#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/59/7005970.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_7005970
loop_
_publ_author_name
'Hill, Anthony F.'
'Smith, Matthew K.'
_publ_section_title
;
 A homoleptic hydrotris(methimazolyl)borate complex of titanium.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3363
_journal_page_last               3364
_journal_paper_doi               10.1039/b707265a
_journal_year                    2007
_chemical_formula_sum            'C18.5 H28 B Cl7 N6 O S3 Ti'
_chemical_formula_weight         747.52
_chemical_name_systematic
;
?
;
_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
_cell_angle_alpha                75.65(3)
_cell_angle_beta                 72.60(3)
_cell_angle_gamma                72.72(3)
_cell_formula_units_Z            2
_cell_length_a                   10.409(2)
_cell_length_b                   13.165(3)
_cell_length_c                   13.445(3)
_cell_measurement_reflns_used    34699
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      31.00
_cell_measurement_theta_min      2.91
_cell_volume                     1653.0(7)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        'X -Seed'
_computing_molecular_graphics    'X-Seed / POV-Ray'
_computing_publication_material  'Microsoft Office 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       ' φ and ω scans with CCD '
_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  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34902
_diffrn_reflns_theta_full        27.62
_diffrn_reflns_theta_max         27.62
_diffrn_reflns_theta_min         2.95
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.039
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.809
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             766
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         7629
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0530P)²+0.9767P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1145
_reflns_number_gt                5638
_reflns_number_total             7629
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b707265a.txt
_cod_data_source_block           c:mks62
_cod_original_cell_volume        1653.0(6)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C18.50 H28 B Cl7 N6 O S3 Ti'
_cod_database_code               7005970
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.5000 0.0000 0.0000 0.02490(14) Uani 1 2 d S . .
Cl1 Cl 0.03960(7) 0.55120(5) 0.31203(5) 0.03569(16) Uani 1 1 d . . .
O1 O -0.16815(18) 0.44154(15) 0.50379(14) 0.0362(4) Uani 1 1 d . . .
C1 C -0.3062(3) 0.4714(3) 0.5725(2) 0.0455(7) Uani 1 1 d . . .
H1A H -0.3632 0.5377 0.5385 0.055 Uiso 1 1 calc R . .
H1B H -0.3010 0.4832 0.6410 0.055 Uiso 1 1 calc R . .
B1 B 0.4187(3) 0.3314(2) -0.0723(2) 0.0318(6) Uani 1 1 d . . .
Ti2 Ti 0.0000 0.5000 0.5000 0.02572(14) Uani 1 2 d S . .
Cl2 Cl 0.15538(7) 0.32473(5) 0.48102(5) 0.03508(15) Uani 1 1 d . . .
C2 C -0.3642(4) 0.3760(3) 0.5874(3) 0.0629(10) Uani 1 1 d . . .
H2A H -0.4669 0.3962 0.6070 0.075 Uiso 1 1 calc R . .
H2B H -0.3308 0.3174 0.6427 0.075 Uiso 1 1 calc R . .
Cl3 Cl 0.64727(13) 0.14167(8) 0.35017(9) 0.0776(3) Uani 1 1 d . . .
C3 C -0.3096(4) 0.3429(4) 0.4807(4) 0.0781(13) Uani 1 1 d . . .
H3A H -0.3726 0.3832 0.4340 0.094 Uiso 1 1 calc R . .
H3B H -0.2997 0.2645 0.4871 0.094 Uiso 1 1 calc R . .
Cl4 Cl 0.57036(12) 0.35791(9) 0.22926(9) 0.0775(3) Uani 1 1 d . . .
C4 C -0.1700(3) 0.3703(3) 0.4375(3) 0.0492(8) Uani 1 1 d . . .
H4A H -0.0941 0.3041 0.4416 0.059 Uiso 1 1 calc R . .
H4B H -0.1591 0.4071 0.3628 0.059 Uiso 1 1 calc R . .
Cl5 Cl 0.07303(12) 0.09827(10) 0.76359(10) 0.0916(4) Uani 1 1 d . . .
C5 C 0.5117(4) 0.2467(3) 0.3108(3) 0.0610(9) Uani 1 1 d . . .
H5A H 0.4651 0.2190 0.2726 0.073 Uiso 1 1 calc R . .
H5B H 0.4424 0.2702 0.3746 0.073 Uiso 1 1 calc R . .
