#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/15/7011553.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_7011553
loop_
_publ_author_name
'Liu, Hong-Ke'
'Sun, Wei-Yin'
'Tang, Wen-Xia'
'Tan, Hai-Yan'
'Zhang, Hua-Xin'
'Tong, Ye-Xiang'
'Yu, Xiao-Lan'
'Kang, Bei-Sheng'
_publ_section_title
;
 Assembly of supermolecular complexes with tripodal ligand titmb and
 tib: a 2D rhombic grid network assembled from 2-connected tib
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3886
_journal_paper_doi               10.1039/b201446g
_journal_year                    2002
_chemical_formula_sum            'C18 H22 N6 O2'
_chemical_formula_weight         354.42
_space_group_IT_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.20(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.590(4)
_cell_length_b                   16.384(3)
_cell_length_c                   11.721(2)
_cell_measurement_temperature    293(2)
_cell_volume                     3489.3(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.731
_diffrn_measured_fraction_theta_max 0.731
_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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12786
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.800699
_exptl_absorpt_correction_T_min  1.000000
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.125
_refine_diff_density_rms         0.031
_refine_ls_extinction_coef       0.0021(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0692P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1351
_reflns_number_gt                3724
_reflns_number_total             7487
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b201446g.txt
_cod_data_source_block           ll2
_cod_database_code               7011553
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
_atom_site_disorder_assembly
_atom_site_disorder_group
N9 N 0.07674(9) 0.42519(9) 0.51614(12) 0.0472(4) Uani 1 1 d . . .
C26 C 0.17919(11) 0.36707(11) 0.33770(15) 0.0481(5) Uani 1 1 d . . .
H26A H 0.1336 0.3546 0.2909 0.058 Uiso 1 1 calc R . .
N8 N 0.40245(9) 0.38376(10) 0.66781(12) 0.0506(4) Uani 1 1 d . . .
C25 C 0.18370(11) 0.42671(11) 0.42271(15) 0.0450(5) Uani 1 1 d . . .
C27 C 0.24091(11) 0.32558(11) 0.32069(14) 0.0452(5) Uani 1 1 d . . .
C23 C 0.31476(11) 0.40311(12) 0.47800(15) 0.0474(5) Uani 1 1 d . . .
N11 N 0.22197(10) 0.30215(9) 0.10910(12) 0.0513(4) Uani 1 1 d . . .
N7 N 0.44045(10) 0.29322(11) 0.80612(14) 0.0622(5) Uani 1 1 d . . .
C30 C 0.01195(12) 0.38719(13) 0.48240(18) 0.0592(6) Uani 1 1 d . . .
H30A H -0.0149 0.3869 0.4059 0.071 Uiso 1 1 calc R . .
C28 C 0.30841(11) 0.34393(11) 0.39192(14) 0.0474(5) Uani 1 1 d . . .
H28A H 0.3502 0.3161 0.3818 0.057 Uiso 1 1 calc R . .
C22 C 0.38938(11) 0.42362(13) 0.55289(15) 0.0584(6) Uani 1 1 d . . .
H22A H 0.4274 0.4069 0.5124 0.070 Uiso 1 1 calc R . .
H22B H 0.3930 0.4823 0.5638 0.070 Uiso 1 1 calc R . .
C33 C 0.23472(12) 0.26338(11) 0.22375(15) 0.0555(6) Uani 1 1 d . . .
H33A H 0.2797 0.2316 0.2353 0.067 Uiso 1 1 calc R . .
H33B H 0.1945 0.2264 0.2268 0.067 Uiso 1 1 calc R . .
C24 C 0.25225(12) 0.44442(11) 0.49157(15) 0.0500(5) Uani 1 1 d . . .
H24A H 0.2562 0.4850 0.5481 0.060 Uiso 1 1 calc R . .
C32 C 0.04537(14) 0.36621(13) 0.66355(18) 0.0634(6) Uani 1 1 d . . .
H32A H 0.0462 0.3478 0.7389 0.076 Uiso 1 1 calc R . .
N10 N -0.00953(10) 0.35040(11) 0.56865(16) 0.0679(5) Uani 1 1 d . . .
C35 C 0.15964(13) 0.30123(14) 0.02781(18) 0.0670(6) Uani 1 1 d . . .
