##############################################################################
# #
# This CIF contains the data in a paper accepted for publication in #
# Acta Crystallographica Section E. It conforms to the requirements of #
# Notes for Authors for Acta Crystallographica Section E, and has been #
# peer reviewed under the auspices of the IUCr Commission on Journals. #
# #
# Full details of the Crystallographic Information File format #
# are given in the paper "The Crystallographic Information File (CIF): #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H. #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. #
# #
# The current version of the core CIF dictionary is obtainable from #
# ftp://ftp.iucr.org/pub/cif_core.dic. #
# #
# Software is freely available for graphical display of the structure(s) #
# in this CIF. For information consult the CIF software page #
# http://www.iucr.org/resources/cif/software. #
# #
# This file may be used for bona fide research purposes within the #
# scientific community so long as proper attribution is given to the journal #
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##############################################################################
data_I
_audit_creation_method 'SHELXL-2016/6'
_chemical_name_systematic
;
Dichloro-tetrakis[\m-4-(ammoniomethyl)cyclohexane-1-carboxylato-\
O,O']dicopper(II) dichloride hexahydrate
;
_chemical_name_common ?
_chemical_formula_moiety 'C32 H60 Cl2 Cu2 N4 O8, 2(Cl), 6(H2 O)'
_chemical_formula_sum 'C32 H72 Cl4 Cu2 N4 O14'
_chemical_formula_iupac '[Cu2 Cl2 (C8 H15 N O2)4 ] (Cl2) , 6H2 O'
_chemical_formula_weight 1005.81
_chemical_melting_point ?
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_name_H-M_alt 'P 21/n'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 14.7100(11)
_cell_length_b 10.7163(6)
_cell_length_c 14.9312(12)
_cell_angle_alpha 90
_cell_angle_beta 91.828(10)
_cell_angle_gamma 90
_cell_volume 2352.5(3)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 8000
_cell_measurement_theta_min 2.25
_cell_measurement_theta_max 25.90
_cell_measurement_temperature 153(2)
_exptl_crystal_description plate
_exptl_crystal_colour green
_exptl_crystal_size_max 0.34
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.20
_exptl_crystal_density_diffrn 1.420
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_F_000 1060
_exptl_absorpt_coefficient_mu 1.192
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(MULABS; Spek, 2009)
;
_shelx_estimated_absorpt_T_min ?
_shelx_estimated_absorpt_T_max ?
_exptl_absorpt_correction_T_min 0.712
_exptl_absorpt_correction_T_max 1.000
_diffrn_ambient_temperature 153(2)
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator 'plane graphite'
_diffrn_measurement_device_type 'STOE IPDS 1'
_diffrn_measurement_device '1 circle goniometer'
_diffrn_measurement_method '\f rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 18018
_diffrn_reflns_av_R_equivalents 0.0907
_diffrn_reflns_theta_min 2.340
_diffrn_reflns_theta_max 25.898
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
_refine_special_details ?
_reflns_number_total 4545
_reflns_number_gt 3172
_reflns_threshold_expression 'I > 2\s(I)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.0907
_refine_ls_R_factor_gt 0.0666
_refine_ls_wR_factor_gt 0.1846
_refine_ls_wR_factor_ref 0.1964
_refine_ls_goodness_of_fit_ref 1.019
_refine_ls_restrained_S_all 1.018
_refine_ls_number_reflns 4545
_refine_ls_number_parameters 273
_refine_ls_number_restraints 9
_refine_ls_hydrogen_treatment mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1331P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 1.797
_refine_diff_density_min -0.927
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
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'
'Cl' 'Cl' 0.1484 0.1585
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cu' 'Cu' 0.3201 1.2651
'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'
_computing_data_collection
;
EXPOSE in IPDS-I (Stoe & Cie, 2004)
;
_computing_cell_refinement
;
CELL in IPDS-I (Stoe & Cie, 2004)
;
_computing_data_reduction
;
INTEGRATE in IPDS-I (Stoe & Cie, 2004)
;
_computing_structure_solution
;
SHELXS2016/6 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2016/6 (Sheldrick, 2015)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2008)
;
_computing_publication_material
;
SHELXL2016/6 (Sheldrick, 2015), PLATON (Spek, 2009) and
publCIF (Westrip, 2010)
;
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu1 0.57200(3) 0.53341(6) 0.55087(4) 0.0195(2) Uani d 1 . .
Cl Cl1 0.69386(7) 0.59126(13) 0.66374(7) 0.0253(3) Uani d 1 . .
O O1 0.5727(3) 0.3572(4) 0.5833(3) 0.0384(10) Uani d 1 . .
O O2 0.4505(3) 0.3014(4) 0.5009(3) 0.0369(10) Uani d 1 . .
O O3 0.6477(2) 0.4905(4) 0.4471(2) 0.0297(9) Uani d 1 . .
O O4 0.5250(2) 0.4381(5) 0.3640(3) 0.0445(12) Uani d 1 . .
N N1 0.6876(3) -0.1791(5) 0.8123(3) 0.0339(11) Uani d 1 . .
H H1A 0.715646 -0.207468 0.762784 0.051 Uiso calc 1 . .
H H1B 0.688742 -0.239545 0.855069 0.051 Uiso calc 1 . .
H H1C 0.717108 -0.110116 0.833690 0.051 Uiso calc 1 . .
N N2 0.6727(3) 0.1961(6) -0.0237(3) 0.0451(14) Uani d 1 . .
H H2A 0.674668 0.130093 0.014673 0.068 Uiso calc 1 . .
H H2B 0.702133 0.175997 -0.074399 0.068 Uiso calc 1 . .
H H2C 0.613684 0.215079 -0.038025 0.068 Uiso calc 1 . .
C C1 0.5154(3) 0.2771(5) 0.5551(3) 0.0244(11) Uani d 1 . .
C C2 0.5225(4) 0.1471(5) 0.5916(4) 0.0299(12) Uani d 1 . .
H H2 0.490146 0.089283 0.548741 0.036 Uiso calc 1 . .
C C3 0.6224(4) 0.1033(6) 0.6034(4) 0.0377(14) Uani d 1 . .
H H3A 0.650187 0.098871 0.543974 0.045 Uiso calc 1 . .
H H3B 0.657016 0.165255 0.640008 0.045 Uiso calc 1 . .
C C4 0.6295(4) -0.0230(6) 0.6482(4) 0.0388(14) Uani d 1 . .
H H4A 0.694444 -0.045681 0.657197 0.047 Uiso calc 1 . .
H H4B 0.600371 -0.086743 0.608849 0.047 Uiso calc 1 . .
C C5 0.5841(3) -0.0227(5) 0.7379(4) 0.0288(12) Uani d 1 . .
H H5 0.614942 0.042295 0.776158 0.035 Uiso calc 1 . .
C C6 0.4837(4) 0.0149(6) 0.7258(6) 0.0472(18) Uani d 1 . .
H H6A 0.451049 -0.048267 0.688621 0.057 Uiso calc 1 . .
H H6B 0.455311 0.017746 0.784995 0.057 Uiso calc 1 . .
C C7 0.4754(3) 0.1418(6) 0.6811(4) 0.0372(14) Uani d 1 . .
H H7A 0.502404 0.205796 0.721666 0.045 Uiso calc 1 . .
H H7B 0.410239 0.162109 0.671203 0.045 Uiso calc 1 . .
C C8 0.5915(4) -0.1465(6) 0.7881(4) 0.0397(14) Uani d 1 . .
H H8A 0.556328 -0.141231 0.843406 0.048 Uiso calc 1 . .
H H8B 0.564509 -0.213527 0.750187 0.048 Uiso calc 1 . .
C C9 0.6099(3) 0.4514(5) 0.3760(3) 0.0244(11) Uani d 1 . .
C C10 0.6679(3) 0.4182(5) 0.2966(3) 0.0244(11) Uani d 1 . .
H H10 0.733515 0.427604 0.315003 0.029 Uiso calc 1 . .
C C11 0.6461(4) 0.5081(6) 0.2187(4) 0.0288(12) Uani d 1 . .
H H11A 0.579838 0.507245 0.204844 0.035 Uiso calc 1 . .
H H11B 0.663545 0.593965 0.236560 0.035 Uiso calc 1 . .
C C12 0.6970(4) 0.4710(6) 0.1351(3) 0.0299(12) Uani d 1 . .
H H12A 0.681611 0.530032 0.085930 0.036 Uiso calc 1 . .
H H12B 0.763338 0.475985 0.147985 0.036 Uiso calc 1 . .
C C13 0.6722(3) 0.3405(5) 0.1063(3) 0.0262(12) Uani d 1 . .
H H13 0.604822 0.337427 0.095228 0.031 Uiso calc 1 . .
C C14 0.6965(4) 0.2495(6) 0.1830(4) 0.0332(13) Uani d 1 . .
H H14A 0.677871 0.164112 0.164965 0.040 Uiso calc 1 . .
H H14B 0.763281 0.249287 0.193720 0.040 Uiso calc 1 . .
C C15 0.6507(4) 0.2838(6) 0.2693(4) 0.0319(12) Uani d 1 . .
H H15A 0.584401 0.270120 0.261501 0.038 Uiso calc 1 . .
H H15B 0.673527 0.227990 0.317868 0.038 Uiso calc 1 . .
C C16 0.7174(4) 0.3051(6) 0.0196(4) 0.0347(14) Uani d 1 . .
H H16A 0.714618 0.376924 -0.022083 0.042 Uiso calc 1 . .
H H16B 0.782239 0.285487 0.032601 0.042 Uiso calc 1 . .
Cl Cl2 0.53120(11) 0.73439(19) 0.07190(12) 0.0537(5) Uani d 1 . .
O O1W 0.3515(3) 0.3850(6) 0.0849(3) 0.0600(14) Uani d 1 . .
H H1WA 0.385(4) 0.405(9) 0.038(3) 0.090 Uiso d 1 . .
H H1WB 0.393(4) 0.383(9) 0.130(3) 0.090 Uiso d 1 . .
O O2W 0.1694(4) 0.5612(6) 0.5040(4) 0.0651(15) Uani d 1 . .
H H2WA 0.134(5) 0.589(9) 0.548(5) 0.098 Uiso d 1 . .
H H2WB 0.222(3) 0.602(8) 0.514(6) 0.098 Uiso d 1 . .
O O3W 0.1194(3) 0.1039(6) 0.3118(3) 0.0619(15) Uani d 1 . .
H H3WA 0.104(5) 0.075(8) 0.259(3) 0.093 Uiso d 1 . .
