#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:26:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179328 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/25/4322530.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_4322530
loop_
_publ_author_name
'Lena Kakaliou'
Scanlon
'Baixin Qian'
'Sung W. Baek'
'Milton R. Smith'
'Douglas H. Motry'
_publ_section_title
;
 Five- and Six-Coordinate Group 4 Compounds Stabilized by β-Ketiminate
 and Diketiminate Ligands: Syntheses and Comparisons between Solid-State
 and Solution Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5964
_journal_page_last               5977
_journal_paper_doi               10.1021/ic981364j
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C25 H39 N5 Ti'
_chemical_formula_weight         457.51
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                102.53
_cell_angle_beta                 93.59
_cell_angle_gamma                102.5190(10)
_cell_formula_units_Z            2
_cell_length_a                   8.69720(10)
_cell_length_b                   10.51620(10)
_cell_length_c                   15.53630(10)
_cell_measurement_temperature    173(2)
_cell_volume                     1345.16(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13940
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    0.337
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.161
_refine_ls_goodness_of_fit_obs   1.213
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         6100
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_restrained_S_obs      1.213
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_obs          0.0431
_refine_ls_shift/esd_max         -0.018
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1534
_refine_ls_wR_factor_obs         0.1460
_reflns_number_observed          5099
_reflns_number_total             6100
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981364j_03.cif
_cod_data_source_block           (TTP)Ti(NMe2)3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] 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^)+(0.1000P)^2^+0.0000P] 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        1345.12(2)
_cod_database_code               4322530
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ti1 Ti 0.45360(3) 0.77617(3) 0.71306(2) 0.02285(12) Uani 1 d . .
N5 N 0.5576(2) 0.7553(2) 0.60410(11) 0.0329(4) Uani 1 d . .
N3 N 0.5525(2) 0.6536(2) 0.75661(12) 0.0376(4) Uani 1 d . .
N4 N 0.2475(2) 0.7174(2) 0.64617(11) 0.0333(4) Uani 1 d . .
N2 N 0.5504(2) 0.98210(15) 0.75801(10) 0.0243(3) Uani 1 d . .
N1 N 0.3343(2) 0.8090(2) 0.83673(10) 0.0272(3) Uani 1 d . .
C25 C 0.5013(3) 0.7851(3) 0.52121(15) 0.0513(6) Uani 1 d . .
H25A H 0.3968(3) 0.8003(3) 0.52485(15) 0.077 Uiso 1 calc R .
H25B H 0.4986(3) 0.7106(3) 0.47235(15) 0.077 Uiso 1 calc R .
H25C H 0.5719(3) 0.8638(3) 0.51227(15) 0.077 Uiso 1 calc R .
C24 C 0.7165(3) 0.7315(3) 0.5975(2) 0.0491(6) Uani 1 d . .
H24A H 0.7540(3) 0.7118(3) 0.6515(2) 0.074 Uiso 1 calc R .
H24B H 0.7870(3) 0.8101(3) 0.5884(2) 0.074 Uiso 1 calc R .
H24C H 0.7127(3) 0.6570(3) 0.5485(2) 0.074 Uiso 1 calc R .
C21 C 0.5320(4) 0.5138(3) 0.7119(3) 0.0763(10) Uani 1 d . .
H21A H 0.4598(4) 0.4931(3) 0.6588(3) 0.114 Uiso 1 calc R .
H21B H 0.4900(4) 0.4582(3) 0.7505(3) 0.114 Uiso 1 calc R .
H21C H 0.6326(4) 0.4976(3) 0.6970(3) 0.114 Uiso 1 calc R .
C20 C 0.6612(3) 0.6915(3) 0.8382(2) 0.0540(6) Uani 1 d . .
H20A H 0.6718(3) 0.7846(3) 0.8655(2) 0.081 Uiso 1 calc R .
H20B H 0.7630(3) 0.6767(3) 0.8247(2) 0.081 Uiso 1 calc R .
H20C H 0.6202(3) 0.6381(3) 0.8783(2) 0.081 Uiso 1 calc R .
C22 C 0.1819(3) 0.5974(3) 0.5778(2) 0.0579(7) Uani 1 d . .
H22A H 0.2575(3) 0.5427(3) 0.5702(2) 0.087 Uiso 1 calc R .
H22B H 0.1581(3) 0.6212(3) 0.5231(2) 0.087 Uiso 1 calc R .
H22C H 0.0866(3) 0.5485(3) 0.5946(2) 0.087 Uiso 1 calc R .
