##############################################################################
# #
# 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 #
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# #
# This file may be used for bona fide research purposes within the #
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data_I
_database_code_depnum_ccdc_archive 'CCDC 1521075'
_audit_creation_method 'SHELXL-2014/7'
_journal_date_recd_electronic 2016-11-30
_journal_date_accepted 2016-12-06
_journal_name_full 'Acta Crystallographica, Section E'
_journal_year 2017
_journal_volume 73
_journal_issue 1
_journal_page_first 31
_journal_page_last 34
_journal_paper_category GM
_journal_paper_doi 10.1107/S2056989016019563
_journal_coeditor_code ZL2687
_publ_contact_author_name 'Elizabeth T. Papish'
_publ_contact_author_address
;
Department of Chemistry
University of Alabama
250 Hackberry Lane
Tuscaloosa, AL 35487-0336
USA
;
_publ_contact_author_email 'etpapish@ua.edu'
_publ_contact_author_fax ?
_publ_contact_author_phone ?
_publ_section_title
;\
Crystal structure of
(perchlorato-\kO)(1,4,7,10-tetraazacyclododecane-\k^4^N)\
copper(II) perchlorate
;
_publ_section_title_footnote .
loop_
_publ_author_name
_publ_author_footnote
_publ_author_address
'Gray, Jessica L.' .
;
Department of Chemistry
University of Alabama
250 Hackberry Lane
Tuscaloosa, AL 35487-0336
USA
;
'Gerlach, Deidra L.' .
;
Department of Chemistry
University of Alabama
250 Hackberry Lane
Tuscaloosa, AL 35487-0336
USA
;
'Papish, Elizabeth T.' .
;
Department of Chemistry
University of Alabama
250 Hackberry Lane
Tuscaloosa, AL 35487-0336
USA
;
_publ_section_synopsis
;\
The crystal structure of
(perchlorato-\kO)(1,4,7,10-tetraazacyclododecane-\k^4^N)\
copper(II) perchlorate is reported. The crystal was grown from a solution of
methanol at ambient temperature which resulted in no co-crystallization of
solvent.
;
_chemical_name_systematic
;
(Perchlorato-\kO)(1,4,7,10-tetraazacyclododecane-\k^4^N)copper(II)
perchlorate
;
_chemical_name_common '[Cu cyclen](ClO4)2'
_chemical_formula_moiety 'C8 H20 Cl1 Cu N4 O4 +, Cl1 O4 -'
_chemical_formula_sum 'C8 H20 Cl2 Cu N4 O8'
_chemical_formula_iupac '[Cu (Cl O4) (C8 H20 N4)] Cl1 O4'
_chemical_formula_weight 434.72
_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 8.9387(2)
_cell_length_b 15.0607(4)
_cell_length_c 11.9235(3)
_cell_angle_alpha 90
_cell_angle_beta 92.9490(10)
_cell_angle_gamma 90
_cell_volume 1603.05(7)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9899
_cell_measurement_theta_min 2.2815
_cell_measurement_theta_max 35.8550
_cell_measurement_temperature 173(2)
_exptl_crystal_description block
_exptl_crystal_colour purple
_exptl_crystal_size_max 0.230
_exptl_crystal_size_mid 0.210
_exptl_crystal_size_min 0.180
_exptl_crystal_density_diffrn 1.801
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_F_000 892
_exptl_absorpt_coefficient_mu 1.741
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2014)
;
_shelx_estimated_absorpt_T_min 0.690
_shelx_estimated_absorpt_T_max 0.745
_exptl_absorpt_correction_T_min 0.6672
_exptl_absorpt_correction_T_max 0.7471
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_device_type 'Bruker SMART APEXII CCD'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 43306
_diffrn_reflns_av_R_equivalents 0.0208
_diffrn_reflns_theta_min 2.180
_diffrn_reflns_theta_max 36.160
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -24
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 12
_refine_special_details ?
_reflns_number_total 7519
_reflns_number_gt 6655
_reflns_threshold_expression 'I > 2\s(I)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.0297
_refine_ls_R_factor_gt 0.0247
_refine_ls_wR_factor_gt 0.0652
_refine_ls_wR_factor_ref 0.0675
_refine_ls_goodness_of_fit_ref 1.022
_refine_ls_restrained_S_all 1.022
_refine_ls_number_reflns 7519
_refine_ls_number_parameters 221
_refine_ls_number_restraints 6
_refine_ls_hydrogen_treatment mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+0.4526P] 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 0.003
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.596
_refine_diff_density_min -0.438
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_extinction_coef 0.0025(3)
_refine_ls_extinction_expression
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0061 0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0106 0.0060
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'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'
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_cell_refinement
;
SAINT-Plus (Bruker, 2013)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2013)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015) and
SHELXLE (H\"ubschle et al., 2011)
;
_computing_molecular_graphics ?
_computing_publication_material ?
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
C C1 0.42855(13) 0.41595(9) 0.83806(10) 0.0315(2) Uani d 1 . .
H H1A 0.5240 0.4277 0.8813 0.038 Uiso calc 1 . .
H H1B 0.4043 0.3521 0.8450 0.038 Uiso calc 1 . .
C C2 0.30439(15) 0.47211(10) 0.88238(9) 0.0341(2) Uani d 1 . .
H H2A 0.2850 0.4540 0.9601 0.041 Uiso calc 1 . .
H H2B 0.3344 0.5354 0.8835 0.041 Uiso calc 1 . .
C C3 0.07219(14) 0.38402(9) 0.83922(11) 0.0330(2) Uani d 1 . .
H H3A 0.0198 0.3977 0.9083 0.040 Uiso calc 1 . .
H H3B 0.1353 0.3308 0.8533 0.040 Uiso calc 1 . .
C C4 -0.04050(12) 0.36717(8) 0.74254(13) 0.0353(3) Uani d 1 . .
H H4A -0.0945 0.3110 0.7554 0.042 Uiso calc 1 . .
H H4B -0.1148 0.4160 0.7378 0.042 Uiso calc 1 . .
C C5 0.08786(13) 0.27094(7) 0.60632(10) 0.0297(2) Uani d 1 . .
H H5A 0.0006 0.2334 0.5836 0.036 Uiso calc 1 . .
