#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/12/2211224.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2211224
loop_
_publ_author_name
'Rabe, Gerd W.'
'Zhang-Presse, Mei'
'Riederer, Florian A.'
'Rheingold, Arnold L.'
_publ_section_title
;Di-μ-chloro-bis{chloro[hydrotris(pyrazol-1-yl)borato)](tetrahydrofuran)ytterbium(III)}
 toluene solvate
;
_journal_coeditor_code           WM2039
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3149
_journal_page_last               m3151
_journal_paper_doi               10.1107/S1600536806044096
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Yb2 (C9 H10 B N6)2 Cl4 (C4 H8 O)2], C7 H8'
_chemical_formula_moiety         'C26 H36 B2 Cl4 N12 O2 Yb2, C7 H8'
_chemical_formula_sum            'C33 H44 B2 Cl4 N12 O2 Yb2'
_chemical_formula_weight         1150.30
_chemical_name_systematic
;
Di-μ-chloro-bis{chloro[hydrotris(pyrazol-1-
yl)borato)](tetrahydrofuran)ytterbium(III)] toluene solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.733(4)
_cell_angle_beta                 105.648(4)
_cell_angle_gamma                103.250(4)
_cell_formula_units_Z            1
_cell_length_a                   9.209(3)
_cell_length_b                   10.919(3)
_cell_length_c                   11.881(3)
_cell_measurement_reflns_used    5645
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      2.15
_cell_volume                     1046.7(5)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'SMART (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XP in SHELXTL (Bruker, 2005)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'φ and ω'
_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  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6253
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    4.742
_exptl_absorpt_correction_T_max  0.789
_exptl_absorpt_correction_T_min  0.574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.825
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             560
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .10
_exptl_crystal_size_min          .05
_refine_diff_density_max         2.985
_refine_diff_density_min         -2.795
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.08P)²+0.69P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                4053
_reflns_number_total             4221
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wm2039.cif
_cod_data_source_block           I
_cod_database_code               2211224
