#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:10:53 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179470 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/67/4336740.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_4336740
loop_
_publ_author_name
'Klaus Pokorny'
'Matthias Schmeisser'
'Frank Hampel'
'Achim Zahl'
'Ralph Puchta'
'Rudi van Eldik'
_publ_contact_author_name
;
;
_publ_section_title
;
 Coordination of Terpyridine to Li+ in Two Different Ionic Liquids
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13167
_journal_page_last               13178
_journal_paper_doi               10.1021/ic4020724
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C30 H22 Cl2 Li2 N6 O8'
_chemical_formula_sum            'C30 H22 Cl2 Li2 N6 O8'
_chemical_formula_weight         679.32
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2012-05-08
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.05.04 svn.r2321, GUI svn.r4222)
;
_cell_angle_alpha                103.254(8)
_cell_angle_beta                 108.437(8)
_cell_angle_gamma                108.812(9)
_cell_formula_units_Z            1
_cell_length_a                   8.6325(7)
_cell_length_b                   9.6777(11)
_cell_length_c                   10.5904(9)
_cell_measurement_reflns_used    2008
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      24.9995
_cell_measurement_theta_min      3.3385
_cell_volume                     738.47(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'J. Appl. Cryst. (2007). 40, 609-613'
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector_area_resol_mean 10.6144
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega    3.00  107.00   1.0000    7.9700
omega____ theta____ kappa____ phi______ frames
    -       21.8076   57.0000   60.0000 104

  2 omega   -5.00   99.00   1.0000    7.9700
omega____ theta____ kappa____ phi______ frames
    -       21.8076   57.0000 -180.0000 104

  3 omega  -21.00   83.00   1.0000    7.9700
omega____ theta____ kappa____ phi______ frames
    -       21.8076   77.0000  -60.0000 104
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0178299000
_diffrn_orient_matrix_UB_12      -0.0747345000
_diffrn_orient_matrix_UB_13      0.0054523000
_diffrn_orient_matrix_UB_21      -0.0506745000
_diffrn_orient_matrix_UB_22      -0.0366910000
_diffrn_orient_matrix_UB_23      -0.0753319000
_diffrn_orient_matrix_UB_31      0.0793444000
_diffrn_orient_matrix_UB_32      0.0028030000
_diffrn_orient_matrix_UB_33      -0.0080407000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3692
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.35
_diffrn_source                   'SuperNova (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    0.284
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.956
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       block
_exptl_crystal_F_000             348
_exptl_crystal_recrystallization_method 'crystallized from [emim]ClO4'
_exptl_crystal_size_max          0.3412
_exptl_crystal_size_mid          0.2438
_exptl_crystal_size_min          0.0664
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0427
_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)+(0.0424P)²+0.2806P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1132
_reflns_number_gt                2084
_reflns_number_total             2600
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4020724_si_001.cif
_cod_data_source_block           ac_ms01
_cod_original_cell_volume        738.47(12)
_cod_database_code               4336740
#BEGIN Tags that were not found in dictionaries:
_chemical_oxdiff_formula         'C30 H22 Cl Li N6 O4'
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.01
#END Tags that were not found in dictionaries
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Li1 Li 0.9701(6) 0.8416(5) 0.6159(4) 0.0355(10) Uani 1 1 d .
C12 C 0.7104(3) 0.9195(3) 0.7512(3) 0.0355(6) Uani 1 1 d .
H12 H 0.6766 0.9569 0.6785 0.043 Uiso 1 1 calc R
C13 C 0.6359(3) 0.9319(3) 0.8494(3) 0.0385(6) Uani 1 1 d .
H13 H 0.5561 0.9782 0.8437 0.046 Uiso 1 1 calc R
C14 C 0.6835(3) 0.8737(3) 0.9552(3) 0.0397(6) Uani 1 1 d .
H14 H 0.6354 0.8796 1.0223 0.048 Uiso 1 1 calc R
C15 C 0.8029(3) 0.8067(3) 0.9612(3) 0.0367(6) Uani 1 1 d .
H15 H 0.8354 0.7660 1.0317 0.044 Uiso 1 1 calc R
C16 C 0.8740(3) 0.8005(3) 0.8604(2) 0.0299(6) Uani 1 1 d .