H H5B 0.1415 0.2431 0.6720 0.036 Uiso calc 1 . .
C C6 0.19107(16) 0.27947(8) 0.51035(10) 0.0345(2) Uani d 1 . .
H H6A 0.2356 0.2209 0.4943 0.041 Uiso calc 1 . .
H H6B 0.1335 0.2998 0.4420 0.041 Uiso calc 1 . .
C C7 0.44486(13) 0.30541(7) 0.60226(11) 0.0302(2) Uani d 1 . .
H H7A 0.5046 0.2707 0.5500 0.036 Uiso calc 1 . .
H H7B 0.4126 0.2651 0.6620 0.036 Uiso calc 1 . .
C C8 0.53867(12) 0.38048(8) 0.65356(12) 0.0315(2) Uani d 1 . .
H H8A 0.6201 0.3558 0.7037 0.038 Uiso calc 1 . .
H H8B 0.5847 0.4147 0.5934 0.038 Uiso calc 1 . .
H H1 0.4734(19) 0.4937(9) 0.7172(14) 0.038 Uiso d 1 . .
H H2 0.1146(18) 0.5097(10) 0.8063(14) 0.038 Uiso d 1 . .
H H3 -0.0155(19) 0.3802(12) 0.5781(13) 0.038 Uiso d 1 . .
H H4 0.3389(19) 0.3719(11) 0.4820(12) 0.038 Uiso d 1 . .
N N1 0.44205(10) 0.43993(6) 0.71871(8) 0.02310(15) Uani d 1 . .
N N2 0.16614(10) 0.46012(7) 0.80849(8) 0.02595(16) Uani d 1 . .
N N3 0.03746(11) 0.36146(6) 0.63546(9) 0.02866(19) Uani d 1 . .
N N4 0.31208(12) 0.34444(6) 0.54087(8) 0.02774(18) Uani d 1 . .
O O1 0.19181(10) 0.55583(5) 0.55695(6) 0.02513(14) Uani d 1 . .
O O2 0.40695(9) 0.63197(6) 0.62923(8) 0.03461(19) Uani d 1 . .
O O3 0.17927(13) 0.64843(8) 0.71488(9) 0.0461(3) Uani d 1 . .
O O4 0.21084(11) 0.71021(6) 0.53609(9) 0.0388(2) Uani d 1 . .
O O5 0.24547(13) 0.44353(6) 0.31635(7) 0.0375(2) Uani d 1 . .
O O6 0.36978(11) 0.40926(8) 0.15317(8) 0.0381(2) Uani d 1 . .
O O7 0.21333(13) 0.30342(6) 0.23229(9) 0.0411(2) Uani d 1 . .
O O8 0.10864(11) 0.42926(7) 0.14227(8) 0.0380(2) Uani d 1 . .
Cl Cl1 0.24776(3) 0.63777(2) 0.61025(2) 0.02082(4) Uani d 1 . .
Cl Cl2 0.23354(3) 0.39588(2) 0.21099(2) 0.02216(5) Uani d 1 . .
Cu Cu1 0.23119(2) 0.42802(2) 0.65438(2) 0.01773(3) Uani 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
C1 0.0265(5) 0.0390(6) 0.0278(5) -0.0022(4) -0.0100(4) 0.0095(4)
C2 0.0368(6) 0.0465(7) 0.0184(4) -0.0037(5) -0.0038(4) -0.0015(4)
C3 0.0296(5) 0.0328(5) 0.0375(6) 0.0004(4) 0.0110(4) 0.0077(4)
C4 0.0176(4) 0.0285(5) 0.0600(8) -0.0005(4) 0.0049(5) 0.0049(5)
C5 0.0299(5) 0.0191(4) 0.0386(5) -0.0049(3) -0.0117(4) 0.0052(4)
C6 0.0523(7) 0.0237(5) 0.0266(5) -0.0087(5) -0.0064(5) -0.0022(4)
C7 0.0307(5) 0.0206(4) 0.0402(6) 0.0008(4) 0.0099(4) 0.0013(4)
C8 0.0199(4) 0.0252(5) 0.0501(7) -0.0006(3) 0.0081(4) 0.0014(4)
N1 0.0190(3) 0.0217(3) 0.0282(4) -0.0023(3) -0.0021(3) 0.0033(3)
N2 0.0241(4) 0.0280(4) 0.0259(4) 0.0011(3) 0.0030(3) 0.0013(3)
N3 0.0236(4) 0.0208(4) 0.0400(5) -0.0022(3) -0.0134(3) 0.0065(3)
N4 0.0403(5) 0.0208(4) 0.0224(4) -0.0040(3) 0.0032(3) 0.0018(3)
O1 0.0361(4) 0.0155(3) 0.0227(3) -0.0025(3) -0.0091(3) -0.0012(2)
O2 0.0213(4) 0.0348(4) 0.0466(5) -0.0019(3) -0.0095(3) 0.0080(4)
O3 0.0542(6) 0.0452(6) 0.0408(5) -0.0136(5) 0.0192(4) -0.0216(4)
O4 0.0420(5) 0.0181(3) 0.0538(5) -0.0016(3) -0.0219(4) 0.0084(3)
O5 0.0614(6) 0.0281(4) 0.0222(3) 0.0054(4) -0.0054(4) -0.0058(3)
O6 0.0258(4) 0.0516(6) 0.0371(4) -0.0021(4) 0.0033(3) 0.0019(4)
O7 0.0536(6) 0.0203(4) 0.0493(5) -0.0032(4) 0.0031(5) -0.0015(4)
O8 0.0302(4) 0.0538(6) 0.0295(4) 0.0164(4) -0.0042(3) -0.0005(4)
Cl1 0.02111(9) 0.01695(8) 0.02384(9) -0.00122(7) -0.00426(7) -0.00201(7)
Cl2 0.02481(10) 0.02058(9) 0.02081(9) 0.00237(7) -0.00149(7) -0.00166(7)
Cu1 0.01806(5) 0.01641(5) 0.01824(5) -0.00136(3) -0.00382(4) 0.00267(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
C1 N1 . 1.4791(14) ?
C1 C2 . 1.5122(19) ?
C1 H1A . 0.9900 ?
C1 H1B . 0.9900 ?