_cod_database_fobs_code          2211224
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Yb Yb1 0.352000(18) 0.432548(15) 0.303116(15) 0.01902(10) Uani d . 1
Cl Cl1 0.35125(13) 0.42505(11) 0.52895(10) 0.0254(2) Uani d . 1
Cl Cl2 0.30855(16) 0.65200(13) 0.29849(14) 0.0348(3) Uani d . 1
O O1 0.0858(4) 0.3452(3) 0.2884(3) 0.0245(7) Uani d . 1
N N1 0.1777(4) 0.3181(4) 0.0876(4) 0.0235(8) Uani d . 1
N N2 0.2036(5) 0.2223(4) 0.0025(4) 0.0231(8) Uani d . 1
N N3 0.5186(4) 0.4346(4) 0.1779(4) 0.0230(8) Uani d . 1
N N4 0.4979(5) 0.3258(4) 0.0778(4) 0.0227(8) Uani d . 1
N N5 0.3854(5) 0.2163(4) 0.2630(4) 0.0234(8) Uani d . 1
N N6 0.3793(5) 0.1415(4) 0.1480(4) 0.0236(8) Uani d . 1
C C1 0.0350(5) 0.3282(5) 0.0266(5) 0.0282(10) Uani d . 1
H H1A -0.0146 0.3874 0.0630 0.034 Uiso calc R 1
C C2 -0.0275(6) 0.2392(5) -0.0969(5) 0.0300(11) Uani d . 1
H H2A -0.1249 0.2262 -0.1595 0.036 Uiso calc R 1
C C3 0.0821(7) 0.1740(5) -0.1085(5) 0.0313(12) Uani d . 1
H H3A 0.0737 0.1064 -0.1822 0.038 Uiso calc R 1
C C4 0.6361(5) 0.5352(5) 0.1815(5) 0.0262(10) Uani d . 1
H H4A 0.6746 0.6240 0.2412 0.031 Uiso calc R 1
C C5 0.6946(6) 0.4935(5) 0.0874(5) 0.0282(10) Uani d . 1
H H5A 0.7792 0.5452 0.0711 0.034 Uiso calc R 1
C C6 0.6030(6) 0.3602(5) 0.0224(5) 0.0270(10) Uani d . 1
H H6A 0.6122 0.3023 -0.0493 0.032 Uiso calc R 1
C C7 0.4114(6) 0.1450(5) 0.3369(5) 0.0274(10) Uani d . 1
H H7A 0.4222 0.1739 0.4226 0.033 Uiso calc R 1
C C8 0.4207(6) 0.0219(5) 0.2707(5) 0.0312(11) Uani d . 1
H H8A 0.4373 -0.0479 0.3007 0.037 Uiso calc R 1
C C9 0.4002(6) 0.0243(5) 0.1521(5) 0.0279(10) Uani d . 1
H H9A 0.4007 -0.0455 0.0841 0.034 Uiso calc R 1
C C10 -0.0080(6) 0.4216(5) 0.3385(5) 0.0291(10) Uani d . 1
H H10A -0.0439 0.4729 0.2858 0.035 Uiso calc R 1
H H10B 0.0555 0.4852 0.4248 0.035 Uiso calc R 1
C C11 -0.1500(6) 0.3166(6) 0.3369(6) 0.0374(12) Uani d . 1
H H11A -0.1297 0.3050 0.4189 0.045 Uiso calc R 1
H H11B -0.2477 0.3420 0.3157 0.045 Uiso calc R 1
C C12 -0.1650(6) 0.1896(5) 0.2362(5) 0.0349(12) Uani d . 1
H H12A -0.2207 0.1080 0.2485 0.042 Uiso calc R 1
H H12B -0.2227 0.1873 0.1518 0.042 Uiso calc R 1
C C13 0.0067(6) 0.2018(5) 0.2548(5) 0.0274(10) Uani d . 1
H H13A 0.0523 0.1701 0.3225 0.033 Uiso calc R 1
H H13B 0.0170 0.1489 0.1769 0.033 Uiso calc R 1
C C40 0.9745(18) 0.1517(12) 0.5721(11) 0.046(3) Uani d P 0.50
C C41 0.9213(14) 0.0283(11) 0.5096(9) 0.033(2) Uani d P 0.50
C C42 0.8019(11) 0.0678(9) 0.5189(8) 0.060(2) Uani d . 1
C C43 1.0911(8) 0.1120(6) 0.5620(5) 0.0449(15) Uani d . 1
