#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/10/4301058.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_4301058
loop_
_publ_author_name
'Adams, Nico'
'Bigmore, Helen R.'
'Blundell, Timothy L.'
'Boyd, Catherine L.'
'Dubberley, Stuart R.'
'Sealey, Andrew J.'
'Cowley, Andrew R.'
'Skinner, Michael E. G.'
'Mountford, Philip'
_publ_section_title
;
 New Titanium Imido Synthons: Syntheses and Supramolecular Structures
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2882
_journal_page_last               2894
_journal_paper_doi               10.1021/ic050011z
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         ' C10 H15 Cl6 N3 Ti1 . 0.5 (C6 H6) '
_chemical_formula_sum            'C13 H18 Cl6 N3 Ti'
_chemical_formula_weight         476.92
_chemical_name_systematic        'Ti(NC6Cl4H)Cl2(NHMe2)2 . 0.5(C6H6)'
_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
_cell_angle_alpha                115.6105(9)
_cell_angle_beta                 90.7721(8)
_cell_angle_gamma                106.112(1)
_cell_formula_units_Z            2
_cell_length_a                   7.3945(1)
_cell_length_b                   12.7544(2)
_cell_length_c                   12.9622(2)
_cell_measurement_reflns_used    4470
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     1046.45(3)
_computing_cell_refinement
; 

 Denzo/Scalepack (Otwinowski & Minor, 1996) 

;
_computing_data_collection
; 

 COLLECT (Nonius BV, 1997) 

;
_computing_data_reduction
; 

 Denzo/Scalepack (Otwinowski & Minor, 1996) 

;
_computing_molecular_graphics
; 

 CAMERON (Watkin et al 1996) 

;
_computing_publication_material
; 

 CRYSTALS (Watkin et al 2001) 

;
_computing_structure_refinement
; 

 CRYSTALS (Watkin et al 2001) 

;
_computing_structure_solution
; 

 SIR97 (Altomare et al, 1999) 

;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
; 

Enraf Nonius Kappa CCD 

;
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.02
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8769
_diffrn_reflns_theta_full        27.386
_diffrn_reflns_theta_max         27.524
_diffrn_reflns_theta_min         2.915
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.175
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 

 Denzo/Scalepack (Otwinowski & Minor, 1996) 

;
_exptl_crystal_colour            ' orange '
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             482.000
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.87
_refine_diff_density_min         -0.62
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0539
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3727
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.009
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;

Method = Prince modified Chebychev polynomial, (Watkin, 1994) 