C2 N2 . 1.4913(15) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 N2 . 1.4781(16) ?
C3 C4 . 1.513(2) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C4 N3 . 1.4881(18) ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C5 N3 . 1.4826(15) ?
C5 C6 . 1.5118(19) ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C6 N4 . 1.4898(15) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C7 N4 . 1.4835(16) ?
C7 C8 . 1.5174(17) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C8 N1 . 1.4901(15) ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
N1 Cu1 . 2.0061(9) ?
N1 H1 . 0.858(14) ?
N2 Cu1 . 2.0145(9) ?
N2 H2 . 0.876(14) ?
N3 Cu1 . 2.0036(9) ?
N3 H3 . 0.859(13) ?
N4 Cu1 . 2.0099(10) ?
N4 H4 . 0.859(13) ?
O1 Cl1 . 1.4644(7) ?
O1 Cu1 . 2.2664(7) ?
O2 Cl1 . 1.4320(8) ?
O3 Cl1 . 1.4267(10) ?
O4 Cl1 . 1.4321(9) ?
O5 Cl2 . 1.4459(9) ?
O6 Cl2 . 1.4441(10) ?
O7 Cl2 . 1.4285(9) ?
O8 Cl2 . 1.4409(9) ?
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
N1 C1 C2 . . 107.30(9) ?
N1 C1 H1A . . 110.3 ?
C2 C1 H1A . . 110.3 ?
N1 C1 H1B . . 110.3 ?
C2 C1 H1B . . 110.3 ?
H1A C1 H1B . . 108.5 ?
N2 C2 C1 . . 109.06(9) ?
N2 C2 H2A . . 109.9 ?
C1 C2 H2A . . 109.9 ?
N2 C2 H2B . . 109.9 ?
C1 C2 H2B . . 109.9 ?
H2A C2 H2B . . 108.3 ?
N2 C3 C4 . . 107.81(10) ?
N2 C3 H3A . . 110.1 ?
C4 C3 H3A . . 110.1 ?
N2 C3 H3B . . 110.1 ?
C4 C3 H3B . . 110.1 ?
H3A C3 H3B . . 108.5 ?
N3 C4 C3 . . 109.92(9) ?
N3 C4 H4A . . 109.7 ?
C3 C4 H4A . . 109.7 ?
N3 C4 H4B . . 109.7 ?
C3 C4 H4B . . 109.7 ?
H4A C4 H4B . . 108.2 ?
N3 C5 C6 . . 107.69(9) ?
N3 C5 H5A . . 110.2 ?
C6 C5 H5A . . 110.2 ?
N3 C5 H5B . . 110.2 ?
C6 C5 H5B . . 110.2 ?
H5A C5 H5B . . 108.5 ?
N4 C6 C5 . . 109.55(9) ?
N4 C6 H6A . . 109.8 ?
C5 C6 H6A . . 109.8 ?
N4 C6 H6B . . 109.8 ?
C5 C6 H6B . . 109.8 ?
H6A C6 H6B . . 108.2 ?
N4 C7 C8 . . 108.37(9) ?
N4 C7 H7A . . 110.0 ?
C8 C7 H7A . . 110.0 ?
N4 C7 H7B . . 110.0 ?
C8 C7 H7B . . 110.0 ?
H7A C7 H7B . . 108.4 ?
N1 C8 C7 . . 109.56(9) ?
N1 C8 H8A . . 109.8 ?
C7 C8 H8A . . 109.8 ?
N1 C8 H8B . . 109.8 ?
C7 C8 H8B . . 109.8 ?
H8A C8 H8B . . 108.2 ?
C1 N1 C8 . . 115.66(9) ?
C1 N1 Cu1 . . 102.97(7) ?
C8 N1 Cu1 . . 107.77(7) ?
C1 N1 H1 . . 107.1(11) ?
C8 N1 H1 . . 110.9(12) ?
Cu1 N1 H1 . . 112.2(11) ?
C3 N2 C2 . . 114.31(10) ?
C3 N2 Cu1 . . 103.55(7) ?
C2 N2 Cu1 . . 107.38(7) ?
C3 N2 H2 . . 111.3(12) ?
C2 N2 H2 . . 109.4(12) ?
Cu1 N2 H2 . . 110.7(11) ?
C5 N3 C4 . . 114.55(9) ?
C5 N3 Cu1 . . 102.42(7) ?
C4 N3 Cu1 . . 108.34(7) ?
C5 N3 H3 . . 106.1(12) ?
C4 N3 H3 . . 113.6(12) ?
Cu1 N3 H3 . . 111.3(12) ?
C7 N4 C6 . . 114.37(9) ?
C7 N4 Cu1 . . 102.84(7) ?
C6 N4 Cu1 . . 107.10(8) ?
C7 N4 H4 . . 110.1(12) ?
C6 N4 H4 . . 110.2(12) ?
Cu1 N4 H4 . . 112.0(12) ?
Cl1 O1 Cu1 . . 116.92(4) ?
O3 Cl1 O2 . . 109.65(7) ?
O3 Cl1 O4 . . 111.02(7) ?
O2 Cl1 O4 . . 109.85(6) ?
O3 Cl1 O1 . . 108.78(6) ?
O2 Cl1 O1 . . 109.36(5) ?
O4 Cl1 O1 . . 108.14(5) ?
O7 Cl2 O8 . . 109.87(7) ?
O7 Cl2 O6 . . 109.78(7) ?
O8 Cl2 O6 . . 109.12(6) ?
O7 Cl2 O5 . . 109.49(6) ?
O8 Cl2 O5 . . 109.95(6) ?
O6 Cl2 O5 . . 108.61(6) ?
N3 Cu1 N1 . . 151.33(4) ?
N3 Cu1 N4 . . 87.11(4) ?
N1 Cu1 N4 . . 87.14(4) ?
N3 Cu1 N2 . . 86.24(4) ?
N1 Cu1 N2 . . 86.52(4) ?
N4 Cu1 N2 . . 153.54(4) ?
N3 Cu1 O1 . . 104.87(3) ?
N1 Cu1 O1 . . 103.78(3) ?
N4 Cu1 O1 . . 103.79(3) ?
N2 Cu1 O1 . . 102.66(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
N1 C1 C2 N2 . . . . 54.05(13) ?