H H3WB 0.073(4) 0.148(8) 0.329(5) 0.093 Uiso d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cu1 0.0152(3) 0.0291(4) 0.0144(3) 0.0005(2) 0.0036(2) 0.0010(2)
Cl1 0.0213(6) 0.0352(8) 0.0193(6) -0.0045(5) 0.0001(4) 0.0005(5)
O1 0.035(2) 0.039(3) 0.041(2) -0.0092(18) -0.0129(17) 0.0117(19)
O2 0.035(2) 0.033(2) 0.041(2) 0.0018(17) -0.0158(17) -0.0035(19)
O3 0.0195(16) 0.050(3) 0.0195(17) -0.0029(16) 0.0022(13) -0.0049(17)
O4 0.0187(18) 0.088(4) 0.027(2) -0.0061(19) 0.0057(14) -0.018(2)
N1 0.031(2) 0.032(3) 0.038(3) 0.007(2) -0.0064(19) 0.001(2)
N2 0.041(3) 0.056(4) 0.039(3) 0.001(3) 0.018(2) -0.019(3)
C1 0.024(2) 0.031(3) 0.018(2) 0.004(2) 0.0067(19) 0.004(2)
C2 0.032(3) 0.025(3) 0.032(3) 0.001(2) -0.008(2) -0.003(2)
C3 0.032(3) 0.048(4) 0.034(3) 0.015(3) 0.016(2) 0.011(3)
C4 0.039(3) 0.040(4) 0.038(3) 0.015(3) -0.001(2) 0.003(3)
C5 0.020(2) 0.029(3) 0.037(3) 0.001(2) -0.002(2) 0.004(2)
C6 0.022(3) 0.036(4) 0.084(5) 0.002(2) 0.010(3) 0.022(4)
C7 0.019(2) 0.037(4) 0.056(4) 0.007(2) 0.010(2) 0.019(3)
C8 0.028(3) 0.040(4) 0.051(4) 0.005(3) 0.004(2) 0.009(3)
C9 0.022(2) 0.030(3) 0.022(2) 0.001(2) 0.0045(19) 0.004(2)
C10 0.014(2) 0.039(3) 0.021(2) 0.001(2) 0.0046(17) 0.000(2)
C11 0.034(3) 0.029(3) 0.024(3) 0.002(2) 0.008(2) -0.001(2)
C12 0.032(3) 0.037(4) 0.021(3) 0.004(2) 0.010(2) 0.004(2)
C13 0.020(2) 0.035(3) 0.024(2) 0.004(2) 0.0101(18) -0.006(2)
C14 0.031(3) 0.030(3) 0.039(3) 0.002(2) 0.011(2) 0.000(3)
C15 0.036(3) 0.031(3) 0.030(3) 0.003(2) 0.011(2) 0.002(2)
C16 0.029(3) 0.047(4) 0.028(3) 0.003(2) 0.013(2) -0.012(3)
Cl2 0.0453(9) 0.0647(13) 0.0518(10) -0.0012(8) 0.0122(7) 0.0128(9)
O1W 0.062(3) 0.068(4) 0.051(3) 0.008(3) 0.014(2) 0.021(3)
O2W 0.048(3) 0.075(4) 0.071(4) 0.012(3) -0.008(3) -0.019(3)
O3W 0.052(3) 0.081(4) 0.053(3) 0.018(3) 0.000(2) -0.034(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 Cu1 3_666 2.6649(11) y
Cu1 O1 . 1.950(4) y
Cu1 O2 3_666 1.955(4) y
Cu1 O4 3_666 1.965(4) y
Cu1 O3 . 1.991(3) y
Cu1 Cl1 . 2.4990(12) y
O1 C1 . 1.265(7) ?
O2 C1 . 1.258(6) ?
O3 C9 . 1.255(6) ?
O4 C9 . 1.264(6) ?
N1 C8 . 1.489(7) ?
N1 H1A . 0.9100 ?
N1 H1B . 0.9100 ?
N1 H1C . 0.9100 ?
N2 C16 . 1.479(8) ?
N2 H2A . 0.9100 ?
N2 H2B . 0.9100 ?
N2 H2C . 0.9100 ?
C1 C2 . 1.499(8) ?
C2 C7 . 1.526(8) ?
C2 C3 . 1.547(7) ?
C2 H2 . 1.0000 ?
C3 C4 . 1.512(9) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C4 C5 . 1.515(8) ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C5 C8 . 1.526(8) ?
C5 C6 . 1.536(7) ?
C5 H5 . 1.0000 ?
C6 C7 . 1.518(9) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C9 C10 . 1.526(6) ?
C10 C15 . 1.516(8) ?
C10 C11 . 1.536(7) ?
C10 H10 . 1.0000 ?
C11 C12 . 1.527(7) ?
C11 H11A . 0.9900 ?
C11 H11B . 0.9900 ?
C12 C13 . 1.505(8) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C13 C16 . 1.522(7) ?
C13 C14 . 1.538(8) ?
C13 H13 . 1.0000 ?
C14 C15 . 1.518(7) ?
C14 H14A . 0.9900 ?
C14 H14B . 0.9900 ?
C15 H15A . 0.9900 ?
C15 H15B . 0.9900 ?
C16 H16A . 0.9900 ?
C16 H16B . 0.9900 ?
O1W H1WA . 0.89(2) ?
O1W H1WB . 0.90(2) ?
O2W H2WA . 0.90(2) ?
O2W H2WB . 0.90(2) ?
O3W H3WA . 0.88(2) ?
O3W H3WB . 0.88(2) ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Cu1 O2 . 3_666 167.02(15) y
O1 Cu1 O4 . 3_666 89.3(2) y
O2 Cu1 O4 3_666 3_666 89.9(2) y
O1 Cu1 O3 . . 88.33(18) y
O2 Cu1 O3 3_666 . 89.60(18) y
O4 Cu1 O3 3_666 . 167.27(15) y
O1 Cu1 Cl1 . . 94.31(11) y
O2 Cu1 Cl1 3_666 . 98.68(11) y
O4 Cu1 Cl1 3_666 . 92.57(11) y
O3 Cu1 Cl1 . . 100.08(10) y
O1 Cu1 Cu1 . 3_666 83.04(11) y
O2 Cu1 Cu1 3_666 3_666 84.05(11) y
O4 Cu1 Cu1 3_666 3_666 80.24(11) y
O3 Cu1 Cu1 . 3_666 87.06(10) y
Cl1 Cu1 Cu1 . 3_666 172.34(4) y
C1 O1 Cu1 . . 125.2(3) ?
C1 O2 Cu1 . 3_666 123.8(4) ?
C9 O3 Cu1 . . 119.4(3) ?
C9 O4 Cu1 . 3_666 128.7(3) ?
C8 N1 H1A . . 109.5 ?
C8 N1 H1B . . 109.5 ?
H1A N1 H1B . . 109.5 ?
C8 N1 H1C . . 109.5 ?
H1A N1 H1C . . 109.5 ?
H1B N1 H1C . . 109.5 ?
C16 N2 H2A . . 109.5 ?
C16 N2 H2B . . 109.5 ?
H2A N2 H2B . . 109.5 ?
C16 N2 H2C . . 109.5 ?
H2A N2 H2C . . 109.5 ?
H2B N2 H2C . . 109.5 ?
O2 C1 O1 . . 123.9(5) ?
O2 C1 C2 . . 118.0(5) ?
O1 C1 C2 . . 118.1(4) ?
C1 C2 C7 . . 108.9(5) ?
C1 C2 C3 . . 112.2(5) ?
C7 C2 C3 . . 110.2(4) ?
C1 C2 H2 . . 108.5 ?
C7 C2 H2 . . 108.5 ?
C3 C2 H2 . . 108.5 ?
C4 C3 C2 . . 112.0(5) ?
C4 C3 H3A . . 109.2 ?
C2 C3 H3A . . 109.2 ?
C4 C3 H3B . . 109.2 ?
C2 C3 H3B . . 109.2 ?
H3A C3 H3B . . 107.9 ?
C3 C4 C5 . . 111.3(5) ?
C3 C4 H4A . . 109.4 ?
C5 C4 H4A . . 109.4 ?
C3 C4 H4B . . 109.4 ?
C5 C4 H4B . . 109.4 ?
H4A C4 H4B . . 108.0 ?
C4 C5 C8 . . 113.9(5) ?
C4 C5 C6 . . 110.2(5) ?
C8 C5 C6 . . 109.8(5) ?
C4 C5 H5 . . 107.5 ?
C8 C5 H5 . . 107.5 ?
C6 C5 H5 . . 107.5 ?
C7 C6 C5 . . 110.5(5) ?
C7 C6 H6A . . 109.6 ?
C5 C6 H6A . . 109.6 ?
C7 C6 H6B . . 109.6 ?
C5 C6 H6B . . 109.6 ?
H6A C6 H6B . . 108.1 ?
C6 C7 C2 . . 112.7(5) ?
C6 C7 H7A . . 109.0 ?
C2 C7 H7A . . 109.0 ?
C6 C7 H7B . . 109.0 ?
C2 C7 H7B . . 109.0 ?
H7A C7 H7B . . 107.8 ?
N1 C8 C5 . . 112.0(5) ?
N1 C8 H8A . . 109.2 ?
C5 C8 H8A . . 109.2 ?
N1 C8 H8B . . 109.2 ?
C5 C8 H8B . . 109.2 ?
H8A C8 H8B . . 107.9 ?
O3 C9 O4 . . 124.6(5) ?
O3 C9 C10 . . 119.4(4) ?
O4 C9 C10 . . 116.0(4) ?
C15 C10 C9 . . 109.8(4) ?
C15 C10 C11 . . 111.3(4) ?
C9 C10 C11 . . 109.5(4) ?
C15 C10 H10 . . 108.7 ?
C9 C10 H10 . . 108.7 ?
C11 C10 H10 . . 108.7 ?
C12 C11 C10 . . 111.1(4) ?
C12 C11 H11A . . 109.4 ?
C10 C11 H11A . . 109.4 ?
C12 C11 H11B . . 109.4 ?
C10 C11 H11B . . 109.4 ?
H11A C11 H11B . . 108.0 ?
C13 C12 C11 . . 110.8(4) ?
C13 C12 H12A . . 109.5 ?
C11 C12 H12A . . 109.5 ?
C13 C12 H12B . . 109.5 ?
C11 C12 H12B . . 109.5 ?
H12A C12 H12B . . 108.1 ?
C12 C13 C16 . . 111.5(5) ?
C12 C13 C14 . . 109.2(4) ?
C16 C13 C14 . . 112.2(5) ?
C12 C13 H13 . . 107.9 ?
C16 C13 H13 . . 107.9 ?
C14 C13 H13 . . 107.9 ?
C15 C14 C13 . . 112.3(5) ?
C15 C14 H14A . . 109.1 ?
C13 C14 H14A . . 109.1 ?
C15 C14 H14B . . 109.1 ?
C13 C14 H14B . . 109.1 ?
H14A C14 H14B . . 107.9 ?
C10 C15 C14 . . 112.5(5) ?
C10 C15 H15A . . 109.1 ?
C14 C15 H15A . . 109.1 ?
C10 C15 H15B . . 109.1 ?
C14 C15 H15B . . 109.1 ?
H15A C15 H15B . . 107.8 ?
N2 C16 C13 . . 111.6(5) ?
N2 C16 H16A . . 109.3 ?
C13 C16 H16A . . 109.3 ?
N2 C16 H16B . . 109.3 ?
C13 C16 H16B . . 109.3 ?
H16A C16 H16B . . 108.0 ?
H1WA O1W H1WB . . 102(3) ?
H2WA O2W H2WB . . 103(3) ?
H3WA O3W H3WB . . 106(3) ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Cu1 O2 C1 O1 3_666 . . . 1.1(7) ?
Cu1 O2 C1 C2 3_666 . . . 178.1(4) ?
Cu1 O1 C1 O2 . . . . 0.9(7) ?
Cu1 O1 C1 C2 . . . . -176.1(4) ?
O2 C1 C2 C7 . . . . -94.2(6) ?
O1 C1 C2 C7 . . . . 82.9(6) ?
O2 C1 C2 C3 . . . . 143.5(5) ?
O1 C1 C2 C3 . . . . -39.4(7) ?
C1 C2 C3 C4 . . . . 174.7(5) ?
C7 C2 C3 C4 . . . . 53.1(7) ?
C2 C3 C4 C5 . . . . -56.3(7) ?
C3 C4 C5 C8 . . . . -178.1(5) ?
C3 C4 C5 C6 . . . . 57.9(7) ?
C4 C5 C6 C7 . . . . -57.2(8) ?
