#------------------------------------------------------------------------------
#$Date: 2017-03-04 15:24:37 +0200 (Sat, 04 Mar 2017) $
#$Revision: 193457 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/50/4345040.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_4345040
loop_
_publ_author_name
'Brown, Andrew'
'Saber, Mohamed'
'Van den Heuvel, Willem'
'Schulte, Kelsey'
'Soncini, Alessandro'
'Dunbar, Kim R.'
_publ_section_title
;
 Titanium(III) Member of the Family of Trigonal Building Blocks with
 Scorpionate and Cyanide Ligands.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1031
_journal_page_last               1035
_journal_paper_doi               10.1021/acs.inorgchem.6b02643
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C26 H42 B N10 Ti'
_chemical_formula_weight         553.40
_chemical_name_common
'Tetraethylammonium Tricyano[tris(3,5-dimethylpyrazol-1-yl)hydroborate]Titanium(III)'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_symmetry_space_group_name_Hall  'P 2ac -2'
_symmetry_space_group_name_H-M   'P m n 21'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.634(2)
_cell_length_b                   8.1814(16)
_cell_length_c                   15.620(3)
_cell_measurement_reflns_used    3736
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.604
_cell_measurement_theta_min      1.304
_cell_volume                     1486.7(5)
_computing_cell_refinement       'SMART V5.625 (Bruker, 2000)'
_computing_data_collection       'SMART V5.625 (Bruker, 2000)'
_computing_data_reduction        'SAINT V6.32 (Bruker, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'profile data from ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17184
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.604
_diffrn_reflns_theta_min         1.304
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.321
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       Block
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 1645 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.013(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3736
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0257
_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)+(0.0551P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.965
_reflns_number_gt                3595
_reflns_number_total             3736
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b02643_si_004.cif
_cod_data_source_block           AJ009A
_cod_depositor_comments          'Adding full bibliography for 4345040.cif.'
_cod_original_cell_volume        1486.8(5)
_cod_database_code               4345040
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y, z'
'x+1/2, -y, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ti1 Ti 0.0000 0.86120(5) 0.80185(2) 0.01468(11) Uani 1 2 d S T P
N1 N 0.0000 0.5961(3) 0.96449(17) 0.0329(6) Uani 1 2 d S T P
C1 C 0.0000 0.6814(3) 0.90450(16) 0.0210(5) Uani 1 2 d S T P
B1 B 0.0000 0.7980(3) 0.59843(17) 0.0163(5) Uani 1 2 d S T P
N2 N 0.22363(17) 1.0490(3) 0.89135(14) 0.0397(5) Uani 1 1 d . . .
C2 C 0.14141(16) 0.9882(2) 0.86387(11) 0.0216(4) Uani 1 1 d . . .
N3 N 0.0000 1.0379(2) 0.70116(13) 0.0168(4) Uani 1 2 d S T P
C3 C 0.0000 1.3083(3) 0.7747(2) 0.0288(6) Uani 1 2 d S T P
H3A H 0.0273 1.4178 0.7595 0.029(13) Uiso 0.5 1 calc R . P
H3B H 0.0509 1.2611 0.8181 0.040(15) Uiso 0.5 1 calc R . P
H3C H -0.0782 1.3157 0.7977 0.032(12) Uiso 0.5 1 calc R . P
N4 N 0.0000 0.9829(2) 0.61758(13) 0.0156(4) Uani 1 2 d S T P
C4 C 0.0000 1.2025(3) 0.69716(18) 0.0200(5) Uani 1 2 d S T P
H10 H 0.335(2) 0.522(3) 0.6598(16) 0.034(6) Uiso 1 1 d . . .
N5 N 0.12472(12) 0.72825(18) 0.72647(9) 0.0162(3) Uani 1 1 d . . .
C5 C 0.0000 1.2517(3) 0.61222(18) 0.0214(5) Uani 1 2 d S T P
N6 N 0.10719(12) 0.71831(17) 0.63967(9) 0.0154(3) Uani 1 1 d . . .
