .
C61 C 0.3083(6) 0.5126(5) 0.4915(5) 0.0697(19) Uani 1 1 d . . .
H61 H 0.2943 0.4629 0.5155 0.084 Uiso 1 1 calc R . .
B1 B 0.1284(6) 0.4468(4) 0.1967(4) 0.0448(14) Uani 1 1 d . . .
B2 B 0.1004(6) 0.2099(5) 0.4104(5) 0.0510(16) Uani 1 1 d . . .
B3 B 0.3113(6) 0.1544(5) 0.1725(4) 0.0500(16) Uani 1 1 d . . .
C1S C 0.305(2) -0.0955(15) 0.4384(14) 0.201(8) Uiso 1 1 d . . .
C2S C 0.384(3) -0.044(3) 0.491(3) 0.332(17) Uiso 1 1 d . . .
C3S C 0.505(4) 0.020(3) 0.530(2) 0.165(12) Uiso 0.5 1 d P . .
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 1.916(4) . ?
Hf O3 1.918(4) . ?
Hf O1 1.922(4) . ?
Hf C55 2.214(7) . ?
O1 B1 1.365(7) . ?
O2 B2 1.374(8) . ?
O3 B3 1.362(8) . ?
C1 C2 1.405(8) . ?
C1 C6 1.408(8) . ?
C1 B1 1.589(9) . ?
C2 C3 1.389(9) . ?
C2 C7 1.515(9) . ?
C3 C4 1.384(10) . ?
C4 C5 1.377(10) . ?
C4 C8 1.510(9) . ?
C5 C6 1.391(9) . ?
C6 C9 1.533(9) . ?
C10 C11 1.401(8) . ?
C10 C15 1.405(9) . ?
C10 B1 1.576(9) . ?
C11 C12 1.409(9) . ?
C11 C16 1.508(9) . ?
C12 C13 1.375(10) . ?
C13 C14 1.374(11) . ?
C13 C17 1.524(10) . ?
C14 C15 1.394(9) . ?
C15 C18 1.524(9) . ?
C19 C20 1.402(8) . ?
C19 C24 1.417(8) . ?
C19 B2 1.567(10) . ?
C20 C21 1.401(9) . ?
C20 C25 1.516(9) . ?
C21 C22 1.380(9) . ?
C22 C23 1.366(10) . ?
C22 C26 1.512(10) . ?
C23 C24 1.406(9) . ?
C24 C27 1.518(9) . ?
C28 C29 1.407(10) . ?
C28 C33 1.411(10) . ?
C28 B2 1.568(10) . ?
C29 C30 1.386(11) . ?
C29 C34 1.507(11) . ?
C30 C31 1.386(17) . ?
C31 C32 1.377(17) . ?
C31 C35 1.520(15) . ?
C32 C33 1.404(13) . ?
C33 C36 1.495(13) . ?
C37 C38 1.415(8) . ?
C37 C42 1.419(8) . ?
C37 B3 1.578(10) . ?
C38 C39 1.392(9) . ?
C38 C43 1.517(9) . ?
C39 C40 1.383(10) . ?
C40 C41 1.372(10) . ?
C40 C44 1.516(10) . ?
C41 C42 1.399(10) . ?
C42 C45 1.520(9) . ?
C46 C51 1.403(8) . ?
C46 C47 1.406(9) . ?
C46 B3 1.574(9) . ?
C47 C48 1.394(9) . ?
C47 C52 1.528(9) . ?
C48 C49 1.386(10) . ?
C49 C50 1.368(9) . ?
C49 C53 1.519(9) . ?
C50 C51 1.396(9) . ?
C51 C54 1.516(9) . ?
C55 C56 1.497(10) . ?
C56 C61 1.385(10) . ?
C56 C57 1.400(11) . ?
C57 C58 1.374(11) . ?
C58 C59 1.382(11) . ?
C59 C60 1.368(11) . ?
C60 C61 1.404(11) . ?
C1S C2S 1.19(4) . ?
C2S C3S 1.41(5) 2_656 ?
C2S C3S 1.54(5) . ?
C3S C3S 1.00(6) 2_656 ?
C3S C2S 1.41(5) 2_656 ?
