#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:14:31 +0100 (vie 25 de mar de 2016) $
#$Revision: 180067 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/13/7051380.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_7051380
loop_
_publ_author_name
'Carmalt, Claire J.'
'Mileham, John D.'
'White, Andrew J. P.'
'Williams, David J.'
_publ_section_title
;
 Synthesis and characterisation of a bridging nitrido complex of
 titanium
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              929
_journal_paper_doi               10.1039/b008211m
_journal_volume                  24
_journal_year                    2000
_chemical_formula_sum            'C46 H61 Cl13 N6 Ti2'
_chemical_formula_weight         1254.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 107.11(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.101(6)
_cell_length_b                   14.916(3)
_cell_length_c                   17.108(4)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      10.84
_cell_volume                     6122(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4606
_diffrn_reflns_theta_max         60.00
_diffrn_reflns_theta_min         3.49
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.719
_exptl_absorpt_correction_T_max  0.6053
_exptl_absorpt_correction_T_min  0.1342
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       'hexagonal needles'
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.048
_refine_ls_goodness_of_fit_obs   1.084
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         4268
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.084
_refine_ls_restrained_S_obs      1.084
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_obs          0.0664
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1142P)²+18.2158P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1897
_refine_ls_wR_factor_obs         0.1702
_reflns_number_observed          3653
_reflns_number_total             4490
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b008211m.txt
_cod_data_source_block           CC0002
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' 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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1142P)^2^+18.2158P] 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^)+(0.1142P)^2^+18.2158P] 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        6121.5(24)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7051380
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ti1 Ti 0.0000 0.08488(7) 0.2500 0.0217(3) Uani 1 d S .
Ti2 Ti 0.0000 0.32415(7) 0.2500 0.0236(3) Uani 1 d S .
Cl1 Cl 0.0000 -0.08261(10) 0.2500 0.0375(4) Uani 1 d S .
Cl2 Cl -0.09417(5) 0.07776(7) 0.17234(7) 0.0332(3) Uani 1 d . .
Cl3 Cl -0.07182(5) 0.34441(8) 0.12793(7) 0.0352(3) Uani 1 d . .
N1 N 0.0000 0.2060(3) 0.2500 0.0253(11) Uani 1 d S .
N2 N 0.0000 0.4837(4) 0.2500 0.045(2) Uani 1 d S .
N3 N 0.0249(2) 0.0821(2) 0.1373(2) 0.0264(8) Uani 1 d . .
N4 N 0.0610(2) 0.3306(3) 0.1800(2) 0.0296(9) Uani 1 d . .
C1 C -0.0463(3) 0.5292(4) 0.2453(4) 0.0512(15) Uani 1 d . .
H1A H -0.0800(3) 0.4974(4) 0.2398(4) 0.061 Uiso 1 calc R .
C2 C -0.0467(4) 0.6237(4) 0.2482(4) 0.072(2) Uani 1 d . .
C3 C 0.0000 0.6696(6) 0.2500 0.078(4) Uani 1 d S .
H3A H 0.0000 0.7333(6) 0.2500 0.093 Uiso 1 calc SR .
C4 C -0.1013(5) 0.6695(6) 0.2455(7) 0.120(5) Uani 1 d . .
H4A H -0.1171(5) 0.6406(6) 0.2851(7) 0.180 Uiso 1 d R .
H4B H -0.1276(5) 0.6642(6) 0.1905(7) 0.180 Uiso 1 d R .
H4C H -0.0946(5) 0.7331(6) 0.2595(7) 0.180 Uiso 1 d R .
C5 C 0.0654(2) 0.0278(3) 0.1284(3) 0.0290(10) Uani 1 d . .
H5A H 0.0828(2) -0.0120(3) 0.1718(3) 0.035 Uiso 1 calc R .
C6 C 0.0829(2) 0.0270(4) 0.0588(3) 0.0348(11) Uani 1 d . .
C7 C 0.0570(2) 0.0857(4) -0.0039(3) 0.0374(12) Uani 1 d . .
