#------------------------------------------------------------------------------
#$Date: 2016-03-21 08:22:03 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178604 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/15/4071566.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_4071566
loop_
_publ_author_name
'Lorber, Christian'
'Choukroun, Robert'
'Vendier, Laure'
_publ_section_title
;
 Reactivity of B(C6F5)3with Simple Early Transition Metal Alkoxides:
 Alkoxide-Aryl Exchange, THF Ring-Opening, or Acetonitrile CC Coupling
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5017
_journal_paper_doi               10.1021/om800234z
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C48 H54 B2 F20 O8 Zr2'
_chemical_formula_sum            'C48 H54 B2 F20 O8 Zr2'
_chemical_formula_weight         1342.97
_chemical_name_systematic
;
 ?
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                110.37(2)
_cell_angle_beta                 105.386(18)
_cell_angle_gamma                98.153(18)
_cell_formula_units_Z            1
_cell_length_a                   10.872(2)
_cell_length_b                   11.866(3)
_cell_length_c                   12.017(3)
_cell_measurement_reflns_used    4500
_cell_measurement_temperature    180
_cell_measurement_theta_max      32.0223
_cell_measurement_theta_min      3.193
_cell_measurement_wavelength     0.71073
_cell_volume                     1353.4(6)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       ω-φ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8990
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         3.2
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         4593
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0447P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1023
_reflns_number_gt                3810
_reflns_number_total             4593
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            om800234z_si_002.cif
_cod_data_source_block           (7)
_cod_original_cell_volume        1353.3(6)
_cod_database_code               4071566
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
C1 C -0.0609(3) 0.2428(3) 0.2615(3) 0.0190(7) Uani 1 1 d .
C2 C -0.1284(3) 0.1884(3) 0.3223(3) 0.0225(7) Uani 1 1 d .
C3 C -0.2301(3) 0.2278(3) 0.3611(3) 0.0286(8) Uani 1 1 d .
C4 C -0.2724(3) 0.3232(3) 0.3374(3) 0.0283(8) Uani 1 1 d .
C5 C -0.2130(3) 0.3769(3) 0.2728(3) 0.0265(8) Uani 1 1 d .
C6 C -0.1124(3) 0.3344(3) 0.2355(3) 0.0224(7) Uani 1 1 d .
C7 C 0.1785(3) 0.3066(3) 0.2225(3) 0.0184(7) Uani 1 1 d .
C8 C 0.2666(3) 0.2698(3) 0.1602(3) 0.0193(7) Uani 1 1 d .
C9 C 0.3759(3) 0.3471(3) 0.1651(3) 0.0267(8) Uani 1 1 d .
C10 C 0.4006(3) 0.4733(3) 0.2326(3) 0.0286(8) Uani 1 1 d .
C11 C 0.3176(3) 0.5166(3) 0.2966(3) 0.0264(8) Uani 1 1 d .
C12 C 0.2119(3) 0.4339(3) 0.2928(3) 0.0211(7) Uani 1 1 d .
O1 O 0.1264(2) 0.12140(18) 0.27805(19) 0.0184(5) Uani 1 1 d .
C14 C 0.2220(3) 0.1678(3) 0.4082(3) 0.0234(7) Uani 1 1 d .
C15 C 0.3626(3) 0.2076(3) 0.4079(3) 0.0298(8) Uani 1 1 d .
H15A H 0.3753 0.1454 0.3384 0.045 Uiso 1 1 calc R
H15B H 0.4254 0.2166 0.4856 0.045 Uiso 1 1 calc R
H15C H 0.3749 0.2856 0.3996 0.045 Uiso 1 1 calc R
C16 C 0.2072(4) 0.0581(3) 0.4454(3) 0.0299(8) Uani 1 1 d .
H16A H 0.1189 0.0348 0.4453 0.045 Uiso 1 1 calc R
H16B H 0.2689 0.081 0.5284 0.045 Uiso 1 1 calc R
H16C H 0.2245 -0.011 0.3862 0.045 Uiso 1 1 calc R
C17 C 0.1906(4) 0.2774(3) 0.4988(3) 0.0317(8) Uani 1 1 d .
H17A H 0.1908 0.3426 0.4689 0.048 Uiso 1 1 calc R
H17B H 0.2561 0.3078 0.5811 0.048 Uiso 1 1 calc R
H17C H 0.1051 0.2508 0.5032 0.048 Uiso 1 1 calc R
O2 O -0.0035(2) 0.10098(18) 0.08298(18) 0.0176(5) Uani 1 1 d .
O4 O 0.0250(2) 0.1635(2) -0.1408(2) 0.0248(5) Uani 1 1 d .
C20 C 0.0771(3) 0.2653(3) -0.1690(3) 0.0248(7) Uani 1 1 d .
C21 C 0.0926(4) 0.3850(3) -0.0597(3) 0.0344(9) Uani 1 1 d .
