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#$Date: 2016-03-22 10:32:06 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178874 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/03/4110304.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_4110304
loop_
_publ_author_name
'Antek G. Wong-Foy'
'Olivier Lebel'
'Adam J. Matzger'
_publ_contact_author_address
;Department of Chemistry
University of Michigan
930 N. University Ave.
Ann Arbor, MI 48109
;
_publ_contact_author_email       matzger@umich.edu
_publ_contact_author_name        'Adam J. Matzger'
_publ_section_title
;
 Porous Crystal Derived from a Tricarboxylate Linker with Two Distinct
 Binding Motifs
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15740
_journal_page_last               15741
_journal_paper_doi               10.1021/ja0753952
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C30 H18 Cu3 O14'
_chemical_formula_sum            'C30 H14 Cu3 O14'
_chemical_formula_weight         793.10
_chemical_name_common            UMCM-150
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           194
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      194
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   18.3532(11)
_cell_length_b                   18.3532(11)
_cell_length_c                   40.667(3)
_cell_measurement_reflns_used    24515
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      66.7
_cell_measurement_theta_min      6.5
_cell_volume                     11863.1(13)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'CrystalClear 1.4'
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku RAXIS-SPIDER'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.1370
_diffrn_reflns_av_sigmaI/netI    0.1071
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            44060
_diffrn_reflns_theta_full        66.59
_diffrn_reflns_theta_max         66.59
_diffrn_reflns_theta_min         6.53
_exptl_absorpt_coefficient_mu    1.182
_exptl_absorpt_correction_T_max  0.7979
_exptl_absorpt_correction_T_min  0.7979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    0.666
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2358
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
;
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         3899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1576
_refine_ls_R_factor_gt           0.0898
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1912
_refine_ls_wR_factor_ref         0.2217
_reflns_number_gt                2360
_reflns_number_total             3899
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0753952-file003.cif
_cod_data_source_block           UMCM150
_cod_original_cell_volume        11862.9(14)
_cod_database_code               4110304
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-x+y, y, z'
'y, x, z+1/2'
'x, x-y, z'
'x-y, -y, z+1/2'
'-y, -x, z'
'-x, -x+y, z+1/2'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'
'x-y, -y, -z'
'-y, -x, -z-1/2'
'-x, -x+y, -z'
'-x+y, y, -z-1/2'
'y, x, -z'
'x, x-y, -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
Cu1 Cu 0.52432(3) 0.47568(3) 0.52559(2) 0.0355(3) Uani 1 2 d S . .
Cu2 Cu 0.88530(9) 0.94265(5) 0.2500 0.0482(5) Uani 1 4 d S . .
O1 O 0.4127(2) 0.4378(2) 0.54367(8) 0.0494(10) Uani 1 1 d . . .
O2 O 0.5753(3) 0.4247(3) 0.56540(16) 0.163(3) Uani 1 2 d S . .
O3 O 0.62914(18) 0.51978(19) 0.50058(8) 0.0489(10) Uani 1 1 d . . .
O4A O 0.8913(17) 0.891(2) 0.2888(4) 0.077(5) Uani 0.53(4) 1 d P A 1
O4B O 0.8649(9) 0.8463(16) 0.2785(5) 0.044(6) Uani 0.47(4) 1 d P A 2
C1 C 0.6398(3) 0.5514(3) 0.47155(12) 0.0411(13) Uani 1 1 d . . .
C2 C 0.7223(3) 0.5776(3) 0.45686(12) 0.0431(14) Uani 1 1 d . . .
C3 C 0.7785(2) 0.5570(4) 0.47077(16) 0.0460(19) Uani 1 2 d S . .
H1 H 0.7639 0.5278 0.4906 0.055 Uiso 1 2 calc SR . .
C4 C 0.7454(3) 0.6211(3) 0.42802(11) 0.0511(14) Uani 1 1 d . . .
