#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:48:10 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179129 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/91/4309127.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_4309127
loop_
_publ_author_name
'Errun Ding'
'Bin Du'
'Fu-Chen Liu'
'Shengming Liu'
'Edward A. Meyers'
'Sheldon G. Shore'
_publ_section_title
;
Preparation and Crystal Structures of a Series of Titanium(III) 9-BBN
Hydroborate Complexes Containing Ti...H Agostic Interactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4871
_journal_page_last               4878
_journal_paper_doi               10.1021/ic050422f
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C32 H64 B3 O2 Ti'
_chemical_formula_weight         561.16
_chemical_name_systematic
; 
 ? 
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.02
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.4241(2)
_cell_length_b                   10.24600(10)
_cell_length_c                   18.5408(2)
_cell_measurement_temperature    200(2)
_cell_volume                     3301.90(6)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_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  0.0165
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7317
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.285
_exptl_absorpt_correction_T_max  0.9776
_exptl_absorpt_correction_T_min  0.9478
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         3779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0476P)²+2.4828P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0968
_reflns_number_gt                3214
_reflns_number_total             3779
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050422fsi20050321_092335_1.cif
_cod_data_source_block           out
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3301.91(6)
_cod_database_code               4309127
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
Ti Ti 0.5000 0.36541(3) 1.2500 0.01950(11) Uani 1 2 d S . .
B10 B 0.57972(9) 0.29831(15) 1.15391(8) 0.0239(3) Uani 1 1 d . . .
H2 H 0.5436(9) 0.2345(15) 1.1970(8) 0.024(4) Uiso 1 1 d . . .
H1 H 0.5715(10) 0.4003(17) 1.1839(9) 0.031(4) Uiso 1 1 d . . .
C11 C 0.66875(8) 0.25852(15) 1.15353(8) 0.0275(3) Uani 1 1 d . . .
H11A H 0.6945(10) 0.2563(17) 1.2024(10) 0.032(4) Uiso 1 1 d . . .
C12 C 0.67557(10) 0.12112(17) 1.12124(9) 0.0363(4) Uani 1 1 d . . .
H12B H 0.7306(12) 0.099(2) 1.1172(10) 0.048(5) Uiso 1 1 d . . .
H12A H 0.6577(10) 0.0561(19) 1.1560(10) 0.039(5) Uiso 1 1 d . . .
C13 C 0.63134(10) 0.09871(18) 1.04795(10) 0.0390(4) Uani 1 1 d . . .
H13A H 0.6608(11) 0.1350(18) 1.0086(10) 0.041(5) Uiso 1 1 d . . .
H13B H 0.6273(12) -0.001(2) 1.0385(11) 0.051(6) Uiso 1 1 d . . .
C14 C 0.55022(9) 0.15689(17) 1.04188(9) 0.0341(3) Uani 1 1 d . . .
H14B H 0.5174(11) 0.099(2) 1.0695(10) 0.045(5) Uiso 1 1 d . . .
H14A H 0.5307(11) 0.1546(18) 0.9893(11) 0.044(5) Uiso 1 1 d . . .
C15 C 0.54371(8) 0.29686(15) 1.07198(8) 0.0270(3) Uani 1 1 d . . .
H15A H 0.4885(10) 0.3210(17) 1.0684(9) 0.031(4) Uiso 1 1 d . . .
C16 C 0.58549(9) 0.40222(18) 1.02991(9) 0.0337(3) Uani 1 1 d . . .
H16B H 0.5721(11) 0.487(2) 1.0478(10) 0.041(5) Uiso 1 1 d . . .
H16A H 0.5684(11) 0.4028(19) 0.9790(11) 0.041(5) Uiso 1 1 d . . .
C17 C 0.67364(9) 0.39265(19) 1.03530(9) 0.0350(4) Uani 1 1 d . . .
H17A H 0.6945(11) 0.4730(19) 1.0198(10) 0.040(5) Uiso 1 1 d . . .
H17B H 0.6903(11) 0.3240(19) 1.0026(10) 0.039(5) Uiso 1 1 d . . .
C18 C 0.70922(9) 0.36569(17) 1.11187(9) 0.0331(3) Uani 1 1 d . . .
H18B H 0.7632(11) 0.3465(18) 1.1094(10) 0.040(5) Uiso 1 1 d . . .
H18A H 0.7068(10) 0.4494(18) 1.1405(9) 0.033(4) Uiso 1 1 d . . .
B20 B 0.5000 0.6017(2) 1.2500 0.0253(4) Uani 1 2 d S . .