C8 C5 C6 C7 . . . . 176.5(6) ?
C5 C6 C7 C2 . . . . 55.9(8) ?
C1 C2 C7 C6 . . . . -176.8(5) ?
C3 C2 C7 C6 . . . . -53.3(7) ?
C4 C5 C8 N1 . . . . 63.3(7) ?
C6 C5 C8 N1 . . . . -172.5(5) ?
Cu1 O3 C9 O4 . . . . 1.0(8) ?
Cu1 O3 C9 C10 . . . . -179.8(4) ?
Cu1 O4 C9 O3 3_666 . . . -2.3(9) ?
Cu1 O4 C9 C10 3_666 . . . 178.5(4) ?
O3 C9 C10 C15 . . . . 122.8(5) ?
O4 C9 C10 C15 . . . . -57.9(6) ?
O3 C9 C10 C11 . . . . -114.7(5) ?
O4 C9 C10 C11 . . . . 64.5(6) ?
C15 C10 C11 C12 . . . . -53.7(6) ?
C9 C10 C11 C12 . . . . -175.2(4) ?
C10 C11 C12 C13 . . . . 58.9(6) ?
C11 C12 C13 C16 . . . . 176.2(4) ?
C11 C12 C13 C14 . . . . -59.3(5) ?
C12 C13 C14 C15 . . . . 56.5(6) ?
C16 C13 C14 C15 . . . . -179.4(5) ?
C9 C10 C15 C14 . . . . 172.3(4) ?
C11 C10 C15 C14 . . . . 50.9(6) ?
C13 C14 C15 C10 . . . . -52.9(6) ?
C12 C13 C16 N2 . . . . -162.4(5) ?
C14 C13 C16 N2 . . . . 74.9(6) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1A Cl1 1_545 0.91 2.63 3.316(5) 133
N1 H1C Cl1 2_646 0.91 2.52 3.394(5) 160
N2 H2B Cl1 2_645 0.91 2.25 3.123(5) 160
N2 H2C Cl2 3_665 0.91 2.24 3.151(6) 179
N1 H1B O1W 3_656 0.91 1.90 2.760(7) 156
N2 H2A O2W 4_665 0.91 2.06 2.789(9) 137
O1W H1WA Cl2 3_665 0.89(2) 2.57(8) 3.218(6) 130(8)
O2W H2WA Cl2 4_576 0.90(2) 2.46(7) 3.176(6) 137(9)
O2W H2WB O3 3_666 0.90(2) 2.22(8) 2.820(6) 124(8)
O3W H3WA Cl1 4_565 0.88(2) 2.66(6) 3.258(5) 127(6)
O3W H3WB Cl2 2_545 0.88(2) 2.35(3) 3.182(5) 158(7)
_shelx_hkl_file
;
-18 0 1 15.57 20.36
18 0 -1 -4.01 20.81
-18 0 2 193.61 21.34
18 -1 -1 1.94 19.84
-18 1 1 -1.14 19.82
-17 0 1 231.87 18.02
17 0 -1 211.03 18.96
-17 0 1 188.38 18.71
-17 0 2 0.80 17.21
17 0 -2 29.84 24.47
-17 0 2 18.75 23.55
-17 0 3 336.81 25.54
17 0 -3 360.28 27.34
-17 0 3 373.53 26.67
-17 0 4 -24.39 23.77
17 0 -4 3.94 24.19
-17 0 5 45.03 27.05
17 0 -5 46.61 19.77
17 0 -6 -13.15 27.22
-17 0 6 11.21 27.40
-17 1 1 23.88 23.51
-17 -1 1 -10.48 18.20
-17 1 1 12.47 24.04
-17 -1 1 -1.33 16.87
17 -1 -1 3.59 24.14
17 1 -1 13.67 25.86
-17 1 2 122.03 24.17
17 1 -2 148.53 26.42
-17 -1 2 112.50 26.48
17 -1 -2 112.21 24.73
-17 1 2 119.09 24.46
-17 -1 2 149.43 24.09
17 1 -3 109.76 25.94
-17 -1 3 100.28 24.38
-17 -1 3 115.86 25.47
17 -1 -3 65.09 24.73
-17 1 3 94.76 17.33
17 1 -4 72.45 27.22
-17 -1 4 56.85 26.17
-17 1 4 83.01 25.47
17 -1 -4 61.02 17.49
-17 1 5 -5.04 19.24
17 1 -5 20.11 19.70
-17 -1 5 -1.98 19.44
17 -1 -5 -32.93 27.17
-17 -1 6 122.51 28.58
17 -1 -6 104.39 19.93
-17 1 6 114.71 27.85
17 1 -6 144.68 28.72
-17 2 1 8.65 16.73
-17 2 1 9.20 16.89
-17 -2 1 -20.68 26.94
17 -2 -1 4.22 16.96
-17 -2 1 8.89 16.84
17 2 -1 27.80 27.03
-17 -2 2 32.84 26.60
-17 2 2 4.76 23.50
-17 -2 2 18.34 24.19
17 -2 -2 3.74 17.06
-17 2 2 5.00 17.19
17 2 -2 26.63 27.21
17 2 -3 30.97 19.34
-17 -2 3 16.94 19.44
17 -2 -3 37.28 16.90
-17 2 3 17.93 25.52
-17 -2 3 17.45 17.60
-17 -2 4 4.01 19.83
17 2 -4 -11.52 21.86
17 -2 -4 40.02 26.48
-17 2 4 0.95 18.88
-17 -2 4 -3.10 21.28
-17 2 5 51.76 19.02
-17 -2 5 26.99 28.26
17 2 -5 36.86 30.32
17 -2 -5 24.55 19.45
17 2 -6 26.40 20.82
-17 -3 1 218.52 27.28
17 3 -1 264.83 34.25
-17 3 1 169.85 20.86
17 -3 -1 224.24 21.16
-17 -3 1 226.48 33.16
-17 3 1 223.85 20.69
17 -3 -2 29.82 19.50
-17 -3 2 67.43 32.35
17 3 -2 31.22 33.02
-17 3 2 20.34 19.43
-17 -3 2 63.87 19.63
-17 -3 3 12.25 31.95
-17 -3 3 6.37 28.23
17 3 -3 23.93 32.07
17 -3 -3 12.78 27.42
-17 3 3 -0.07 26.84
17 3 -4 241.27 24.23
-17 -3 4 182.73 29.41
-17 3 4 185.91 27.75
-17 -3 4 186.38 23.67
17 -3 -4 196.92 28.24
17 -3 -5 31.74 19.39
-17 -4 1 -17.93 28.40
-17 -4 1 -1.16 23.98
-17 4 1 -14.41 27.59
17 4 -1 -6.12 24.45
-17 4 1 1.20 27.84
17 -4 -1 9.53 27.98
17 -4 -2 18.42 27.97
-17 -4 2 -2.19 20.47
17 4 -2 32.74 23.94
-17 4 2 0.94 27.50
-17 -4 2 24.31 23.78
-17 -4 3 20.57 28.77
16 0 -1 11.31 20.92
-16 0 1 6.57 20.22
-16 0 1 -26.77 20.73
-16 0 2 212.85 15.68
16 0 -2 265.50 22.67
-16 0 2 199.36 16.15
-16 0 3 -7.94 16.43
16 0 -3 -6.15 16.84
-16 0 4 22.94 23.10
16 0 -4 13.94 23.73
16 0 -5 8.67 23.51
-16 0 5 -15.34 23.80
16 0 -6 467.00 20.14
-16 0 6 445.33 19.60
-16 0 7 -4.14 24.24
16 0 -7 9.84 23.38
-16 0 8 6.86 28.20
16 0 -8 17.54 26.82
-16 0 9 -2.46 20.68
-16 -1 1 198.69 21.62
-16 1 1 180.99 15.24
-16 -1 1 211.35 22.35
16 1 -1 221.38 23.14
16 -1 -1 208.54 21.86
-16 1 1 231.33 21.27
-16 -1 2 11.12 23.23
-16 1 2 -9.37 19.96
-16 -1 2 -4.40 14.39
16 1 -2 10.35 23.59
16 -1 -2 -21.24 22.14
-16 -1 3 166.84 25.97
-16 -1 3 146.53 22.75
16 1 -3 203.20 26.15
-16 1 3 153.22 17.21
16 -1 -3 161.79 24.54
16 1 -4 10.38 24.75
-16 1 4 13.06 23.02
-16 -1 4 13.65 23.54
16 -1 -4 17.46 23.10
16 1 -5 136.12 25.22
16 -1 -5 137.76 23.82
-16 -1 5 102.35 24.34
-16 1 5 116.56 23.73
-16 1 6 2.01 16.61
-16 -1 6 -11.61 24.71
16 1 -6 0.96 17.21
16 -1 -6 -7.21 16.30
16 1 -7 14.60 24.59
16 -1 -7 35.44 16.31
-16 1 7 28.41 24.07
-16 -1 7 4.65 18.23
-16 1 8 45.07 19.75
16 1 -8 57.46 27.90
16 -1 -8 49.35 26.87
-16 -1 8 61.06 20.90
16 2 -1 -11.73 27.09
-16 2 1 -3.92 16.44
-16 -2 1 21.67 26.49
16 -2 -1 -11.15 16.77
-16 -2 1 -7.71 23.82
-16 2 1 -5.72 16.42
-16 -2 2 280.46 25.12
-16 -2 2 289.27 19.52
16 2 -2 292.70 20.47
16 -2 -2 280.98 19.12
-16 2 2 249.27 24.91
-16 2 3 22.90 16.28
16 -2 -3 -12.31 16.79
-16 -2 3 18.04 18.30
-16 -2 3 19.17 16.75
16 2 -3 12.69 18.51
16 -2 -4 -2.86 16.53
-16 -2 4 22.11 16.88
-16 2 4 -0.17 23.14
-16 -2 4 11.46 17.98
16 2 -4 16.88 18.16
16 2 -5 2.51 18.21
-16 -2 5 6.27 17.06
16 -2 -5 -22.62 23.44
-16 2 5 3.24 16.53
-16 2 6 -7.02 23.59
-16 -2 6 1.71 17.46
16 -2 -6 9.52 16.42
16 2 -6 9.73 25.41
16 -2 -7 11.43 25.11
-16 -2 7 5.88 20.68
-16 2 7 -4.28 25.50
16 2 -7 6.10 20.58
16 -2 -8 39.00 26.67
-16 2 8 14.61 19.50
-16 -2 8 -12.19 29.89
16 2 -8 7.96 29.00
16 3 -1 15.43 27.98
-16 3 1 -1.34 16.81
-16 3 1 4.51 16.45
-16 -3 1 -3.99 16.78
-16 -3 1 12.97 27.47
16 -3 -1 10.65 16.58
16 -3 -2 140.70 16.77
-16 3 2 144.98 23.28
-16 -3 2 113.19 19.88
-16 -3 2 120.32 17.52
16 3 -2 121.01 20.66
16 -3 -3 48.28 17.03
-16 -3 3 70.45 19.46
-16 3 3 74.78 22.98
-16 -3 3 26.27 24.75
16 3 -3 50.49 19.87
-16 -3 4 10.46 24.39
-16 3 4 -2.07 16.24
16 3 -4 7.92 19.18
16 -3 -4 -9.26 16.73
-16 -3 4 -9.22 19.19
-16 3 5 40.52 23.78
-16 -3 5 46.41 27.31
16 3 -5 50.29 27.76
-16 -3 5 71.84 24.81
16 -3 -5 46.10 23.98
-16 -3 6 65.25 18.57
-16 3 6 72.21 16.86
16 -3 -6 50.55 17.31
16 3 -6 76.45 28.98
-16 3 7 8.58 19.13
-16 -3 7 -3.42 21.24
16 3 -7 -8.79 21.67
16 -3 -7 -5.72 27.39
16 4 -1 15.98 29.22
-16 4 1 30.74 23.76
-16 -4 1 13.69 24.33
-16 -4 1 21.56 29.09
16 -4 -1 68.16 23.95
-16 -4 2 55.08 28.87
16 -4 -2 50.60 24.09
-16 -4 2 58.25 24.37
16 4 -2 64.81 29.05
-16 4 2 32.26 23.83
16 4 -3 44.93 28.48
-16 -4 3 -11.41 28.45
-16 4 3 20.52 16.58
16 -4 -3 6.43 23.71
-16 -4 3 45.69 24.25
16 -4 -4 94.90 24.10
16 4 -4 91.16 28.98
-16 4 4 60.91 16.87
-16 -4 4 77.06 28.75
-16 -4 4 64.46 18.15
16 -4 -5 24.13 19.22
-16 -4 5 7.32 20.82
-16 4 5 -11.24 27.43
16 4 -5 47.05 30.17
-16 -4 5 -13.73 30.42
-16 4 6 17.90 27.45
-16 -4 6 8.29 30.56
-16 -4 6 26.65 22.83
16 4 -6 57.23 22.51
16 -4 -6 11.97 27.79
-16 5 1 -5.72 17.44
16 -5 -1 5.93 19.59
-16 -5 1 -2.04 17.45
-16 -5 1 -11.69 31.46
-16 5 2 44.69 27.78
16 -5 -2 48.09 19.65
16 5 -2 34.54 31.92
-16 -5 2 44.73 31.25
-16 -5 2 45.19 20.20
-16 -5 3 126.96 21.55
16 -5 -3 171.81 20.54
-16 -5 3 155.76 33.72
16 5 -3 171.39 34.72
-16 5 3 115.23 28.74
-16 5 4 -14.20 27.92
16 5 -4 -3.61 33.35
16 -5 -4 0.97 19.73
-16 -5 4 -12.70 30.04
-16 -5 4 15.26 32.97
-16 -5 5 61.71 23.20
-16 5 5 26.06 28.54
-16 -5 5 73.60 30.37
16 -5 -5 45.27 28.40
16 5 -5 66.10 23.72
-16 -6 1 63.31 29.22
-16 6 1 39.30 20.74
-16 -6 1 47.40 24.24
16 -6 -1 55.26 20.47
-16 6 2 2.91 20.48
-15 0 1 334.05 22.45
15 0 -1 363.36 22.91
-15 0 1 365.48 21.57
-15 0 2 6.54 13.86
15 0 -2 -13.30 20.47
15 0 -3 522.35 18.37
-15 0 3 488.16 17.50
15 0 -4 0.32 14.04
-15 0 4 3.14 13.77
-15 0 5 57.84 14.20
15 0 -5 50.31 14.65
15 0 -6 -12.49 20.00
-15 0 6 -10.51 20.50
-15 0 7 176.76 24.77
15 0 -7 200.41 23.99
-15 0 8 -12.17 24.53
15 0 -8 2.57 23.42
15 0 -9 373.06 18.73
-15 0 9 371.97 26.74
-15 0 10 3.02 29.01
15 0 -10 -0.63 27.02
-15 1 1 96.93 14.61
15 -1 -1 114.41 20.54
-15 1 1 101.42 20.63
-15 -1 1 100.47 15.75
15 1 -1 134.06 15.78
-15 -1 1 114.63 14.76
15 1 -2 200.20 22.20
-15 -1 2 190.59 21.72
-15 1 2 163.05 20.62
15 -1 -2 175.10 21.30
-15 -1 2 176.13 15.06