H2 H 0.7091 0.6362 0.4182 0.061 Uiso 1 1 calc R . .
C5 C 0.8219(2) 0.6439(5) 0.41280(17) 0.053(2) Uani 1 2 d S . .
C6 C 0.8479(3) 0.6957(6) 0.3816(2) 0.062(2) Uani 1 2 d S . .
C7 C 0.8974(3) 0.7947(5) 0.32460(19) 0.054(2) Uani 1 2 d S . .
C8 C 0.9244(3) 0.8487(5) 0.29520(19) 0.047(2) Uani 1 2 d S . .
C9A C 0.9008(11) 0.6877(13) 0.3583(4) 0.073(5) Uani 0.49(2) 1 d P B 1
H3A H 0.9188 0.6491 0.3617 0.088 Uiso 0.49(2) 1 calc PR B 1
C10A C 0.9264(11) 0.7403(13) 0.3294(4) 0.071(6) Uani 0.49(2) 1 d P B 1
H4A H 0.9625 0.7371 0.3142 0.085 Uiso 0.49(2) 1 calc PR B 1
C9B C 0.8198(12) 0.7475(16) 0.3745(4) 0.086(8) Uani 0.51(2) 1 d P . 2
H3B H 0.7831 0.7518 0.3891 0.103 Uiso 0.51(2) 1 calc PR B 2
C10B C 0.8424(12) 0.7948(14) 0.3467(4) 0.084(7) Uani 0.51(2) 1 d P . 2
H4B H 0.8190 0.8287 0.3427 0.101 Uiso 0.51(2) 1 calc PR B 2
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'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
O1 Cu1 O1 89.5(2) . 11_665
O1 Cu1 O3 169.73(14) . .
O1 Cu1 O3 90.08(14) 11_665 .
O1 Cu1 O3 90.08(14) . 11_665
O1 Cu1 O3 169.73(14) 11_665 11_665
O3 Cu1 O3 88.53(19) . 11_665
O1 Cu1 O2 99.16(19) . .
O1 Cu1 O2 99.15(19) 11_665 .
O3 Cu1 O2 91.05(19) . .
O3 Cu1 O2 91.05(19) 11_665 .
O1 Cu1 Cu1 86.79(10) . 13_666
O1 Cu1 Cu1 86.80(10) 11_665 13_666
O3 Cu1 Cu1 82.93(10) . 13_666
O3 Cu1 Cu1 82.93(10) 11_665 13_666
O2 Cu1 Cu1 171.6(2) . 13_666
O4A Cu2 O4A 64.7(18) . 9_565
O4A Cu2 O4A 174.1(17) . 24_566
O4A Cu2 O4A 115.0(17) 9_565 24_566
O4A Cu2 O4A 115.0(17) . 16_556
O4A Cu2 O4A 174.1(17) 9_565 16_556
O4A Cu2 O4A 64.7(18) 24_566 16_556
O4A Cu2 O4B 86.8(16) . 9_565
O4A Cu2 O4B 24.6(4) 9_565 9_565
O4A Cu2 O4B 94.2(18) 24_566 9_565
O4A Cu2 O4B 157.8(4) 16_556 9_565
O4A Cu2 O4B 157.8(4) . 24_566
O4A Cu2 O4B 94.2(18) 9_565 24_566
O4A Cu2 O4B 24.6(4) 24_566 24_566
O4A Cu2 O4B 86.8(16) 16_556 24_566
O4B Cu2 O4B 71.3(17) 9_565 24_566
O4A Cu2 O4B 24.6(4) . .
O4A Cu2 O4B 86.7(16) 9_565 .
O4A Cu2 O4B 157.8(4) 24_566 .
O4A Cu2 O4B 94.2(18) 16_556 .
O4B Cu2 O4B 105.5(16) 9_565 .
O4B Cu2 O4B 161.2(8) 24_566 .