N2 C3 C4 N3 . . . . 50.52(13) ?
N3 C5 C6 N4 . . . . 53.24(12) ?
N4 C7 C8 N1 . . . . 51.48(13) ?
C2 C1 N1 C8 . . . . -169.09(9) ?
C2 C1 N1 Cu1 . . . . -51.82(10) ?
C7 C8 N1 C1 . . . . 89.34(12) ?
C7 C8 N1 Cu1 . . . . -25.21(11) ?
C4 C3 N2 C2 . . . . -166.49(10) ?
C4 C3 N2 Cu1 . . . . -50.00(10) ?
C1 C2 N2 C3 . . . . 87.01(12) ?
C1 C2 N2 Cu1 . . . . -27.24(11) ?
C6 C5 N3 C4 . . . . -168.48(9) ?
C6 C5 N3 Cu1 . . . . -51.42(9) ?
C3 C4 N3 C5 . . . . 89.53(11) ?
C3 C4 N3 Cu1 . . . . -24.09(11) ?
C8 C7 N4 C6 . . . . -165.51(10) ?
C8 C7 N4 Cu1 . . . . -49.77(10) ?
C5 C6 N4 C7 . . . . 87.24(12) ?
C5 C6 N4 Cu1 . . . . -26.00(11) ?
Cu1 O1 Cl1 O3 . . . . -58.89(8) ?
Cu1 O1 Cl1 O2 . . . . 60.85(7) ?
Cu1 O1 Cl1 O4 . . . . -179.55(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 H1 O6 3_666 0.860(10)
2.50(2) 3.1710(10)
135.0(10)
N1 H1 O2 . 0.860(10)
2.390(10)
3.0930(10)
139.0(10)
N2 H2 O8 3_566 0.88(2) 2.31(2) 3.0500(10)
142.0(10)
N2 H2 O3 . 0.88(2) 2.44(2) 3.052(2) 127.0(10)
N3 H3 O1 3_566 0.86(2) 2.400(10)
3.2450(10)
169(2)
N3 H3 O4 3_566 0.86(2) 2.55(2) 3.1320(10)
126.0(10)
N4 H4 O5 . 0.86(2) 2.360(10)
3.0960(10)
143.0(10)
_shelx_hkl_file
;
1 0 0 -6.80 0.40
1 0 0 -5.80 0.50
-1 0 0 -5.30 0.50
2 0 0 9999.00 171.58
-2 0 0 9546.75 168.48
-2 0 0 9272.77 170.28
3 0 0 -2.60 0.50
-3 0 0 -3.50 0.30
-3 0 0 -2.50 0.50
-3 0 0 -2.70 0.30
3 0 0 -2.80 0.50
-3 0 0 -2.10 0.50
-4 0 0 3811.02 69.29
-4 0 0 3813.12 67.99
4 0 0 3771.42 69.39
4 0 0 4003.30 68.19
-4 0 0 3640.14 68.39
-5 0 0 -0.50 0.70
5 0 0 -0.30 0.40
5 0 0 0.60 0.60
5 0 0 0.80 0.80
-5 0 0 -0.40 0.40
-5 0 0 -0.50 0.20
-5 0 0 2.10 0.70
-5 0 0 -0.60 0.50
-5 0 0 -0.70 0.50
-5 0 0 -0.40 0.50
-6 0 0 2722.93 47.60
-6 0 0 2709.23 47.80
6 0 0 2735.63 48.40
-6 0 0 2791.32 47.30
6 0 0 2732.43 49.70
-6 0 0 2747.03 47.70
6 0 0 2453.55 49.10
-6 0 0 2730.33 49.40
-7 0 0 0.30 0.60
7 0 0 0.30 0.90
-7 0 0 0.10 0.90
-7 0 0 2.50 1.00
8 0 0 171.88 5.40
-8 0 0 169.78 4.20
-8 0 0 170.88 4.80
-8 0 0 166.38 4.60
-9 0 0 -0.80 1.20
-9 0 0 -0.60 1.10
-10 0 0 249.18 6.80
-10 0 0 246.08 6.50
-11 0 0 -0.10 1.30
-11 0 0 -1.90 1.30
-12 0 0 23.90 2.50
-12 0 0 30.60 2.90
-13 0 0 1.60 1.70
-13 0 0 -0.20 1.70
-14 0 0 39.10 3.60
-14 0 0 34.30 3.20
0 -1 0 -1.30 0.10
1 -1 0 23.00 0.80
1 -1 0 26.70 0.90
1 -1 0 24.50 0.80
-1 -1 0 23.90 0.90
1 -1 0 23.00 0.80
-1 -1 0 23.00 0.80
-1 -1 0 23.80 0.60
-1 -1 0 24.40 0.90
-1 1 0 24.50 0.90
-1 1 0 23.80 0.80
-1 1 0 23.70 0.80
1 1 0 24.00 0.60
-1 1 0 23.20 0.80
1 1 0 24.10 0.80
1 1 0 22.70 0.90
1 1 0 23.40 0.80
2 -1 0 99.09 2.40
2 -1 0 96.49 2.50
2 -1 0 96.99 2.20
-2 -1 0 101.19 2.60
-2 -1 0 97.19 2.60
2 -1 0 99.69 2.60
2 1 0 96.49 2.60
-2 1 0 96.69 2.60
2 1 0 97.89 2.50
-2 1 0 93.39 2.20
-2 1 0 100.69 2.60
-2 1 0 97.69 2.30
2 1 0 97.19 2.30
-3 -1 0 1281.77 22.70
-3 -1 0 1252.87 22.20
3 -1 0 1181.18 22.50
-3 -1 0 1222.88 22.80
3 -1 0 1253.57 22.20
3 -1 0 1229.78 22.80
-3 1 0 1259.67 22.20
-3 1 0 1225.38 22.70
3 1 0 1205.58 22.70
3 1 0 1243.88 22.20
3 1 0 1231.48 22.60
-3 1 0 1242.08 22.60
-4 -1 0 25.70 1.40
4 -1 0 26.90 1.70
4 -1 0 27.30 1.80
-4 -1 0 26.90 1.70
-4 -1 0 27.00 1.70
-4 -1 0 27.50 1.10
4 -1 0 27.20 1.50