Cl6 Cl -0.0117(2) 0.08438(11) 0.58149(10) 0.1204(6) Uani 1 1 d . . .
C6 C -0.0416(4) 0.1578(3) 0.6818(3) 0.0585(9) Uani 1 1 d . . .
H6A H -0.0315 0.2321 0.6493 0.070 Uiso 1 1 calc R . .
H6B H -0.1380 0.1628 0.7251 0.070 Uiso 1 1 calc R . .
Cl7 Cl 0.1077(2) 0.6021(2) -0.08740(19) 0.0724(5) Uani 0.50 1 d P . .
C7 C 0.0012(9) 0.5569(8) 0.0356(8) 0.063(2) Uani 0.50 1 d PD . .
Cl8 Cl -0.0464(3) 0.4413(2) 0.0333(3) 0.0798(7) Uani 0.50 1 d P . .
S11 S 0.56203(7) 0.10801(5) 0.09821(5) 0.02965(15) Uani 1 1 d . . .
N11 N 0.5693(2) 0.29149(16) -0.05916(16) 0.0297(5) Uani 1 1 d . . .
C11 C 0.6312(3) 0.2063(2) 0.00477(19) 0.0286(5) Uani 1 1 d . . .
N12 N 0.7654(2) 0.20899(18) -0.01521(18) 0.0352(5) Uani 1 1 d . . .
C12 C 0.6693(3) 0.3464(2) -0.1206(2) 0.0376(6) Uani 1 1 d . . .
H12 H 0.6549 0.4094 -0.1728 0.045 Uiso 1 1 calc R . .
C13 C 0.7894(3) 0.2959(2) -0.0940(2) 0.0421(7) Uani 1 1 d . . .
H13 H 0.8752 0.3161 -0.1238 0.050 Uiso 1 1 calc R . .
C14 C 0.8661(3) 0.1327(3) 0.0388(3) 0.0499(8) Uani 1 1 d . . .
H14A H 0.8388 0.1396 0.1136 0.075 Uiso 1 1 calc R . .
H14B H 0.9577 0.1478 0.0063 0.075 Uiso 1 1 calc R . .
H14C H 0.8699 0.0590 0.0330 0.075 Uiso 1 1 calc R . .
S21 S 0.60214(7) 0.09858(5) -0.17874(5) 0.03047(15) Uani 1 1 d . . .
N21 N 0.4004(2) 0.29160(17) -0.16573(16) 0.0305(5) Uani 1 1 d . . .
C21 C 0.4646(3) 0.2014(2) -0.20864(19) 0.0294(5) Uani 1 1 d . . .
N22 N 0.4027(2) 0.20468(19) -0.28494(17) 0.0345(5) Uani 1 1 d . . .
C22 C 0.2961(3) 0.3505(2) -0.2167(2) 0.0399(6) Uani 1 1 d . . .
H22 H 0.2345 0.4176 -0.2023 0.048 Uiso 1 1 calc R . .
C23 C 0.2971(3) 0.2965(2) -0.2897(2) 0.0417(7) Uani 1 1 d . . .
H23 H 0.2364 0.3177 -0.3357 0.050 Uiso 1 1 calc R . .
C24 C 0.4397(4) 0.1219(3) -0.3506(2) 0.0491(8) Uani 1 1 d . . .
H24A H 0.5373 0.1127 -0.3892 0.074 Uiso 1 1 calc R . .
H24B H 0.3812 0.1443 -0.4012 0.074 Uiso 1 1 calc R . .
H24C H 0.4251 0.0534 -0.3055 0.074 Uiso 1 1 calc R . .
S31 S 0.25943(6) 0.11623(5) 0.00881(5) 0.03094(15) Uani 1 1 d . . .
N31 N 0.3147(2) 0.30083(16) 0.03345(16) 0.0301(5) Uani 1 1 d . . .
C31 C 0.2543(3) 0.2170(2) 0.0723(2) 0.0307(5) Uani 1 1 d . . .
N32 N 0.1834(2) 0.22502(18) 0.17328(18) 0.0370(5) Uani 1 1 d . . .
C32 C 0.2810(3) 0.3611(2) 0.1131(2) 0.0396(6) Uani 1 1 d . . .
H32 H 0.3097 0.4249 0.1073 0.048 Uiso 1 1 calc R . .
C33 C 0.2014(3) 0.3143(2) 0.1992(2) 0.0427(7) Uani 1 1 d . . .