C6 C 0.0000 1.1117(3) 0.56381(18) 0.0193(5) Uani 1 2 d S T P
N7 N 0.0000 -0.0499(3) 0.15592(13) 0.0171(4) Uani 1 2 d S T P
C7 C 0.0000 1.0919(4) 0.46851(19) 0.0262(6) Uani 1 2 d S T P
H7A H 0.0000 1.191(5) 0.440(2) 0.032(9) Uiso 1 2 d S . P
H7B H 0.065(2) 1.032(3) 0.4489(16) 0.032(6) Uiso 1 1 d . . .
C8 C 0.2703(2) 0.6283(3) 0.83018(14) 0.0304(5) Uani 1 1 d . . .
H8A H 0.3188 0.7228 0.8436 0.098(15) Uiso 1 1 calc R . .
H8B H 0.3163 0.5282 0.8334 0.15(2) Uiso 1 1 calc R . .
H8C H 0.2070 0.6220 0.8715 0.067(12) Uiso 1 1 calc R . .
C9 C 0.22274(16) 0.6463(2) 0.74245(13) 0.0192(4) Uani 1 1 d . . .
C10 C 0.26718(16) 0.5849(2) 0.66646(12) 0.0205(4) Uani 1 1 d . . .
H5 H 0.0000 1.355(4) 0.590(2) 0.025(9) Uiso 1 2 d S . P
C11 C 0.19198(16) 0.6321(2) 0.60255(12) 0.0184(4) Uani 1 1 d . . .
C12 C 0.19913(17) 0.5991(2) 0.50880(12) 0.0251(4) Uani 1 1 d . . .
H12A H 0.1319 0.5358 0.4908 0.039(7) Uiso 1 1 calc R . .
H12B H 0.2692 0.5369 0.4965 0.065(10) Uiso 1 1 calc R . .
H12C H 0.2011 0.7030 0.4776 0.027(6) Uiso 1 1 calc R . .
C13 C 0.0000 -0.0761(3) 0.25244(17) 0.0267(6) Uani 1 2 d S T P
H13A H 0.0686 -0.0218 0.2768 0.032 Uiso 0.5 1 calc R U P
H13B H -0.0686 -0.0218 0.2768 0.032 Uiso 0.5 1 calc R U P
C14 C 0.0000 -0.2530(4) 0.2806(2) 0.0425(8) Uani 1 2 d S T P
H14A H -0.0273 -0.2603 0.3398 0.036(14) Uiso 0.5 1 calc R . P
H14B H 0.0782 -0.2968 0.2770 0.017(10) Uiso 0.5 1 calc R . P
H14C H -0.0509 -0.3164 0.2432 0.09(3) Uiso 0.5 1 calc R . P
C15 C 0.0000 0.1341(3) 0.14335(19) 0.0205(6) Uani 1 2 d S T P
H15A H -0.0686 0.1798 0.1722 0.025 Uiso 0.5 1 calc R U P
H15B H 0.0686 0.1798 0.1722 0.025 Uiso 0.5 1 calc R U P
H18A H 0.274(3) -0.136(3) 0.113(2) 0.047(9) Uiso 1 1 d . . .
C16 C 0.0000 0.1910(4) 0.0518(2) 0.0291(6) Uani 1 2 d S T P
H18B H 0.228(3) -0.087(4) 0.201(3) 0.053(9) Uiso 1 1 d . . .
C17 C 0.10378(15) -0.1278(2) 0.11373(14) 0.0224(4) Uani 1 1 d . . .
H17A H 0.0990 -0.2477 0.1215 0.027 Uiso 1 1 calc R U .
H17B H 0.1004 -0.1055 0.0515 0.027 Uiso 1 1 calc R U .
H18C H 0.219(3) 0.048(5) 0.131(3) 0.073(10) Uiso 1 1 d . . .
C18 C 0.21807(18) -0.0700(3) 0.1472(2) 0.0391(6) Uani 1 1 d . . .
H16A H 0.060(2) 0.159(3) 0.0245(18) 0.032(7) Uiso 1 1 d . . .
H16B H 0.0000 0.306(6) 0.047(3) 0.040(10) Uiso 1 2 d S . P
H1 H 0.0000 0.774(3) 0.5268(18) 0.012(7) Uiso 1 2 d S . P
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'
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
N3 Ti1 N5 86.53(6) . .