C23 C 0.1396(3) 0.8055(3) 0.6613(2) 0.0460(6) Uani 1 d . .
H23A H 0.1885(3) 0.8838(3) 0.7071(2) 0.069 Uiso 1 calc R .
H23B H 0.0438(3) 0.7593(3) 0.6793(2) 0.069 Uiso 1 calc R .
H23C H 0.1152(3) 0.8316(3) 0.6075(2) 0.069 Uiso 1 calc R .
C5 C 0.5593(3) 1.2236(2) 0.8146(2) 0.0396(5) Uani 1 d . .
H5A H 0.6409(3) 1.2317(2) 0.7760(2) 0.059 Uiso 1 calc R .
H5B H 0.6034(3) 1.2692(2) 0.8744(2) 0.059 Uiso 1 calc R .
H5C H 0.4768(3) 1.2628(2) 0.7962(2) 0.059 Uiso 1 calc R .
C4 C 0.4910(2) 1.0761(2) 0.81045(12) 0.0268(4) Uani 1 d . .
C3 C 0.3718(2) 1.0477(2) 0.86328(13) 0.0300(4) Uani 1 d . .
H3A H 0.3314(2) 1.1194(2) 0.89032(13) 0.036 Uiso 1 calc R .
C2 C 0.3039(2) 0.9215(2) 0.88103(13) 0.0313(4) Uani 1 d . .
C1 C 0.1970(3) 0.9243(2) 0.9545(2) 0.0535(7) Uani 1 d . .
H1A H 0.1579(3) 0.8348(2) 0.9613(2) 0.080 Uiso 1 calc R .
H1B H 0.1093(3) 0.9605(2) 0.9395(2) 0.080 Uiso 1 calc R .
H1C H 0.2560(3) 0.9793(2) 1.0091(2) 0.080 Uiso 1 calc R .
C6 C 0.2716(2) 0.6880(2) 0.86567(13) 0.0298(4) Uani 1 d . .
C11 C 0.1457(2) 0.5889(2) 0.81500(14) 0.0370(5) Uani 1 d . .
H11A H 0.1009(2) 0.6008(2) 0.76224(14) 0.044 Uiso 1 calc R .
C10 C 0.0864(3) 0.4716(2) 0.84297(14) 0.0392(5) Uani 1 d . .
H10A H 0.0015(3) 0.4071(2) 0.80881(14) 0.047 Uiso 1 calc R .
C9 C 0.1521(3) 0.4499(2) 0.92095(14) 0.0349(4) Uani 1 d . .
C8 C 0.2788(3) 0.5480(2) 0.97005(14) 0.0413(5) Uani 1 d . .
H8A H 0.3253(3) 0.5351(2) 1.02204(14) 0.050 Uiso 1 calc R .
C7 C 0.3382(3) 0.6661(2) 0.94302(14) 0.0396(5) Uani 1 d . .
H7A H 0.4231(3) 0.7305(2) 0.97729(14) 0.048 Uiso 1 calc R .
C12 C 0.0855(3) 0.3247(2) 0.9529(2) 0.0436(5) Uani 1 d . .
H12A H -0.0012(3) 0.2681(2) 0.9111(2) 0.065 Uiso 1 calc R .
H12B H 0.0487(3) 0.3496(2) 1.0097(2) 0.065 Uiso 1 calc R .
H12C H 0.1669(3) 0.2772(2) 0.9581(2) 0.065 Uiso 1 calc R .
C13 C 0.6968(2) 1.0315(2) 0.72355(12) 0.0266(4) Uani 1 d . .
C18 C 0.8399(2) 1.0305(2) 0.76744(13) 0.0305(4) Uani 1 d . .
H18A H 0.8412(2) 0.9971(2) 0.81813(13) 0.037 Uiso 1 calc R .
C17 C 0.9832(2) 1.0799(2) 0.7358(2) 0.0381(5) Uani 1 d . .
H17A H 1.0783(2) 1.0786(2) 0.7661(2) 0.046 Uiso 1 calc R .
C16 C 0.9866(3) 1.1301(2) 0.6610(2) 0.0450(5) Uani 1 d . .
C15 C 0.8414(3) 1.1292(3) 0.6165(2) 0.0493(6) Uani 1 d . .
H15A H 0.8405(3) 1.1610(3) 0.5651(2) 0.059 Uiso 1 calc R .
C14 C 0.6983(3) 1.0818(2) 0.64738(15) 0.0399(5) Uani 1 d . .
H14A H 0.6033(3) 1.0836(2) 0.61718(15) 0.048 Uiso 1 calc R .
