#------------------------------------------------------------------------------
#$Date: 2015-07-11 00:58:09 +0300 (Sat, 11 Jul 2015) $
#$Revision: 143626 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/51/7035125.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_7035125
loop_
_publ_author_name
'Pedrosa, Sergio'
'Vidal, Fernando'
'Lee, Lucia Myongwon'
'Vargas-Baca, Ignacio'
'Gómez-Sal, Pilar'
'Mosquera, Marta E. G.'
_publ_section_title
;
 Imido-pyridine Ti(iv) compounds: synthesis of unusual imido-amido
 heterobimetallic derivatives.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11119
_journal_page_last               11128
_journal_paper_doi               10.1039/c5dt01320h
_journal_volume                  44
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C22 H32 Cl2 Li2 N6 O1'
_chemical_formula_sum            'C22 H32 Cl2 Li2 N6 O'
_chemical_formula_weight         481.32
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2014-10-20T12:57:23-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-03-27 deposited with the CCDC.
2015-05-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.46(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.457(11)
_cell_length_b                   28.056(8)
_cell_length_c                   9.083(7)
_cell_measurement_reflns_used    234
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      3.13
_cell_measurement_wavelength     0.71073
_cell_volume                     2621(4)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.01
_diffrn_orient_matrix_UB_12      0
_diffrn_orient_matrix_UB_13      0
_diffrn_orient_matrix_UB_21      0
_diffrn_orient_matrix_UB_22      0.01
_diffrn_orient_matrix_UB_23      0
_diffrn_orient_matrix_UB_31      0
_diffrn_orient_matrix_UB_32      0
_diffrn_orient_matrix_UB_33      0.01
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1527
_diffrn_reflns_av_unetI/netI     0.0684
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            37790
_diffrn_reflns_theta_full        25.57
_diffrn_reflns_theta_max         25.57
_diffrn_reflns_theta_min         3.1
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.22
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.514
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.201
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         4882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0670P)²+2.8382P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1516
_refine_ls_wR_factor_ref         0.1797
_reflns_number_gt                3274
_reflns_number_total             4882
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c5dt01320h1.cif
_cod_data_source_block           3b
_cod_depositor_comments
'Adding full bibliography for 7035122--7035125.cif.'
_cod_original_cell_volume        2621(3)
_cod_database_code               7035125
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Li1 Li -0.2874(6) -0.3713(2) 0.9306(7) 0.0345(13) Uani 1 1 d .
Li2 Li -0.0379(6) -0.3725(2) 0.8148(6) 0.0324(13) Uani 1 1 d .
Cl1 Cl -0.15774(9) -0.30601(3) 0.88123(10) 0.0385(3) Uani 1 1 d .
Cl2 Cl -0.17896(9) -0.43598(3) 0.84699(10) 0.0353(3) Uani 1 1 d .
N3 N -0.0025(3) -0.36214(10) 0.6052(3) 0.0289(6) Uani 1 1 d .
N5 N 0.1361(3) -0.38017(10) 0.9540(3) 0.0316(7) Uani 1 1 d .
O1 O -0.4535(3) -0.36981(9) 0.8003(3) 0.0476(7) Uani 1 1 d .
N6 N 0.1412(3) -0.46233(11) 0.9501(3) 0.0423(8) Uani 1 1 d .
H6A H 0.0747 -0.4621 0.8788 0.051 Uiso 1 1 calc R
H6B H 0.1753 -0.489 0.9835 0.051 Uiso 1 1 calc R
N4 N 0.0071(3) -0.27955(12) 0.6102(4) 0.0426(8) Uani 1 1 d .
N1 N -0.3065(3) -0.37066(10) 1.1507(3) 0.0349(7) Uani 1 1 d .
N2 N -0.2983(4) -0.28858(13) 1.1760(5) 0.0450(9) Uani 1 1 d .
C7 C 0.0100(3) -0.32184(12) 0.5327(4) 0.0304(8) Uani 1 1 d .
C11 C 0.0025(4) -0.40329(13) 0.5316(4) 0.0327(8) Uani 1 1 d .
C13 C 0.1928(4) -0.42034(12) 1.0102(4) 0.0329(8) Uani 1 1 d .
C17 C 0.1899(4) -0.33883(14) 1.0082(4) 0.0378(9) Uani 1 1 d .
C8 C 0.0292(4) -0.32205(14) 0.3858(4) 0.0392(9) Uani 1 1 d .
C14 C 0.3030(4) -0.41980(16) 1.1224(5) 0.0428(10) Uani 1 1 d .
C10 C 0.0185(4) -0.40701(13) 0.3861(4) 0.0377(9) Uani 1 1 d .