O4A Cu2 O4B 94.2(18) . 16_556
O4A Cu2 O4B 157.8(4) 9_565 16_556
O4A Cu2 O4B 86.8(16) 24_566 16_556
O4A Cu2 O4B 24.6(4) 16_556 16_556
O4B Cu2 O4B 161.2(8) 9_565 16_556
O4B Cu2 O4B 105.5(16) 24_566 16_556
O4B Cu2 O4B 71.3(17) . 16_556
C1 O1 Cu1 121.1(3) 13_666 .
C1 O3 Cu1 124.0(3) . .
C8 O4A Cu2 132.1(11) . .
C8 O4B Cu2 120.3(12) . .
O1 C1 O3 125.1(5) 13_666 .
O1 C1 C2 120.1(4) 13_666 .
O3 C1 C2 114.9(5) . .
C4 C2 C3 117.2(5) . .
C4 C2 C1 120.7(5) . .
C3 C2 C1 122.1(5) . .
C2 C3 C2 123.6(7) . 7_655
C2 C3 H1 118.2 . .
C2 C3 H1 118.2 7_655 .
C2 C4 C5 122.0(5) . .
C2 C4 H2 119.0 . .
C5 C4 H2 119.0 . .
C4 C5 C4 118.1(6) . 7_655
C4 C5 C6 120.9(3) . .
C4 C5 C6 120.9(3) 7_655 .
C9B C6 C9B 97.3(19) . 7_655
C9B C6 C9A 49.9(8) . 7_655
C9B C6 C9A 117.6(9) 7_655 7_655
C9B C6 C9A 117.6(9) . .
C9B C6 C9A 49.9(8) 7_655 .
C9A C6 C9A 95.1(15) 7_655 .
C9B C6 C5 121.5(7) . .
C9B C6 C5 121.5(7) 7_655 .
C9A C6 C5 120.8(8) 7_655 .
C9A C6 C5 120.8(7) . .
C10B C7 C10B 96.7(16) . 7_655
C10B C7 C10A 48.6(7) . 7_655
C10B C7 C10A 118.2(9) 7_655 7_655
C10B C7 C10A 118.2(9) . .
C10B C7 C10A 48.6(7) 7_655 .
C10A C7 C10A 98.7(16) 7_655 .
C10B C7 C8 122.6(7) . .
C10B C7 C8 122.6(7) 7_655 .
C10A C7 C8 119.2(7) 7_655 .
C10A C7 C8 119.2(7) . .
O4A C8 O4A 108(3) . 7_655
O4A C8 O4B 38.8(6) . .
O4A C8 O4B 125.9(8) 7_655 .
O4A C8 O4B 125.9(8) . 7_655
O4A C8 O4B 38.8(6) 7_655 7_655
O4B C8 O4B 115(2) . 7_655
O4A C8 C7 119.4(7) . .
O4A C8 C7 119.4(7) 7_655 .
O4B C8 C7 114.7(6) . .
O4B C8 C7 114.7(6) 7_655 .
C6 C9A C10A 119.2(12) . .
C6 C9A H3A 120.4 . .
C10A C9A H3A 120.4 . .
C7 C10A C9A 119.4(11) . .
C7 C10A H4A 120.3 . .
C9A C10A H4A 120.3 . .
C6 C9B C10B 122.5(12) . .
C6 C9B C9B 41.4(9) . 7_655
C10B C9B C9B 90.8(9) . 7_655
C6 C9B H3B 118.7 . .
C10B C9B H3B 118.7 . .
C9B C9B H3B 140.0 7_655 .
C7 C10B C9B 122.8(12) . .
C7 C10B C10B 41.7(8) . 7_655
C9B C10B C10B 89.2(8) . 7_655
C7 C10B H4B 118.6 . .
C9B C10B H4B 118.6 . .
C10B C10B H4B 142.7 7_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.948(3) .
Cu1 O1 1.948(3) 11_665
Cu1 O3 1.958(3) .