4 1 0 26.50 1.50
-4 1 0 24.60 1.70
-4 1 0 25.70 1.40
-4 1 0 30.10 1.50
-4 1 0 25.20 1.70
4 1 0 25.40 1.60
4 1 0 27.60 1.80
-5 -1 0 1314.77 23.10
-5 -1 0 1262.47 23.40
5 -1 0 1277.37 24.60
-5 -1 0 1291.47 23.10
-5 -1 0 1297.57 23.30
-5 -1 0 1305.77 25.00
5 -1 0 1274.37 23.90
-5 -1 0 1295.97 24.70
5 -1 0 1273.57 24.90
-5 -1 0 1304.47 23.80
-5 1 0 1292.77 24.90
5 1 0 1289.47 23.90
5 1 0 1290.27 24.60
-5 1 0 1297.27 23.80
-5 1 0 1287.67 23.40
-5 1 0 1307.87 23.30
5 1 0 1308.07 24.90
-5 1 0 1324.07 23.10
6 -1 0 37.50 2.60
-6 -1 0 36.90 1.50
-6 -1 0 38.10 2.50
-6 -1 0 37.00 1.70
-6 -1 0 39.90 1.60
6 -1 0 36.70 2.10
6 -1 0 32.10 2.30
-6 -1 0 38.50 2.60
6 1 0 35.30 2.10
-6 1 0 38.20 1.90
-6 1 0 36.00 1.80
6 1 0 37.00 2.40
-6 1 0 37.80 2.60
-6 1 0 38.60 2.50
-6 1 0 36.90 1.80
-6 1 0 36.00 1.50
6 1 0 37.60 2.60
-7 -1 0 485.25 13.00
-7 -1 0 452.05 9.00
-7 -1 0 443.16 9.50
-7 -1 0 451.55 9.40
7 -1 0 468.05 10.30
7 1 0 457.85 10.20
-7 1 0 459.75 9.00
-7 1 0 447.06 9.50
-7 1 0 448.46 9.40
-7 1 0 450.55 9.50
-8 -1 0 215.38 5.60
-8 -1 0 217.28 5.00
8 -1 0 223.28 6.30
-8 -1 0 207.48 5.30
-8 1 0 218.98 5.70
8 1 0 222.08 6.30
-8 1 0 211.78 5.40
-8 1 0 208.38 5.00
-9 -1 0 391.56 8.90
-9 -1 0 409.16 9.20
-9 1 0 404.16 9.00
-9 1 0 405.96 9.20
-10 -1 0 71.79 3.50
-10 -1 0 73.29 3.30
-10 1 0 78.89 3.40
-10 1 0 69.09 3.50
-11 -1 0 170.28 5.40
-11 -1 0 172.48 5.60
-11 1 0 184.08 5.60
-11 1 0 174.08 5.70
-12 -1 0 13.10 2.10
-12 -1 0 18.30 2.30
-12 1 0 15.40 2.30
-12 1 0 14.00 2.10
-13 -1 0 94.89 4.50
-13 -1 0 101.39 4.90
-13 1 0 101.69 4.90
-13 1 0 99.89 4.50
-14 -1 0 60.19 4.30
-14 -1 0 53.69 3.90
-14 1 0 57.49 3.80
-14 1 0 58.49 4.20
0 -2 0 1416.16 26.20
0 -2 0 1383.26 27.00
0 -2 0 1530.45 27.00
0 2 0 1455.35 26.60
0 2 0 1385.46 26.70
0 2 0 1478.75 26.60
0 2 0 1505.35 27.00
1 -2 0 4162.58 77.49
1 -2 0 4476.55 77.99
-1 -2 0 4404.56 78.99
-1 -2 0 4223.88 78.29
1 -2 0 4315.27 78.59
1 -2 0 4272.17 78.39
-1 -2 0 4456.65 76.59
1 2 0 4509.05 78.99
-1 2 0 4418.76 77.59
1 2 0 4346.77 78.19
-1 2 0 4198.78 77.89
-1 2 0 4307.97 78.09
1 2 0 4538.15 76.69
-1 2 0 4391.46 78.39
2 -2 0 889.71 16.20
-2 -2 0 886.61 16.10
-2 -2 0 898.31 15.90
-2 -2 0 893.71 16.40
2 -2 0 893.41 16.10
2 -2 0 900.61 16.40
-2 -2 0 897.21 16.50
2 -2 0 905.11 16.40
2 2 0 899.11 16.40
2 2 0 857.11 15.90
-2 2 0 902.61 16.40
-2 2 0 887.21 16.30
-2 2 0 904.71 16.10
-2 2 0 900.51 16.10
2 2 0 879.81 16.10
-3 -2 0 285.77 6.20
3 -2 0 275.97 5.80
3 -2 0 276.07 5.70
-3 -2 0 274.57 5.80
-3 -2 0 280.57 6.40
3 -2 0 286.27 6.30
-3 -2 0 271.47 5.30
3 -2 0 272.37 6.10
-3 2 0 279.57 5.80
3 2 0 277.97 6.20
3 2 0 272.67 6.30
-3 2 0 281.27 5.70
-3 2 0 279.77 6.20
3 2 0 277.67 5.80
-3 2 0 260.27 6.10
-4 -2 0 168.68 4.90
4 -2 0 174.48 4.70
-4 -2 0 169.18 4.70
-4 -2 0 173.78 3.80
4 -2 0 170.18 4.80
-4 -2 0 172.98 4.20
4 -2 0 171.08 4.30
-4 -2 0 171.28 3.70
-4 -2 0 179.88 4.00
4 2 0 176.08 4.30
4 2 0 172.88 4.60
-4 2 0 171.48 4.80
-4 2 0 175.08 4.10
4 2 0 173.78 4.80
-4 2 0 161.48 4.60
-4 2 0 179.08 4.30
-5 -2 0 517.55 9.90
5 -2 0 511.25 10.50
-5 -2 0 509.15 9.60
-5 -2 0 515.35 11.20
5 -2 0 509.25 11.40
-5 -2 0 521.55 9.70
5 -2 0 502.65 11.10
-5 -2 0 500.95 10.40
