#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:47:24 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179764 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/60/7006037.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_7006037
loop_
_publ_author_name
'Johnson, Andrew L.'
'Davidson, Matthew G.'
'Mahon, Mary F.'
_publ_section_title
;
 Reactivity of boranes with a titanium(IV) amine tris(phenolate)
 alkoxide complex; formation of a Ti(IV) tetrahydroborate complex, a
 Ti(III) dimer and a Ti(IV) hydroxide Lewis acid adduct.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5405
_journal_page_last               5411
_journal_paper_doi               10.1039/b708378e
_journal_year                    2007
_chemical_formula_sum            'C34 H42 B N O3 Ti'
_chemical_formula_weight         571.40
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   14.1580(2)
_cell_length_b                   14.1580(2)
_cell_length_c                   26.3930(6)
_cell_measurement_reflns_used    23103
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.69
_cell_volume                     4581.66(14)
_computing_data_reduction
'Denzo and Scalepack (otwinowski&Minor, 1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       KappaCCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            23103
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.69
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_T_max  0.8586
_exptl_absorpt_correction_T_min  0.6092
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.0011(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2311
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.661
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.127
_refine_ls_shift/su_mean         0.027
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0646P)²+7.1940P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1343
_reflns_number_gt                1803
_reflns_number_total             2311
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b708378e.txt
_cod_data_source_block           Compound-3
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7006037
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Ti1 Ti 0.0000 0.0000 0.16769(3) 0.0318(3) Uani 1 3 d S . .
O1 O 0.04064(19) 0.14266(18) 0.17815(8) 0.0372(6) Uani 1 1 d . . .
N1 N 0.0000 0.0000 0.25835(15) 0.0302(9) Uani 1 3 d S . .
B1 B 0.0000 0.0000 0.0832(3) 0.0499(18) Uani 1 3 d S . .
H1B H 0.0000 0.0000 0.043(3) 0.07(3) Uiso 1 3 d S . .
H2B H -0.062(3) 0.018(4) 0.1003(18) 0.063(13) Uiso 1 1 d . . .
C1 C 0.0201(3) 0.2026(2) 0.21235(12) 0.0342(7) Uani 1 1 d . . .
C2 C -0.0156(3) 0.2728(3) 0.19528(13) 0.0395(8) Uani 1 1 d . . .
C3 C -0.0367(3) 0.3309(3) 0.23176(14) 0.0433(8) Uani 1 1 d . . .
H3 H -0.0624 0.3795 0.2221 0.052 Uiso 1 1 d R . .
C4 C -0.0215(3) 0.3227(3) 0.28328(14) 0.0418(8) Uani 1 1 d . . .
C5 C 0.0146(3) 0.2521(3) 0.29874(12) 0.0374(7) Uani 1 1 d . . .
H5 H 0.0246 0.2447 0.3342 0.045 Uiso 1 1 d R . .
C6 C 0.0353(3) 0.1910(2) 0.26342(11) 0.0333(7) Uani 1 1 d . . .
C7 C -0.0319(4) 0.2819(3) 0.13966(14) 0.0514(9) Uani 1 1 d . . .
H7A H -0.0551 0.3344 0.1347 0.062 Uiso 1 1 d R . .
H7B H -0.0871 0.2121 0.1272 0.062 Uiso 1 1 d R . .
H7C H 0.0349 0.3047 0.1216 0.062 Uiso 1 1 d R . .
C8 C -0.0444(4) 0.3880(3) 0.32161(16) 0.0553(10) Uani 1 1 d . . .
H8A H -0.0310 0.3719 0.3553 0.066 Uiso 1 1 d R . .
H8B H -0.1190 0.3707 0.3188 0.066 Uiso 1 1 d R . .
H8C H 0.0029 0.4642 0.3147 0.066 Uiso 1 1 d R . .
C9 C 0.0739(2) 0.1138(2) 0.27850(9) 0.0328(7) Uani 1 1 d . . .
H9A H 0.0752 0.1111 0.3148 0.039 Uiso 1 1 d R . .
H9B H 0.1463 0.1414 0.2656 0.039 Uiso 1 1 d R . .
C101 C -0.0703(2) -0.0627(2) 0.43279(9) 0.069(3) Uani 0.50 1 d PRD A -1
C102 C -0.1035(2) -0.0029(2) 0.42909(9) 0.068(3) Uani 0.50 1 d PRD A -1
C104 C 0.0514(2) 0.1426(2) 0.42819(9) 0.083(4) Uani 0.50 1 d PRD A -1
C103 C -0.0638(2) 0.0873(2) 0.42486(9) 0.089(3) Uani 0.50 1 d PRD A -1
C105 C 0.0915(2) 0.2029(2) 0.44414(9) 0.138(7) Uani 0.50 1 d PRD . .