-15 1 3 3.04 19.72
15 -1 -3 2.78 20.06
-15 -1 3 10.48 14.18
15 1 -3 18.02 21.16
-15 -1 4 124.67 14.60
15 1 -4 123.72 21.48
-15 1 4 118.92 19.76
15 -1 -4 140.93 14.80
15 1 -5 0.87 20.67
-15 -1 5 13.77 14.04
15 -1 -5 11.51 13.85
-15 1 5 13.14 13.84
-15 1 6 71.57 14.66
15 -1 -6 112.31 20.19
15 1 -6 78.24 21.30
-15 -1 6 76.89 15.19
15 1 -7 80.42 23.84
-15 1 7 37.80 23.94
-15 -1 7 44.31 17.76
15 -1 -7 67.00 16.52
-15 1 8 234.05 24.94
15 1 -8 211.41 25.48
-15 -1 8 205.26 18.93
15 -1 -8 232.20 24.46
-15 1 9 -4.83 17.51
15 1 -9 6.96 24.30
15 -1 -9 -6.11 23.51
-15 -1 9 -2.16 18.37
-15 1 10 93.28 29.56
15 -1 -10 138.61 27.74
-15 -1 10 105.19 22.25
15 1 -10 148.49 28.64
-15 -2 1 59.88 22.37
-15 2 1 40.65 14.81
15 2 -1 58.76 23.05
15 -2 -1 72.72 20.62
-15 -2 1 42.77 14.87
-15 -2 2 -13.10 22.18
-15 -2 2 -0.24 14.08
-15 2 2 -7.71 19.49
15 -2 -2 8.81 13.93
15 2 -2 -14.46 22.48
15 -2 -3 60.13 20.27
-15 -2 3 76.69 14.68
-15 -2 3 34.51 15.84
15 2 -3 66.96 16.04
-15 2 3 38.99 14.29
15 -2 -4 20.19 19.95
-15 2 4 31.04 13.86
15 2 -4 12.54 15.90
-15 -2 4 18.15 20.14
-15 -2 5 195.48 21.58
15 -2 -5 168.46 15.11
-15 2 5 189.11 20.30
15 2 -5 218.65 16.70
-15 -2 6 90.32 23.11
-15 2 6 53.36 23.90
15 -2 -6 84.19 16.86
15 2 -6 93.07 18.22
-15 -2 7 -11.51 18.08
15 2 -7 7.73 25.07
15 -2 -7 -18.45 23.58
-15 2 7 13.30 16.50
-15 -2 8 106.81 19.02
15 -2 -8 144.59 24.13
-15 2 8 84.80 24.45
15 2 -8 133.37 18.54
-15 -2 9 92.58 19.72
-15 2 9 110.91 18.05
15 -2 -9 119.60 26.23
15 2 -9 97.06 27.52
15 -2 -10 20.28 27.65
-15 -2 10 7.84 30.96
-15 2 10 41.51 27.92
15 2 -10 25.36 28.93
-15 -3 1 4.86 16.44
15 -3 -1 4.89 14.14
-15 -3 1 17.58 19.96
-15 3 1 24.11 19.47
15 3 -1 7.50 16.50
15 3 -2 280.90 25.14
15 -3 -2 239.08 15.75
-15 -3 2 238.72 21.63
-15 -3 2 271.99 24.14
-15 3 2 226.28 20.92
-15 -3 3 38.97 20.72
15 3 -3 32.69 23.71
15 -3 -3 19.04 20.34
-15 -3 3 61.39 23.04
-15 3 3 43.26 19.69
-15 -3 4 26.24 14.99
-15 3 4 28.38 19.62
15 3 -4 26.40 16.50
-15 -3 4 15.02 16.46
15 -3 -4 40.91 20.23
15 -3 -5 2.52 16.63
-15 3 5 -18.91 21.70
-15 -3 5 4.47 22.94
15 3 -5 9.75 18.64
-15 3 6 -4.87 17.09
15 3 -6 25.51 26.52
-15 -3 6 30.96 25.19
15 -3 -6 18.20 16.98
-15 -3 7 290.25 20.07
15 -3 -7 255.59 18.02
-15 3 7 238.13 24.87
15 3 -7 320.55 27.53
15 3 -8 73.20 19.41
-15 3 8 75.16 24.29
15 -3 -8 72.00 24.42
-15 -3 8 67.37 26.82
-15 3 9 23.97 28.06
-15 -3 9 36.56 31.26
15 3 -9 16.22 30.17
15 -3 -9 56.73 27.59
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11 -1 -5 446.16 17.00
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11 -1 -6 39.99 10.31
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11 1 -7 44.07 17.71
11 -1 -7 49.89 12.57
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11 -1 -8 101.27 12.85
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11 -1 -9 124.36 13.00
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11 -1 -10 188.52 15.83
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11 1 -11 113.78 21.06
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11 -1 -12 24.67 20.85
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11 -1 -13 16.44 24.53
11 1 -14 193.64 27.54
11 -1 -14 186.15 26.80
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11 2 -1 18.70 14.72
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11 -2 -1 16.75 9.91
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11 2 -2 151.31 16.23
11 -2 -2 160.49 14.87
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11 2 -3 252.05 13.77
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11 -2 -3 324.73 15.91
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11 -2 -4 14.26 14.17
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11 -2 -5 31.63 10.17
11 2 -5 26.41 15.16
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11 2 -6 44.61 18.44
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11 -2 -6 64.85 17.60
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11 -2 -7 52.08 17.68
11 -2 -8 8.20 12.53
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11 2 -8 4.74 17.97
11 2 -9 138.47 18.36
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11 -2 -9 131.76 13.17
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11 -2 -11 15.82 14.90
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11 -2 -13 194.65 25.20
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11 2 -14 10.17 29.32
11 -2 -14 17.38 19.82
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11 -3 -1 77.83 14.17
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11 -3 -2 28.35 14.18
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11 -3 -3 98.12 10.87
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11 -3 -4 48.37 14.81
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11 -3 -5 66.90 12.88
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11 -3 -6 119.26 18.10
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11 -3 -7 49.43 17.97
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11 -3 -8 248.89 19.40
11 -3 -9 99.54 13.35
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11 -3 -10 25.55 21.19
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11 3 -11 150.86 16.97
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11 -3 -11 167.86 22.29
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11 -3 -12 64.96 25.20
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11 -3 -13 106.59 25.67
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11 -4 -7 502.55 21.27
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11 -4 -8 -0.68 12.83
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11 4 -9 29.06 16.03
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11 -4 -9 30.20 15.46
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11 -4 -10 315.04 17.11
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11 -4 -11 2.41 23.49
11 4 -11 19.88 18.31
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11 -4 -12 295.77 26.56
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9 -5 3 21.61 14.46
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9 -5 4 69.51 15.74
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9 5 10 126.05 16.37
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9 5 11 220.11 17.10
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9 -6 0 239.81 12.78
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9 7 12 9.96 29.58
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9 -8 0 0.10 17.80
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9 9 5 20.96 22.86
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10 -1 0 9.73 9.52
10 1 0 7.40 9.86
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10 -1 3 352.95 13.33
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10 -1 9 45.17 12.71
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10 -1 10 9.18 17.48
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-10 -1 -11 14.72 21.88
-10 1 -11 6.23 21.58
10 -1 11 5.48 14.87
10 1 11 4.81 22.02
10 -1 12 9.92 21.02
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10 1 12 11.94 21.61
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10 -1 13 41.82 24.39
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10 1 13 29.83 18.21
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10 -1 14 21.11 17.79
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10 -2 2 520.98 17.44
10 2 2 490.95 18.93
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10 -2 4 531.56 18.84
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-10 -2 -6 789.26 21.64
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-10 -2 -12 9.40 15.50
-10 2 -12 12.35 15.33
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-10 2 -13 21.58 26.02
10 -2 13 32.24 24.37
-10 -2 -13 79.56 25.61
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-10 2 -14 47.96 21.27
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10 -3 0 1140.65 20.98
10 -3 1 17.99 13.78
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10 -3 4 43.30 10.71
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-10 -3 -4 44.51 10.86
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-10 -3 -8 194.57 19.48
-10 -3 -8 183.58 19.68
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-10 3 -9 308.92 19.32
