#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:37:37 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178525 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/29/4062930.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_4062930
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/om049771s
_journal_year                    2004
_chemical_formula_sum            'C48 H90 B20 Cl2 Na2 O7 Zr'
_chemical_formula_weight         1203.50
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 101.953(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9343(12)
_cell_length_b                   24.1026(19)
_cell_length_c                   17.6490(13)
_cell_measurement_temperature    293(2)
_cell_volume                     6631.3(9)
_diffrn_ambient_temperature      293(2)
_exptl_crystal_density_diffrn    1.205
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4062930
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Zr Zr 0.5000 0.16434(3) 0.2500 0.0482(2) Uani 1 2 d S . .
C1 C 0.3343(3) 0.1812(2) 0.1521(3) 0.0540(12) Uani 1 1 d . . .
C2 C 0.3257(3) 0.1467(2) 0.2177(3) 0.0519(11) Uani 1 1 d . . .
C3 C 0.3044(3) 0.1564(2) 0.0726(3) 0.0645(14) Uani 1 1 d . . .
H3A H 0.2941 0.1861 0.0348 0.077 Uiso 1 1 calc R . .
H3B H 0.3497 0.1332 0.0607 0.077 Uiso 1 1 calc R . .
C4 C 0.1596(4) 0.1241(3) -0.0006(3) 0.0838(18) Uani 1 1 d . . .
H4A H 0.1648 0.1471 -0.0417 0.101 Uiso 1 1 calc R . .
C5 C 0.0874(5) 0.0920(4) -0.0055(4) 0.109(3) Uani 1 1 d . . .
H5A H 0.0445 0.0927 -0.0501 0.131 Uiso 1 1 calc R . .
C6 C 0.0788(4) 0.0583(3) 0.0571(5) 0.099(2) Uani 1 1 d . . .
H6A H 0.0302 0.0364 0.0538 0.118 Uiso 1 1 calc R . .
C7 C 0.1419(3) 0.0575(3) 0.1231(4) 0.0761(16) Uani 1 1 d . . .
H7A H 0.1353 0.0357 0.1650 0.091 Uiso 1 1 calc R . .
C8 C 0.2162(3) 0.0894(2) 0.1273(3) 0.0634(13) Uani 1 1 d . . .
C9 C 0.2249(3) 0.1227(2) 0.0653(3) 0.0613(13) Uani 1 1 d . . .
C10 C 0.2867(3) 0.0901(2) 0.1988(3) 0.0620(13) Uani 1 1 d . . .
H10A H 0.2639 0.0769 0.2424 0.074 Uiso 1 1 calc R . .
H10B H 0.3314 0.0645 0.1915 0.074 Uiso 1 1 calc R . .
O1 O 0.5420(3) 0.2100(2) -0.0514(3) 0.1031(14) Uani 1 1 d U A 1
C11 C 0.4848(6) 0.2554(5) -0.0536(6) 0.194(6) Uani 1 1 d U A 1
H11A H 0.4264 0.2418 -0.0610 0.233 Uiso 1 1 calc R A 1
H11B H 0.4980 0.2752 -0.0048 0.233 Uiso 1 1 calc R A 1
C12 C 0.4919(7) 0.2909(5) -0.1134(7) 0.178(5) Uani 1 1 d U A 1
H12A H 0.4904 0.3293 -0.0971 0.214 Uiso 1 1 calc R A 1
H12B H 0.4454 0.2849 -0.1577 0.214 Uiso 1 1 calc R A 1
C13 C 0.5707(7) 0.2787(5) -0.1323(8) 0.225(8) Uani 1 1 d U A 1
H13A H 0.6105 0.3092 -0.1181 0.269 Uiso 1 1 calc R A 1
H13B H 0.5636 0.2719 -0.1874 0.269 Uiso 1 1 calc R A 1
