#------------------------------------------------------------------------------
#$Date: 2015-03-09 17:37:50 +0200 (Mon, 09 Mar 2015) $
#$Revision: 133705 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/14/4061480.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_4061480
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         'C108 H134 B6 O8 Zr2, 4(C5 H12)'
_chemical_formula_sum            'C128 H182 B6 O8 Zr2'
_chemical_formula_weight         2096.04
_chemical_name_common            '[{Zr(OH)(OBMes2)3}2].4(pentane)'
_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'
_cell_angle_alpha                99.632(1)
_cell_angle_beta                 115.774(1)
_cell_angle_gamma                94.824(1)
_cell_formula_units_Z            1
_cell_length_a                   14.0750(3)
_cell_length_b                   15.3388(3)
_cell_length_c                   16.1859(4)
_cell_measurement_temperature    173(2)
_cell_volume                     3053.63(12)
_diffrn_ambient_temperature      173(2)
_exptl_crystal_density_diffrn    1.14
_cod_database_code               4061480
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 0.02382(4) 0.06261(4) 0.11290(4) 0.0281(2) Uani 1 1 d . . .
B1 B 0.1402(6) 0.2745(4) 0.1932(5) 0.0336(16) Uani 1 1 d . . .
B2 B 0.1690(6) -0.0216(5) 0.2902(5) 0.0368(17) Uani 1 1 d . . .
B3 B -0.2062(5) 0.0967(5) 0.0987(5) 0.0308(15) Uani 1 1 d . . .
O1 O 0.1067(3) 0.1841(3) 0.1530(3) 0.0374(10) Uani 1 1 d . . .
O2 O 0.0905(3) -0.0044(3) 0.2080(3) 0.0403(11) Uani 1 1 d . . .
O3 O -0.1034(3) 0.0875(3) 0.1286(3) 0.0366(10) Uani 1 1 d . . .
O4 O 0.0938(4) 0.0063(3) 0.0265(3) 0.0434(11) Uani 1 1 d . . .
H4 H 0.169(10) -0.001(8) 0.049(8) 0.13(4) Uiso 1 1 d . . .
C1 C 0.0546(5) 0.3295(4) 0.2023(4) 0.0378(15) Uani 1 1 d . . .
C2 C 0.0193(5) 0.3934(4) 0.1473(5) 0.0438(17) Uani 1 1 d . . .
C3 C -0.0587(6) 0.4400(5) 0.1532(6) 0.060(2) Uani 1 1 d . . .
H3 H -0.0819 0.4828 0.1157 0.072 Uiso 1 1 calc R . .
C4 C -0.1037(6) 0.4267(5) 0.2113(7) 0.065(2) Uani 1 1 d . . .
C5 C -0.0697(6) 0.3634(5) 0.2647(6) 0.056(2) Uani 1 1 d . . .
H5 H -0.1011 0.3525 0.3043 0.067 Uiso 1 1 calc R . .
C6 C 0.0089(5) 0.3151(4) 0.2622(5) 0.0435(16) Uani 1 1 d . . .
C7 C 0.0611(7) 0.4085(5) 0.0786(6) 0.060(2) Uani 1 1 d . . .
H7A H 0.0293 0.3577 0.0238 0.09 Uiso 1 1 calc R . .
H7B H 0.1392 0.4137 0.1091 0.09 Uiso 1 1 calc R . .
H7C H 0.0418 0.4639 0.0582 0.09 Uiso 1 1 calc R . .
C8 C -0.1885(8) 0.4787(7) 0.2162(9) 0.097(4) Uani 1 1 d . . .
H8A H -0.2109 0.4603 0.2612 0.145 Uiso 0.5 1 calc PR . .
H8B H -0.2505 0.4665 0.1538 0.145 Uiso 0.5 1 calc PR . .
H8C H -0.1591 0.5432 0.2369 0.145 Uiso 0.5 1 calc PR . .
H8D H -0.2028 0.5197 0.1734 0.145 Uiso 0.5 1 calc PR . .