H7A H 0.0674(2) 0.0861(4) -0.0530(3) 0.045 Uiso 1 calc R .
C8 C 0.0159(2) 0.1435(3) 0.0048(3) 0.0339(11) Uani 1 d . .
C9 C 0.0011(2) 0.1390(3) 0.0764(3) 0.0302(10) Uani 1 d . .
H9A H -0.0273(2) 0.1781(3) 0.0828(3) 0.036 Uiso 1 calc R .
C10 C 0.1287(3) -0.0352(5) 0.0533(4) 0.053(2) Uani 1 d . .
H10A H 0.1219(3) -0.0951(5) 0.0720(4) 0.079 Uiso 1 d R .
H10B H 0.1646(3) -0.0127(5) 0.0879(4) 0.079 Uiso 1 d R .
H10C H 0.1296(3) -0.0386(5) -0.0035(4) 0.079 Uiso 1 d R .
C11 C -0.0128(3) 0.2084(4) -0.0613(4) 0.053(2) Uani 1 d . .
H11A H -0.0287(3) 0.1756(4) -0.1125(4) 0.079 Uiso 1 d R .
H11B H 0.0141(3) 0.2527(4) -0.0690(4) 0.079 Uiso 1 d R .
H11C H -0.0426(3) 0.2391(4) -0.0457(4) 0.079 Uiso 1 d R .
C12 C 0.1048(2) 0.2733(3) 0.2008(3) 0.0331(11) Uani 1 d . .
H12A H 0.1099(2) 0.2362(3) 0.2476(3) 0.040 Uiso 1 calc R .
C13 C 0.1424(2) 0.2670(4) 0.1559(3) 0.0395(12) Uani 1 d . .
C14 C 0.1355(3) 0.3223(4) 0.0895(4) 0.0495(14) Uani 1 d . .
H14A H 0.1615(3) 0.3201(4) 0.0590(4) 0.059 Uiso 1 calc R .
C15 C 0.0907(3) 0.3814(4) 0.0665(4) 0.0478(14) Uani 1 d . .
C16 C 0.0549(2) 0.3829(4) 0.1138(3) 0.0394(12) Uani 1 d . .
H16A H 0.0241(2) 0.4231(4) 0.0990(3) 0.047 Uiso 1 calc R .
C17 C 0.1897(3) 0.2012(4) 0.1809(5) 0.056(2) Uani 1 d . .
H17A H 0.2246(3) 0.2331(4) 0.2064(5) 0.083 Uiso 1 d R .
H17B H 0.1928(3) 0.1690(4) 0.1325(5) 0.083 Uiso 1 d R .
H17C H 0.1825(3) 0.1583(4) 0.2200(5) 0.083 Uiso 1 d R .
C18 C 0.0807(4) 0.4422(6) -0.0066(5) 0.083(3) Uani 1 d . .
H18A H 0.1165(4) 0.4585(6) -0.0147(5) 0.124 Uiso 1 d R .
H18B H 0.0614(4) 0.4965(6) 0.0025(5) 0.124 Uiso 1 d R .
H18C H 0.0577(4) 0.4109(6) -0.0552(5) 0.124 Uiso 1 d R .
C20 C 0.1638(4) 0.8866(5) 0.3657(6) 0.079(2) Uani 1 d . .
H20A H 0.1233(4) 0.8774(5) 0.3400(6) 0.095 Uiso 0.60 calc PR 1
H20B H 0.1685(4) 0.9423(5) 0.3985(6) 0.095 Uiso 0.60 calc PR 1
H20C H 0.1796(4) 0.9417(5) 0.3912(6) 0.095 Uiso 0.40 d PR 2
H20D H 0.1240(4) 0.8899(5) 0.3541(6) 0.095 Uiso 0.40 d PR 2
Cl21 Cl 0.18998(14) 0.7974(2) 0.4301(2) 0.1038(9) Uani 1 d . .