H3 H 0.5265(9) 0.5192(16) 1.2939(9) 0.028(4) Uiso 1 1 d . . .
C21 C 0.56471(9) 0.69268(15) 1.21895(9) 0.0301(3) Uani 1 1 d . . .
H21A H 0.6050(11) 0.6408(18) 1.1997(10) 0.036(5) Uiso 1 1 d . . .
C22 C 0.52713(11) 0.77436(17) 1.15647(9) 0.0383(4) Uani 1 1 d . . .
H22A H 0.5146(11) 0.715(2) 1.1159(11) 0.045(5) Uiso 1 1 d . . .
H22B H 0.5661(13) 0.833(2) 1.1385(12) 0.058(6) Uiso 1 1 d . . .
C23 C 0.45563(12) 0.85064(17) 1.17444(10) 0.0420(4) Uani 1 1 d . . .
H23B H 0.4289(12) 0.879(2) 1.1302(12) 0.051(6) Uiso 1 1 d . . .
H23A H 0.4716(11) 0.932(2) 1.2011(10) 0.041(5) Uiso 1 1 d . . .
C24 C 0.39880(10) 0.77463(17) 1.21789(10) 0.0388(4) Uani 1 1 d . . .
H24B H 0.3699(12) 0.716(2) 1.1820(11) 0.048(5) Uiso 1 1 d . . .
H24A H 0.3597(12) 0.836(2) 1.2370(11) 0.053(6) Uiso 1 1 d . . .
O30 O 0.60037(5) 0.31365(9) 1.31886(5) 0.0251(2) Uani 1 1 d . . .
C31 C 0.66331(9) 0.40082(17) 1.34236(11) 0.0371(4) Uani 1 1 d . . .
H31B H 0.6420(11) 0.462(2) 1.3745(11) 0.048(5) Uiso 1 1 d . . .
H31A H 0.6791(12) 0.449(2) 1.2986(12) 0.055(6) Uiso 1 1 d . . .
C32 C 0.72462(11) 0.3140(2) 1.37906(13) 0.0518(5) Uani 1 1 d . . .
H32B H 0.7537(13) 0.358(2) 1.4179(13) 0.060(6) Uiso 1 1 d . . .
H32A H 0.7638(18) 0.274(3) 1.3402(17) 0.103(10) Uiso 1 1 d . . .
C33 C 0.68010(12) 0.19781(19) 1.40298(12) 0.0491(5) Uani 1 1 d . . .
H33A H 0.7114(12) 0.120(2) 1.4089(11) 0.053(6) Uiso 1 1 d . . .
H33B H 0.6531(16) 0.231(3) 1.4537(15) 0.084(8) Uiso 1 1 d . . .
C34 C 0.61985(9) 0.18057(15) 1.34110(10) 0.0317(3) Uani 1 1 d . . .
H34B H 0.5741(11) 0.1422(17) 1.3565(10) 0.036(5) Uiso 1 1 d . . .
H34A H 0.6385(12) 0.1354(19) 1.3024(11) 0.046(5) Uiso 1 1 d . . .
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'
B B 0.0013 0.0007 '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'
Ti Ti 0.2776 0.4457 '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
_geom_angle_publ_flag
O30 Ti O30 151.55(5) 2_657 . ?
O30 Ti B20 104.22(3) 2_657 . ?
O30 Ti B20 104.22(3) . . ?
O30 Ti B10 83.29(5) 2_657 2_657 ?
O30 Ti B10 88.74(5) . 2_657 ?
B20 Ti B10 106.41(4) . 2_657 ?
O30 Ti B10 88.74(5) 2_657 . ?
O30 Ti B10 83.29(5) . . ?
B20 Ti B10 106.41(4) . . ?
B10 Ti B10 147.18(8) 2_657 . ?
O30 Ti H2 81.6(5) 2_657 . ?
O30 Ti H2 77.9(5) . . ?
B20 Ti H2 136.2(5) . . ?
B10 Ti H2 117.3(5) 2_657 . ?
B10 Ti H2 29.8(5) . . ?
O30 Ti H1 102.2(5) 2_657 . ?
O30 Ti H1 83.3(5) . . ?
B20 Ti H1 78.8(5) . . ?
B10 Ti H1 171.4(5) 2_657 . ?
B10 Ti H1 28.5(5) . . ?
H2 Ti H1 57.8(7) . . ?
O30 Ti H3 130.4(5) 2_657 . ?
O30 Ti H3 77.2(5) . . ?