H8E H -0.1631 0.5135 0.2808 0.145 Uiso 0.5 1 calc PR . .
H8F H -0.2546 0.4368 0.1977 0.145 Uiso 0.5 1 calc PR . .
C9 C 0.0441(6) 0.2502(5) 0.3247(5) 0.0536(19) Uani 1 1 d . . .
H9A H 0.0724 0.2823 0.3906 0.08 Uiso 1 1 calc R . .
H9B H 0.1002 0.2223 0.3159 0.08 Uiso 1 1 calc R . .
H9C H -0.0171 0.2037 0.3085 0.08 Uiso 1 1 calc R . .
C10 C 0.2594(5) 0.3180(4) 0.2226(4) 0.0371(15) Uani 1 1 d . . .
C11 C 0.3057(5) 0.2992(4) 0.1611(5) 0.0425(16) Uani 1 1 d . . .
C12 C 0.4092(6) 0.3426(5) 0.1868(6) 0.056(2) Uani 1 1 d . . .
H12 H 0.439 0.33 0.1444 0.067 Uiso 1 1 calc R . .
C13 C 0.4694(6) 0.4032(5) 0.2718(6) 0.059(2) Uani 1 1 d . . .
C14 C 0.4240(6) 0.4199(4) 0.3318(5) 0.0510(19) Uani 1 1 d . . .
H14 H 0.4651 0.4601 0.3914 0.061 Uiso 1 1 calc R . .
C15 C 0.3213(5) 0.3804(4) 0.3086(5) 0.0411(16) Uani 1 1 d . . .
C16 C 0.2461(7) 0.2341(6) 0.0662(5) 0.060(2) Uani 1 1 d . . .
H16A H 0.2817 0.2433 0.0273 0.09 Uiso 1 1 calc R . .
H16B H 0.1721 0.2444 0.0349 0.09 Uiso 1 1 calc R . .
H16C H 0.2457 0.1724 0.0749 0.09 Uiso 1 1 calc R . .
C17 C 0.5815(7) 0.4496(6) 0.2965(9) 0.095(4) Uani 1 1 d . . .
H17A H 0.5986 0.4285 0.2448 0.142 Uiso 0.5 1 calc PR . .
H17B H 0.6338 0.4353 0.3542 0.142 Uiso 0.5 1 calc PR . .
H17C H 0.5842 0.5147 0.3062 0.142 Uiso 0.5 1 calc PR . .
H17D H 0.6125 0.4906 0.3587 0.142 Uiso 0.5 1 calc PR . .
H17E H 0.5773 0.4837 0.2493 0.142 Uiso 0.5 1 calc PR . .
H17F H 0.6269 0.4043 0.2973 0.142 Uiso 0.5 1 calc PR . .
C18 C 0.2811(6) 0.4047(5) 0.3802(5) 0.0508(18) Uani 1 1 d . . .
H18A H 0.3375 0.4466 0.4363 0.076 Uiso 1 1 calc R . .
H18B H 0.2617 0.3502 0.3977 0.076 Uiso 1 1 calc R . .
H18C H 0.218 0.433 0.3533 0.076 Uiso 1 1 calc R . .
C19 C 0.2373(5) 0.0644(4) 0.3701(4) 0.0393(16) Uani 1 1 d . . .
C20 C 0.3123(5) 0.1233(4) 0.3625(5) 0.0406(16) Uani 1 1 d . . .
C21 C 0.3700(6) 0.2003(4) 0.4345(5) 0.0495(19) Uani 1 1 d . . .
H21 H 0.4215 0.2396 0.4287 0.059 Uiso 1 1 calc R . .
C22 C 0.3540(7) 0.2206(5) 0.5136(5) 0.060(2) Uani 1 1 d . . .
C23 C 0.2786(7) 0.1625(5) 0.5195(5) 0.060(2) Uani 1 1 d . . .
H23 H 0.2658 0.176 0.5728 0.072 Uiso 1 1 calc R . .