Cl22 Cl 0.1952(4) 0.8994(6) 0.2913(4) 0.110(3) Uani 0.60 d P 1
Cl23 Cl 0.1886(8) 0.8646(12) 0.2719(15) 0.219(11) Uani 0.40 d P 2
C30 C 0.2938(4) 0.9452(7) 0.1052(8) 0.106(4) Uani 1 d . .
H30A H 0.3306(4) 0.9239(7) 0.1023(8) 0.127 Uiso 1 calc R .
H30B H 0.2656(4) 0.8994(7) 0.0793(8) 0.127 Uiso 1 calc R .
Cl31 Cl 0.27791(11) 1.0427(2) 0.0538(2) 0.1072(8) Uani 1 d . .
Cl32 Cl 0.29590(15) 0.9586(3) 0.2090(3) 0.158(2) Uani 1 d . .
C40 C 0.3179(9) 0.8145(17) -0.0888(15) 0.140(11) Uani 0.50 d PD 1
H40A H 0.3164(80) 0.7741(91) -0.1345(90) 0.210 Uiso 0.50 calc PR 1
H40B H 0.3563(19) 0.8179(156) -0.0528(41) 0.210 Uiso 0.50 calc PR 1
H40C H 0.3054(62) 0.8744(71) -0.1099(128) 0.210 Uiso 0.50 calc PR 1
C41 C 0.2835(4) 0.7823(7) -0.0451(6) 0.123(5) Uani 1 d D .
H41A H 0.3071(4) 0.8049(7) -0.0749(6) 0.147 Uiso 0.50 calc PR 2
C42 C 0.3049(3) 0.7256(6) 0.0210(6) 0.110(4) Uani 1 d D .
H42A H 0.3430(3) 0.7081(6) 0.0345(6) 0.133 Uiso 1 calc R .
C43 C 0.2724(4) 0.6939(6) 0.0677(6) 0.129(6) Uani 1 d D .
H43A H 0.2878(4) 0.6568(6) 0.1139(6) 0.155 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 '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
N1 Ti1 N3 91.07(9) . . ?
N1 Ti1 N3 91.07(9) . 2 ?
N3 Ti1 N3 177.9(2) . 2 ?
N1 Ti1 Cl2 92.59(4) . 2 ?
N3 Ti1 Cl2 89.80(11) . 2 ?
N3 Ti1 Cl2 90.11(11) 2 2 ?
N1 Ti1 Cl2 92.59(4) . . ?
N3 Ti1 Cl2 90.11(11) . . ?
N3 Ti1 Cl2 89.80(11) 2 . ?
Cl2 Ti1 Cl2 174.82(7) 2 . ?
N1 Ti1 Cl1 180.0 . . ?
N3 Ti1 Cl1 88.93(9) . . ?
N3 Ti1 Cl1 88.93(9) 2 . ?
Cl2 Ti1 Cl1 87.41(4) 2 . ?
Cl2 Ti1 Cl1 87.41(4) . . ?
N1 Ti2 N4 92.49(10) . . ?
N1 Ti2 N4 92.49(10) . 2 ?
N4 Ti2 N4 175.0(2) . 2 ?
N1 Ti2 Cl3 97.41(4) . 2 ?
N4 Ti2 Cl3 90.18(11) . 2 ?
N4 Ti2 Cl3 89.18(11) 2 2 ?
N1 Ti2 Cl3 97.41(4) . . ?
N4 Ti2 Cl3 89.18(11) . . ?
N4 Ti2 Cl3 90.18(11) 2 . ?
Cl3 Ti2 Cl3 165.18(8) 2 . ?
N1 Ti2 N2 180.0 . . ?
N4 Ti2 N2 87.51(10) . . ?
N4 Ti2 N2 87.51(10) 2 . ?
Cl3 Ti2 N2 82.59(4) 2 . ?
Cl3 Ti2 N2 82.59(4) . . ?
Ti2 N1 Ti1 180.0 . . ?
C1 N2 C1 118.5(7) 2 . ?