C14 C 0.6025(6) 0.2291(4) -0.0885(7) 0.179(5) Uani 1 1 d U A 1
H14A H 0.6159 0.2008 -0.1233 0.214 Uiso 1 1 calc R A 1
H14B H 0.6546 0.2377 -0.0511 0.214 Uiso 1 1 calc R A 1
O2 O 0.4391(4) 0.0899(2) -0.0660(3) 0.1169(17) Uani 1 1 d U A 2
C21 C 0.4020(8) 0.0399(4) -0.0598(6) 0.162(4) Uani 1 1 d U A 2
H21A H 0.4448 0.0108 -0.0554 0.195 Uiso 1 1 calc R A 2
H21B H 0.3781 0.0392 -0.0136 0.195 Uiso 1 1 calc R A 2
C22 C 0.3364(10) 0.0304(6) -0.1257(9) 0.230(7) Uani 1 1 d U A 2
H22A H 0.3442 -0.0054 -0.1485 0.276 Uiso 1 1 calc R A 2
H22B H 0.2807 0.0310 -0.1118 0.276 Uiso 1 1 calc R A 2
C23 C 0.3425(12) 0.0718(7) -0.1761(8) 0.272(10) Uani 1 1 d U A 2
H23A H 0.2860 0.0862 -0.1989 0.326 Uiso 1 1 calc R A 2
H23B H 0.3690 0.0583 -0.2174 0.326 Uiso 1 1 calc R A 2
C24 C 0.3930(11) 0.1132(7) -0.1339(7) 0.320(13) Uani 1 1 d U A 2
H24A H 0.4320 0.1285 -0.1640 0.384 Uiso 1 1 calc R A 2
H24B H 0.3569 0.1429 -0.1219 0.384 Uiso 1 1 calc R A 2
O3 O 0.6640(3) 0.0927(2) -0.0150(3) 0.1168(17) Uani 1 1 d U A 1
C31 C 0.6646(8) 0.0687(5) -0.0891(6) 0.178(5) Uani 1 1 d U A 1
H31A H 0.6525 0.0293 -0.0885 0.214 Uiso 1 1 calc R A 1
H31B H 0.6213 0.0860 -0.1288 0.214 Uiso 1 1 calc R A 1
C32 C 0.7465(8) 0.0776(5) -0.1042(7) 0.178(5) Uani 1 1 d U A 1
H32A H 0.7456 0.1089 -0.1389 0.214 Uiso 1 1 calc R A 1
H32B H 0.7655 0.0451 -0.1284 0.214 Uiso 1 1 calc R A 1
C33 C 0.8032(7) 0.0885(6) -0.0315(7) 0.209(6) Uani 1 1 d U A 1
H33A H 0.8430 0.1180 -0.0369 0.251 Uiso 1 1 calc R A 1
H33B H 0.8358 0.0555 -0.0127 0.251 Uiso 1 1 calc R A 1
C34 C 0.7508(6) 0.1045(6) 0.0198(6) 0.176(5) Uani 1 1 d U A 1
H34A H 0.7672 0.0843 0.0681 0.211 Uiso 1 1 calc R A 1
H34B H 0.7577 0.1438 0.0309 0.211 Uiso 1 1 calc R A 1
O4 O 0.0000 -0.0556(13) 0.2500 0.387(13) Uani 1 2 d SU . 2
C41 C 0.0603(17) 0.0002(12) 0.3019(12) 0.326(14) Uani 1 1 d U B 2
H41A H 0.0576 -0.0044 0.3559 0.392 Uiso 1 1 calc R B 2
H41B H 0.1196 -0.0055 0.2985 0.392 Uiso 1 1 calc R B 2
C42 C 0.042(3) 0.0546(11) 0.2837(13) 0.41(4) Uani 1 1 d U . 2
H42A H 0.0891 0.0722 0.2665 0.492 Uiso 1 1 calc R . 2
H42B H 0.0308 0.0744 0.3285 0.492 Uiso 1 1 calc R . 2
B3 B 0.3505(3) 0.1642(3) 0.3057(3) 0.0556(14) Uani 1 1 d . . .
H3 H 0.3482 0.1276 0.3425 0.067 Uiso 1 1 calc R . .
B4 B 0.4219(4) 0.2207(2) 0.3336(3) 0.0539(13) Uani 1 1 d . . .
H4 H 0.4679 0.2166 0.3891 0.065 Uiso 1 1 calc R . .
B5 B 0.4420(3) 0.2586(2) 0.2518(3) 0.0549(13) Uani 1 1 d . . .
B6 B 0.3829(4) 0.2387(2) 0.1571(3) 0.0556(14) Uani 1 1 d . . .
H6 H 0.4021 0.2474 0.1019 0.067 Uiso 1 1 calc R . .
B7 B 0.2728(4) 0.2424(3) 0.1643(4) 0.0654(16) Uani 1 1 d . . .
H7 H 0.2179 0.2494 0.1161 0.078 Uiso 1 1 calc R . .