C24 C 0.2199(6) 0.0847(5) 0.4504(5) 0.0489(18) Uani 1 1 d . . .
C25 C 0.3369(6) 0.1041(5) 0.2801(5) 0.0468(17) Uani 1 1 d . . .
H25A H 0.3221 0.0391 0.2547 0.07 Uiso 1 1 calc R . .
H25B H 0.4126 0.1275 0.301 0.07 Uiso 1 1 calc R . .
H25C H 0.2919 0.1333 0.2311 0.07 Uiso 1 1 calc R . .
C26 C 0.4173(9) 0.3045(6) 0.5895(6) 0.090(3) Uani 1 1 d . . .
H26A H 0.4664 0.3368 0.5721 0.135 Uiso 0.5 1 calc PR . .
H26B H 0.4585 0.2879 0.6494 0.135 Uiso 0.5 1 calc PR . .
H26C H 0.368 0.3433 0.5962 0.135 Uiso 0.5 1 calc PR . .
H26D H 0.3955 0.3086 0.6397 0.135 Uiso 0.5 1 calc PR . .
H26E H 0.4034 0.3574 0.5624 0.135 Uiso 0.5 1 calc PR . .
H26F H 0.494 0.3021 0.6156 0.135 Uiso 0.5 1 calc PR . .
C27 C 0.1405(7) 0.0216(6) 0.4615(5) 0.067(2) Uani 1 1 d . . .
H27A H 0.1359 0.047 0.5191 0.101 Uiso 1 1 calc R . .
H27B H 0.164 -0.0365 0.4656 0.101 Uiso 1 1 calc R . .
H27C H 0.0699 0.0134 0.407 0.101 Uiso 1 1 calc R . .
C28 C 0.1852(5) -0.1213(4) 0.2935(4) 0.0348(14) Uani 1 1 d . . .
C29 C 0.2850(5) -0.1412(4) 0.3560(4) 0.0396(15) Uani 1 1 d . . .
C30 C 0.3001(6) -0.2293(5) 0.3525(5) 0.0462(17) Uani 1 1 d . . .
H30 H 0.3679 -0.2409 0.3938 0.055 Uiso 1 1 calc R . .
C31 C 0.2210(7) -0.3009(5) 0.2917(5) 0.055(2) Uani 1 1 d . . .
C32 C 0.1232(7) -0.2824(5) 0.2322(5) 0.058(2) Uani 1 1 d . . .
H32 H 0.0676 -0.3309 0.1897 0.069 Uiso 1 1 calc R . .
C33 C 0.1034(5) -0.1953(4) 0.2326(5) 0.0425(16) Uani 1 1 d . . .
C34 C 0.3789(5) -0.0706(5) 0.4282(5) 0.0499(18) Uani 1 1 d . . .
H34A H 0.4405 -0.0993 0.4596 0.075 Uiso 1 1 calc R . .
H34B H 0.3596 -0.039 0.4751 0.075 Uiso 1 1 calc R . .
H34C H 0.3975 -0.0275 0.3969 0.075 Uiso 1 1 calc R . .
C35 C 0.2422(9) -0.3967(5) 0.2895(8) 0.089(3) Uani 1 1 d . . .
H35A H 0.3155 -0.396 0.3368 0.133 Uiso 0.5 1 calc PR . .
H35B H 0.2333 -0.4244 0.2269 0.133 Uiso 0.5 1 calc PR . .
H35C H 0.1913 -0.4313 0.3033 0.133 Uiso 0.5 1 calc PR . .
H35D H 0.1779 -0.4385 0.2412 0.133 Uiso 0.5 1 calc PR . .
H35E H 0.2601 -0.4101 0.3511 0.133 Uiso 0.5 1 calc PR . .
H35F H 0.3021 -0.4031 0.2747 0.133 Uiso 0.5 1 calc PR . .
C36 C -0.0087(6) -0.1849(5) 0.1657(6) 0.064(2) Uani 1 1 d . . .
H36A H -0.0071 -0.1633 0.1126 0.096 Uiso 1 1 calc R . .