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-10 -3 -12 25.78 25.69
-10 3 -13 51.90 24.61
-10 -3 -13 98.11 26.56
10 3 13 66.01 26.39
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10 -3 13 70.77 24.05
-10 -3 -13 59.30 26.10
-10 3 -14 60.96 28.19
-10 -3 -14 72.37 21.75
10 3 14 83.57 21.14
-10 3 -14 40.46 30.21
10 -3 14 56.73 27.96
-10 -3 -14 87.82 21.22
10 4 0 178.95 13.13
-10 -4 0 156.40 12.61
-10 4 0 177.22 15.78
-10 -4 0 168.16 11.72
10 -4 0 195.39 15.38
10 -4 1 190.19 15.22
-10 4 -1 162.85 11.57
-10 -4 -1 182.63 15.14
-10 -4 -1 144.37 12.60
10 -4 2 10.36 10.07
-10 -4 -2 11.47 15.82
-10 4 -2 12.80 9.58
-10 4 -2 15.60 13.93
-10 -4 -2 11.35 13.68
10 -4 3 279.85 16.50
-10 -4 -3 224.07 13.19
-10 4 -3 267.44 15.54
-10 4 -3 215.26 11.79
-10 -4 -3 260.14 16.23
-10 -4 -4 64.98 14.51
10 -4 4 53.39 10.93
-10 4 -4 65.01 14.48
-10 -4 -4 39.26 11.62
-10 4 -4 50.91 10.51
-10 -4 -5 140.30 18.59
-10 4 -5 142.67 18.28
-10 -4 -5 123.12 14.51
-10 4 -5 160.00 17.71
10 4 6 40.54 17.71
-10 -4 -6 42.68 13.03
-10 4 -6 64.53 18.30
-10 4 -6 64.22 17.58
-10 -4 -6 51.01 13.48
10 4 7 18.24 17.74
-10 -4 -7 29.78 18.66
-10 -4 -7 19.59 18.00
-10 4 -7 17.46 18.11
-10 4 -7 33.94 16.68
-10 -4 -8 131.11 18.43
-10 -4 -8 110.74 19.23
10 4 8 84.22 18.54
-10 4 -8 86.06 14.18
-10 4 -8 111.08 12.72
-10 -4 -9 140.20 16.83
10 4 9 141.77 16.49
-10 4 -9 178.84 23.21
-10 -4 -9 188.47 16.45
-10 4 -9 187.98 21.38
-10 -4 -10 223.34 22.67
-10 -4 -10 188.83 16.95
-10 4 -10 196.34 16.94
-10 4 -10 191.69 21.12
10 4 10 126.94 22.98
-10 4 -11 74.48 20.42
-10 4 -11 72.60 22.44
10 4 11 58.14 22.20
-10 -4 -11 99.93 22.19
-10 -4 -11 81.79 15.89
-10 4 -12 23.01 16.96
-10 -4 -12 27.89 25.85
-10 4 -12 23.47 25.91
10 4 12 22.71 25.64
-10 -4 -12 11.50 26.01
-10 4 -13 1.50 24.16
-10 -4 -13 22.78 26.18
-10 4 -13 19.24 18.41
10 4 13 38.65 27.43
-10 -4 -13 3.50 27.85
-10 -5 0 374.39 15.50
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-10 -5 0 468.73 17.78
10 -5 0 479.71 14.03
10 -5 1 153.13 11.66
-10 -5 -1 140.85 17.57
-10 5 -1 176.61 16.04
-10 -5 -1 153.16 11.40
10 -5 2 446.97 17.91
-10 5 -2 423.78 16.74
-10 -5 -2 382.40 19.52
-10 5 -2 403.44 17.30
-10 -5 -2 362.02 13.65
-10 5 -3 96.98 17.55
-10 -5 -3 68.62 14.32
-10 5 -3 104.43 18.07
10 -5 3 100.24 12.96
-10 -5 -3 75.01 17.38
-10 -5 -4 194.90 17.94
10 -5 4 187.65 19.51
-10 5 -4 181.04 18.56
-10 5 -4 198.58 18.44
-10 -5 -4 188.58 20.24
-10 -5 -5 43.04 17.28
10 5 5 34.21 17.50
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-10 -5 -5 55.27 19.28
-10 -5 -6 20.98 19.15
-10 -5 -6 6.03 17.43
-10 5 -6 12.56 13.17
10 5 6 13.35 17.11
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10 5 7 -11.68 17.60
-10 -5 -7 7.00 17.45
-10 5 -7 18.95 13.21
-10 -5 -7 13.41 13.30
-10 5 -7 10.58 12.29
-10 -5 -8 56.66 15.34
-10 -5 -8 66.07 16.13
10 5 8 32.15 15.00
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-10 -5 -9 43.30 21.40
-10 -5 -9 29.16 15.91
-10 5 -9 35.47 22.31
10 5 9 28.26 21.19
-10 5 -9 35.99 20.73
10 5 10 189.83 16.99
-10 -5 -10 246.12 17.14
-10 -5 -10 218.60 17.27
-10 5 -10 240.76 18.00
-10 5 -10 266.70 21.95
-10 5 -11 22.74 26.37
-10 -5 -11 5.48 25.54
10 5 11 7.56 25.14
-10 -5 -11 -9.59 26.12
-10 5 -11 7.48 24.02
-10 -5 -12 132.79 19.06
-10 5 -12 114.33 27.29
10 5 12 109.15 18.76
-10 -5 -12 160.86 26.82
-10 5 -12 115.51 17.89
-10 -5 -13 256.16 30.82
-10 5 -13 163.27 32.25
10 5 13 152.86 30.97
-10 -5 -13 207.04 22.42
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10 -6 0 128.41 13.77
10 -6 1 825.41 19.34
-10 -6 -1 804.01 26.25
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-10 -6 -1 778.79 23.06
10 -6 2 34.77 18.09
-10 6 -2 15.22 17.38
-10 6 -2 27.58 18.57
-10 -6 -2 26.84 20.22
-10 -6 -2 26.66 12.01
10 -6 3 66.80 13.35
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-10 6 -3 71.15 18.42
-10 -6 -3 49.68 20.42
-10 -6 -3 65.74 17.14
-10 -6 -4 382.07 19.44
10 -6 4 427.24 22.00
-10 6 -4 386.29 20.52
-10 6 -4 424.55 20.73
-10 -6 -4 415.09 22.33
-10 -6 -5 15.97 17.21
10 6 5 6.25 17.02
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-10 -6 -5 10.29 14.11
-10 6 -6 6.13 12.89
-10 -6 -6 -8.80 19.18
10 6 6 -0.63 16.92
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10 6 7 30.58 20.98
-10 -6 -7 74.16 14.66
-10 -6 -7 48.89 16.49
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-10 6 -7 75.59 21.70
-10 -6 -8 -6.88 15.00
-10 -6 -8 -0.65 16.02
10 6 8 2.96 14.67
-10 6 -8 3.81 23.03
-10 6 -8 8.64 21.30
-10 -6 -9 141.80 22.45
-10 -6 -9 158.51 23.45
-10 6 -9 178.41 17.74
10 6 9 142.73 21.91
-10 6 -9 190.45 22.56
10 6 10 14.58 17.81
-10 -6 -10 30.33 17.59
-10 -6 -10 35.50 26.06
-10 6 -10 44.85 25.03
-10 6 -10 36.02 26.85
-10 6 -11 232.11 21.47
-10 -6 -11 236.29 26.82
10 6 11 214.22 26.35
-10 -6 -11 172.68 19.73
-10 6 -11 262.26 26.28
-10 -6 -12 60.47 20.86
-10 6 -12 32.72 31.39
10 6 12 45.79 20.51
-10 -6 -12 25.89 30.25
-10 6 -12 41.33 28.49
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10 -7 0 383.86 21.08
10 -7 1 63.74 18.35
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-10 -7 -1 66.68 21.03
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10 -7 2 587.98 23.08
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10 -7 3 55.98 19.15
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-10 -7 -3 37.98 17.07
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10 -7 4 16.28 19.14
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-10 -7 -5 105.44 17.24
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-10 -7 -6 40.64 14.49
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10 7 6 33.04 14.42
-10 -7 -6 29.83 23.35
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10 7 7 23.35 20.42
-10 -7 -7 -5.56 20.69
-10 7 -7 13.49 22.85
-10 -7 -7 -1.15 22.82
-10 7 -7 1.80 22.12
-10 -7 -8 25.03 20.99
-10 -7 -8 41.02 16.15
10 7 8 15.29 22.68
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-10 -7 -9 78.44 25.05
-10 -7 -9 83.67 26.85
-10 7 -9 59.29 28.04
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10 7 9 50.31 24.99
-10 -7 -10 177.64 26.31
-10 -7 -10 128.66 19.71
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10 7 10 134.19 26.11
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10 7 11 0.18 29.00
-10 7 -11 7.58 22.19
-10 -7 -11 1.48 20.21
-10 -7 -11 -7.07 21.56
-10 7 -11 -17.09 29.65
-10 8 0 10.12 24.31
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10 -8 0 9.64 21.53
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10 -8 1 325.58 24.28
-10 -8 -1 301.48 26.43
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-10 -8 -1 298.20 23.25
10 -8 2 16.47 21.78
-10 -8 -2 14.51 23.95
-10 8 -2 -2.37 23.71
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-10 -8 -2 1.90 20.29
10 -8 3 77.71 23.04
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-10 -8 -3 62.57 20.53
-10 -8 -4 2.82 20.31
10 -8 4 7.14 22.90
-10 8 -4 8.23 22.45
-10 -8 -4 6.91 16.68
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-10 -8 -5 12.24 14.44
-10 -8 -5 5.77 23.65
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-10 8 -5 14.80 23.00
-10 -8 -6 63.71 21.19
-10 8 -6 75.48 23.91
-10 -8 -6 54.85 23.79
10 8 6 47.82 14.89
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-10 -8 -7 13.26 24.47
-10 8 -7 4.63 19.88
-10 -8 -7 3.88 27.03
-10 8 -7 11.75 26.48
10 8 7 7.89 24.40
-10 -8 -8 4.15 24.55
10 8 8 -7.92 24.45
-10 -8 -8 23.44 26.78
-10 8 -8 -11.62 28.06
-10 8 -8 11.60 26.60
-10 -8 -9 28.38 27.11
-10 -8 -9 42.53 29.08
10 8 9 17.49 27.05
-10 8 -9 43.78 21.35
-10 8 -9 38.10 32.00
-10 -8 -10 -3.02 20.42
-10 -8 -10 -2.57 31.01
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10 8 10 6.25 20.17
10 -9 0 19.88 15.65
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-10 -9 0 28.82 21.52
10 -9 1 7.15 15.46
-10 -9 -1 5.49 23.32
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-10 -9 -1 -1.64 20.81
10 -9 2 418.80 25.87
-10 -9 -2 273.89 26.28
-10 9 -2 297.37 26.23
-10 9 -2 364.33 25.25
-10 -9 -2 332.93 24.39
10 -9 3 -3.10 27.00
-10 -9 -3 2.25 27.16
-10 9 -3 -17.31 27.57
-10 9 -3 10.05 26.37
-10 -9 -3 6.11 23.87
10 -9 4 29.12 27.55
-10 -9 -4 5.15 27.02
-10 9 -4 14.80 27.72
-10 9 -4 19.11 19.19
-10 -9 -4 15.45 24.16
-10 -9 -5 35.59 24.25
-10 -9 -5 33.51 27.07
-10 9 -5 23.45 26.63
-10 9 -5 30.37 19.37