H35A H 0.1179 0.2721 0.0352 0.080 Uiso 1 1 calc R . .
C29 C 0.11582(11) 0.47063(12) 0.44040(17) 0.0551(5) Uani 1 1 d . . .
H29A H 0.1297 0.5237 0.4746 0.066 Uiso 1 1 calc R . .
H29B H 0.0831 0.4792 0.3652 0.066 Uiso 1 1 calc R . .
C20 C 0.41121(12) 0.35911(13) 0.85125(17) 0.0633(6) Uani 1 1 d . . .
H20A H 0.4080 0.3646 0.9290 0.076 Uiso 1 1 calc R . .
C21 C 0.43407(12) 0.31114(13) 0.69506(17) 0.0587(6) Uani 1 1 d . . .
H21A H 0.4498 0.2771 0.6416 0.070 Uiso 1 1 calc R . .
N12 N 0.16361(14) 0.34584(13) -0.06374(16) 0.0827(7) Uani 1 1 d . . .
C19 C 0.38776(12) 0.41487(13) 0.76801(16) 0.0601(6) Uani 1 1 d . . .
H19A H 0.3658 0.4648 0.7770 0.072 Uiso 1 1 calc R . .
C31 C 0.09809(13) 0.41212(13) 0.63273(16) 0.0615(6) Uani 1 1 d . . .
H31A H 0.1408 0.4312 0.6817 0.074 Uiso 1 1 calc R . .
C34 C 0.26947(15) 0.35103(14) 0.06748(19) 0.0711(7) Uani 1 1 d . . .
H34A H 0.3174 0.3641 0.1043 0.085 Uiso 1 1 calc R . .
C36 C 0.23281(19) 0.37682(15) -0.0384(2) 0.0823(8) Uani 1 1 d . . .
H36A H 0.2524 0.4111 -0.0873 0.099 Uiso 1 1 calc R . .
N5 N 0.07802(9) 0.56948(9) 0.00188(13) 0.0510(4) Uani 1 1 d . . .
C7 C 0.22453(13) 0.67852(11) 0.33658(15) 0.0484(5) Uani 1 1 d . . .
N3 N 0.23455(11) 0.68456(10) 0.55054(14) 0.0544(5) Uani 1 1 d . . .
C5 C 0.29809(11) 0.63085(11) 0.20349(16) 0.0465(5) Uani 1 1 d . . .
C9 C 0.17295(12) 0.58467(11) 0.18236(15) 0.0450(5) Uani 1 1 d . . .
C10 C 0.23864(13) 0.58431(11) 0.14661(16) 0.0498(5) Uani 1 1 d . . .
H10B H 0.2435 0.5523 0.0831 0.060 Uiso 1 1 calc R . .
C8 C 0.16617(11) 0.63245(11) 0.27743(15) 0.0490(5) Uani 1 1 d . . .
H8A H 0.1217 0.6334 0.3017 0.059 Uiso 1 1 calc R . .
N2 N 0.40823(9) 0.55222(10) 0.18574(15) 0.0552(5) Uani 1 1 d . . .
C6 C 0.28982(13) 0.67698(11) 0.29850(16) 0.0523(6) Uani 1 1 d . . .
H6A H 0.3293 0.7078 0.3379 0.063 Uiso 1 1 calc R . .
N4 N 0.29695(13) 0.61968(10) 0.70454(15) 0.0643(5) Uani 1 1 d . . .
N6 N 0.04778(11) 0.58225(12) -0.18966(15) 0.0754(6) Uani 1 1 d . . .
C13 C 0.30104(12) 0.65897(12) 0.60822(17) 0.0555(5) Uani 1 1 d . . .
H13A H 0.3446 0.6679 0.5831 0.067 Uiso 1 1 calc R . .
C11 C 0.21794(14) 0.73003(13) 0.44050(16) 0.0715(7) Uani 1 1 d . . .
H11A H 0.2514 0.7760 0.4458 0.086 Uiso 1 1 calc R . .
H11B H 0.1683 0.7515 0.4288 0.086 Uiso 1 1 calc R . .
C17 C 0.04667(13) 0.64419(13) -0.0215(2) 0.0696(7) Uani 1 1 d . . .