C19 C 1.1431(4) 1.1833(4) 0.6284(2) 0.0755(9) Uani 1 d . .
H19A H 1.1234(4) 1.2137(4) 0.5757(2) 0.113 Uiso 1 calc R .
H19B H 1.1989(4) 1.1133(4) 0.6154(2) 0.113 Uiso 1 calc R .
H19C H 1.2061(4) 1.2567(4) 0.6736(2) 0.113 Uiso 1 calc R .
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'
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
_geom_angle_publ_flag
N3 Ti1 N4 121.27(8) . . ?
N3 Ti1 N5 92.75(8) . . ?
N4 Ti1 N5 91.50(7) . . ?
N3 Ti1 N2 119.40(7) . . ?
N4 Ti1 N2 118.35(7) . . ?
N5 Ti1 N2 95.63(7) . . ?
N3 Ti1 N1 89.53(7) . . ?
N4 Ti1 N1 88.27(7) . . ?
N5 Ti1 N1 177.46(6) . . ?
N2 Ti1 N1 82.27(6) . . ?
C24 N5 C25 109.0(2) . . ?
C24 N5 Ti1 125.04(14) . . ?
C25 N5 Ti1 125.15(14) . . ?
C21 N3 C20 112.1(2) . . ?
C21 N3 Ti1 124.4(2) . . ?
C20 N3 Ti1 123.5(2) . . ?
C22 N4 C23 112.6(2) . . ?
C22 N4 Ti1 129.4(2) . . ?
C23 N4 Ti1 117.95(14) . . ?
C4 N2 C13 115.84(15) . . ?
C4 N2 Ti1 129.09(12) . . ?
C13 N2 Ti1 114.95(11) . . ?
C2 N1 C6 117.3(2) . . ?
C2 N1 Ti1 128.05(12) . . ?
C6 N1 Ti1 114.36(12) . . ?
N2 C4 C3 124.2(2) . . ?
N2 C4 C5 119.3(2) . . ?
C3 C4 C5 116.4(2) . . ?
C4 C3 C2 127.6(2) . . ?
N1 C2 C3 121.8(2) . . ?
N1 C2 C1 122.2(2) . . ?
C3 C2 C1 116.0(2) . . ?
C11 C6 C7 118.4(2) . . ?
C11 C6 N1 120.7(2) . . ?
C7 C6 N1 120.9(2) . . ?
C6 C11 C10 120.5(2) . . ?
C9 C10 C11 121.2(2) . . ?
C8 C9 C10 117.8(2) . . ?
C8 C9 C12 120.7(2) . . ?
C10 C9 C12 121.5(2) . . ?
C9 C8 C7 121.4(2) . . ?
C6 C7 C8 120.7(2) . . ?
C18 C13 C14 118.7(2) . . ?
C18 C13 N2 119.5(2) . . ?
C14 C13 N2 121.9(2) . . ?
C13 C18 C17 120.3(2) . . ?
C16 C17 C18 121.7(2) . . ?
C17 C16 C15 117.6(2) . . ?
C17 C16 C19 120.6(2) . . ?
C15 C16 C19 121.7(2) . . ?
C14 C15 C16 121.5(2) . . ?
C15 C14 C13 120.2(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 N3 1.909(2) . ?
Ti1 N4 1.919(2) . ?
Ti1 N5 1.962(2) . ?
Ti1 N2 2.090(2) . ?
Ti1 N1 2.237(2) . ?
N5 C24 1.462(3) . ?
N5 C25 1.469(3) . ?
N3 C21 1.451(3) . ?
N3 C20 1.459(3) . ?
N4 C22 1.440(3) . ?
N4 C23 1.450(3) . ?
N2 C4 1.354(2) . ?
N2 C13 1.448(2) . ?
N1 C2 1.322(3) . ?
N1 C6 1.448(2) . ?
C5 C4 1.521(2) . ?
C4 C3 1.384(3) . ?
C3 C2 1.423(3) . ?
C2 C1 1.516(3) . ?
C6 C11 1.395(3) . ?
C6 C7 1.387(3) . ?
C11 C10 1.400(3) . ?
C10 C9 1.392(3) . ?
C9 C8 1.386(3) . ?
C9 C12 1.518(3) . ?
C8 C7 1.400(3) . ?
C13 C18 1.384(3) . ?
C13 C14 1.397(3) . ?
C18 C17 1.405(3) . ?
C17 C16 1.376(3) . ?
C16 C15 1.398(4) . ?
C16 C19 1.517(3) . ?
C15 C14 1.392(3) . ?