H33 H 0.1642 0.3378 0.2656 0.051 Uiso 1 1 calc R . .
C34 C 0.1029(4) 0.1507(3) 0.2453(2) 0.0535(8) Uani 1 1 d . . .
H34A H 0.0184 0.1597 0.2226 0.080 Uiso 1 1 calc R . .
H34B H 0.0777 0.1663 0.3172 0.080 Uiso 1 1 calc R . .
H34C H 0.1584 0.0763 0.2443 0.080 Uiso 1 1 calc R . .
H7A H -0.089(3) 0.608(4) 0.061(4) 0.050 Uiso 0.50 1 d PD . .
H7B H 0.058(4) 0.541(5) 0.088(3) 0.050 Uiso 0.50 1 d PD . .
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'
S S 0.1246 0.1234 '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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.180
-1 0 0 0.140
0 1 0 0.120
0 -1 0 0.140
0 0 1 0.120
0 0 -1 0.140
1 0 2 0.121
-2 0 -3 0.125
2 -3 0 0.122
0 -9 -10 0.144
-1 19 18 0.147
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
S11 Ti1 S11 180 . 2_655 ?
S11 Ti1 S31 85.64(3) . 2_655 ?
S11 Ti1 S31 94.36(3) 2_655 2_655 ?
S11 Ti1 S31 94.36(3) . . ?
S11 Ti1 S31 85.64(3) 2_655 . ?
S31 Ti1 S31 180 2_655 . ?
S11 Ti1 S21 86.24(3) . 2_655 ?
S11 Ti1 S21 93.76(3) 2_655 2_655 ?
S31 Ti1 S21 94.36(4) 2_655 2_655 ?
S31 Ti1 S21 85.64(4) . 2_655 ?
S11 Ti1 S21 93.76(3) . . ?
S11 Ti1 S21 86.24(3) 2_655 . ?
S31 Ti1 S21 85.64(4) 2_655 . ?
S31 Ti1 S21 94.36(4) . . ?
S21 Ti1 S21 180 2_655 . ?
C4 O1 C1 109.1(2) . . ?
C4 O1 Ti2 126.89(17) . . ?
C1 O1 Ti2 124.01(16) . . ?
O1 C1 C2 103.4(3) . . ?
N11 B1 N31 110.6(2) . . ?
N11 B1 N21 112.4(2) . . ?
N31 B1 N21 112.2(2) . . ?
O1 Ti2 O1 180 2_566 . ?
O1 Ti2 Cl1 89.93(6) 2_566 2_566 ?
O1 Ti2 Cl1 90.07(6) . 2_566 ?
O1 Ti2 Cl1 90.07(6) 2_566 . ?
O1 Ti2 Cl1 89.93(6) . . ?
Cl1 Ti2 Cl1 180 2_566 . ?
O1 Ti2 Cl2 89.31(6) 2_566 . ?
O1 Ti2 Cl2 90.69(6) . . ?
Cl1 Ti2 Cl2 89.47(4) 2_566 . ?
Cl1 Ti2 Cl2 90.53(4) . . ?
O1 Ti2 Cl2 90.69(6) 2_566 2_566 ?
O1 Ti2 Cl2 89.31(6) . 2_566 ?
Cl1 Ti2 Cl2 90.53(4) 2_566 2_566 ?
Cl1 Ti2 Cl2 89.47(4) . 2_566 ?
Cl2 Ti2 Cl2 180 . 2_566 ?
C1 C2 C3 102.9(3) . . ?
C2 C3 C4 105.0(3) . . ?
O1 C4 C3 105.5(3) . . ?
Cl4 C5 Cl3 112.5(2) . . ?
Cl5 C6 Cl6 112.1(2) . . ?
Cl8 Cl7 C7 20.4(4) 2_565 . ?
Cl8 C7 Cl8 89.1(7) 2_565 . ?
Cl8 C7 Cl7 22.7(4) 2_565 . ?
Cl8 C7 Cl7 111.7(6) . . ?
Cl8 C7 C7 61.9(6) 2_565 2_565 ?
Cl8 C7 C7 27.2(3) . 2_565 ?
Cl7 C7 C7 84.5(6) . 2_565 ?
C7 Cl8 Cl7 136.9(8) 2_565 2_565 ?
C7 Cl8 C7 90.9(7) 2_565 . ?
Cl7 Cl8 C7 132.0(6) 2_565 . ?
C7 Cl8 Cl8 63.3(7) 2_565 2_565 ?