H17A H 0.0389 0.6830 0.0325 0.084 Uiso 1 1 calc R . .
N1 N 0.46349(10) 0.43805(11) 0.15427(17) 0.0709(5) Uani 1 1 d . . .
C15 C 0.10892(12) 0.53495(14) 0.11732(16) 0.0633(6) Uani 1 1 d . . .
H15A H 0.1252 0.4795 0.1082 0.076 Uiso 1 1 calc R . .
H15B H 0.0709 0.5329 0.1626 0.076 Uiso 1 1 calc R . .
C16 C 0.07704(12) 0.53472(13) -0.10223(17) 0.0613(6) Uani 1 1 d . . .
H16A H 0.0951 0.4827 -0.1112 0.074 Uiso 1 1 calc R . .
C3 C 0.43059(13) 0.50455(14) 0.1080(2) 0.0657(6) Uani 1 1 d . . .
H3A H 0.4236 0.5172 0.0291 0.079 Uiso 1 1 calc R . .
C4 C 0.37043(13) 0.63051(12) 0.1640(2) 0.0659(6) Uani 1 1 d . . .
H4B H 0.3614 0.6425 0.0812 0.079 Uiso 1 1 calc R . .
H4C H 0.4019 0.6731 0.2049 0.079 Uiso 1 1 calc R . .
C18 C 0.02921(12) 0.65068(14) -0.1377(2) 0.0729(7) Uani 1 1 d . . .
H18A H 0.0072 0.6963 -0.1778 0.088 Uiso 1 1 calc R . .
C12 C 0.18506(14) 0.65996(15) 0.6136(2) 0.0684(7) Uani 1 1 d . . .
H12B H 0.1345 0.6686 0.5956 0.082 Uiso 1 1 calc R . .
C2 C 0.46206(13) 0.44486(15) 0.2703(2) 0.0728(7) Uani 1 1 d . . .
H2A H 0.4815 0.4066 0.3271 0.087 Uiso 1 1 calc R . .
C14 C 0.22395(17) 0.62049(14) 0.7076(2) 0.0706(7) Uani 1 1 d . . .
H14A H 0.2039 0.5971 0.7662 0.085 Uiso 1 1 calc R . .
C1 C 0.42885(13) 0.51417(15) 0.2908(2) 0.0733(7) Uani 1 1 d . . .
H1B H 0.4214 0.5326 0.3624 0.088 Uiso 1 1 calc R . .
O1W O 0.53946(8) 0.20391(9) 0.98045(12) 0.0721(4) Uani 1 1 d . . .
O2W O 0.58169(9) 0.34602(10) 0.11064(13) 0.0866(5) Uani 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 0.0000 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'
O O 0.0106 0.0060 '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
C30 N9 C31 106.11(18) . . ?
C30 N9 C29 126.01(16) . . ?
C31 N9 C29 127.87(18) . . ?
C27 C26 C25 121.60(17) . . ?
C21 N8 C19 106.62(16) . . ?
C21 N8 C22 126.44(18) . . ?
C19 N8 C22 126.89(17) . . ?
C26 C25 C24 118.32(18) . . ?
C26 C25 C29 120.75(17) . . ?
C24 C25 C29 120.92(17) . . ?
C26 C27 C28 118.66(17) . . ?
C26 C27 C33 120.36(17) . . ?
C28 C27 C33 120.96(18) . . ?
C24 C23 C28 118.79(17) . . ?
C24 C23 C22 120.93(18) . . ?
C28 C23 C22 120.25(19) . . ?
C35 N11 C34 106.41(19) . . ?
C35 N11 C33 126.8(2) . . ?
C34 N11 C33 126.62(17) . . ?
C21 N7 C20 104.30(18) . . ?
N10 C30 N9 112.82(18) . . ?
C27 C28 C23 121.16(19) . . ?
N8 C22 C23 112.73(16) . . ?
N11 C33 C27 111.72(15) . . ?
C23 C24 C25 121.45(17) . . ?
C31 C32 N10 110.42(19) . . ?
C30 N10 C32 104.13(19) . . ?
N12 C35 N11 112.7(2) . . ?
N9 C29 C25 112.25(16) . . ?
C19 C20 N7 110.60(18) . . ?
N7 C21 N8 112.25(19) . . ?