C1 N2 Ti2 120.8(4) 2 . ?
C1 N2 Ti2 120.8(4) . . ?
C9 N3 C5 118.3(4) . . ?
C9 N3 Ti1 119.5(3) . . ?
C5 N3 Ti1 122.1(3) . . ?
C16 N4 C12 118.0(4) . . ?
C16 N4 Ti2 123.7(3) . . ?
C12 N4 Ti2 118.0(3) . . ?
N2 C1 C2 121.7(7) . . ?
C3 C2 C1 119.4(8) . . ?
C3 C2 C4 122.8(7) . . ?
C1 C2 C4 117.7(9) . . ?
C2 C3 C2 119.1(9) 2 . ?
N3 C5 C6 123.0(5) . . ?
C5 C6 C7 117.5(5) . . ?
C5 C6 C10 120.2(5) . . ?
C7 C6 C10 122.3(5) . . ?
C8 C7 C6 120.3(4) . . ?
C9 C8 C7 117.9(5) . . ?
C9 C8 C11 120.2(5) . . ?
C7 C8 C11 121.9(5) . . ?
N3 C9 C8 122.9(5) . . ?
N4 C12 C13 122.0(5) . . ?
C14 C13 C12 118.5(5) . . ?
C14 C13 C17 121.7(5) . . ?
C12 C13 C17 119.8(5) . . ?
C13 C14 C15 120.7(5) . . ?
C16 C15 C14 117.3(5) . . ?
C16 C15 C18 120.0(6) . . ?
C14 C15 C18 122.8(5) . . ?
N4 C16 C15 123.5(5) . . ?
Cl22 C20 Cl21 113.0(5) . . ?
Cl21 C20 Cl23 104.2(6) . . ?
Cl31 C30 Cl32 111.0(6) . . ?
C40 C41 C43 120.1(12) . 7_565 ?
C40 C41 C42 119.8(11) . . ?
C43 C41 C42 120.1(7) 7_565 . ?
C43 C42 C41 121.7(6) . . ?
C42 C43 C41 118.2(7) . 7_565 ?
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 N1 1.806(5) . ?
Ti1 N3 2.196(4) . ?
Ti1 N3 2.196(4) 2 ?
Ti1 Cl2 2.3486(13) 2 ?
Ti1 Cl2 2.3486(13) . ?
Ti1 Cl1 2.498(2) . ?
Ti2 N1 1.763(5) . ?
Ti2 N4 2.206(4) . ?
Ti2 N4 2.206(4) 2 ?
Ti2 Cl3 2.3425(14) 2 ?
Ti2 Cl3 2.3425(14) . ?
Ti2 N2 2.380(6) . ?
N2 C1 1.327(7) 2 ?
N2 C1 1.327(7) . ?
N3 C9 1.340(6) . ?
N3 C5 1.342(6) . ?
N4 C16 1.347(7) . ?
N4 C12 1.355(7) . ?
C1 C2 1.410(9) . ?
C2 C3 1.351(10) . ?
C2 C4 1.520(14) . ?
C3 C2 1.351(10) 2 ?
C5 C6 1.386(7) . ?
C6 C7 1.390(8) . ?
C6 C10 1.502(8) . ?
C7 C8 1.385(8) . ?
C8 C9 1.384(7) . ?
C8 C11 1.503(8) . ?
C12 C13 1.384(7) . ?
C13 C14 1.372(8) . ?
C13 C17 1.503(8) . ?
C14 C15 1.391(9) . ?
C15 C16 1.376(8) . ?
C15 C18 1.504(9) . ?
C20 Cl22 1.694(10) . ?
C20 Cl21 1.728(8) . ?
C20 Cl23 1.91(2) . ?
C30 Cl31 1.685(12) . ?
C30 Cl32 1.773(13) . ?
C40 C41 1.384(10) . ?
C41 C43 1.387(8) 7_565 ?
C41 C42 1.387(8) . ?
C42 C43 1.384(9) . ?
C43 C41 1.387(8) 7_565 ?