B20 Ti H3 29.9(5) . . ?
B10 Ti H3 93.3(5) 2_657 . ?
B10 Ti H3 115.6(5) . . ?
H2 Ti H3 139.7(7) . . ?
H1 Ti H3 88.1(7) . . ?
C15 B10 C11 107.93(11) . . ?
C15 B10 Ti 119.40(9) . . ?
C11 B10 Ti 132.58(10) . . ?
C15 B10 H2 115.1(7) . . ?
C11 B10 H2 113.8(7) . . ?
Ti B10 H2 48.3(7) . . ?
C15 B10 H1 113.4(8) . . ?
C11 B10 H1 111.8(8) . . ?
Ti B10 H1 47.2(8) . . ?
H2 B10 H1 94.5(11) . . ?
C12 C11 C18 113.99(13) . . ?
C12 C11 B10 109.60(12) . . ?
C18 C11 B10 107.32(12) . . ?
C12 C11 H11A 107.1(10) . . ?
C18 C11 H11A 106.4(10) . . ?
B10 C11 H11A 112.4(10) . . ?
C13 C12 C11 115.78(13) . . ?
C13 C12 H12B 109.1(11) . . ?
C11 C12 H12B 109.8(12) . . ?
C13 C12 H12A 108.3(11) . . ?
C11 C12 H12A 109.0(11) . . ?
H12B C12 H12A 104.2(16) . . ?
C14 C13 C12 114.29(13) . . ?
C14 C13 H13A 108.8(11) . . ?
C12 C13 H13A 110.0(11) . . ?
C14 C13 H13B 108.6(12) . . ?
C12 C13 H13B 108.8(11) . . ?
H13A C13 H13B 106.1(16) . . ?
C13 C14 C15 115.18(13) . . ?
C13 C14 H14B 107.0(11) . . ?
C15 C14 H14B 108.0(11) . . ?
C13 C14 H14A 107.9(11) . . ?
C15 C14 H14A 110.0(11) . . ?
H14B C14 H14A 108.6(16) . . ?
C16 C15 C14 114.66(13) . . ?
C16 C15 B10 107.78(12) . . ?
C14 C15 B10 108.48(12) . . ?
C16 C15 H15A 106.4(10) . . ?
C14 C15 H15A 107.6(10) . . ?
B10 C15 H15A 112.1(10) . . ?
C17 C16 C15 115.30(13) . . ?
C17 C16 H16B 107.6(11) . . ?
C15 C16 H16B 108.7(11) . . ?
C17 C16 H16A 107.5(11) . . ?
C15 C16 H16A 111.9(12) . . ?
H16B C16 H16A 105.3(16) . . ?
C18 C17 C16 114.17(13) . . ?
C18 C17 H17A 107.3(11) . . ?
C16 C17 H17A 109.0(11) . . ?
C18 C17 H17B 108.9(11) . . ?
C16 C17 H17B 110.0(11) . . ?
H17A C17 H17B 107.2(15) . . ?
C17 C18 C11 115.00(13) . . ?
C17 C18 H18B 109.0(11) . . ?
C11 C18 H18B 111.1(11) . . ?
C17 C18 H18A 107.7(10) . . ?
C11 C18 H18A 107.7(10) . . ?
H18B C18 H18A 105.9(15) . . ?
C21 B20 C21 108.79(17) 2_657 . ?
C21 B20 Ti 125.61(9) 2_657 . ?
C21 B20 Ti 125.61(9) . . ?
C21 B20 H3 113.6(7) 2_657 . ?
C21 B20 H3 113.2(8) . . ?
Ti B20 H3 47.1(8) . . ?
C22 C21 C24 114.02(14) . 2_657 ?
C22 C21 B20 108.31(12) . . ?
C24 C21 B20 107.90(12) 2_657 . ?
C22 C21 H21A 107.6(11) . . ?
C24 C21 H21A 107.9(11) 2_657 . ?
B20 C21 H21A 111.1(11) . . ?
C23 C22 C21 115.15(14) . . ?
C23 C22 H22A 110.1(12) . . ?
C21 C22 H22A 107.6(12) . . ?
C23 C22 H22B 110.6(13) . . ?
C21 C22 H22B 108.7(13) . . ?
H22A C22 H22B 104.0(17) . . ?
C22 C23 C24 114.94(14) . . ?
C22 C23 H23B 108.9(13) . . ?
C24 C23 H23B 108.2(13) . . ?
C22 C23 H23A 109.4(11) . . ?