N3 Ti1 N5 86.53(6) . 3
N5 Ti1 N5 84.30(8) . 3
N3 Ti1 C2 90.27(6) . .
N5 Ti1 C2 88.58(6) . .
N5 Ti1 C2 172.36(6) 3 .
N3 Ti1 C2 90.27(6) . 3
N5 Ti1 C2 172.36(6) . 3
N5 Ti1 C2 88.58(6) 3 3
C2 Ti1 C2 98.38(10) . 3
N3 Ti1 C1 179.94(9) . .
N5 Ti1 C1 93.51(6) . .
N5 Ti1 C1 93.51(6) 3 .
C2 Ti1 C1 89.70(7) . .
C2 Ti1 C1 89.70(7) 3 .
N1 C1 Ti1 174.2(2) . .
N4 B1 N6 109.43(13) . .
N4 B1 N6 109.43(13) . 3
N6 B1 N6 107.37(19) . 3
N4 B1 H1 111.0(15) . .
N6 B1 H1 109.8(8) . .
N6 B1 H1 109.8(8) 3 .
N2 C2 Ti1 173.53(17) . .
C4 N3 N4 106.3(2) . .
C4 N3 Ti1 135.24(17) . .
N4 N3 Ti1 118.41(14) . .
C4 C3 H3A 109.5 . .
C4 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C4 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C6 N4 N3 109.6(2) . .
C6 N4 B1 130.3(2) . .
N3 N4 B1 120.18(18) . .
N3 C4 C5 109.5(2) . .
N3 C4 C3 122.9(2) . .
C5 C4 C3 127.6(2) . .
C9 N5 N6 106.22(14) . .
C9 N5 Ti1 135.89(13) . .
N6 N5 Ti1 117.89(10) . .
C6 C5 C4 106.5(2) . .
C6 C5 H5 124(2) . .
C4 C5 H5 129(2) . .
C11 N6 N5 110.36(14) . .
C11 N6 B1 129.27(16) . .
N5 N6 B1 120.36(15) . .
N4 C6 C5 108.0(2) . .
N4 C6 C7 122.4(3) . .
C5 C6 C7 129.6(3) . .
C17 N7 C17 105.59(18) 3 .
C17 N7 C15 111.14(13) 3 .
C17 N7 C15 111.13(13) . .
C17 N7 C13 111.79(14) 3 .
C17 N7 C13 111.79(13) . .
C15 N7 C13 105.5(2) . .
C6 C7 H7A 113(2) . .
C6 C7 H7B 112.0(16) . .
H7A C7 H7B 107(2) . .
C9 C8 H8A 109.5 . .
C9 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C9 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N5 C9 C10 109.70(17) . .
N5 C9 C8 122.41(17) . .
C10 C9 C8 127.88(16) . .
C11 C10 C9 106.29(16) . .
C11 C10 H10 126.8(15) . .
C9 C10 H10 126.9(15) . .
N6 C11 C10 107.43(16) . .
N6 C11 C12 124.01(17) . .
C10 C11 C12 128.56(17) . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C14 C13 N7 115.0(2) . .
C14 C13 H13A 108.5 . .
N7 C13 H13A 108.5 . .
C14 C13 H13B 108.5 . .
N7 C13 H13B 108.5 . .
H13A C13 H13B 107.5 . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C16 C15 N7 115.5(2) . .
C16 C15 H15A 108.4 . .
N7 C15 H15A 108.4 . .
C16 C15 H15B 108.4 . .
N7 C15 H15B 108.4 . .
H15A C15 H15B 107.5 . .
C15 C16 H16A 112.1(18) . .
C15 C16 H16B 113(2) . .
H16A C16 H16B 105(2) . .
C18 C17 N7 114.85(17) . .
C18 C17 H17A 108.6 . .
N7 C17 H17A 108.6 . .
C18 C17 H17B 108.6 . .
N7 C17 H17B 108.6 . .
H17A C17 H17B 107.5 . .
C17 C18 H18A 102.8(18) . .
C17 C18 H18B 114(2) . .
H18A C18 H18B 111(3) . .
C17 C18 H18C 103(2) . .