C C44 0.7890(15) -0.0736(13) 0.4458(13) 0.043(3) Uani d P 0.50
B B1 0.3613(7) 0.1931(5) 0.0376(5) 0.0252(11) Uani d . 1
H H1B1 0.3648 0.1244 -0.0361 0.030 Uiso calc R 1
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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 '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'
N N 0.0061 0.0033 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Yb1 N5 . . 92.19(13)
O1 Yb1 N3 . . 141.94(12)
N5 Yb1 N3 . . 76.65(13)
O1 Yb1 N1 . . 69.09(12)
N5 Yb1 N1 . . 78.96(14)
N3 Yb1 N1 . . 73.06(13)
O1 Yb1 Cl2 . . 89.91(9)
N5 Yb1 Cl2 . . 168.16(11)
N3 Yb1 Cl2 . . 94.61(10)
N1 Yb1 Cl2 . . 90.94(10)
O1 Yb1 Cl1 . 2_666 142.07(8)
N5 Yb1 Cl1 . 2_666 96.67(10)
N3 Yb1 Cl1 . 2_666 75.89(9)
N1 Yb1 Cl1 . 2_666 148.82(9)
Cl2 Yb1 Cl1 . 2_666 88.77(4)
O1 Yb1 Cl1 . . 71.34(8)
N5 Yb1 Cl1 . . 86.47(10)
N3 Yb1 Cl1 . . 141.95(9)
N1 Yb1 Cl1 . . 137.01(9)
Cl2 Yb1 Cl1 . . 105.23(4)
Cl1 Yb1 Cl1 2_666 . 72.50(4)
O1 Yb1 Yb1 . 2_666 106.85(8)
N5 Yb1 Yb1 . 2_666 91.93(10)
N3 Yb1 Yb1 . 2_666 109.75(9)
N1 Yb1 Yb1 . 2_666 169.70(9)
Cl2 Yb1 Yb1 . 2_666 98.61(3)
Cl1 Yb1 Yb1 2_666 2_666 36.31(2)
Cl1 Yb1 Yb1 . 2_666 36.19(3)
Yb1 Cl1 Yb1 2_666 . 107.50(4)
C13 O1 C10 . . 109.7(3)
C13 O1 Yb1 . . 122.2(3)
C10 O1 Yb1 . . 126.4(3)
N2 N1 C1 . . 105.8(4)
N2 N1 Yb1 . . 124.5(3)
C1 N1 Yb1 . . 129.6(3)
C3 N2 N1 . . 110.4(4)
C3 N2 B1 . . 129.8(4)
N1 N2 B1 . . 119.5(4)
C4 N3 N4 . . 106.0(4)
C4 N3 Yb1 . . 130.5(3)
N4 N3 Yb1 . . 123.4(3)
C6 N4 N3 . . 109.6(4)
C6 N4 B1 . . 129.6(4)
N3 N4 B1 . . 120.7(4)
C7 N5 N6 . . 107.0(4)
C7 N5 Yb1 . . 131.2(3)
N6 N5 Yb1 . . 121.7(3)
C9 N6 N5 . . 108.9(4)
C9 N6 B1 . . 127.9(4)
N5 N6 B1 . . 123.1(4)
N1 C1 C2 . . 110.1(5)
N1 C1 H1A . . 124.9
C2 C1 H1A . . 124.9
C3 C2 C1 . . 105.2(4)
C3 C2 H2A . . 127.4
C1 C2 H2A . . 127.4
N2 C3 C2 . . 108.4(5)
N2 C3 H3A . . 125.8
C2 C3 H3A . . 125.8
N3 C4 C5 . . 111.3(5)
N3 C4 H4A . . 124.3
C5 C4 H4A . . 124.3
C6 C5 C4 . . 104.7(4)
C6 C5 H5A . . 127.6
C4 C5 H5A . . 127.6
N4 C6 C5 . . 108.4(4)
N4 C6 H6A . . 125.8
C5 C6 H6A . . 125.8
N5 C7 C8 . . 110.5(5)
N5 C7 H7A . . 124.8
C8 C7 H7A . . 124.8
C9 C8 C7 . . 104.5(4)
C9 C8 H8A . . 127.7
C7 C8 H8A . . 127.7
N6 C9 C8 . . 109.1(4)
N6 C9 H9A . . 125.5
C8 C9 H9A . . 125.5
O1 C10 C11 . . 105.2(4)
O1 C10 H10A . . 110.7
C11 C10 H10A . . 110.7
O1 C10 H10B . . 110.7
C11 C10 H10B . . 110.7
H10A C10 H10B . . 108.8
C12 C11 C10 . . 103.6(4)
C12 C11 H11A . . 111.1
C10 C11 H11A . . 111.1
C12 C11 H11B . . 111.0
C10 C11 H11B . . 111.0
H11A C11 H11B . . 109.0
C13 C12 C11 . . 102.2(4)