C9 C 0.0311(4) -0.36456(15) 0.3141(5) 0.0425(10) Uani 1 1 d .
C16 C 0.2957(4) -0.33473(14) 1.1184(5) 0.0451(10) Uani 1 1 d .
C15 C 0.3526(4) -0.37713(16) 1.1761(5) 0.0492(11) Uani 1 1 d .
C19 C -0.5329(5) -0.41100(19) 0.7652(7) 0.0597(13) Uani 1 1 d .
C22 C -0.5295(5) -0.3287(2) 0.7574(7) 0.0671(15) Uani 1 1 d .
C21 C -0.6379(5) -0.34394(19) 0.6433(7) 0.0844(18) Uani 1 1 d .
H21A H -0.628 -0.3317 0.5461 0.101 Uiso 1 1 calc R
H21B H -0.7192 -0.3321 0.6662 0.101 Uiso 1 1 calc R
C20 C -0.6376(5) -0.39647(18) 0.6421(7) 0.0815(18) Uani 1 1 d .
H20A H -0.7208 -0.4088 0.6579 0.098 Uiso 1 1 calc R
H20B H -0.6209 -0.4084 0.5471 0.098 Uiso 1 1 calc R
C12 C 0.0182(6) -0.45445(18) 0.3095(6) 0.0587(12) Uani 1 1 d .
C18 C 0.3470(5) -0.28653(16) 1.1759(7) 0.0732(15) Uani 1 1 d .
H18A H 0.4218 -0.2908 1.2534 0.11 Uiso 1 1 calc R
H18B H 0.2807 -0.2697 1.2154 0.11 Uiso 1 1 calc R
H18C H 0.3711 -0.2685 1.0953 0.11 Uiso 1 1 calc R
C5 C -0.3045(3) -0.33238(13) 1.2398(4) 0.0343(8) Uani 1 1 d .
C1 C -0.3166(4) -0.41357(14) 1.2116(5) 0.0386(9) Uani 1 1 d .
C4 C -0.3123(4) -0.33739(16) 1.3900(4) 0.0430(10) Uani 1 1 d .
C2 C -0.3243(4) -0.42180(15) 1.3575(4) 0.0433(10) Uani 1 1 d .
C3 C -0.3212(4) -0.38196(17) 1.4476(5) 0.0464(11) Uani 1 1 d .
C6 C -0.3328(8) -0.4713(2) 1.4175(8) 0.0704(16) Uani 1 1 d .
H11 H -0.010(4) -0.4313(13) 0.588(4) 0.036(10) Uiso 1 1 d .
H9 H 0.040(5) -0.3668(16) 0.218(6) 0.074(16) Uiso 1 1 d .
H4 H -0.315(4) -0.3086(14) 1.444(4) 0.044(11) Uiso 1 1 d .
H1 H -0.318(4) -0.4381(13) 1.144(4) 0.036(10) Uiso 1 1 d .
H3 H -0.326(4) -0.3878(14) 1.546(5) 0.046(11) Uiso 1 1 d .
H14 H 0.331(4) -0.4496(15) 1.161(4) 0.046(11) Uiso 1 1 d .
H4B H -0.020(5) -0.2543(17) 0.546(5) 0.064(14) Uiso 1 1 d .
H17 H 0.146(4) -0.3112(13) 0.968(4) 0.034(10) Uiso 1 1 d .
H4A H -0.029(4) -0.2789(14) 0.687(5) 0.039(12) Uiso 1 1 d .
H2B H -0.276(4) -0.2659(15) 1.230(5) 0.044(13) Uiso 1 1 d .
H2A H -0.267(5) -0.2880(15) 1.087(5) 0.060(14) Uiso 1 1 d .
H8 H 0.039(4) -0.2907(14) 0.341(4) 0.038(10) Uiso 1 1 d .
H6D H -0.305(7) -0.496(2) 1.354(8) 0.11(2) Uiso 1 1 d .
H6E H -0.270(8) -0.473(3) 1.518(9) 0.15(3) Uiso 1 1 d .
H6C H -0.406(7) -0.481(3) 1.412(8) 0.12(3) Uiso 1 1 d .
H12C H -0.035(5) -0.4780(19) 0.350(6) 0.081(17) Uiso 1 1 d .
H12B H -0.022(7) -0.452(2) 0.193(8) 0.13(2) Uiso 1 1 d .
H12A H 0.107(7) -0.468(2) 0.324(7) 0.12(2) Uiso 1 1 d .
H22A H -0.483(7) -0.303(3) 0.743(8) 0.13(3) Uiso 1 1 d .
H19A H -0.484(5) -0.4376(19) 0.746(6) 0.078(17) Uiso 1 1 d .