-10 -9 -6 11.06 24.36
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10 9 6 23.14 24.37
-10 -9 -6 -3.62 27.05
-10 9 -6 18.24 26.27
-10 -9 -7 2.86 26.64
10 9 7 37.27 26.28
-10 9 -7 -9.12 29.81
-10 -9 -7 11.76 21.73
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10 9 8 -13.22 28.67
-10 -9 -8 5.27 28.42
-10 -9 -8 7.65 21.94
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10 -10 0 -4.25 18.31
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-10 -10 0 1.84 24.84
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10 -10 1 172.32 20.32
-10 10 -1 172.51 28.77
-10 10 -1 157.51 27.55
-10 -10 -1 148.55 32.29
-10 -10 -1 146.47 26.37
10 -10 2 10.80 27.39
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-10 10 -2 14.95 19.47
-10 -10 -2 12.06 25.56
-10 -10 -2 34.36 24.18
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10 -10 3 54.10 28.63
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-10 -10 -3 52.48 26.41
-10 -10 -3 44.98 24.82
-10 10 -4 74.07 28.91
-10 -10 -4 66.49 21.66
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-10 -10 -5 5.55 27.84
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11 0 0 -3.25 13.71
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11 0 1 67.50 10.37
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11 0 2 -3.53 9.92
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-11 0 -2 0.39 9.73
11 0 3 504.87 15.41
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-11 0 -4 3.46 14.27
-11 0 -4 2.58 14.25
-11 0 -5 339.45 14.00
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-11 0 -6 10.15 17.43
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-11 0 -7 11.28 18.17
-11 0 -7 1.00 17.87
-11 0 -8 -1.47 17.76
-11 0 -8 2.79 12.59
-11 0 -9 37.54 12.81
-11 0 -9 33.45 17.96
11 0 9 19.00 12.86
-11 0 -10 -7.37 21.37
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11 0 10 -4.26 21.35
-11 0 -11 103.53 15.36
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11 0 11 66.74 15.50
-11 0 -12 -12.12 17.70
-11 0 -12 2.69 25.34
11 0 12 0.77 17.49
-11 0 -13 142.68 18.17
-11 0 -13 83.16 18.73
11 0 13 81.89 18.48
11 0 14 21.06 28.41
-11 0 -14 12.23 28.55
-11 0 -14 -10.39 20.54
11 -1 0 5.27 9.91
11 1 0 20.89 14.28
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11 -1 1 5.50 13.62
11 1 1 6.39 10.16
-11 -1 -1 9.53 10.04
-11 1 -1 -4.51 13.59
-11 1 -1 23.66 13.21
-11 -1 -1 11.09 9.95
11 -1 2 190.66 15.87
11 1 2 166.30 12.36
-11 -1 -2 157.10 11.79
-11 1 -2 183.39 15.45
-11 1 -2 197.83 15.75
-11 -1 -2 197.15 15.54
11 -1 3 111.58 15.73
-11 1 -3 87.10 15.32
-11 -1 -3 98.18 15.31
-11 1 -3 74.86 11.49
-11 -1 -3 108.65 15.31
-11 -1 -4 148.35 15.81
-11 1 -4 92.72 16.02
-11 1 -4 179.02 16.06
-11 -1 -4 125.73 16.21
-11 1 -5 35.10 10.77
-11 -1 -5 47.68 14.97
-11 1 -5 34.95 10.84
-11 -1 -5 39.77 11.15
-11 -1 -6 182.42 14.57
-11 1 -6 169.06 18.48
-11 -1 -6 156.20 13.81
-11 1 -6 178.76 13.74
-11 -1 -7 104.64 18.49
-11 1 -7 89.41 13.06
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-11 1 -7 94.46 13.05
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-11 -1 -8 -1.24 12.72
11 1 8 -4.45 12.91
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-11 -1 -8 0.31 12.84
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-11 -1 -9 20.29 12.89
11 1 9 23.34 12.83
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-11 -1 -9 25.01 18.08
-11 1 -10 -5.31 20.96
-11 -1 -10 -5.58 21.72
-11 -1 -10 -9.68 21.77
11 1 10 19.35 21.17
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-11 1 -11 -10.45 20.73
-11 1 -11 6.32 21.52
-11 -1 -11 -13.65 15.62
-11 -1 -11 23.69 21.24
11 -1 11 6.08 20.65
11 1 11 10.84 21.81
-11 1 -12 14.89 17.25
-11 -1 -12 22.36 17.73
11 1 12 23.28 17.83
-11 1 -12 8.72 25.31
-11 -1 -12 39.24 17.85
11 -1 12 19.86 17.35
-11 1 -13 15.09 17.49
-11 -1 -13 36.07 25.23
11 -1 13 5.49 17.24
-11 1 -13 11.31 25.36
11 1 13 -8.15 25.54
-11 -1 -13 24.86 17.73
-11 -1 -14 275.00 30.48
-11 1 -14 214.71 22.34
-11 -1 -14 252.51 30.50
11 1 14 164.18 30.72
11 -2 0 39.25 9.45
11 2 0 26.37 10.75
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11 -2 1 46.97 13.93
11 2 1 20.94 15.12
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11 -2 2 42.12 14.20
11 2 2 23.84 15.13
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-11 -2 -2 11.84 14.25
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11 -2 3 40.07 15.23
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-11 -2 -3 59.69 14.93
-11 2 -3 82.75 14.58
-11 -2 -3 51.79 11.13
11 -2 4 183.55 16.54
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-11 2 -4 200.67 16.09
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11 2 8 91.82 18.49
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-11 -2 -8 74.15 18.71
-11 2 -8 84.76 17.82
-11 2 -9 197.57 21.61
-11 -2 -9 187.20 16.28
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11 2 9 132.79 22.80
-11 2 -9 187.48 16.38
-11 2 -10 6.88 20.34
-11 -2 -10 6.69 15.43
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11 2 10 3.56 15.40
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-11 -2 -11 -18.41 21.89
11 2 11 1.49 21.66
-11 2 -12 120.41 24.41
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11 2 12 108.62 26.02
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11 -2 13 136.60 25.28
11 2 13 149.95 19.72
11 -3 0 70.47 14.15
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11 -3 1 73.54 10.40
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11 -3 3 158.07 11.79
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11 -3 4 215.12 14.56
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11 3 7 68.71 18.40
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11 3 8 100.92 18.44
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-11 -3 -9 -2.15 21.75
-11 3 -9 8.60 15.23
11 3 9 13.10 21.32
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-11 -3 -10 15.75 21.27
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11 3 11 86.46 25.95
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11 3 12 49.40 26.29
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11 3 13 95.42 21.57
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11 4 0 213.64 13.66
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11 -4 1 231.41 12.06
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11 -4 2 24.77 12.24
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11 -4 3 350.10 15.22
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11 -4 4 130.02 13.26
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11 -7 1 387.81 18.28
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11 -8 0 539.83 26.00
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11 -8 2 -2.13 22.60
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11 -8 4 46.93 16.85
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11 -9 1 137.76 27.00
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12 4 11 16.28 25.52
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12 -5 0 265.05 14.14
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12 -5 1 209.09 18.30
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12 -5 2 -2.42 12.21
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12 -6 1 323.28 22.60
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12 -6 2 192.48 22.42
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12 7 9 3.18 19.51
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12 -8 0 7.42 24.85
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12 -8 2 27.05 18.78
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12 -8 3 163.34 28.16
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12 -8 4 9.32 27.53
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12 -9 0 155.69 27.04
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12 -9 1 63.65 27.00
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13 0 1 795.05 24.18
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13 -1 2 673.05 23.24
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13 -1 3 8.18 17.23
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13 -2 0 200.98 18.04
13 2 0 136.92 14.81
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13 -2 1 322.48 19.75
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13 -2 2 80.80 17.66