 W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 

 0.766 0.432 0.436 

;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0521
_refine_ls_wR_factor_gt          0.0408
_refine_ls_wR_factor_ref         0.0408
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              14
_reflns_limit_k_min              -16
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                3728
_reflns_number_total             4805
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ic050011zsi20050104_034133_5.cif
_cod_data_source_block           COMPOUND_11
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic ' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1046.45
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C13 H18 Cl6 N3 Ti1 '
_cod_database_code               4301058
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_occupancy
_atom_site_adp_type
_atom_site_attached_hydrogens
Ti1 Ti 0.03381(5) 0.02529(3) 0.25870(3) 0.0166 1.0000 Uani .
N1 N 0.2427(2) 0.14358(17) 0.30819(16) 0.0217 1.0000 Uani .
N2 N 0.1120(3) -0.09902(17) 0.31267(16) 0.0230 1.0000 Uani .
N3 N -0.1244(2) 0.10460(17) 0.18304(16) 0.0228 1.0000 Uani .
C1 C 0.3980(3) 0.24660(18) 0.35655(18) 0.0190 1.0000 Uani .
C2 C 0.5014(3) 0.28360(19) 0.46549(18) 0.0204 1.0000 Uani .
C3 C 0.6576(3) 0.3892(2) 0.51454(19) 0.0242 1.0000 Uani .
C4 C 0.7136(3) 0.4616(2) 0.4583(2) 0.0257 1.0000 Uani .
C5 C 0.6146(3) 0.42616(19) 0.3514(2) 0.0236 1.0000 Uani .
C6 C 0.4613(3) 0.31910(19) 0.29918(18) 0.0205 1.0000 Uani .
C7 C -0.0380(4) -0.2182(2) 0.2756(2) 0.0353 1.0000 Uani .
C8 C 0.2967(3) -0.1192(2) 0.2838(2) 0.0335 1.0000 Uani .
C9 C -0.3259(3) 0.0309(3) 0.1322(2) 0.0388 1.0000 Uani .
C10 C -0.1112(4) 0.2334(2) 0.2589(2) 0.0321 1.0000 Uani .
Cl1 Cl 0.02846(9) -0.11429(5) 0.06822(5) 0.0305 1.0000 Uani .
Cl2 Cl -0.16605(8) 0.05330(6) 0.39934(5) 0.0298 1.0000 Uani .
Cl3 Cl 0.42852(8) 0.19431(5) 0.53476(5) 0.0291 1.0000 Uani .
Cl4 Cl 0.78693(9) 0.43322(6) 0.64620(5) 0.0360 1.0000 Uani .
Cl5 Cl 0.68878(9) 0.51610(6) 0.28248(6) 0.0364 1.0000 Uani .
Cl6 Cl 0.34607(8) 0.27055(5) 0.16239(5) 0.0285 1.0000 Uani .
H1 H 0.1255 -0.05851 0.38769 0.0284 1.0000 Uiso .
H2 H -0.0632 0.10313 0.12584 0.0289 1.0000 Uiso .
H41 H 0.8244 0.5386 0.4949 0.0279 1.0000 Uiso .
H71 H -0.1622 -0.2040 0.2953 0.0433 1.0000 Uiso .
H72 H -0.0032 -0.2625 0.3164 0.0433 1.0000 Uiso .
H73 H -0.0500 -0.2686 0.1901 0.0433 1.0000 Uiso .
H81 H 0.3975 -0.0384 0.3090 0.0433 1.0000 Uiso .
H82 H 0.3320 -0.1634 0.3246 0.0433 1.0000 Uiso .
H83 H 0.2852 -0.1694 0.1983 0.0433 1.0000 Uiso .
H91 H -0.3338 -0.0561 0.0811 0.0449 1.0000 Uiso .
H92 H -0.4030 0.0343 0.1957 0.0449 1.0000 Uiso .
H93 H -0.3766 0.0646 0.0856 0.0449 1.0000 Uiso .
H101 H 0.0250 0.2826 0.2929 0.0414 1.0000 Uiso .
H102 H -0.1880 0.2372 0.3226 0.0414 1.0000 Uiso .
H103 H -0.1616 0.2675 0.2125 0.0414 1.0000 Uiso .
C11 C -0.0390(12) 0.4258(7) 0.0496(7) 0.0584(18) 0.5000 Uiso .
C12 C 0.1325(13) 0.4994(11) 0.0446(11) 0.093(3) 0.5000 Uiso .
C13 C 0.1293(13) 0.5718(9) -0.013(1) 0.083(3) 0.5000 Uiso .
C14 C -0.0484(11) 0.5608(6) -0.0595(6) 0.0498(15) 0.5000 Uiso .
C15 C -0.2146(13) 0.4863(11) -0.0568(11) 0.101(4) 0.5000 Uiso .
C16 C -0.2119(13) 0.4233(12) 0.0034(12) 0.112(4) 0.5000 Uiso .