C24 C23 H23A 109.3(11) . . ?
H23B C23 H23A 105.7(16) . . ?
C23 C24 C21 115.40(14) . 2_657 ?
C23 C24 H24B 105.5(12) . . ?
C21 C24 H24B 109.8(12) 2_657 . ?
C23 C24 H24A 110.1(12) . . ?
C21 C24 H24A 109.0(12) 2_657 . ?
H24B C24 H24A 106.6(17) . . ?
C31 O30 C34 109.47(11) . . ?
C31 O30 Ti 126.02(9) . . ?
C34 O30 Ti 124.07(8) . . ?
O30 C31 C32 105.45(14) . . ?
O30 C31 H31B 105.7(12) . . ?
C32 C31 H31B 113.4(12) . . ?
O30 C31 H31A 107.4(12) . . ?
C32 C31 H31A 115.2(12) . . ?
H31B C31 H31A 108.9(17) . . ?
C33 C32 C31 103.61(15) . . ?
C33 C32 H32B 113.8(14) . . ?
C31 C32 H32B 112.4(13) . . ?
C33 C32 H32A 104.7(16) . . ?
C31 C32 H32A 111.9(16) . . ?
H32B C32 H32A 110(2) . . ?
C32 C33 C34 102.36(15) . . ?
C32 C33 H33A 112.7(13) . . ?
C34 C33 H33A 110.3(13) . . ?
C32 C33 H33B 105.0(14) . . ?
C34 C33 H33B 111.0(14) . . ?
H33A C33 H33B 114.6(19) . . ?
O30 C34 C33 103.96(13) . . ?
O30 C34 H34B 106.8(11) . . ?
C33 C34 H34B 111.9(11) . . ?
O30 C34 H34A 109.5(12) . . ?
C33 C34 H34A 112.4(13) . . ?
H34B C34 H34A 111.8(16) . . ?
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
Ti O30 2.1580(9) 2_657 ?
Ti O30 2.1580(9) . ?
Ti B20 2.421(2) . ?
Ti B10 2.4337(15) 2_657 ?
Ti B10 2.4337(15) . ?
Ti H2 1.857(15) . ?
Ti H1 1.843(17) . ?
Ti H3 1.819(16) . ?
B10 C15 1.603(2) . ?
B10 C11 1.604(2) . ?
B10 H2 1.237(16) . ?
B10 H1 1.197(17) . ?
C11 C12 1.538(2) . ?
C11 C18 1.541(2) . ?
C11 H11A 0.982(18) . ?
C12 C13 1.532(2) . ?
C12 H12B 0.99(2) . ?
C12 H12A 0.992(19) . ?
C13 C14 1.531(2) . ?
C13 H13A 0.99(2) . ?
C13 H13B 1.04(2) . ?
C14 C15 1.546(2) . ?
C14 H14B 0.99(2) . ?
C14 H14A 1.010(19) . ?
C15 C16 1.544(2) . ?
C15 H15A 0.991(18) . ?
C16 C17 1.535(2) . ?
C16 H16B 0.96(2) . ?
C16 H16A 0.97(2) . ?
C17 C18 1.534(2) . ?
C17 H17A 0.95(2) . ?
C17 H17B 0.99(2) . ?
C18 H18B 0.97(2) . ?
C18 H18A 1.011(19) . ?
B20 C21 1.601(2) 2_657 ?
B20 C21 1.601(2) . ?
B20 H3 1.240(16) . ?
C21 C22 1.538(2) . ?
C21 C24 1.541(2) 2_657 ?
C21 H21A 0.968(19) . ?
C22 C23 1.527(3) . ?
C22 H22A 0.98(2) . ?
C22 H22B 0.98(2) . ?
C23 C24 1.532(3) . ?
C23 H23B 0.96(2) . ?
C23 H23A 1.00(2) . ?
C24 C21 1.541(2) 2_657 ?
C24 H24B 1.00(2) . ?
C24 H24A 1.01(2) . ?
O30 C31 1.4572(18) . ?
O30 C34 1.4577(17) . ?
C31 C32 1.515(2) . ?
C31 H31B 0.96(2) . ?
C31 H31A 1.00(2) . ?
C32 C33 1.504(3) . ?
C32 H32B 0.96(2) . ?
C32 H32A 1.10(3) . ?
C33 C34 1.510(2) . ?
C33 H33A 0.97(2) . ?
C33 H33B 1.13(3) . ?
C34 H34B 0.950(19) . ?
C34 H34A 0.93(2) . ?