H36B H -0.0346 -0.1415 0.1992 0.096 Uiso 1 1 calc R . .
H36C H -0.0567 -0.2431 0.1423 0.096 Uiso 1 1 calc R . .
C37 C -0.2850(4) 0.0825(4) -0.0094(4) 0.0308(13) Uani 1 1 d . . .
C38 C -0.3776(5) 0.0154(4) -0.0530(4) 0.0341(14) Uani 1 1 d . . .
C39 C -0.4556(5) 0.0125(5) -0.1435(4) 0.0402(16) Uani 1 1 d . . .
H39 H -0.5178 -0.0328 -0.1715 0.048 Uiso 1 1 calc R . .
C40 C -0.4455(5) 0.0741(5) -0.1947(4) 0.0406(16) Uani 1 1 d . . .
C41 C -0.3512(5) 0.1359(4) -0.1542(4) 0.0400(16) Uani 1 1 d . . .
H41 H -0.3412 0.1763 -0.1894 0.048 Uiso 1 1 calc R . .
C42 C -0.2702(5) 0.1410(4) -0.0634(4) 0.0355(14) Uani 1 1 d . . .
C43 C -0.3931(6) -0.0540(5) -0.0012(5) 0.0451(16) Uani 1 1 d . . .
H43A H -0.4525 -0.1023 -0.0455 0.068 Uiso 1 1 calc R . .
H43B H -0.4094 -0.0255 0.0488 0.068 Uiso 1 1 calc R . .
H43C H -0.3273 -0.0789 0.0266 0.068 Uiso 1 1 calc R . .
C44 C -0.5327(6) 0.0739(6) -0.2901(5) 0.062(2) Uani 1 1 d . . .
H44A H -0.593 0.0258 -0.3073 0.093 Uiso 0.5 1 calc PR . .
H44B H -0.5054 0.0637 -0.3366 0.093 Uiso 0.5 1 calc PR . .
H44C H -0.557 0.1319 -0.2889 0.093 Uiso 0.5 1 calc PR . .
H44D H -0.5106 0.1218 -0.3146 0.093 Uiso 0.5 1 calc PR . .
H44E H -0.5982 0.0839 -0.2853 0.093 Uiso 0.5 1 calc PR . .
H44F H -0.5466 0.0157 -0.3329 0.093 Uiso 0.5 1 calc PR . .
C45 C -0.1724(6) 0.2125(5) -0.0241(5) 0.0500(18) Uani 1 1 d . . .
H45A H -0.1132 0.1859 -0.0281 0.075 Uiso 1 1 calc R . .
H45B H -0.1522 0.2393 0.0419 0.075 Uiso 1 1 calc R . .
H45C H -0.188 0.2591 -0.0604 0.075 Uiso 1 1 calc R . .
C46 C -0.2469(5) 0.1231(4) 0.1770(4) 0.0339(14) Uani 1 1 d . . .
C47 C -0.3121(5) 0.1897(4) 0.1721(5) 0.0388(15) Uani 1 1 d . . .
C48 C -0.3417(5) 0.2132(5) 0.2436(5) 0.0451(17) Uani 1 1 d . . .
H48 H -0.3844 0.2586 0.2399 0.054 Uiso 1 1 calc R . .
C49 C -0.3117(5) 0.1736(5) 0.3193(5) 0.0479(18) Uani 1 1 d . . .
C50 C -0.2489(5) 0.1074(5) 0.3227(5) 0.0473(18) Uani 1 1 d . . .
H50 H -0.227 0.0792 0.3745 0.057 Uiso 1 1 calc R . .
C51 C -0.2172(5) 0.0808(5) 0.2535(4) 0.0417(16) Uani 1 1 d . . .
C52 C -0.3489(6) 0.2388(5) 0.0936(5) 0.0470(17) Uani 1 1 d . . .
H52A H -0.3966 0.1963 0.0339 0.071 Uiso 1 1 calc R . .