C35 N12 C36 104.1(2) . . ?
C20 C19 N8 106.23(19) . . ?
C32 C31 N9 106.51(19) . . ?
C36 C34 N11 105.9(2) . . ?
C34 C36 N12 110.8(2) . . ?
C16 N5 C17 106.01(17) . . ?
C16 N5 C15 127.01(17) . . ?
C17 N5 C15 126.95(18) . . ?
C6 C7 C8 118.62(18) . . ?
C6 C7 C11 119.93(19) . . ?
C8 C7 C11 121.5(2) . . ?
C13 N3 C12 106.9(2) . . ?
C13 N3 C11 127.0(2) . . ?
C12 N3 C11 126.1(2) . . ?
C6 C5 C10 118.3(2) . . ?
C6 C5 C4 120.44(19) . . ?
C10 C5 C4 121.28(19) . . ?
C10 C9 C8 118.99(17) . . ?
C10 C9 C15 120.08(18) . . ?
C8 C9 C15 120.9(2) . . ?
C9 C10 C5 121.29(18) . . ?
C7 C8 C9 121.0(2) . . ?
C3 N2 C1 106.35(17) . . ?
C3 N2 C4 127.22(18) . . ?
C1 N2 C4 126.4(2) . . ?
C7 C6 C5 121.78(18) . . ?
C13 N4 C14 104.82(19) . . ?
C16 N6 C18 104.09(17) . . ?
N4 C13 N3 111.7(2) . . ?
N3 C11 C7 112.87(16) . . ?
C18 C17 N5 106.2(2) . . ?
C3 N1 C2 103.8(2) . . ?
N5 C15 C9 111.78(16) . . ?
N6 C16 N5 112.47(19) . . ?
N1 C3 N2 113.0(2) . . ?
N2 C4 C5 112.13(17) . . ?
C17 C18 N6 111.2(2) . . ?
C14 C12 N3 106.2(2) . . ?
C1 C2 N1 110.7(2) . . ?
C12 C14 N4 110.3(2) . . ?
C2 C1 N2 106.2(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
N9 C30 1.339(2) . ?
N9 C31 1.357(2) . ?
N9 C29 1.464(2) . ?
C26 C27 1.384(3) . ?
C26 C25 1.385(2) . ?
N8 C21 1.336(2) . ?
N8 C19 1.360(2) . ?
N8 C22 1.470(2) . ?
C25 C24 1.387(3) . ?
C25 C29 1.504(3) . ?
C27 C28 1.385(3) . ?
C27 C33 1.512(2) . ?
C23 C24 1.383(3) . ?
C23 C28 1.386(2) . ?
C23 C22 1.514(3) . ?
N11 C35 1.336(3) . ?
N11 C34 1.357(3) . ?
N11 C33 1.460(2) . ?
N7 C21 1.315(2) . ?
N7 C20 1.365(3) . ?
C30 N10 1.310(3) . ?
C32 C31 1.344(3) . ?
C32 N10 1.366(3) . ?
C35 N12 1.313(3) . ?
C20 C19 1.340(3) . ?
N12 C36 1.356(3) . ?
C34 C36 1.351(3) . ?
N5 C16 1.343(2) . ?
N5 C17 1.358(2) . ?
N5 C15 1.467(2) . ?
C7 C6 1.379(3) . ?
C7 C8 1.382(3) . ?
C7 C11 1.508(3) . ?
N3 C13 1.344(2) . ?
N3 C12 1.358(3) . ?
N3 C11 1.465(3) . ?
C5 C6 1.381(3) . ?
C5 C10 1.391(3) . ?
C5 C4 1.512(3) . ?
C9 C10 1.372(3) . ?
C9 C8 1.389(3) . ?
C9 C15 1.509(3) . ?
N2 C3 1.331(3) . ?
N2 C1 1.361(2) . ?
N2 C4 1.459(2) . ?
N4 C13 1.316(3) . ?
N4 C14 1.365(3) . ?
N6 C16 1.310(2) . ?
N6 C18 1.355(3) . ?
C17 C18 1.336(3) . ?
N1 C3 1.309(3) . ?
N1 C2 1.371(3) . ?
C12 C14 1.348(3) . ?
C2 C1 1.338(3) . ?