H21A H 0.0082 0.3893 -0.0505 0.052 Uiso 1 1 calc R
H21B H 0.1274 0.4546 -0.0756 0.052 Uiso 1 1 calc R
H21C H 0.1522 0.387 0.0163 0.052 Uiso 1 1 calc R
C22 C 0.2084(4) 0.2500(4) -0.1845(4) 0.0374(9) Uani 1 1 d .
H22A H 0.2646 0.246 -0.1102 0.056 Uiso 1 1 calc R
H22B H 0.2498 0.3197 -0.1967 0.056 Uiso 1 1 calc R
H22C H 0.1941 0.1746 -0.2564 0.056 Uiso 1 1 calc R
O3 O -0.2510(2) 0.0882(2) -0.1416(2) 0.0245(5) Uani 1 1 d .
C24 C -0.3712(3) 0.1286(3) -0.1558(3) 0.0281(8) Uani 1 1 d .
C25 C -0.4567(5) 0.0591(5) -0.1075(6) 0.0741(17) Uani 1 1 d .
H25A H -0.4697 -0.0288 -0.1514 0.111 Uiso 1 1 calc R
H25B H -0.5406 0.0788 -0.1218 0.111 Uiso 1 1 calc R
H25C H -0.414 0.0833 -0.0188 0.111 Uiso 1 1 calc R
C26 C -0.4388(4) 0.1009(4) -0.2936(4) 0.0489(11) Uani 1 1 d .
H26A H -0.38 0.1423 -0.3227 0.073 Uiso 1 1 calc R
H26B H -0.5173 0.1302 -0.3029 0.073 Uiso 1 1 calc R
H26C H -0.4619 0.0128 -0.3425 0.073 Uiso 1 1 calc R
C27 C -0.3343(4) 0.2685(4) -0.0809(4) 0.0479(11) Uani 1 1 d .
H27A H -0.2931 0.2875 0.007 0.072 Uiso 1 1 calc R
H27B H -0.4125 0.2982 -0.0925 0.072 Uiso 1 1 calc R
H27C H -0.274 0.3083 -0.11 0.072 Uiso 1 1 calc R
Zr1 Zr -0.08446(3) 0.04847(3) -0.10954(3) 0.01750(12) Uani 1 1 d .
B1 B 0.0579(4) 0.1976(3) 0.2133(3) 0.0186(8) Uani 1 1 d .
F2 F -0.0957(2) 0.09208(17) 0.34715(19) 0.0334(5) Uani 1 1 d .
F3 F -0.2887(2) 0.1717(2) 0.4202(2) 0.0424(6) Uani 1 1 d .
F4 F -0.3703(2) 0.3636(2) 0.3740(2) 0.0424(6) Uani 1 1 d .
F5 F -0.2552(2) 0.46870(18) 0.2453(2) 0.0378(5) Uani 1 1 d .
F6 F -0.06470(18) 0.38659(17) 0.16655(18) 0.0283(4) Uani 1 1 d .
F8 F 0.25116(18) 0.14471(16) 0.09359(17) 0.0266(4) Uani 1 1 d .
F9 F 0.45792(19) 0.30203(19) 0.1044(2) 0.0366(5) Uani 1 1 d .
F10 F 0.5032(2) 0.55189(19) 0.2351(2) 0.0422(6) Uani 1 1 d .
F11 F 0.3406(2) 0.63883(17) 0.3634(2) 0.0369(5) Uani 1 1 d .
F12 F 0.14206(18) 0.48561(16) 0.36639(18) 0.0280(4) Uani 1 1 d .
C28 C -0.0199(4) 0.2603(4) -0.2886(3) 0.0375(9) Uani 1 1 d .
H28A H -0.0281 0.1853 -0.3583 0.056 Uiso 1 1 calc R
H28B H 0.0114 0.331 -0.3045 0.056 Uiso 1 1 calc R
H28C H -0.1046 0.2615 -0.2787 0.056 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C6 C1 C2 113.0(3) . .
C6 C1 B1 121.7(3) . .
C2 C1 B1 125.1(3) . .
F2 C2 C3 115.6(3) . .
F2 C2 C1 120.4(3) . .
C3 C2 C1 124.0(3) . .
F3 C3 C4 119.7(3) . .
F3 C3 C2 120.4(3) . .
C4 C3 C2 119.9(3) . .
F4 C4 C3 121.3(3) . .
F4 C4 C5 120.1(3) . .
C3 C4 C5 118.6(3) . .
F5 C5 C6 120.7(3) . .
F5 C5 C4 119.7(3) . .
C6 C5 C4 119.5(3) . .
F6 C6 C1 119.1(3) . .
F6 C6 C5 116.0(3) . .
C1 C6 C5 124.9(3) . .
C12 C7 C8 112.8(3) . .
C12 C7 B1 128.6(3) . .
C8 C7 B1 118.5(2) . .
C9 C8 F8 114.9(3) . .
C9 C8 C7 125.7(3) . .
F8 C8 C7 119.3(3) . .
F9 C9 C8 121.3(3) . .
F9 C9 C10 120.0(3) . .
C8 C9 C10 118.6(3) . .