H52B H -0.2866 0.267 0.0893 0.071 Uiso 1 1 calc R . .
H52C H -0.3876 0.2853 0.1064 0.071 Uiso 1 1 calc R . .
C53 C -0.3463(7) 0.2001(6) 0.3945(6) 0.068(2) Uani 1 1 d . . .
H53A H -0.3174 0.1648 0.4423 0.102 Uiso 0.5 1 calc PR . .
H53B H -0.4248 0.1886 0.3662 0.102 Uiso 0.5 1 calc PR . .
H53C H -0.3194 0.2642 0.4241 0.102 Uiso 0.5 1 calc PR . .
H53D H -0.3903 0.2469 0.3794 0.102 Uiso 0.5 1 calc PR . .
H53E H -0.2829 0.2231 0.4556 0.102 Uiso 0.5 1 calc PR . .
H53F H -0.3883 0.1475 0.3976 0.102 Uiso 0.5 1 calc PR . .
C54 C -0.1524(6) 0.0061(6) 0.2620(5) 0.057(2) Uani 1 1 d . . .
H54A H -0.0819 0.0291 0.2683 0.085 Uiso 1 1 calc R . .
H54B H -0.19 -0.0428 0.2056 0.085 Uiso 1 1 calc R . .
H54C H -0.1433 -0.0166 0.3177 0.085 Uiso 1 1 calc R . .
C55 C -0.3241(15) 0.4541(15) -0.0734(14) 0.183(8) Uani 1 1 d . . .
H55A H -0.3001 0.5175 -0.0402 0.275 Uiso 1 1 calc R . .
H55B H -0.328 0.4474 -0.1362 0.275 Uiso 1 1 calc R . .
H55C H -0.2732 0.4183 -0.0377 0.275 Uiso 1 1 calc R . .
C56 C -0.422(2) 0.425(2) -0.082(2) 0.287(19) Uani 1 1 d . . .
H56A H -0.4101 0.4434 -0.016 0.344 Uiso 1 1 calc R . .
H56B H -0.4638 0.4689 -0.114 0.344 Uiso 1 1 calc R . .
C57 C -0.4936(18) 0.3564(14) -0.1128(13) 0.142(6) Uani 1 1 d . . .
H57A H -0.452 0.3111 -0.0844 0.171 Uiso 1 1 calc R . .
H57B H -0.5102 0.3402 -0.1801 0.171 Uiso 1 1 calc R . .
C58 C -0.5942(18) 0.3283(17) -0.1164(19) 0.212(11) Uani 1 1 d . . .
H58A H -0.5814 0.3476 -0.0504 0.254 Uiso 1 1 calc R . .
H58B H -0.6402 0.3686 -0.1509 0.254 Uiso 1 1 calc R . .
C59 C -0.658(2) 0.2502(18) -0.1474(18) 0.219(11) Uani 1 1 d . . .
H59A H -0.7219 0.2568 -0.1383 0.328 Uiso 1 1 calc R . .
H59B H -0.6206 0.2071 -0.1124 0.328 Uiso 1 1 calc R . .
H59C H -0.6799 0.2282 -0.2146 0.328 Uiso 1 1 calc R . .
C60 C -0.1469(13) 0.4530(15) 0.4975(13) 0.158(7) Uani 1 1 d . . .
H60A H -0.1669 0.4957 0.5368 0.237 Uiso 1 1 calc R . .
H60B H -0.2118 0.4186 0.4424 0.237 Uiso 1 1 calc R . .
H60C H -0.1019 0.4859 0.4765 0.237 Uiso 1 1 calc R . .
C61 C -0.092(3) 0.3966(18) 0.548(2) 0.265(15) Uani 1 1 d . . .
H61A H -0.0324 0.4407 0.6004 0.318 Uiso 1 1 calc R . .
H61B H -0.1402 0.3796 0.5748 0.318 Uiso 1 1 calc R . .
C62 C -0.0470(13) 0.3274(14) 0.5501(14) 0.151(6) Uani 1 1 d . . .