-5 -2 0 500.15 11.40
-5 -2 0 497.25 9.80
-5 2 0 523.95 10.00
-5 2 0 518.75 10.50
-5 2 0 481.15 11.00
-5 2 0 521.75 9.90
-5 2 0 518.25 10.30
-5 2 0 521.35 11.40
5 2 0 522.85 11.20
-5 2 0 533.05 9.70
5 2 0 522.65 10.50
5 2 0 527.35 11.50
6 -2 0 159.98 4.60
-6 -2 0 158.58 3.70
-6 -2 0 155.68 3.90
6 -2 0 155.88 5.30
-6 -2 0 150.48 4.10
-6 -2 0 161.98 5.40
-6 -2 0 164.28 3.60
-6 -2 0 154.68 3.70
-6 -2 0 157.88 5.20
6 -2 0 155.48 5.10
-6 -2 0 152.28 3.90
-6 2 0 161.98 5.30
6 2 0 164.38 5.70
-6 2 0 147.59 4.00
6 2 0 152.68 4.50
-6 2 0 153.28 3.90
-6 2 0 161.38 3.70
-7 -2 0 159.88 4.30
-7 -2 0 162.68 3.90
-7 -2 0 154.38 4.30
7 -2 0 166.58 5.00
-7 2 0 153.88 4.20
-7 2 0 159.88 3.90
7 2 0 161.08 4.90
-7 2 0 157.08 4.40
-8 -2 0 79.69 3.20
-8 -2 0 86.89 3.00
-8 -2 0 83.09 2.70
8 -2 0 85.79 3.70
8 2 0 85.39 3.60
-8 2 0 84.69 3.10
-8 2 0 84.29 3.10
-8 2 0 94.19 2.80
-9 -2 0 12.60 1.50
-9 -2 0 6.40 1.50
-9 2 0 8.90 1.60
-9 2 0 9.60 1.50
-10 -2 0 31.60 2.60
-10 -2 0 32.20 2.50
-10 2 0 28.10 2.30
-10 2 0 28.80 2.40
-11 -2 0 6.20 1.70
-11 -2 0 3.20 1.70
-11 2 0 5.10 1.80
-11 2 0 5.00 1.60
-12 -2 0 2.80 1.60
-12 -2 0 -1.20 1.40
-12 2 0 1.40 1.60
-12 2 0 -0.60 1.70
-13 -2 0 29.50 3.10
-13 -2 0 29.60 2.90
-13 2 0 24.00 2.90
-13 2 0 30.50 2.90
-14 -2 0 3.50 1.70
-14 -2 0 2.40 2.00
-14 2 0 0.40 1.90
-14 2 0 -0.30 1.90
0 -3 0 -3.30 0.30
0 -3 0 -3.60 0.30
0 -3 0 -3.00 0.30
0 3 0 -2.90 0.30
0 3 0 -3.20 0.40
0 3 0 -2.30 0.40
0 3 0 -1.60 0.40
1 -3 0 65.19 1.80
1 -3 0 67.49 1.90
-1 -3 0 65.59 1.60
-1 -3 0 66.69 1.90
-1 -3 0 66.89 1.90
1 -3 0 65.09 1.80
1 -3 0 68.09 1.90
1 3 0 68.49 1.90
-1 3 0 66.99 1.80
1 3 0 67.99 1.70
-1 3 0 68.79 1.90
-1 3 0 66.89 1.90
-1 3 0 65.99 1.80
1 3 0 69.49 1.90
2 -3 0 7.20 0.80
-2 -3 0 8.00 0.80
-2 -3 0 7.00 0.50
-2 -3 0 7.60 0.90
2 -3 0 7.00 0.80
2 -3 0 7.00 0.80
2 3 0 8.50 0.90
2 3 0 8.00 0.60
-2 3 0 8.20 0.80
2 3 0 8.60 0.80
-2 3 0 10.90 1.00
-2 3 0 7.10 0.80
2 3 0 7.00 0.70
-3 -3 0 1.90 0.70
3 -3 0 1.50 0.60
3 -3 0 1.20 0.60
-3 -3 0 1.60 0.40
-3 -3 0 1.70 0.60
3 -3 0 1.50 0.60
-3 -3 0 0.60 0.50
-3 3 0 2.20 0.60
-3 3 0 1.70 0.60
3 3 0 2.40 0.70
3 3 0 1.90 0.70
3 3 0 1.20 0.50
-3 3 0 2.70 0.70
-3 3 0 1.30 0.60
-4 -3 0 46.60 1.50
-4 -3 0 47.60 2.30
4 -3 0 43.10 2.00
-4 -3 0 47.80 1.60
4 -3 0 46.20 1.90
4 -3 0 45.80 2.30
-4 -3 0 45.40 2.40
-4 -3 0 46.20 1.90
-4 -3 0 47.10 1.70
4 -3 0 49.60 2.30
-4 3 0 46.50 2.20
-4 3 0 46.80 1.70
-4 3 0 45.50 2.00
-4 3 0 49.20 2.20
-4 3 0 46.80 1.70
4 3 0 46.50 1.90
4 3 0 41.60 2.20
-4 3 0 48.50 1.90
4 3 0 47.80 2.20
5 -3 0 209.28 5.90
-5 -3 0 213.48 4.70
5 -3 0 205.18 5.70
-5 -3 0 207.58 4.50
-5 -3 0 205.98 4.80
-5 -3 0 211.28 4.50
5 -3 0 199.78 5.20
-5 -3 0 213.48 6.10
-5 -3 0 203.78 5.80
5 3 0 204.88 5.70
-5 3 0 199.48 5.00
5 3 0 210.38 5.20
5 3 0 207.78 5.90
-5 3 0 200.38 4.70
-5 3 0 211.18 4.50
-5 3 0 207.68 5.70
-5 3 0 210.48 5.80
-5 3 0 204.58 4.70
-6 -3 0 380.06 7.40
6 -3 0 385.46 9.30
-6 -3 0 378.66 9.30
-6 -3 0 371.46 7.90
-6 -3 0 376.66 7.40
6 -3 0 379.76 9.50
-6 -3 0 375.76 7.80
-6 -3 0 370.06 7.50
-6 -3 0 371.16 9.60
6 -3 0 372.96 8.50
-6 3 0 365.06 7.80
-6 3 0 370.66 7.50
-6 3 0 373.66 8.20
6 3 0 373.46 8.50