H18A C18 H18C 112(3) . .
H18B C18 H18C 114(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 N3 2.136(2) .
Ti1 N5 2.1621(14) .
Ti1 N5 2.1621(14) 3
Ti1 C2 2.1737(19) .
Ti1 C2 2.1737(19) 3
Ti1 C1 2.176(3) .
N1 C1 1.168(4) .
B1 N4 1.542(3) .
B1 N6 1.548(2) .
B1 N6 1.548(2) 3
B1 H1 1.14(3) .
N2 C2 1.161(3) .
N3 C4 1.348(3) .
N3 N4 1.381(3) .
C3 C4 1.490(4) .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
N4 C6 1.347(3) .
C4 C5 1.386(4) .
N5 C9 1.346(2) .
N5 N6 1.3735(19) .
C5 C6 1.372(4) .
C5 H5 0.92(4) .
N6 C11 1.344(2) .
C6 C7 1.497(4) .
N7 C17 1.516(2) 3
N7 C17 1.516(2) .
N7 C15 1.518(3) .
N7 C13 1.523(3) .
C7 H7A 0.93(4) .
C7 H7B 0.95(3) .
C8 C9 1.485(3) .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 C10 1.389(3) .
C10 C11 1.382(3) .
C10 H10 0.95(3) .
C11 C12 1.491(2) .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 C14 1.512(4) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 C16 1.504(4) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C16 H16A 0.86(3) .
C16 H16B 0.94(5) .
C17 C18 1.505(3) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C18 H18A 1.00(3) .
C18 H18B 0.86(4) .
C18 H18C 1.00(4) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
C4 N3 N4 C6 0.000(1) .
Ti1 N3 N4 C6 180.000(1) .
C4 N3 N4 B1 180.000(1) .
Ti1 N3 N4 B1 0.000(1) .
N6 B1 N4 C6 121.30(13) .
N6 B1 N4 C6 -121.30(13) 3
N6 B1 N4 N3 -58.70(13) .
N6 B1 N4 N3 58.70(13) 3
N4 N3 C4 C5 0.000(2) .
Ti1 N3 C4 C5 180.000(1) .
N4 N3 C4 C3 180.000(2) .
Ti1 N3 C4 C3 0.000(2) .
N3 C4 C5 C6 0.000(2) .
C3 C4 C5 C6 180.000(2) .
C9 N5 N6 C11 0.13(18) .
Ti1 N5 N6 C11 180.00(11) .
C9 N5 N6 B1 179.13(16) .
Ti1 N5 N6 B1 -1.0(2) .
N4 B1 N6 C11 -122.10(19) .
N6 B1 N6 C11 119.22(18) 3
N4 B1 N6 N5 59.1(2) .
N6 B1 N6 N5 -59.6(2) 3
N3 N4 C6 C5 0.000(2) .
B1 N4 C6 C5 180.000(2) .
N3 N4 C6 C7 180.000(2) .
B1 N4 C6 C7 0.000(2) .
C4 C5 C6 N4 0.000(2) .
C4 C5 C6 C7 180.000(2) .
N6 N5 C9 C10 0.03(19) .
Ti1 N5 C9 C10 -179.80(13) .
N6 N5 C9 C8 -179.46(17) .
Ti1 N5 C9 C8 0.7(3) .
N5 C9 C10 C11 -0.2(2) .
C8 C9 C10 C11 179.28(19) .
N5 N6 C11 C10 -0.25(19) .
B1 N6 C11 C10 -179.13(17) .
N5 N6 C11 C12 -179.69(16) .
B1 N6 C11 C12 1.4(3) .
C9 C10 C11 N6 0.3(2) .
C9 C10 C11 C12 179.67(18) .
C17 N7 C13 C14 59.06(13) 3
C17 N7 C13 C14 -59.07(13) .
C15 N7 C13 C14 180.000(0) .
C17 N7 C15 C16 -58.64(13) 3
C17 N7 C15 C16 58.64(13) .
C13 N7 C15 C16 180.000(0) .
C17 N7 C17 C18 -179.01(16) 3
C15 N7 C17 C18 60.4(3) .
C13 N7 C17 C18 -57.2(2) .