C22 C 1.0047(3) 0.7316(3) 0.8585(2) 0.0305(6) Uani 1 1 d .
C23 C 1.0793(3) 0.6765(3) 0.9620(3) 0.0380(6) Uani 1 1 d .
H23 H 1.0485 0.6809 1.0390 0.046 Uiso 1 1 calc R
C24 C 1.1991(4) 0.6154(3) 0.9482(3) 0.0424(7) Uani 1 1 d .
H24 H 1.2520 0.5799 1.0171 0.051 Uiso 1 1 calc R
C25 C 1.2405(3) 0.6068(3) 0.8322(3) 0.0401(6) Uani 1 1 d .
H25 H 1.3191 0.5635 0.8205 0.048 Uiso 1 1 calc R
C26 C 1.1623(3) 0.6645(3) 0.7328(3) 0.0313(6) Uani 1 1 d .
C32 C 1.1978(3) 0.6643(3) 0.6037(2) 0.0310(6) Uani 1 1 d .
C33 C 1.3004(3) 0.5925(3) 0.5639(3) 0.0422(7) Uani 1 1 d .
H33 H 1.3461 0.5378 0.6154 0.051 Uiso 1 1 calc R
C34 C 1.3329(4) 0.6044(3) 0.4462(3) 0.0460(7) Uani 1 1 d .
H34 H 1.4023 0.5587 0.4183 0.055 Uiso 1 1 calc R
C35 C 1.2622(3) 0.6838(3) 0.3708(3) 0.0438(7) Uani 1 1 d .
H35 H 1.2841 0.6943 0.2922 0.053 Uiso 1 1 calc R
C36 C 1.1576(4) 0.7479(3) 0.4143(3) 0.0404(6) Uani 1 1 d .
H36 H 1.1073 0.7996 0.3615 0.048 Uiso 1 1 calc R
N11 N 0.8279(3) 0.8568(2) 0.7554(2) 0.0309(5) Uani 1 1 d .
N21 N 1.0485(3) 0.7265(2) 0.74713(19) 0.0291(5) Uani 1 1 d .
N31 N 1.1247(3) 0.7396(2) 0.5286(2) 0.0340(5) Uani 1 1 d .
O1 O 0.7491(3) 0.7945(3) 0.4424(2) 0.0731(8) Uani 1 1 d .
O2 O 0.6265(3) 0.6766(2) 0.1959(2) 0.0715(7) Uani 1 1 d .
O3 O 0.8742(2) 0.9224(2) 0.31136(18) 0.0394(5) Uani 1 1 d .
O4 O 0.5885(3) 0.8933(3) 0.2951(3) 0.0690(7) Uani 1 1 d .
Cl1 Cl 0.70964(8) 0.82243(7) 0.31237(6) 0.0322(2) 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'
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 0.0060 '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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-12 0 8 0.1038 -12.0000 0.0000 8.0000 0.2576 0.0054 -1.0165
2 -13 7 0.1727 2.0000 -13.0000 7.0000 0.9741 -0.1517 0.0660
-1 13 -2 0.1625 -1.0000 13.0000 -2.0000 -0.9646 -0.2756 -0.0268
-2 1 14 0.0358 -2.0000 1.0000 14.0000 0.0373 -0.9900 -0.2685
12 -1 -7 0.1006 12.0000 -1.0000 -7.0000 -0.1774 -0.0441 1.0056
-2 -12 5 0.1585 -2.0000 -12.0000 5.0000 0.9597 0.1650 -0.2325
11 -5 2 0.1391 11.0000 -5.0000 2.0000 0.1884 -0.5246 0.8427
5 2 -15 0.0405 5.0000 2.0000 -15.0000 -0.3204 0.8032 0.5229
7 -13 -2 0.1774 7.0000 -13.0000 -2.0000 0.8358 0.2729 0.5351
-7 13 2 0.1774 -7.0000 13.0000 2.0000 -0.8358 -0.2729 -0.5351
-5 -2 15 0.0419 -5.0000 -2.0000 15.0000 0.3204 -0.8032 -0.5229
5 1 -15 0.0441 5.0000 1.0000 -15.0000 -0.2457 0.8399 0.5201
-5 -1 15 0.0441 -5.0000 -1.0000 15.0000 0.2457 -0.8399 -0.5201
3 -6 -11 0.0938 3.0000 -6.0000 -11.0000 0.3349 0.8968 0.3097
-3 6 11 0.0938 -3.0000 6.0000 11.0000 -0.3349 -0.8968 -0.3097
5 0 -14 0.0332 5.0000 -0.0000 -14.0000 -0.1655 0.8013 0.5093
-5 0 14 0.0332 -5.0000 0.0000 14.0000 0.1655 -0.8013 -0.5093
11 -4 0 0.1187 11.0000 -4.0000 -0.0000 0.1028 -0.4107 0.8616
-11 4 0 0.1187 -11.0000 4.0000 0.0000 -0.1028 0.4107 -0.8616
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
N21 Li1 N11 75.48(15) . .