Cu1 O3 1.958(3) 11_665
Cu1 O2 2.291(7) .
Cu1 Cu1 2.5927(17) 13_666
Cu2 O4A 1.873(11) .
Cu2 O4A 1.873(11) 9_565
Cu2 O4A 1.873(11) 24_566
Cu2 O4A 1.873(11) 16_556
Cu2 O4B 1.986(13) 9_565
Cu2 O4B 1.986(13) 24_566
Cu2 O4B 1.986(13) .
Cu2 O4B 1.987(13) 16_556
O1 C1 1.242(5) 13_666
O3 C1 1.286(5) .
O4A C8 1.228(13) .
O4B C8 1.268(13) .
C1 O1 1.242(5) 13_666
C1 C2 1.468(6) .
C2 C4 1.362(6) .
C2 C3 1.384(5) .
C3 C2 1.384(5) 7_655
C3 H1 0.9300 .
C4 C5 1.394(6) .
C4 H2 0.9300 .
C5 C4 1.394(6) 7_655
C5 C6 1.512(9) .
C6 C9B 1.320(16) .
C6 C9B 1.320(16) 7_655
C6 C9A 1.415(17) 7_655
C6 C9A 1.415(17) .
C7 C10B 1.351(14) .
C7 C10B 1.351(14) 7_655
C7 C10A 1.361(16) 7_655
C7 C10A 1.361(15) .
C7 C8 1.472(9) .
C8 O4A 1.228(13) 7_655
C8 O4B 1.268(13) 7_655
C9A C10A 1.443(18) .
C9A H3A 0.9300 .
C10A H4A 0.9300 .
C9B C10B 1.360(17) .
C9B C9B 1.98(3) 7_655
C9B H3B 0.9300 .
C10B C10B 2.02(3) 7_655
C10B H4B 0.9300 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O1 Cu1 O1 C1 84.8(4) 11_665 13_666
O3 Cu1 O1 C1 -2.8(10) . 13_666
O3 Cu1 O1 C1 -84.9(4) 11_665 13_666
O2 Cu1 O1 C1 -176.0(4) . 13_666
Cu1 Cu1 O1 C1 -2.0(4) 13_666 13_666
O1 Cu1 O3 C1 -1.0(10) . .
O1 Cu1 O3 C1 -88.5(4) 11_665 .
O3 Cu1 O3 C1 81.3(4) 11_665 .
O2 Cu1 O3 C1 172.4(4) . .
Cu1 Cu1 O3 C1 -1.7(4) 13_666 .
O4A Cu2 O4A C8 -146(3) 9_565 .
O4A Cu2 O4A C8 -58(3) 24_566 .
O4A Cu2 O4A C8 27(5) 16_556 .
O4B Cu2 O4A C8 -158(3) 9_565 .
O4B Cu2 O4A C8 -165.8(13) 24_566 .
O4B Cu2 O4A C8 62(2) . .
O4B Cu2 O4A C8 41(4) 16_556 .
O4A Cu2 O4B C8 -47.5(14) . .
O4A Cu2 O4B C8 -73.1(11) 9_565 .
O4A Cu2 O4B C8 119(4) 24_566 .
O4A Cu2 O4B C8 101(3) 16_556 .
O4B Cu2 O4B C8 -89.2(16) 9_565 .
O4B Cu2 O4B C8 -167(2) 24_566 .
O4B Cu2 O4B C8 110(2) 16_556 .
Cu1 O3 C1 O1 4.0(7) . 13_666
Cu1 O3 C1 C2 -177.7(3) . .
O1 C1 C2 C4 6.4(8) 13_666 .
O3 C1 C2 C4 -172.0(5) . .
O1 C1 C2 C3 -171.3(5) 13_666 .
O3 C1 C2 C3 10.3(8) . .
