#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/08/7110847.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_7110847
loop_
_publ_author_name
'Braunschweig, Holger'
'Koblinski, Carsten von'
'Englert, Ulli'
_publ_section_title
;
 Synthesis and structure of the first boron-bridged constrained geometry
 complexes
;
_journal_issue                   12
_journal_name_full               'Chemical Communications'
_journal_page_first              1049
_journal_paper_doi               10.1039/b000380h
_journal_year                    2000
_chemical_compound_source        'see paper'
_chemical_formula_sum            'C21 H35 B N4 Ti'
_chemical_formula_weight         402.25
_chemical_name_common
; Complex 1

;
_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                101.94(2)
_cell_angle_beta                 102.32(4)
_cell_angle_gamma                103.37(4)
_cell_formula_units_Z            2.00
_cell_length_a                   9.464(6)
_cell_length_b                   9.754(4)
_cell_length_c                   13.596(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    213
_cell_measurement_theta_max      13
_cell_measurement_theta_min      11
_cell_volume                     1148.8(10)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1977)
_computing_data_collection       CAD4_(Enraf-Nonius,_1977)
_computing_data_reduction        PROCESS_MolEN_(Fair,_1990)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device       Enraf_Nonius_CAD4
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4351
_diffrn_reflns_theta_full        25.96
_diffrn_reflns_theta_max         26.0
_diffrn_reflns_theta_min         3.1
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.380
_exptl_absorpt_correction_T_max  0.000
_exptl_absorpt_correction_T_min  0.000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.17
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platelet
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         4068
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0697P)²+0.1442P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1162
_reflns_number_gt                3347
_reflns_number_total             4351
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b000380hsup1.cif
_cod_data_source_block           KV6170799
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0697P)^2^+0.1442P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0697P)^2^+0.1442P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1149(1)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C21 H35 B1 N4 Ti1'
_cod_database_code               7110847
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_calc_flag
_atom_site_refinement_flags
Ti Ti 0.48966(4) 0.31917(4) 0.20166(3) 0.02737(13) Uani 1 d .
N1 N 0.71708(19) 0.3937(2) 0.23969(14) 0.0309(4) Uani 1 d .
N2 N 0.88284(19) 0.6513(2) 0.35117(14) 0.0313(4) Uani 1 d .
N3 N 0.4063(2) 0.2896(2) 0.05588(14) 0.0329(4) Uani 1 d .
N4 N 0.4428(2) 0.1254(2) 0.21870(15) 0.0370(5) Uani 1 d .
C1 C 0.5839(2) 0.5460(2) 0.31686(16) 0.0325(5) Uani 1 d .
C2 C 0.4691(2) 0.5603(3) 0.23669(18) 0.0351(5) Uani 1 d .
H2 H 0.4853 0.6213 0.1889 0.046 Uiso 1 calc R
C3 C 0.3283(3) 0.4728(3) 0.23680(19) 0.0410(6) Uani 1 d .
H3 H 0.2306 0.4610 0.1885 0.053 Uiso 1 calc R
C4 C 0.3520(3) 0.4058(3) 0.31772(19) 0.0432(6) Uani 1 d .
H4 H 0.2740 0.3389 0.3362 0.056 Uiso 1 calc R
C5 C 0.5068(3) 0.4510(3) 0.36781(17) 0.0386(5) Uani 1 d .
H5 H 0.5548 0.4220 0.4283 0.050 Uiso 1 calc R
C10 C 0.8086(2) 0.3252(2) 0.18935(16) 0.0308(5) Uani 1 d .
C11 C 0.8499(3) 0.3647(3) 0.10486(18) 0.0405(6) Uani 1 d .
H11 H 0.8167 0.4429 0.0806 0.053 Uiso 1 calc R
C12 C 0.9370(3) 0.2958(3) 0.0544(2) 0.0505(7) Uani 1 d .
H12 H 0.9642 0.3253 -0.0053 0.066 Uiso 1 calc R
C13 C 0.9855(3) 0.1867(3) 0.0869(2) 0.0542(7) Uani 1 d .
H13 H 1.0484 0.1390 0.0516 0.070 Uiso 1 calc R
C14 C 0.9446(3) 0.1451(3) 0.1698(3) 0.0576(8) Uani 1 d .