N21 Li1 N31 75.88(16) . .
N31 Li1 N11 150.5(2) . .
O1 Li1 N11 91.77(18) . .
O1 Li1 N21 136.7(2) . .
O1 Li1 N31 104.4(2) . .
O1 Li1 O3 105.9(2) . 2_776
O3 Li1 N11 95.93(18) 2_776 .
O3 Li1 N21 116.4(2) 2_776 .
O3 Li1 N31 102.87(19) 2_776 .
N11 C12 C13 123.7(2) . .
C14 C13 C12 118.0(2) . .
C13 C14 C15 119.6(2) . .
C14 C15 C16 119.1(2) . .
C15 C16 C22 123.1(2) . .
N11 C16 C15 122.0(2) . .
N11 C16 C22 114.9(2) . .
C23 C22 C16 124.4(2) . .
N21 C22 C16 114.4(2) . .
N21 C22 C23 121.2(2) . .
C24 C23 C22 118.8(2) . .
C23 C24 C25 119.9(2) . .
C24 C25 C26 118.6(3) . .
C25 C26 C32 123.9(2) . .
N21 C26 C25 121.7(2) . .
N21 C26 C32 114.4(2) . .
C33 C32 C26 122.7(2) . .
N31 C32 C26 115.2(2) . .
N31 C32 C33 122.1(2) . .
C34 C33 C32 118.6(3) . .
C35 C34 C33 119.6(3) . .
C34 C35 C36 118.4(3) . .
N31 C36 C35 123.4(3) . .
C12 N11 Li1 127.9(2) . .
C12 N11 C16 117.7(2) . .
C16 N11 Li1 114.4(2) . .
C22 N21 Li1 120.0(2) . .
C26 N21 Li1 119.68(19) . .
C26 N21 C22 119.7(2) . .
C32 N31 Li1 114.27(19) . .
C36 N31 Li1 128.0(2) . .
C36 N31 C32 117.7(2) . .
Cl1 O1 Li1 137.62(18) . .
Cl1 O3 Li1 136.50(16) . 2_776
O1 Cl1 O3 109.91(12) . .
O2 Cl1 O1 108.90(15) . .
O2 Cl1 O3 109.37(13) . .
O4 Cl1 O1 110.83(15) . .
O4 Cl1 O2 108.11(15) . .
O4 Cl1 O3 109.69(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Li1 N11 2.208(4) .
Li1 N21 2.057(5) .
Li1 N31 2.197(5) .
Li1 O1 2.015(5) .
Li1 O3 2.043(5) 2_776
C12 C13 1.387(3) .
C12 N11 1.333(3) .
C13 C14 1.374(4) .
C14 C15 1.377(4) .
C15 C16 1.389(3) .
C16 C22 1.487(3) .
C16 N11 1.352(3) .
C22 C23 1.394(3) .
C22 N21 1.343(3) .
C23 C24 1.375(4) .
C24 C25 1.376(4) .
C25 C26 1.393(4) .
C26 C32 1.492(3) .
C26 N21 1.335(3) .
C32 C33 1.394(3) .
C32 N31 1.345(3) .
C33 C34 1.382(4) .
C34 C35 1.370(4) .
C35 C36 1.380(4) .
C36 N31 1.341(3) .
O1 Cl1 1.4209(19) .
O2 Cl1 1.420(2) .
O3 Li1 2.043(5) 2_776
O3 Cl1 1.4428(17) .
O4 Cl1 1.413(2) .