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13 -2 4 71.86 13.59
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13 3 11 118.84 29.00
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13 -4 0 166.97 13.39
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13 -4 1 414.14 20.00
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13 -4 4 299.99 17.53
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13 4 10 16.10 19.79
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13 -5 0 230.54 15.79
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13 -5 1 184.81 15.93
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13 -5 2 11.75 14.80
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13 5 10 65.07 28.00
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13 -6 1 34.35 20.76
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13 -6 2 43.17 15.28
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13 -6 3 16.75 21.69
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13 -7 0 141.97 18.10
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13 -7 1 -13.35 25.18
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13 -7 2 7.38 25.43
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13 -7 3 -3.46 26.48
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13 -8 0 37.18 17.83
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13 -8 1 16.94 18.29
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-15 -6 -2 13.24 17.19
-15 6 -3 4.11 27.86
15 -6 3 3.11 27.93
-15 6 -3 -7.83 20.57
-15 -6 -3 6.90 30.91
-15 -6 -3 5.47 25.67
15 -6 4 28.20 30.87
-15 6 -4 72.30 30.11
-15 6 -4 32.53 20.66
-15 -6 -4 -19.02 33.27
-15 -6 -4 11.58 27.64
-15 6 -5 28.72 29.44
-15 6 -5 11.43 31.34
-15 -6 -5 3.52 27.37
-15 -6 -5 -4.66 32.78
15 -7 0 4.57 28.79
-15 -7 0 10.53 33.78
-15 7 0 25.64 21.20
-15 -7 0 20.47 29.03
-15 7 0 2.61 28.79
15 -7 1 55.62 29.57
-15 7 -1 11.37 21.93
-15 7 -1 31.60 29.57
-15 -7 -1 46.95 33.93
-15 -7 -1 28.04 28.90
15 -7 2 2.70 21.35
-15 7 -2 -1.82 21.21
-15 7 -2 5.85 30.47
-15 -7 -2 -8.51 33.93
-15 -7 -2 31.39 27.87
16 0 0 14.22 21.23
-16 0 0 29.06 20.73
-16 0 0 11.47 20.29
16 0 1 6.42 14.92
-16 0 -1 6.09 14.32
-16 0 -1 -3.98 14.95
16 0 2 115.52 24.02
-16 0 -2 93.57 23.91
-16 0 -2 126.16 18.01
-16 0 -3 4.07 17.86
-16 0 -3 -21.59 17.79
-16 0 -4 129.76 18.37
-16 0 -4 138.33 25.55
-16 0 -5 15.53 24.98
-16 0 -5 -15.46 25.17
-16 0 -6 8.61 17.96
-16 0 -6 4.69 17.99
-16 0 -7 41.75 28.67
-16 0 -7 -9.36 20.73
-16 0 -8 216.00 21.87
-16 1 0 5.55 14.35
16 -1 0 -6.18 14.66
16 1 0 -3.59 15.80
-16 1 0 5.99 14.21
-16 -1 0 -8.82 14.48
-16 -1 0 4.98 15.23
16 -1 1 22.31 22.69
16 1 1 -26.85 24.22
-16 -1 -1 -9.58 15.43
-16 1 -1 -6.08 20.53
-16 -1 -1 1.39 22.17
-16 1 -1 -1.94 22.56
16 -1 2 11.21 24.62
-16 1 -2 4.63 24.19
16 1 2 28.34 25.72
-16 -1 -2 22.76 25.30
-16 1 -2 0.07 24.19
-16 -1 -2 14.65 24.02
16 -1 3 59.10 18.36
-16 1 -3 66.92 17.60
-16 1 -3 52.49 24.92
-16 -1 -3 58.39 25.23
-16 -1 -3 45.43 18.27
-16 -1 -4 29.09 25.50
-16 1 -4 22.60 17.44
-16 1 -4 53.17 24.63
-16 -1 -4 18.95 25.12
-16 1 -5 24.83 17.62
-16 -1 -5 20.75 25.57
-16 1 -5 21.43 25.18
-16 -1 -5 21.20 17.87
-16 1 -6 -2.25 25.21
-16 -1 -6 -6.50 18.30
-16 1 -6 10.43 17.70
-16 -1 -6 7.23 25.18
-16 1 -7 149.32 21.45
-16 -1 -7 173.46 29.77
-16 1 -7 208.27 21.31
-16 -1 -7 183.12 29.88
16 -2 0 129.65 24.68
16 2 0 183.91 27.45
-16 -2 0 124.14 27.44
-16 2 0 130.43 24.58
-16 2 0 127.69 17.48
-16 -2 0 149.74 17.82
16 -2 1 21.79 24.32
16 2 1 28.86 19.05
-16 2 -1 49.13 23.61
-16 -2 -1 25.46 26.46
-16 2 -1 13.62 23.93
-16 -2 -1 41.39 24.07
-16 2 -2 24.42 23.89
16 -2 2 4.37 24.30
-16 2 -2 5.93 23.96
-16 -2 -2 -3.41 18.96
-16 -2 -2 7.84 24.16
-16 -2 -3 -16.10 26.54
16 -2 3 -9.94 24.68
-16 2 -3 12.40 24.16
-16 2 -3 24.00 24.37
-16 -2 -3 -11.86 24.72
-16 -2 -4 -7.77 26.45
-16 2 -4 46.83 24.62
-16 2 -4 -0.16 17.70
-16 -2 -4 12.27 24.62
-16 2 -5 5.80 17.74
-16 -2 -5 5.46 18.46
-16 2 -5 -21.14 25.27
-16 -2 -5 21.41 24.69
-16 2 -6 58.71 27.44
-16 -2 -6 65.32 21.48
-16 2 -6 46.74 20.58
-16 -2 -6 32.49 27.29
-16 2 -7 -3.17 29.31
-16 -2 -7 -10.23 29.48
-16 2 -7 12.46 20.40
-16 -2 -7 5.53 28.92
16 -3 0 297.32 25.62
16 3 0 328.19 29.58
-16 3 0 275.56 25.10
-16 -3 0 316.18 29.07
-16 3 0 256.21 18.15
-16 -3 0 263.54 25.22
16 -3 1 26.66 24.04
-16 3 -1 -16.95 24.07
-16 3 -1 -5.92 16.84
-16 -3 -1 13.27 27.46
-16 -3 -1 4.50 23.86
-16 -3 -2 77.46 20.31
16 -3 2 121.94 25.22
-16 3 -2 100.23 17.41
-16 -3 -2 77.42 24.80
-16 3 -2 90.21 17.78
16 -3 3 -6.93 25.08
-16 -3 -3 -8.98 19.41
-16 3 -3 2.66 24.51
-16 3 -3 16.32 17.32
-16 -3 -3 -10.43 24.25
-16 -3 -4 -12.01 27.20
-16 3 -4 -11.39 25.18
-16 3 -4 -8.00 25.05
-16 -3 -4 -7.76 24.22
-16 -3 -5 21.98 29.05
-16 3 -5 22.02 17.90
-16 -3 -5 21.46 17.69
-16 3 -5 15.59 18.42
-16 3 -6 16.70 29.65
-16 -3 -6 35.57 30.89
-16 3 -6 44.77 28.91
-16 -3 -6 49.52 28.29
16 -4 0 21.42 24.16
-16 4 0 11.85 23.89
-16 -4 0 9.51 17.06
-16 4 0 -7.26 23.69
-16 -4 0 -1.74 20.43
-16 -4 -1 250.30 21.84
-16 4 -1 253.03 18.82
16 -4 1 272.69 19.48
-16 4 -1 283.52 25.20
-16 -4 -1 246.05 25.52
16 -4 2 6.24 25.08
-16 -4 -2 8.01 20.06
-16 4 -2 -12.38 24.52
-16 4 -2 -4.53 24.87
-16 -4 -2 -10.44 17.29
16 -4 3 -3.92 18.15
-16 4 -3 14.09 17.71
-16 -4 -3 -1.11 28.20
-16 4 -3 13.49 24.71
-16 -4 -3 -5.75 17.06
16 -4 4 -9.74 29.75
-16 -4 -4 19.65 32.10
-16 4 -4 -15.43 29.18
-16 4 -4 1.28 20.36
-16 -4 -4 5.37 19.78
-16 -4 -5 -5.11 31.67
-16 4 -5 21.78 28.69
-16 -4 -5 -13.47 28.02
-16 4 -5 22.85 29.69
-16 -5 0 76.10 31.91
16 -5 0 88.81 27.07
-16 5 0 66.42 17.81
-16 5 0 90.50 26.82
-16 -5 0 80.13 18.14
16 -5 1 53.97 26.65
-16 -5 -1 33.68 31.64
-16 5 -1 30.58 28.55
-16 -5 -1 64.32 27.99
-16 5 -1 24.97 26.82
16 -5 2 34.15 20.41
-16 -5 -2 3.62 33.27
-16 5 -2 12.20 28.21
-16 5 -2 3.24 20.52
-16 -5 -2 28.81 19.45
16 -5 3 16.75 29.23
-16 5 -3 20.68 28.99
-16 -5 -3 26.55 33.04
-16 5 -3 -8.59 28.56
-16 -5 -3 16.86 19.35
-16 -5 -4 26.07 33.18
-16 -5 -4 26.33 19.69
-16 -6 0 10.73 23.97
-16 6 0 3.42 20.11
-16 6 0 15.79 20.38
-16 -6 0 18.71 28.61
17 0 0 -18.04 25.74
-17 0 0 -17.17 17.17
-17 0 0 4.57 24.79
17 0 1 106.58 26.33
-17 0 -1 96.51 25.89
-17 0 -1 100.58 25.25
17 0 2 -53.39 26.11
-17 0 -2 -36.59 25.49
-17 0 -2 -25.03 25.35
-17 0 -3 177.85 19.05
-17 0 -3 152.88 18.79
-17 0 -4 -20.30 20.84
-17 0 -4 -4.39 28.92
-17 0 -5 81.17 30.06
-17 0 -5 125.83 21.46
-17 -1 0 11.83 26.16
17 -1 0 29.89 24.61
17 1 0 1.05 26.08
-17 1 0 1.66 23.91
-17 1 0 -12.79 23.81
-17 -1 0 -1.20 24.11
17 -1 1 9.72 24.84
17 1 1 6.46 26.22
-17 -1 -1 1.07 26.14
-17 1 -1 4.94 24.21
-17 -1 -1 -12.99 24.76
-17 1 -1 15.59 24.35
17 -1 2 252.79 19.23
-17 1 -2 236.21 18.78
-17 -1 -2 231.50 27.51
-17 1 -2 256.63 26.16
-17 -1 -2 237.46 25.98
17 -1 3 -15.15 18.27
-17 1 -3 -3.26 18.04
-17 1 -3 -17.72 27.25
-17 -1 -3 14.48 26.71
-17 -1 -3 21.29 21.10
-17 -1 -4 0.54 21.20
-17 1 -4 2.76 20.47
-17 -1 -4 -0.91 20.84
-17 1 -4 31.77 28.71
-17 1 -5 -10.31 29.22
-17 -1 -5 10.56 21.25
-17 1 -5 10.41 29.32
-17 -1 -5 -6.78 29.22
-17 2 0 100.63 17.45
17 -2 0 101.20 17.74
17 2 0 103.87 27.82
-17 -2 0 116.36 27.09
-17 2 0 91.73 17.57
-17 -2 0 75.87 24.86
17 -2 1 16.45 25.18
17 2 1 49.20 19.62
-17 -2 -1 24.19 19.36
-17 2 -1 32.74 17.44
-17 -2 -1 15.75 24.52
-17 2 -1 35.42 24.60
17 -2 2 15.84 26.65
-17 2 -2 13.72 26.54
-17 2 -2 -7.85 26.44
-17 -2 -2 7.10 26.53
-17 -2 -2 8.62 19.12
-17 -2 -3 65.90 22.20
17 -2 3 89.76 20.57
-17 2 -3 85.33 20.36
-17 2 -3 86.12 29.02
-17 -2 -3 50.31 28.94
-17 -2 -4 -11.58 22.01
-17 2 -4 15.06 20.64
-17 2 -4 -10.85 29.08
-17 -2 -4 15.52 20.00
17 -3 0 15.14 19.40
17 3 0 -10.81 32.95
-17 -3 0 25.70 32.05
-17 3 0 9.18 19.31
-17 -3 0 3.49 19.89
-17 3 0 -2.80 19.65
17 -3 1 87.19 28.88
-17 3 -1 62.87 28.47
-17 3 -1 112.31 28.25
-17 -3 -1 96.56 28.35
-17 -3 -1 99.43 32.77
-17 -3 -2 9.30 32.26
-17 3 -2 3.46 28.65
17 -3 2 5.52 28.62
-17 3 -2 -14.70 28.67
-17 -3 -2 -0.64 28.15
17 -3 3 27.67 20.48
-17 -3 -3 -2.93 32.15
-17 3 -3 27.31 20.42
-17 3 -3 8.33 28.84
-17 -3 -3 20.04 28.33
-17 -3 -4 88.98 20.45
17 -4 0 282.01 29.88
-17 4 0 199.38 29.57
-17 4 0 239.01 29.03
-17 -4 0 261.13 29.57
-17 -4 0 225.50 25.37
-17 -4 -1 36.58 23.94
17 -4 1 42.59 28.94
-17 4 -1 24.38 28.66
-17 4 -1 32.91 28.14
-17 -4 -1 49.10 28.28
-17 4 -2 95.39 20.67