H14 H 0.9782 0.0666 0.1933 0.075 Uiso 1 calc R
C15 C 0.8567(3) 0.2127(3) 0.2207(2) 0.0459(6) Uani 1 d .
H15 H 0.8281 0.1810 0.2793 0.060 Uiso 1 calc R
C20 C 1.0306(2) 0.6365(3) 0.33997(18) 0.0360(5) Uani 1 d .
H20 H 1.0132 0.5357 0.2994 0.047 Uiso 1 calc R
C21 C 1.1437(3) 0.6589(3) 0.4442(2) 0.0536(7) Uani 1 d .
H21A H 1.1695 0.7607 0.4855 0.070 Uiso 1 calc R
H21B H 1.2352 0.6367 0.4318 0.070 Uiso 1 calc R
H21C H 1.0991 0.5936 0.4825 0.070 Uiso 1 calc R
C22 C 1.0962(3) 0.7364(3) 0.2781(2) 0.0535(7) Uani 1 d .
H22A H 1.0249 0.7145 0.2091 0.070 Uiso 1 calc R
H22B H 1.1918 0.7203 0.2696 0.070 Uiso 1 calc R
H22C H 1.1141 0.8387 0.3157 0.070 Uiso 1 calc R
C23 C 0.8872(2) 0.7966(2) 0.41377(17) 0.0359(5) Uani 1 d .
H23 H 0.9930 0.8559 0.4364 0.047 Uiso 1 calc R
C24 C 0.7995(3) 0.8764(3) 0.3509(2) 0.0530(7) Uani 1 d .
H24A H 0.8311 0.8776 0.2869 0.069 Uiso 1 calc R
H24B H 0.8193 0.9770 0.3926 0.069 Uiso 1 calc R
H24C H 0.6913 0.8261 0.3325 0.069 Uiso 1 calc R
C25 C 0.8391(3) 0.7879(3) 0.5129(2) 0.0509(7) Uani 1 d .
H25A H 0.7314 0.7355 0.4942 0.066 Uiso 1 calc R
H25B H 0.8573 0.8870 0.5567 0.066 Uiso 1 calc R
H25C H 0.8977 0.7356 0.5515 0.066 Uiso 1 calc R
C31 C 0.4657(3) 0.1883(3) -0.00672(19) 0.0447(6) Uani 1 d .
H31A H 0.3818 0.1080 -0.0558 0.058 Uiso 1 calc R
H31B H 0.5303 0.1488 0.0394 0.058 Uiso 1 calc R
H31C H 0.5250 0.2402 -0.0458 0.058 Uiso 1 calc R
C32 C 0.3123(3) 0.3511(3) -0.01093(19) 0.0488(7) Uani 1 d .
H32A H 0.3734 0.4072 -0.0470 0.063 Uiso 1 calc R
H32B H 0.2699 0.4158 0.0317 0.063 Uiso 1 calc R
H32C H 0.2301 0.2720 -0.0626 0.063 Uiso 1 calc R
C41 C 0.3135(3) 0.0046(3) 0.1528(2) 0.0483(6) Uani 1 d .
H41A H 0.3433 -0.0858 0.1410 0.063 Uiso 1 calc R
H41B H 0.2777 0.0248 0.0856 0.063 Uiso 1 calc R
H41C H 0.2324 -0.0063 0.1875 0.063 Uiso 1 calc R
C42 C 0.5020(4) 0.0944(4) 0.3171(2) 0.0634(8) Uani 1 d .
H42A H 0.4240 0.0827 0.3544 0.082 Uiso 1 calc R
H42B H 0.5901 0.1756 0.3602 0.082 Uiso 1 calc R
H42C H 0.5317 0.0041 0.3030 0.082 Uiso 1 calc R
B B 0.7468(3) 0.5380(3) 0.30476(19) 0.0303(5) Uani 1 d .