B8 B 0.2666(4) 0.2688(3) 0.2547(4) 0.0699(17) Uani 1 1 d . . .
H8 H 0.2099 0.2940 0.2577 0.084 Uiso 1 1 calc R . .
B9 B 0.3139(4) 0.2284(3) 0.3357(4) 0.0648(16) Uani 1 1 d . . .
H9 H 0.2906 0.2297 0.3901 0.078 Uiso 1 1 calc R . .
B10 B 0.3708(4) 0.2856(3) 0.3091(4) 0.0651(16) Uani 1 1 d . . .
H10 H 0.3855 0.3222 0.3467 0.078 Uiso 1 1 calc R . .
B11 B 0.3460(4) 0.2936(3) 0.2059(4) 0.0656(16) Uani 1 1 d . . .
H11 H 0.3451 0.3354 0.1809 0.079 Uiso 1 1 calc R . .
B12 B 0.2522(4) 0.1959(3) 0.2483(3) 0.0650(16) Uani 1 1 d . . .
H12 H 0.1869 0.1786 0.2382 0.078 Uiso 1 1 calc R . .
Cl Cl 0.48471(8) 0.08687(5) 0.15109(7) 0.0610(4) Uani 1 1 d . A .
Na Na 0.54794(14) 0.13247(11) 0.02609(12) 0.0811(7) 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
Zr B5 2.455(6) . ?
Zr B5 2.455(6) 2_655 ?
Zr B4 2.516(5) . ?
Zr B4 2.516(5) 2_655 ?
Zr Cl 2.5331(13) 2_655 ?
Zr Cl 2.5331(13) . ?
Zr C2 2.751(4) 2_655 ?
Zr C2 2.751(4) . ?
Zr B3 2.759(5) 2_655 ?
Zr B3 2.759(5) . ?
Zr B6 2.849(5) 2_655 ?
Zr B6 2.849(5) . ?
C1 C2 1.455(6) . ?
C1 C3 1.508(7) . ?
C1 B6 1.583(7) . ?
C1 B7 1.810(7) . ?
C2 C10 1.507(7) . ?
C2 B3 1.579(7) . ?
C2 B12 1.826(7) . ?
C3 C9 1.488(7) . ?
C4 C5 1.374(9) . ?
C4 C9 1.391(7) . ?
C5 C6 1.400(10) . ?
C6 C7 1.372(8) . ?
C7 C8 1.401(7) . ?
C8 C9 1.388(7) . ?
C8 C10 1.505(7) . ?
O1 C14 1.353(8) . ?
O1 C11 1.421(10) . ?
O1 Na 2.306(5) . ?
C11 C12 1.382(11) . ?
C12 C13 1.396(12) . ?
C13 C14 1.456(12) . ?
O2 C21 1.357(9) . ?
O2 C24 1.389(11) . ?
O2 Na 2.352(5) . ?
C21 C22 1.411(13) . ?
C21 C23 2.213(16) . ?
C22 C23 1.354(16) . ?
C23 C24 1.396(15) . ?
O3 C31 1.433(9) . ?
O3 C34 1.420(10) . ?
O3 Na 2.328(5) . ?
C31 C32 1.402(14) . ?
C32 C33 1.432(14) . ?
C33 C34 1.407(11) . ?
O4 C41 1.79(3) . ?
O4 C41 1.79(3) 2 ?
C41 C42 1.37(4) . ?
C42 C42 1.59(7) 2 ?
B3 B4 1.778(8) . ?
B3 B9 1.773(8) . ?
B3 B12 1.847(8) . ?
B3 Na 3.166(6) 2_655 ?
B4 B9 1.739(8) . ?
B4 B10 1.775(8) . ?
B4 B5 1.791(7) . ?
B5 B11 1.788(8) . ?
B5 B10 1.792(8) . ?
B5 B6 1.806(8) . ?
B5 B5 1.862(11) 2_655 ?
B6 B11 1.746(8) . ?
B6 B7 1.788(8) . ?
B7 B8 1.739(9) . ?
B7 B11 1.751(9) . ?
B7 B12 1.940(8) . ?
B8 B9 1.764(9) . ?
B8 B12 1.772(9) . ?
B8 B11 1.776(9) . ?
B8 B10 1.784(9) . ?
B9 B10 1.766(9) . ?
B9 B12 1.825(9) . ?
B10 B11 1.793(9) . ?
Cl Na 2.830(2) . ?
Na B3 3.166(6) 2_655 ?