18 0 0 249.26 22.12
-18 0 0 238.78 30.21
-18 1 0 -7.28 20.45
;
_shelx_hkl_checksum 19365
_shelx_res_file
;
TITL CUCL6 IPDS2 -120DEGC
G:\CuCl_L6\mulabs\CUCL6.res
created by SHELXL-2016/6 at 20:19:44 on 18-Aug-2017
CELL 0.71073 14.71000 10.71630 14.93120 90.00000 91.82800 90.00000
ZERR 2 0.00110 0.00060 0.00120 0.00000 0.01000 0.00000
LATT 1
SYMM -X+ 0.50000, Y+ 0.50000, -Z+ 0.50000
SFAC C H CL CU N O
UNIT 64 144 8 4 8 28
TEMP -120
PLAN 10
FMAP 2
L.S. 9
BOND $H
DFIX 0.88 .02 O1W H1WA O1W H1WB O2W H2WA O2W H2WB O3W H3WA O3W H3WB
DFIX 1.40 .02 H1WA H1WB H2WA H2WB H3WA H3WB
HTAB
EQIV $2 X, Y-1, Z
HTAB N1 CL1_$2
EQIV $3 -X+1, -Y, -Z+1
HTAB N1 O1W_$3
EQIV $4 -X+3/2, Y-1/2, -Z+3/2
HTAB N1 CL1_$4
EQIV $5 X+1/2, -Y+1/2, Z-1/2
HTAB N2 O2W_$5
EQIV $6 -X+3/2, Y-1/2, -Z+1/2
HTAB N2 CL1_$6
EQIV $7 -X+1, -Y+1, -Z
HTAB N2 CL2_$7
HTAB C5 CL1_$4
HTAB O1W CL2_$7
EQIV $8 X-1/2, -Y+3/2, Z+1/2
HTAB O2W CL2_$8
EQIV $1 -X+1, -Y+1, -Z+1
HTAB O2W O3_$1
EQIV $9 X-1/2, -Y+1/2, Z-1/2
HTAB O3W CL1_$9
EQIV $10 -X+1/2, Y-1/2, -Z+1/2
HTAB O3W CL2_$10
CONF
ACTA
WGHT 0.133100
FVAR 0.43332
CU1 4 0.571999 0.533415 0.550868 11.00000 0.01521 0.02911 =
0.01441 0.00099 0.00360 0.00048
CL1 3 0.693858 0.591263 0.663742 11.00000 0.02131 0.03521 =
0.01932 0.00051 0.00011 -0.00451
O1 6 0.572684 0.357161 0.583266 11.00000 0.03482 0.03871 =
0.04068 0.01174 -0.01291 -0.00922
O2 6 0.450508 0.301423 0.500912 11.00000 0.03500 0.03340 =
0.04111 -0.00352 -0.01585 0.00177
O3 6 0.647726 0.490539 0.447096 11.00000 0.01949 0.05023 =
0.01949 -0.00489 0.00222 -0.00292
O4 6 0.524963 0.438094 0.363974 11.00000 0.01871 0.08845 =
0.02651 -0.01836 0.00566 -0.00611
N1 5 0.687592 -0.179073 0.812261 11.00000 0.03142 0.03161 =
0.03816 0.00068 -0.00643 0.00676
AFIX 137
H1A 2 0.715646 -0.207468 0.762784 11.00000 -1.50000
H1B 2 0.688742 -0.239545 0.855069 11.00000 -1.50000
H1C 2 0.717108 -0.110116 0.833690 11.00000 -1.50000
AFIX 0
N2 5 0.672665 0.196075 -0.023704 11.00000 0.04108 0.05601 =
0.03934 -0.01894 0.01823 0.00071
AFIX 137
H2A 2 0.674668 0.130093 0.014673 11.00000 -1.50000
H2B 2 0.702133 0.175997 -0.074399 11.00000 -1.50000
H2C 2 0.613684 0.215079 -0.038025 11.00000 -1.50000
AFIX 0
C1 1 0.515402 0.277130 0.555057 11.00000 0.02441 0.03104 =
0.01810 0.00406 0.00667 0.00361
C2 1 0.522531 0.147070 0.591574 11.00000 0.03241 0.02471 =
0.03208 -0.00288 -0.00777 0.00111
AFIX 13
H2 2 0.490146 0.089283 0.548741 11.00000 -1.20000
AFIX 0
C3 1 0.622436 0.103300 0.603430 11.00000 0.03227 0.04791 =
0.03398 0.01070 0.01637 0.01514
AFIX 23
H3A 2 0.650187 0.098871 0.543974 11.00000 -1.20000
H3B 2 0.657016 0.165255 0.640008 11.00000 -1.20000
AFIX 0
C4 1 0.629540 -0.023042 0.648250 11.00000 0.03881 0.03981 =
0.03759 0.00315 -0.00086 0.01504
AFIX 23
H4A 2 0.694444 -0.045681 0.657197 11.00000 -1.20000
H4B 2 0.600371 -0.086743 0.608849 11.00000 -1.20000
AFIX 0
C5 1 0.584121 -0.022703 0.737930 11.00000 0.02009 0.02908 =
0.03698 0.00372 -0.00208 0.00104
AFIX 13
H5 2 0.614942 0.042295 0.776158 11.00000 -1.20000
AFIX 0
C6 1 0.483721 0.014873 0.725809 11.00000 0.02193 0.03646 =
0.08381 0.02182 0.00956 0.00234
AFIX 23
H6A 2 0.451049 -0.048267 0.688621 11.00000 -1.20000
H6B 2 0.455311 0.017746 0.784995 11.00000 -1.20000
AFIX 0
C7 1 0.475442 0.141777 0.681066 11.00000 0.01933 0.03733 =
0.05558 0.01891 0.01001 0.00701
AFIX 23
H7A 2 0.502404 0.205796 0.721666 11.00000 -1.20000
H7B 2 0.410239 0.162109 0.671203 11.00000 -1.20000
AFIX 0
C8 1 0.591520 -0.146499 0.788111 11.00000 0.02833 0.03997 =
0.05091 0.00886 0.00384 0.00496
AFIX 23
H8A 2 0.556328 -0.141231 0.843406 11.00000 -1.20000
H8B 2 0.564509 -0.213527 0.750187 11.00000 -1.20000
AFIX 0
C9 1 0.609875 0.451404 0.375997 11.00000 0.02191 0.02963 =
0.02180 0.00376 0.00449 0.00127
C10 1 0.667925 0.418153 0.296562 11.00000 0.01383 0.03878 =
0.02093 0.00048 0.00462 0.00097
AFIX 13
H10 2 0.733515 0.427604 0.315003 11.00000 -1.20000
AFIX 0
C11 1 0.646108 0.508073 0.218656 11.00000 0.03378 0.02950 =
0.02358 -0.00114 0.00796 0.00242
AFIX 23
H11A 2 0.579838 0.507245 0.204844 11.00000 -1.20000
H11B 2 0.663545 0.593965 0.236560 11.00000 -1.20000
AFIX 0
C12 1 0.696993 0.471040 0.135139 11.00000 0.03209 0.03701 =
0.02126 0.00430 0.00981 0.00428
AFIX 23
H12A 2 0.681611 0.530032 0.085930 11.00000 -1.20000
H12B 2 0.763338 0.475985 0.147985 11.00000 -1.20000
AFIX 0
C13 1 0.672186 0.340523 0.106322 11.00000 0.01996 0.03498 =
0.02414 -0.00563 0.01006 0.00422
AFIX 13
H13 2 0.604822 0.337427 0.095228 11.00000 -1.20000
AFIX 0
C14 1 0.696518 0.249487 0.182999 11.00000 0.03064 0.03026 =
0.03948 0.00032 0.01123 0.00247
AFIX 23
H14A 2 0.677871 0.164112 0.164965 11.00000 -1.20000
H14B 2 0.763281 0.249287 0.193720 11.00000 -1.20000
AFIX 0
C15 1 0.650748 0.283753 0.269284 11.00000 0.03570 0.03079 =
0.02974 0.00233 0.01148 0.00277
AFIX 23
H15A 2 0.584401 0.270120 0.261501 11.00000 -1.20000
H15B 2 0.673527 0.227990 0.317868 11.00000 -1.20000
AFIX 0
C16 1 0.717385 0.305086 0.019603 11.00000 0.02919 0.04735 =
0.02819 -0.01187 0.01301 0.00251
AFIX 23
H16A 2 0.714618 0.376924 -0.022083 11.00000 -1.20000
H16B 2 0.782239 0.285487 0.032601 11.00000 -1.20000
AFIX 0
CL2 3 0.531204 0.734393 0.071905 11.00000 0.04527 0.06465 =
0.05177 0.01281 0.01220 -0.00124
O1W 6 0.351535 0.385033 0.084903 11.00000 0.06224 0.06768 =
0.05079 0.02149 0.01402 0.00759
H1WA 2 0.384777 0.405410 0.038149 11.00000 -1.50000
H1WB 2 0.393272 0.383056 0.129847 11.00000 -1.50000
O2W 6 0.169373 0.561231 0.504045 11.00000 0.04846 0.07545 =
0.07064 -0.01884 -0.00828 0.01154
H2WA 2 0.134446 0.588825 0.548321 11.00000 -1.50000
H2WB 2 0.222069 0.601670 0.513794 11.00000 -1.50000
O3W 6 0.119368 0.103885 0.311773 11.00000 0.05223 0.08052 =
0.05288 -0.03412 -0.00041 0.01809
H3WA 2 0.103633 0.075011 0.258612 11.00000 -1.50000
H3WB 2 0.072737 0.147803 0.329208 11.00000 -1.50000
HKLF 4
REM CUCL6 IPDS2 -120DEGC
REM R1 = 0.0666 for 3172 Fo > 4sig(Fo) and 0.0907 for all 4545 data
REM 273 parameters refined using 9 restraints
END
WGHT 0.1334 0.0000
REM Instructions for potential hydrogen bonds
HTAB N1 Cl1_$2
HTAB N1 O1W_$3
HTAB N1 Cl1_$4
HTAB N2 O2W_$5
HTAB N2 Cl1_$6
HTAB N2 Cl2_$7
HTAB C5 Cl1_$4
HTAB O1W Cl2_$7
HTAB O2W Cl2_$8
HTAB O2W O3_$1
HTAB O3W Cl1_$9
HTAB O3W Cl2_$10
REM Highest difference peak 1.797, deepest hole -0.927, 1-sigma level 0.143
Q1 1 0.6091 0.4412 0.5789 11.00000 0.05 1.80
Q2 1 0.4639 0.3774 0.4727 11.00000 0.05 1.70
Q3 1 0.5401 0.4379 0.5293 11.00000 0.05 1.49
Q4 1 0.6088 0.6257 0.5739 11.00000 0.05 1.31
Q5 1 0.7351 0.5024 0.6802 11.00000 0.05 1.02
Q6 1 0.0964 0.5648 0.5874 11.00000 0.05 0.99
Q7 1 0.7362 0.6691 0.6788 11.00000 0.05 0.82
Q8 1 0.6637 0.6796 0.6344 11.00000 0.05 0.80
Q9 1 0.6661 0.4933 0.6378 11.00000 0.05 0.62
Q10 1 0.5593 0.8353 0.0912 11.00000 0.05 0.61
;
_shelx_res_checksum 76319
data_Global
_journal_date_recd_electronic 2017-08-28
_journal_date_accepted 2017-08-31
_journal_name_full 'Acta Crystallographica, Section E'
_journal_year 2017
_journal_volume 73
_journal_issue 10
_journal_page_first 1421
_journal_page_last 1425
_journal_paper_category GM
_journal_paper_doi 10.1107/S2056989017012543
_journal_coeditor_code WM5416
_publ_contact_author_name 'Helen Stoeckli-Evans'
_publ_contact_author_address
;
Institute of Physics
University of Neuch\^atel
rue Emile-Argand11
CH-2000 Neuch\^atel
Switzerland
;
_publ_contact_author_email
'helen.stoeckli-evans@unine.ch, altaf_dr@hotmail.com'
_publ_contact_author_fax '+41 32 718 25 11'
_publ_contact_author_phone '+41 32 718 24 26'
_publ_section_title
;\
A copper(II) paddle-wheel structure of tranexamic acid:
dichloro-tetrakis[\m-4-(ammoniomethyl)cyclohexane-1-carboxylato-\
O,O']dicopper(II) dichloride hexahydrate
;
loop_
_publ_author_name
_publ_author_address
'Altaf, Muhammad'
;
Center of Excellence in Nanotechnology,
King Fahd University of Petroleum
& Minerals, 31261 Dahran
Saudi Arabia
;
'Stoeckli-Evans, Helen'
;
Institute of Physics
University of Neuch\^atel
rue Emile-Argand 11
CH-2000 Neuch\^atel
Switzerland
;
_publ_section_synopsis
;
Tranexamic acid is an antifibrinolytic amino acid that exists as a zwitterion
[trans-4-(ammoniomethyl)cyclohexane-1-carboxylate] in the solid state.
Its reaction with copper chloride lead to the formation of a copper(II)
paddle-wheel structure.
;