-6 3 0 371.26 7.80
-7 -3 0 39.60 2.10
-7 -3 0 41.00 1.70
-7 -3 0 38.70 2.00
-7 -3 0 45.60 3.70
7 -3 0 44.30 2.60
-7 -3 0 43.40 1.80
-7 3 0 40.50 1.80
-7 3 0 39.80 2.20
-7 3 0 39.90 2.20
7 3 0 43.80 2.60
8 -3 0 467.75 10.70
-8 -3 0 451.65 9.20
-8 -3 0 457.15 9.90
-8 -3 0 452.95 9.60
-8 3 0 447.86 9.20
8 3 0 470.05 10.70
-8 3 0 453.35 9.70
-8 3 0 441.66 9.70
-9 -3 0 -0.80 0.90
-9 -3 0 0.70 1.20
-9 3 0 1.20 1.10
-9 3 0 -0.70 1.10
-10 -3 0 361.06 8.80
-10 -3 0 365.56 8.50
-10 3 0 355.86 8.60
-10 3 0 361.96 8.80
-11 -3 0 10.50 1.90
-11 -3 0 11.40 1.70
-11 3 0 9.80 1.90
-11 3 0 10.40 1.90
-12 -3 0 129.29 5.10
-12 -3 0 120.69 4.60
-12 3 0 127.49 5.00
-12 3 0 126.59 5.00
-13 -3 0 -0.30 1.40
-13 -3 0 1.70 1.80
-13 3 0 2.30 1.80
-13 3 0 -0.20 1.50
-14 -3 0 140.69 5.80
-14 -3 0 133.79 5.50
-14 3 0 133.19 5.80
-14 3 0 127.69 5.50
0 -4 0 6565.14 124.89
0 -4 0 6867.81 124.39
0 -4 0 7274.57 125.49
0 4 0 7569.44 124.79
0 4 0 7647.73 124.69
0 4 0 6742.43 124.79
0 4 0 6393.36 124.29
1 -4 0 6282.47 110.79
1 -4 0 6006.90 110.29
-1 -4 0 6242.88 111.09
1 -4 0 6063.89 109.69
-1 -4 0 6109.79 110.09
-1 -4 0 5900.21 108.49
1 -4 0 6208.68 109.99
1 4 0 6205.68 110.49
1 4 0 5886.91 109.49
-1 4 0 6513.15 109.79
-1 4 0 6346.17 109.89
1 4 0 6030.30 108.99
-1 4 0 6188.68 110.39
-1 4 0 5673.83 109.89
2 -4 0 148.89 3.60
2 -4 0 143.19 3.60
-2 -4 0 141.79 3.10
-2 -4 0 146.39 3.80
-2 -4 0 145.59 3.70
2 -4 0 144.09 3.60
2 -4 0 148.79 3.60
-2 4 0 149.88 3.60
-2 4 0 144.39 3.60
-2 4 0 144.49 3.50
-2 4 0 145.99 3.60
2 4 0 150.38 3.60
2 4 0 145.89 3.50
2 4 0 145.39 3.20
2 4 0 143.69 3.70
-3 -4 0 1548.25 28.40
-3 -4 0 1585.74 28.60
3 -4 0 1581.14 28.40
-3 -4 0 1490.25 27.30
3 -4 0 1535.65 28.40
3 -4 0 1580.74 28.10
3 -4 0 1589.34 28.00
-3 4 0 1556.84 28.30
-3 4 0 1551.84 28.30
3 4 0 1574.54 28.30
3 4 0 1460.65 27.60
-3 4 0 1575.14 28.10
-3 4 0 1582.14 28.10
3 4 0 1577.24 28.50
3 4 0 1569.94 28.10
4 -4 0 837.52 16.90
-4 -4 0 878.11 15.80
-4 -4 0 842.42 15.40
-4 -4 0 860.81 15.90
-4 -4 0 859.91 17.10
4 -4 0 858.01 16.80
-4 -4 0 862.81 15.70
4 -4 0 845.22 16.40
4 -4 0 841.22 16.20
-4 -4 0 855.71 16.90
-4 -4 0 868.21 15.60
-4 -4 0 843.52 16.30
-4 4 0 905.21 15.70
4 4 0 852.21 16.30
4 4 0 883.01 17.10
-4 4 0 844.62 16.80
-4 4 0 868.81 15.70
4 4 0 865.61 16.80
-4 4 0 836.22 16.70
-4 4 0 869.21 16.30
-4 4 0 845.82 16.30
-5 -4 0 1216.48 22.30
5 -4 0 1229.68 24.00
5 -4 0 1236.88 22.00
-5 -4 0 1214.38 23.90
-5 -4 0 1221.98 22.50
-5 -4 0 1244.18 24.20
5 -4 0 1251.57 23.80
-5 -4 0 1232.18 22.10
5 -4 0 1213.18 23.20
-5 -4 0 1215.78 22.00
-5 -4 0 1278.37 22.20
5 4 0 1230.38 23.10
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-4 -3 -18 95.99 4.80
-4 -3 -18 95.59 4.60
-4 3 -18 97.19 4.60
-4 3 -18 102.89 5.00
6 4 -18 28.20 4.10
5 -4 -18 67.19 4.10
5 -4 -18 63.49 4.10
5 4 -18 69.29 4.10
5 4 -18 67.59 4.00
5 4 -18 61.79 3.80
4 -4 -18 23.40 2.80
4 -4 -18 22.70 2.60
4 4 -18 19.40 2.50
4 4 -18 25.80 2.80
4 4 -18 20.40 2.60
3 -4 -18 31.50 3.20
3 -4 -18 30.90 2.80
3 -4 -18 34.70 3.00
3 4 -18 32.90 3.00
3 4 -18 31.10 3.00
2 -4 -18 28.50 2.80
2 -4 -18 28.40 2.80
2 -4 -18 25.00 2.60
2 4 -18 26.10 2.70
2 4 -18 23.70 2.70