C4 C2 C3 C2 -0.6(11) . 7_655
C1 C2 C3 C2 177.1(4) . 7_655
C3 C2 C4 C5 0.5(9) . .
C1 C2 C4 C5 -177.3(6) . .
C2 C4 C5 C4 -0.3(12) . 7_655
C2 C4 C5 C6 -177.2(7) . .
C4 C5 C6 C9B 26.7(19) . .
C4 C5 C6 C9B -150.1(16) 7_655 .
C4 C5 C6 C9B 150.1(16) . 7_655
C4 C5 C6 C9B -26.7(19) 7_655 7_655
C4 C5 C6 C9A -32.4(16) . 7_655
C4 C5 C6 C9A 150.8(13) 7_655 7_655
C4 C5 C6 C9A -150.9(13) . .
C4 C5 C6 C9A 32.4(16) 7_655 .
Cu2 O4A C8 O4A 58(5) . 7_655
Cu2 O4A C8 O4B -67(2) . .
Cu2 O4A C8 O4B 19(6) . 7_655
Cu2 O4A C8 C7 -161(2) . .
Cu2 O4B C8 O4A 48.4(13) . .
Cu2 O4B C8 O4A -25(5) . 7_655
Cu2 O4B C8 O4B -69(3) . 7_655
Cu2 O4B C8 C7 155.2(11) . .
C10B C7 C8 O4A -6(3) . .
C10B C7 C8 O4A -131(2) 7_655 .
C10A C7 C8 O4A 51(3) 7_655 .
C10A C7 C8 O4A 172(2) . .
C10B C7 C8 O4A 131(2) . 7_655
C10B C7 C8 O4A 6(3) 7_655 7_655
C10A C7 C8 O4A -172(2) 7_655 7_655
C10A C7 C8 O4A -51(3) . 7_655
C10B C7 C8 O4B -49(2) . .
C10B C7 C8 O4B -174(2) 7_655 .
C10A C7 C8 O4B 8(2) 7_655 .
C10A C7 C8 O4B 128.5(19) . .
C10B C7 C8 O4B 174(2) . 7_655
C10B C7 C8 O4B 49(2) 7_655 7_655
C10A C7 C8 O4B -128(2) 7_655 7_655
C10A C7 C8 O4B -8(2) . 7_655
C9B C6 C9A C10A 4(3) . .
C9B C6 C9A C10A -70.8(15) 7_655 .
C9A C6 C9A C10A 51(2) 7_655 .
C5 C6 C9A C10A -177.9(10) . .
C10B C7 C10A C9A -3(3) . .
C10B C7 C10A C9A 70.1(13) 7_655 .
C10A C7 C10A C9A -50(2) 7_655 .
C8 C7 C10A C9A 179.4(11) . .
C6 C9A C10A C7 -2(2) . .
C9B C6 C9B C10B 46(3) 7_655 .
C9A C6 C9B C10B -74.6(18) 7_655 .
C9A C6 C9B C10B -3(3) . .
C5 C6 C9B C10B 179.8(13) . .
C9A C6 C9B C9B -120.2(17) 7_655 7_655
C9A C6 C9B C9B -48.2(10) . 7_655
C5 C6 C9B C9B 134(2) . 7_655
C10B C7 C10B C9B -41(3) 7_655 .
C10A C7 C10B C9B 80.7(19) 7_655 .
C10A C7 C10B C9B 5(3) . .
C8 C7 C10B C9B -177.3(13) . .
C10A C7 C10B C10B 122.0(15) 7_655 7_655
C10A C7 C10B C10B 46.1(10) . 7_655
C8 C7 C10B C10B -136(2) . 7_655
C6 C9B C10B C7 -2(3) . .
C9B C9B C10B C7 26.0(18) 7_655 .
C6 C9B C10B C10B -28(2) . 7_655
C9B C9B C10B C10B -0.005(10) 7_655 7_655
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.041 -0.027 0.000 8171.9 -1.4