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'
N N 0.0061 0.0033 '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
O1 Ti1 O1 117.75(4) 3 . ?
O1 Ti1 O1 117.75(3) 3 2 ?
O1 Ti1 O1 117.75(3) . 2 ?
O1 Ti1 B1 98.71(7) 3 . ?
O1 Ti1 B1 98.71(7) . . ?
O1 Ti1 B1 98.71(7) 2 . ?
O1 Ti1 N1 81.29(7) 3 . ?
O1 Ti1 N1 81.29(7) . . ?
O1 Ti1 N1 81.29(7) 2 . ?
B1 Ti1 N1 180.0 . . ?
O1 Ti1 H2B 128.8(12) 3 . ?
O1 Ti1 H2B 84.9(12) . . ?
O1 Ti1 H2B 81.7(12) 2 . ?
B1 Ti1 H2B 30.1(12) . . ?
N1 Ti1 H2B 149.9(12) . . ?
C1 O1 Ti1 137.8(2) . . ?
C9 N1 C9 108.33(18) 3 . ?
C9 N1 C9 108.33(18) 3 2 ?
C9 N1 C9 108.33(18) . 2 ?
C9 N1 Ti1 110.59(17) 3 . ?
C9 N1 Ti1 110.59(17) . . ?
C9 N1 Ti1 110.59(17) 2 . ?
Ti1 B1 H1B 180.000(4) . . ?
Ti1 B1 H2B 66(2) . . ?
H1B B1 H2B 114(2) . . ?
O1 C1 C6 118.3(3) . . ?
O1 C1 C2 119.6(3) . . ?
C6 C1 C2 122.1(3) . . ?
C3 C2 C1 117.3(3) . . ?
C3 C2 C7 122.5(3) . . ?
C1 C2 C7 120.2(3) . . ?
C4 C3 C2 122.7(3) . . ?
C4 C3 H3 116.7 . . ?
C2 C3 H3 120.6 . . ?
C3 C4 C5 118.3(3) . . ?
C3 C4 C8 121.0(3) . . ?
C5 C4 C8 120.8(3) . . ?
C4 C5 C6 120.9(3) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.6 . . ?
C1 C6 C5 118.8(3) . . ?
C1 C6 C9 118.6(3) . . ?
C5 C6 C9 122.6(3) . . ?
C2 C7 H7A 109.1 . . ?
C2 C7 H7B 109.0 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 110.3 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.4 . . ?
C4 C8 H8A 110.2 . . ?
C4 C8 H8B 109.7 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 108.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 N1 111.9(2) . . ?
C6 C9 H9A 108.4 . . ?
N1 C9 H9A 109.0 . . ?
C6 C9 H9B 108.3 . . ?
N1 C9 H9B 109.7 . . ?
H9A C9 H9B 109.4 . . ?
C102 C101 C105 62.23(16) . 2 ?
C103 C102 C101 133.5 . . ?
C103 C102 C105 149.43(17) . 2 ?
C101 C102 C105 75.55(17) . 2 ?
C105 C104 C103 125.8 . . ?
C102 C103 C104 114.1 . . ?
C104 C105 C102 43.87(15) . 3 ?
C104 C105 C101 19.0 . 3 ?
C102 C105 C101 42.22(11) 3 3 ?
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
Ti1 O1 1.823(2) 3 ?
Ti1 O1 1.823(2) . ?
Ti1 O1 1.823(2) 2 ?
Ti1 B1 2.231(7) . ?
Ti1 N1 2.393(4) . ?
Ti1 H2B 2.06(5) . ?
O1 C1 1.367(4) . ?
N1 C9 1.512(3) 3 ?
N1 C9 1.512(3) . ?
N1 C9 1.512(3) 2 ?
B1 H1B 1.06(8) . ?
B1 H2B 1.13(4) . ?
C1 C6 1.388(4) . ?
C1 C2 1.395(5) . ?
C2 C3 1.392(5) . ?
C2 C7 1.502(5) . ?
C3 C4 1.391(5) . ?
C3 H3 0.9599 . ?
C4 C5 1.393(5) . ?
C4 C8 1.511(5) . ?
C5 C6 1.398(4) . ?
C5 H5 0.9600 . ?
C6 C9 1.500(4) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9602 . ?
C7 H7C 0.9602 . ?
C8 H8A 0.9599 . ?
C8 H8B 0.9602 . ?
C8 H8C 0.9599 . ?
C9 H9A 0.9602 . ?
C9 H9B 0.9598 . ?
C101 C102 1.1600 . ?
C101 C105 1.672(4) 2 ?
C102 C103 1.1153 . ?
C102 C105 1.527(4) 2 ?
C104 C105 0.8619 . ?
C104 C103 1.4152 . ?
C105 C102 1.527(4) 3 ?
C105 C101 1.672(4) 3 ?