Cl7 Cl8 Cl8 159.3(4) 2_565 2_565 ?
C7 Cl8 Cl8 27.6(3) . 2_565 ?
C11 S11 Ti1 106.55(9) . . ?
C11 N11 C12 107.6(2) . . ?
C11 N11 B1 132.0(2) . . ?
C12 N11 B1 120.4(2) . . ?
N12 C11 N11 107.8(2) . . ?
N12 C11 S11 122.5(2) . . ?
N11 C11 S11 129.67(19) . . ?
C11 N12 C13 108.9(2) . . ?
C11 N12 C14 124.9(2) . . ?
C13 N12 C14 126.2(2) . . ?
C13 C12 N11 108.6(2) . . ?
C12 C13 N12 107.2(2) . . ?
C21 S21 Ti1 103.91(9) . . ?
C21 N21 C22 107.8(2) . . ?
C21 N21 B1 132.2(2) . . ?
C22 N21 B1 120.0(2) . . ?
N21 C21 N22 107.5(2) . . ?
N21 C21 S21 129.03(19) . . ?
N22 C21 S21 123.5(2) . . ?
C21 N22 C23 109.6(2) . . ?
C21 N22 C24 125.4(2) . . ?
C23 N22 C24 125.0(2) . . ?
C23 C22 N21 108.4(3) . . ?
C22 C23 N22 106.8(2) . . ?
C31 S31 Ti1 103.03(9) . . ?
C31 N31 C32 107.9(2) . . ?
C31 N31 B1 132.7(2) . . ?
C32 N31 B1 119.0(2) . . ?
N31 C31 N32 107.6(2) . . ?
N31 C31 S31 128.4(2) . . ?
N32 C31 S31 124.0(2) . . ?
C31 N32 C33 109.1(2) . . ?
C31 N32 C34 126.0(2) . . ?
C33 N32 C34 124.9(2) . . ?
C33 C32 N31 108.4(2) . . ?
C32 C33 N32 107.0(2) . . ?
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 S11 2.4837(8) . ?
Ti1 S11 2.4837(8) 2_655 ?
Ti1 S31 2.5025(11) 2_655 ?
Ti1 S31 2.5025(11) . ?
Ti1 S21 2.5169(11) 2_655 ?
Ti1 S21 2.5169(11) . ?
Cl1 Ti2 2.3893(9) . ?
O1 C4 1.452(3) . ?
O1 C1 1.457(3) . ?
O1 Ti2 2.0942(17) . ?
C1 C2 1.495(4) . ?
B1 N11 1.548(4) . ?
B1 N31 1.553(4) . ?
B1 N21 1.555(4) . ?
Ti2 O1 2.0942(17) 2_566 ?
Ti2 Cl1 2.3893(9) 2_566 ?
Ti2 Cl2 2.4152(11) . ?
Ti2 Cl2 2.4152(11) 2_566 ?
C2 C3 1.499(5) . ?
Cl3 C5 1.763(4) . ?
C3 C4 1.511(5) . ?
Cl4 C5 1.747(4) . ?
Cl5 C6 1.747(4) . ?
Cl6 C6 1.751(4) . ?
Cl7 Cl8 0.998(3) 2_565 ?
Cl7 C7 1.769(10) . ?
C7 Cl8 0.904(8) 2_565 ?
C7 Cl8 1.744(9) . ?
C7 C7 1.977(18) 2_565 ?
Cl8 C7 0.904(8) 2_565 ?
Cl8 Cl7 0.998(3) 2_565 ?
Cl8 Cl8 1.952(6) 2_565 ?
S11 C11 1.726(3) . ?
N11 C11 1.354(3) . ?
N11 C12 1.388(3) . ?
C11 N12 1.351(3) . ?
N12 C13 1.381(4) . ?
N12 C14 1.450(4) . ?
C12 C13 1.337(4) . ?
S21 C21 1.723(3) . ?
N21 C21 1.351(3) . ?
N21 C22 1.390(3) . ?
C21 N22 1.351(3) . ?
N22 C23 1.374(4) . ?
N22 C24 1.463(4) . ?
C22 C23 1.344(4) . ?
S31 C31 1.727(3) . ?
N31 C31 1.348(3) . ?
N31 C32 1.390(3) . ?
C31 N32 1.351(3) . ?
N32 C33 1.382(4) . ?
N32 C34 1.459(4) . ?
C32 C33 1.335(4) . ?