H111 H -0.0395 0.3720 0.0873 0.0704 0.5000 Uiso .
H121 H 0.2552 0.5021 0.0805 0.1116 0.5000 Uiso .
H131 H 0.2490 0.6276 -0.019 0.0999 0.5000 Uiso .
H141 H -0.0529 0.6129 -0.0985 0.0597 0.5000 Uiso .
H151 H -0.3367 0.4778 -0.0984 0.1209 0.5000 Uiso .
H161 H -0.3343 0.3749 0.0153 0.1364 0.5000 Uiso .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C   ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'H   ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997
0.0030 International_Tables_Vol_IV_Table_2.2B
'N   ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
'Cl  ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 International_Tables_Vol_IV_Table_2.2B
'Ti  ' 0.2480 0.4460 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050
1.2807 International_Tables_Vol_IV_Table_2.2B
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . Ti1 . N2 . 100.00(8) yes
N1 . Ti1 . N3 . 97.10(8) yes
N2 . Ti1 . N3 . 162.89(7) yes
N1 . Ti1 . Cl1 . 110.54(7) yes
N2 . Ti1 . Cl1 . 87.68(5) yes
N3 . Ti1 . Cl1 . 85.68(5) yes
N1 . Ti1 . Cl2 . 110.92(7) yes
N2 . Ti1 . Cl2 . 86.77(5) yes
N3 . Ti1 . Cl2 . 87.80(5) yes
Cl1 . Ti1 . Cl2 . 138.51(3) yes
Ti1 . N1 . C1 . 173.11(16) yes
Ti1 . N2 . C7 . 114.29(14) yes
Ti1 . N2 . C8 . 115.34(14) yes
C7 . N2 . C8 . 109.81(19) yes
Ti1 . N2 . H1 . 101.57 yes
C7 . N2 . H1 . 108.15 yes
C8 . N2 . H1 . 106.87 yes
Ti1 . N3 . C9 . 115.62(15) yes
Ti1 . N3 . C10 . 114.95(14) yes
C9 . N3 . C10 . 109.86(19) yes
Ti1 . N3 . H2 . 100.74 yes
C9 . N3 . H2 . 106.93 yes
C10 . N3 . H2 . 107.74 yes
N1 . C1 . C2 . 121.04(18) yes
N1 . C1 . C6 . 121.24(18) yes
C2 . C1 . C6 . 117.72(18) yes
C1 . C2 . C3 . 120.62(19) yes
C1 . C2 . Cl3 . 118.11(16) yes
C3 . C2 . Cl3 . 121.28(16) yes
C2 . C3 . C4 . 120.7(2) yes
C2 . C3 . Cl4 . 120.80(18) yes
C4 . C3 . Cl4 . 118.47(16) yes
C3 . C4 . C5 . 119.28(19) yes
C4 . C5 . C6 . 121.0(2) yes
C4 . C5 . Cl5 . 118.45(17) yes
C6 . C5 . Cl5 . 120.57(17) yes
C1 . C6 . C5 . 120.61(19) yes
C1 . C6 . Cl6 . 118.45(15) yes
C5 . C6 . Cl6 . 120.94(16) yes
Ti1 . Cl1 . H2 2_555 135.40 yes
Ti1 . Cl2 . H1 2_556 130.80 yes
N2 . H1 . Cl2 2_556 149.30 yes
N3 . H2 . Cl1 2_555 152.78 yes
C12 . C11 . C16 . 122.2(6) yes
C11 . C12 . C13 . 117.7(6) yes
C12 . C13 . C14 . 116.4(6) yes
C13 . C14 . C15 . 125.4(6) yes
C14 . C15 . C16 . 117.9(6) yes
C11 . C16 . C15 . 120.0(6) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ti1 . N1 . 1.7079(18) yes
Ti1 . N2 . 2.1894(18) yes
Ti1 . N3 . 2.1992(18) yes
Ti1 . Cl1 . 2.3293(6) yes
Ti1 . Cl2 . 2.3319(6) yes
N1 . C1 . 1.367(3) yes
N2 . C7 . 1.480(3) yes
N2 . C8 . 1.483(3) yes
N2 . H1 . 0.870 yes
N3 . C9 . 1.483(3) yes
N3 . C10 . 1.479(3) yes
N3 . H2 . 0.870 yes
C1 . C2 . 1.413(3) yes
C1 . C6 . 1.411(3) yes
C2 . C3 . 1.388(3) yes
C2 . Cl3 . 1.718(2) yes
C3 . C4 . 1.391(3) yes
C3 . Cl4 . 1.724(2) yes
C4 . C5 . 1.382(3) yes
C5 . C6 . 1.389(3) yes
C5 . Cl5 . 1.721(2) yes
C6 . Cl6 . 1.724(2) yes
Cl1 . H2 2_555 2.5922 yes
Cl2 . H1 2_556 2.7428 yes
Ti1 . Ti1 2_555 6.4527(7) yes
Ti1 . Ti1 2_556 6.5720(7) yes
C3 . C5 2_666 3.436(3) yes
C11 . C12 . 1.374(8) yes
C11 . C16 . 1.390(8) yes
C12 . C13 . 1.415(8) yes
C13 . C14 . 1.385(8) yes
C14 . C15 . 1.341(8) yes
C15 . C16 . 1.343(8) yes