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N3 Ti N4 103.44(9)
N3 Ti N1 110.25(9)
N4 Ti N1 106.33(9)
N3 Ti C1 122.66(9)
N4 Ti C1 133.22(9)
N1 Ti C1 67.01(9)
N3 Ti C5 145.47(9)
N4 Ti C5 99.77(9)
N1 Ti C5 86.89(9)
C1 Ti C5 36.26(8)
N3 Ti C2 90.82(9)
N4 Ti C2 151.26(9)
N1 Ti C2 91.44(9)
C1 Ti C2 35.54(8)
C5 Ti C2 57.99(9)
N3 Ti C4 117.72(9)
N4 Ti C4 94.33(9)
N1 Ti C4 120.91(9)
C1 Ti C4 59.04(9)
C5 Ti C4 34.53(9)
C2 Ti C4 56.95(9)
N3 Ti C3 89.09(9)
N4 Ti C3 120.02(9)
N1 Ti C3 123.80(9)
C1 Ti C3 58.52(9)
C5 Ti C3 56.99(9)
C2 Ti C3 34.16(8)
C4 Ti C3 33.64(9)
N3 Ti B 119.47(8)
N4 Ti B 126.01(8)
N1 Ti B 30.94(8)
C1 Ti B 36.18(8)
C5 Ti B 62.28(8)
C2 Ti B 63.03(9)
C4 Ti B 93.18(9)
C3 Ti B 93.29(9)
C10 N1 B 131.67(18)
C10 N1 Ti 124.23(14)
B N1 Ti 102.40(14)
B N2 C20 123.20(19)
B N2 C23 121.99(19)
C20 N2 C23 114.80(17)
C32 N3 C31 110.28(19)
C32 N3 Ti 137.65(17)
C31 N3 Ti 111.64(15)
C41 N4 C42 110.3(2)
C41 N4 Ti 124.81(17)
C42 N4 Ti 122.15(18)
C2 C1 C5 105.4(2)
C2 C1 B 123.89(19)
C5 C1 B 119.4(2)
C2 C1 Ti 75.37(14)
C5 C1 Ti 72.91(13)
B C1 Ti 86.69(14)
C3 C2 C1 109.2(2)
C3 C2 Ti 75.35(15)
C1 C2 Ti 69.09(13)
C4 C3 C2 108.1(2)
C4 C3 Ti 72.01(14)
C2 C3 Ti 70.49(14)
C3 C4 C5 108.0(2)
C3 C4 Ti 74.35(14)
C5 C4 Ti 69.33(13)
C4 C5 C1 109.3(2)
C4 C5 Ti 76.13(14)
C1 C5 Ti 70.83(12)
C11 C10 C15 117.6(2)
C11 C10 N1 121.2(2)
C15 C10 N1 121.2(2)
C12 C11 C10 121.2(3)
C13 C12 C11 120.7(3)
C12 C13 C14 119.0(2)
C13 C14 C15 120.9(3)
C14 C15 C10 120.6(3)
N2 C20 C21 112.9(2)
N2 C20 C22 111.9(2)
C21 C20 C22 111.0(2)
N2 C23 C24 113.00(19)
N2 C23 C25 112.1(2)
C24 C23 C25 111.6(2)
N2 B N1 131.0(2)
N2 B C1 125.4(2)
N1 B C1 103.57(18)
N2 B Ti 175.77(16)
N1 B Ti 46.66(10)
C1 B Ti 57.13(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ti N3 1.9045(19)
Ti N4 1.913(2)
Ti N1 2.020(2)
Ti C1 2.282(2)
Ti C5 2.309(2)
Ti C2 2.364(3)
Ti C4 2.396(2)
Ti C3 2.426(3)
Ti B 2.712(3)
N1 C10 1.414(3)
N1 B 1.428(3)
N2 B 1.409(3)
N2 C20 1.476(3)
N2 C23 1.481(3)
N3 C32 1.451(3)
N3 C31 1.460(3)
N4 C41 1.456(3)
N4 C42 1.457(3)
C1 C2 1.420(3)
C1 C5 1.429(3)
C1 B 1.604(3)
C2 C3 1.408(3)
C3 C4 1.396(4)
C4 C5 1.399(3)
C10 C11 1.388(3)
C10 C15 1.391(3)
C11 C12 1.382(4)
C12 C13 1.369(4)
C13 C14 1.374(4)
C14 C15 1.385(4)
C20 C21 1.523(3)
C20 C22 1.525(3)
C23 C24 1.516(4)
C23 C25 1.524(3)