H62A H -0.0078 0.3406 0.5143 0.181 Uiso 1 1 calc R . .
H62B H -0.1101 0.2818 0.5038 0.181 Uiso 1 1 calc R . .
C63 C 0.016(4) 0.2709(16) 0.601(2) 0.33(2) Uani 1 1 d . . .
H63A H 0.0857 0.3124 0.6381 0.394 Uiso 1 1 calc R . .
H63B H -0.0125 0.2662 0.6461 0.394 Uiso 1 1 calc R . .
C64 C 0.0443(16) 0.2041(14) 0.5945(18) 0.197(10) Uani 1 1 d . . .
H64A H 0.0957 0.1983 0.6571 0.295 Uiso 1 1 calc R . .
H64B H 0.0789 0.2011 0.5533 0.295 Uiso 1 1 calc R . .
H64C H -0.0174 0.1551 0.5678 0.295 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 O2 1.934(4) . ?
Zr O1 1.956(4) . ?
Zr O3 1.974(4) . ?
Zr O4 2.147(5) . ?
Zr O4 2.147(4) 2 ?
B1 O1 1.375(8) . ?
B1 C1 1.572(10) . ?
B1 C10 1.579(10) . ?
B2 O2 1.396(8) . ?
B2 C28 1.572(10) . ?
B2 C19 1.572(10) . ?
B3 O3 1.340(8) . ?
B3 C37 1.576(9) . ?
B3 C46 1.610(9) . ?
O4 Zr 2.147(4) 2 ?
C1 C2 1.411(9) . ?
C1 C6 1.411(10) . ?
C2 C3 1.389(10) . ?
C2 C7 1.504(11) . ?
C3 C4 1.374(12) . ?
C4 C5 1.384(12) . ?
C4 C8 1.513(11) . ?
C5 C6 1.394(10) . ?
C6 C9 1.498(10) . ?
C10 C15 1.404(9) . ?
C10 C11 1.414(9) . ?
C11 C12 1.400(10) . ?
C11 C16 1.512(10) . ?
C12 C13 1.379(11) . ?
C13 C14 1.378(11) . ?
C13 C17 1.525(11) . ?
C14 C15 1.380(10) . ?
C15 C18 1.505(10) . ?
C19 C20 1.392(10) . ?
C19 C24 1.413(10) . ?
C20 C21 1.402(9) . ?
C20 C25 1.506(10) . ?
C21 C22 1.385(12) . ?
C22 C23 1.373(12) . ?
C22 C26 1.512(11) . ?
C23 C24 1.394(11) . ?
C24 C27 1.506(11) . ?
C28 C33 1.416(9) . ?
C28 C29 1.424(9) . ?
C29 C30 1.381(9) . ?
C29 C34 1.509(9) . ?
C30 C31 1.376(10) . ?
C31 C32 1.381(11) . ?
C31 C35 1.521(11) . ?
C32 C33 1.386(10) . ?
C33 C36 1.517(10) . ?
C37 C38 1.410(8) . ?
C37 C42 1.415(9) . ?
C38 C39 1.387(9) . ?
C38 C43 1.516(9) . ?
C39 C40 1.393(10) . ?
C40 C41 1.382(9) . ?
C40 C44 1.498(9) . ?
C41 C42 1.399(9) . ?
C42 C45 1.501(9) . ?
C46 C51 1.413(9) . ?
C46 C47 1.419(9) . ?
C47 C48 1.396(9) . ?
C47 C52 1.506(9) . ?
C48 C49 1.375(10) . ?
C49 C50 1.394(10) . ?
C49 C53 1.508(10) . ?
C50 C51 1.390(10) . ?
C51 C54 1.511(10) . ?
C55 C56 1.36(3) . ?
C56 C57 1.26(2) . ?
C57 C58 1.42(3) . ?
C58 C59 1.31(2) . ?
C60 C61 1.34(3) . ?
C61 C62 1.28(3) . ?
C62 C63 1.39(3) . ?
C63 C64 1.13(2) . ?