C13 C12 H12A . . 111.3
C11 C12 H12A . . 111.3
C13 C12 H12B . . 111.3
C11 C12 H12B . . 111.3
H12A C12 H12B . . 109.2
O1 C13 C12 . . 104.1(4)
O1 C13 H13A . . 110.9
C12 C13 H13A . . 110.9
O1 C13 H13B . . 110.9
C12 C13 H13B . . 110.9
H13A C13 H13B . . 108.9
C41 C40 C43 . . 71.7(9)
C41 C40 C42 . . 55.1(8)
C43 C40 C42 . . 126.9(10)
C40 C41 C42 . . 72.2(10)
C40 C41 C44 . . 143.1(14)
C42 C41 C44 . . 71.0(9)
C40 C41 C43 . . 54.7(8)
C42 C41 C43 . . 126.9(9)
C44 C41 C43 . . 161.9(12)
C40 C41 C43 . 2_756 162.7(13)
C42 C41 C43 . 2_756 125.0(9)
C44 C41 C43 . 2_756 53.9(8)
C43 C41 C43 . 2_756 108.1(8)
C40 C41 C41 . 2_756 109.3(12)
C42 C41 C41 . 2_756 177.6(12)
C44 C41 C41 . 2_756 107.4(12)
C43 C41 C41 . 2_756 54.6(6)
C43 C41 C41 2_756 2_756 53.5(6)
C41 C42 C40 . . 52.7(8)
C41 C42 C44 . . 55.1(8)
C40 C42 C44 . . 107.8(9)
C40 C43 C44 . 2_756 178.8(10)
C40 C43 C41 . . 53.6(8)
C44 C43 C41 2_756 . 127.4(9)
C40 C43 C41 . 2_756 125.4(9)
C44 C43 C41 2_756 2_756 55.6(8)
C41 C43 C41 . 2_756 71.9(8)
C43 C44 C41 2_756 . 70.5(9)
C43 C44 C42 2_756 . 124.3(10)
C41 C44 C42 . . 53.8(8)
N2 B1 N4 . . 107.8(4)
N2 B1 N6 . . 110.0(4)
N4 B1 N6 . . 109.2(4)
N2 B1 H1B1 . . 109.9
N4 B1 H1B1 . . 109.9
N6 B1 H1B1 . . 109.9
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Yb1 O1 . 2.358(3) y
Yb1 N5 . 2.387(4) y
Yb1 N3 . 2.409(4) y
Yb1 N1 . 2.413(4) y
Yb1 Cl2 . 2.5307(14) y
Yb1 Cl1 2_666 2.7010(12) y
Yb1 Cl1 . 2.7082(13) y
Yb1 Yb1 2_666 4.3622(12) ?
Cl1 Yb1 2_666 2.7010(12) ?
O1 C13 . 1.457(5) ?
O1 C10 . 1.461(6) ?
N1 N2 . 1.358(6) ?
N1 C1 . 1.365(6) ?
N2 C3 . 1.351(7) ?
N2 B1 . 1.531(7) ?
N3 C4 . 1.336(6) ?
N3 N4 . 1.367(5) ?
N4 C6 . 1.349(6) ?
N4 B1 . 1.541(6) ?
N5 C7 . 1.333(6) ?
N5 N6 . 1.367(6) ?
N6 C9 . 1.349(6) ?
N6 B1 . 1.547(7) ?
C1 C2 . 1.394(7) ?
C1 H1A . 0.9500 ?
C2 C3 . 1.377(8) ?
C2 H2A . 0.9500 ?
C3 H3A . 0.9500 ?
C4 C5 . 1.382(7) ?
C4 H4A . 0.9500 ?
C5 C6 . 1.380(7) ?
C5 H5A . 0.9500 ?
C6 H6A . 0.9500 ?
C7 C8 . 1.395(7) ?
C7 H7A . 0.9500 ?
C8 C9 . 1.379(8) ?
C8 H8A . 0.9500 ?
C9 H9A . 0.9500 ?
C10 C11 . 1.520(7) ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
C11 C12 . 1.516(8) ?
C11 H11A . 0.9900 ?
C11 H11B . 0.9900 ?
C12 C13 . 1.505(7) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C40 C41 . 1.251(16) ?
C40 C43 . 1.269(16) ?
C40 C42 . 1.497(16) ?
C41 C42 . 1.290(15) ?
C41 C44 . 1.311(17) ?
C41 C43 . 1.476(12) ?
C41 C43 2_756 1.498(13) ?
C41 C41 2_756 1.75(2) ?
C42 C44 . 1.512(16) ?
C43 C44 2_756 1.285(15) ?
C43 C41 2_756 1.498(13) ?
C44 C43 2_756 1.285(15) ?
B1 H1B1 . 1.0000 ?