H22B H -0.562(6) -0.318(2) 0.855(7) 0.11(2) Uiso 1 1 d .
H19B H -0.567(7) -0.415(2) 0.854(7) 0.11(2) Uiso 1 1 d .
H15 H 0.432(6) -0.3765(18) 1.267(6) 0.093(17) Uiso 1 1 d .
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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 '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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 -2 0.065
3 0 1 0.251
-8 -5 6 0.265
1 -4 7 0.099
0 9 -10 0.127
4 -12 13 0.14
0 -1 -7 0.1
0 1 7 0.068
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O1 Li1 N1 111.4(3)
O1 Li1 Cl2 104.8(3)
N1 Li1 Cl2 117.6(3)
O1 Li1 Cl1 110.6(3)
N1 Li1 Cl1 109.8(3)
Cl2 Li1 Cl1 102.1(2)
O1 Li1 Li2 122.3(3)
N1 Li1 Li2 126.2(3)
Cl2 Li1 Li2 50.95(16)
Cl1 Li1 Li2 51.36(16)
N3 Li2 N5 107.7(3)
N3 Li2 Cl2 116.7(3)
N5 Li2 Cl2 110.6(3)
N3 Li2 Cl1 108.6(3)
N5 Li2 Cl1 112.2(3)
Cl2 Li2 Cl1 100.9(2)
N3 Li2 Li1 130.5(3)
N5 Li2 Li1 121.6(3)
Cl2 Li2 Li1 50.22(16)
Cl1 Li2 Li1 50.89(16)
Li1 Cl1 Li2 77.8(2)
Li1 Cl2 Li2 78.8(2)
C7 N3 C11 118.0(3)
C7 N3 Li2 129.9(3)
C11 N3 Li2 112.0(3)
C13 N5 C17 117.6(3)
C13 N5 Li2 127.9(3)
C17 N5 Li2 113.9(3)
C22 O1 C19 108.9(4)
C22 O1 Li1 126.1(3)
C19 O1 Li1 123.1(3)
C1 N1 C5 117.7(3)
C1 N1 Li1 115.2(3)
C5 N1 Li1 127.1(3)
N3 C7 N4 117.7(3)
N3 C7 C8 121.3(3)
N4 C7 C8 121.0(3)
N3 C11 C10 124.9(3)
N5 C13 N6 117.4(3)
N5 C13 C14 121.5(3)
N6 C13 C14 121.0(3)
N5 C17 C16 125.1(4)
C9 C8 C7 118.8(4)
C15 C14 C13 118.9(4)
C11 C10 C9 115.6(3)
C11 C10 C12 121.7(4)
C9 C10 C12 122.6(4)
C8 C9 C10 121.3(4)
C17 C16 C15 116.2(4)
C17 C16 C18 121.4(4)
C15 C16 C18 122.3(4)
C14 C15 C16 120.6(4)
O1 C19 C20 105.6(4)
O1 C22 C21 106.4(4)
C22 C21 C20 107.3(4)
C19 C20 C21 105.9(4)
N1 C5 N2 117.5(3)
N1 C5 C4 120.9(4)
N2 C5 C4 121.6(4)
N1 C1 C2 125.3(4)
C3 C4 C5 119.3(4)
C1 C2 C3 116.1(4)
C1 C2 C6 121.9(4)
C3 C2 C6 122.0(4)
C4 C3 C2 120.6(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Li1 O1 1.916(7)
Li1 N1 2.045(7)
Li1 Cl2 2.338(6)
Li1 Cl1 2.370(6)
Li1 Li2 2.985(9)
Li2 N3 2.025(6)
Li2 N5 2.030(7)
Li2 Cl2 2.363(6)
Li2 Cl1 2.386(6)
N3 C7 1.327(4)
N3 C11 1.340(4)
N5 C13 1.331(4)
N5 C17 1.343(5)
O1 C22 1.416(5)
O1 C19 1.425(5)
N6 C13 1.368(5)
N4 C7 1.383(5)
N1 C1 1.337(5)
N1 C5 1.342(5)
N2 C5 1.365(5)
C7 C8 1.385(5)
C11 C10 1.366(5)
C13 C14 1.393(6)
C17 C16 1.356(6)
C8 C9 1.361(6)
C14 C15 1.360(6)
C10 C9 1.377(6)
C10 C12 1.502(6)
C16 C15 1.389(6)
C16 C18 1.513(6)
C19 C20 1.473(7)
C22 C21 1.454(7)
C21 C20 1.474(7)
C5 C4 1.389(5)
C1 C2 1.362(6)
C4 C3 1.365(6)
C2 C3 1.383(6)
C2 C6 1.502(7)