F10 C10 C11 120.8(3) . .
F10 C10 C9 120.3(3) . .
C11 C10 C9 118.9(3) . .
F11 C11 C10 119.8(3) . .
F11 C11 C12 120.3(3) . .
C10 C11 C12 120.0(3) . .
F12 C12 C11 115.1(3) . .
F12 C12 C7 121.0(3) . .
C11 C12 C7 123.9(3) . .
C14 O1 B1 127.6(2) . .
C14 O1 Zr1 132.27(17) . 2
B1 O1 Zr1 97.98(16) . 2
O1 C14 C16 105.1(2) . .
O1 C14 C17 111.3(3) . .
C16 C14 C17 110.4(3) . .
O1 C14 C15 109.6(2) . .
C16 C14 C15 110.7(3) . .
C17 C14 C15 109.7(3) . .
B1 O2 Zr1 151.30(19) . .
B1 O2 Zr1 98.76(17) . 2
Zr1 O2 Zr1 106.67(8) . 2
C20 O4 Zr1 164.1(2) . .
O4 C20 C21 107.5(3) . .
O4 C20 C22 106.9(3) . .
C21 C20 C22 112.0(3) . .
O4 C20 C28 109.2(3) . .
C21 C20 C28 109.5(3) . .
C22 C20 C28 111.6(3) . .
C24 O3 Zr1 174.8(2) . .
O3 C24 C25 107.2(3) . .
O3 C24 C26 109.3(3) . .
C25 C24 C26 111.5(4) . .
O3 C24 C27 108.0(3) . .
C25 C24 C27 112.3(4) . .
C26 C24 C27 108.4(3) . .
O4 Zr1 O3 104.62(10) . .
O4 Zr1 O2 103.45(9) . .
O3 Zr1 O2 107.48(9) . .
O4 Zr1 O1 101.37(9) . 2
O3 Zr1 O1 100.90(9) . 2
O2 Zr1 O1 135.69(8) . 2
O4 Zr1 O2 113.77(9) . 2
O3 Zr1 O2 140.41(9) . 2
O2 Zr1 O2 73.33(8) . 2
O1 Zr1 O2 63.18(8) 2 2
O4 Zr1 B1 113.14(10) . 2
O3 Zr1 B1 122.90(10) . 2
O2 Zr1 B1 103.55(9) . 2
O1 Zr1 B1 32.33(9) 2 2
O2 Zr1 B1 31.02(9) 2 2
O4 Zr1 Zr1 113.55(7) . 2
O3 Zr1 Zr1 132.60(7) . 2
O2 Zr1 Zr1 38.06(6) . 2
O1 Zr1 Zr1 98.10(6) 2 2
O2 Zr1 Zr1 35.27(5) 2 2
B1 Zr1 Zr1 65.78(8) 2 2
O2 B1 O1 99.6(2) . .
O2 B1 C1 107.6(2) . .
O1 B1 C1 114.3(3) . .
O2 B1 C7 111.0(2) . .
O1 B1 C7 105.6(2) . .
C1 B1 C7 117.4(2) . .
O2 B1 Zr1 50.22(13) . 2
O1 B1 Zr1 49.69(12) . 2
C1 B1 Zr1 128.2(2) . 2
C7 B1 Zr1 114.40(19) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C6 1.381(5) .
C1 C2 1.402(4) .
C1 B1 1.633(4) .
C2 F2 1.349(4) .
C2 C3 1.389(5) .
C3 F3 1.342(4) .
C3 C4 1.370(5) .
C4 F4 1.343(4) .
C4 C5 1.386(5) .
C5 F5 1.348(4) .
C5 C6 1.382(4) .
C6 F6 1.354(4) .
C7 C12 1.386(4) .
C7 C8 1.393(4) .
C7 B1 1.658(5) .
C8 C9 1.368(5) .
C8 F8 1.379(3) .
C9 F9 1.349(4) .
C9 C10 1.378(5) .
C10 F10 1.335(4) .
C10 C11 1.377(5) .
C11 F11 1.338(4) .
C11 C12 1.381(5) .
C12 F12 1.359(3) .
O1 C14 1.485(4) .
O1 B1 1.533(4) .
O1 Zr1 2.186(2) 2
C14 C16 1.518(5) .
C14 C17 1.527(5) .
C14 C15 1.535(5) .
O2 B1 1.480(4) .
O2 Zr1 2.068(2) .
O2 Zr1 2.208(2) 2
O4 C20 1.445(4) .
O4 Zr1 1.885(2) .
C20 C21 1.512(5) .
C20 C22 1.516(5) .
C20 C28 1.516(5) .
O3 C24 1.444(4) .
O3 Zr1 1.909(2) .
C24 C25 1.510(6) .
C24 C26 1.516(5) .
C24 C27 1.519(5) .
Zr1 O1 2.186(2) 2
Zr1 O2 2.208(2) 2
Zr1 B1 2.839(3) 2
Zr1 Zr1 3.4306(9) 2
B1 Zr1 2.839(3) 2