1 -4 -18 8.90 2.00
1 -4 -18 6.90 2.10
1 4 -18 9.40 2.10
1 4 -18 8.90 2.00
0 -4 -18 14.60 2.30
0 -4 -18 16.90 2.30
0 4 -18 9.60 2.00
0 4 -18 11.90 2.20
0 4 -18 12.20 2.10
-1 -4 -18 0.60 1.80
-1 -4 -18 -0.90 1.60
-1 4 -18 -0.20 1.60
-1 4 -18 0.80 1.60
-1 4 -18 2.70 1.70
-2 -4 -18 9.10 2.10
-2 -4 -18 11.30 2.20
-2 -4 -18 13.60 2.20
-2 4 -18 8.50 2.00
-2 4 -18 8.90 1.90
-2 4 -18 14.20 2.40
-3 -4 -18 4.80 2.00
-3 -4 -18 6.20 1.90
-3 -4 -18 6.00 2.00
-3 4 -18 7.60 1.90
-3 4 -18 5.80 2.10
-3 4 -18 8.20 2.10
-4 -4 -18 4.00 2.00
-4 -4 -18 1.40 2.00
-4 4 -18 1.30 1.70
-4 4 -18 1.90 1.90
5 -5 -18 9.50 2.30
5 -5 -18 6.40 2.10
5 5 -18 8.00 2.20
5 5 -18 9.70 2.10
4 -5 -18 22.80 2.80
4 -5 -18 18.40 2.60
4 5 -18 18.50 2.50
4 5 -18 19.60 2.50
3 -5 -18 42.50 3.50
3 -5 -18 37.20 3.30
3 5 -18 38.50 3.30
3 5 -18 45.20 3.40
2 -5 -18 53.59 3.50
2 -5 -18 57.79 3.80
2 -5 -18 45.60 3.40
2 5 -18 52.69 3.70
2 5 -18 49.00 3.20
1 -5 -18 64.99 3.80
1 -5 -18 64.79 3.70
1 5 -18 63.19 3.80
1 5 -18 69.39 3.70
0 -5 -18 40.80 3.30
0 -5 -18 33.60 3.10
0 5 -18 45.80 3.30
0 5 -18 46.70 3.50
0 5 -18 45.60 3.30
-1 -5 -18 57.59 3.50
-1 -5 -18 56.09 3.60
-1 5 -18 57.19 3.40
-1 5 -18 60.09 3.60
-1 5 -18 49.20 3.60
-2 -5 -18 17.00 2.40
-2 -5 -18 15.80 2.40
-2 -5 -18 21.70 2.60
-2 5 -18 20.60 2.50
-2 5 -18 19.80 2.50
-2 5 -18 20.30 2.70
-3 -5 -18 95.49 4.60
-3 -5 -18 99.19 4.80
-3 5 -18 101.69 5.00
-3 5 -18 93.79 4.50
-4 -5 -18 19.80 2.90
-4 5 -18 21.60 2.70
5 -6 -18 7.60 2.10
5 6 -18 5.40 2.10
4 -6 -18 9.50 2.20
4 -6 -18 11.50 2.30
4 6 -18 13.50 2.50
4 6 -18 14.20 2.30
3 -6 -18 5.00 2.00
3 -6 -18 8.70 2.30
3 6 -18 7.60 2.00
3 6 -18 6.10 1.90
2 -6 -18 2.40 1.80
2 -6 -18 1.20 1.60
2 -6 -18 0.10 1.60
2 6 -18 0.60 1.50
2 6 -18 -0.30 1.50
1 -6 -18 7.20 2.10
1 -6 -18 7.60 2.00
1 6 -18 9.30 2.20
1 6 -18 9.30 2.10
1 6 -18 12.20 2.10
0 -6 -18 2.80 1.80
0 -6 -18 0.00 1.70
0 6 -18 1.80 1.70
0 6 -18 2.60 1.70
0 6 -18 1.70 1.60
-1 -6 -18 4.00 1.90
-1 -6 -18 1.60 1.80
-1 6 -18 2.90 1.80
-1 6 -18 2.90 1.80
-2 -6 -18 9.40 2.20
-2 -6 -18 10.00 2.20
-2 6 -18 10.80 2.30
-2 6 -18 6.60 2.00
-3 -6 -18 7.20 2.10
-3 -6 -18 3.80 1.80
-3 6 -18 8.30 2.00
-3 6 -18 8.00 2.20
-4 6 -18 15.50 3.30
4 -7 -18 1.30 1.70
4 -7 -18 2.00 2.00
4 7 -18 1.50 1.70
4 7 -18 -1.10 2.00
3 -7 -18 13.20 2.40
3 -7 -18 16.90 2.50
3 7 -18 17.40 2.60
3 7 -18 16.80 2.30
2 -7 -18 0.00 1.90
2 -7 -18 1.30 1.70
2 7 -18 2.20 1.80
2 7 -18 0.40 1.60
1 -7 -18 41.50 3.30
1 -7 -18 41.50 3.20
1 7 -18 48.60 3.60
0 -7 -18 2.40 1.70
0 -7 -18 4.00 1.80
0 7 -18 4.30 1.80
0 7 -18 3.80 1.80
-1 -7 -18 35.40 3.10
-1 -7 -18 33.20 3.00
-1 7 -18 36.80 3.20
-1 7 -18 40.30 3.30
-2 -7 -18 12.90 2.30
-2 -7 -18 18.90 2.60
-2 7 -18 16.60 2.40
-2 7 -18 20.50 2.60
-3 -7 -18 35.50 3.20
-3 -7 -18 31.80 4.40
-3 7 -18 26.10 2.80
4 -8 -18 1.40 1.80
4 8 -18 -0.20 1.60
3 -8 -18 15.80 2.40
3 -8 -18 18.60 2.70
3 8 -18 17.10 2.90
2 -8 -18 2.20 1.80
2 -8 -18 1.60 1.90
2 8 -18 4.30 1.90
1 -8 -18 24.90 2.70
1 8 -18 23.90 2.90
1 8 -18 28.60 3.00
0 -8 -18 0.30 1.60
0 -8 -18 -0.90 1.70
0 8 -18 0.90 1.50
0 8 -18 1.20 1.80
-1 -8 -18 13.30 2.30
-1 -8 -18 14.00 2.20
-1 8 -18 10.70 2.10
-1 8 -18 14.10 2.50
-2 -8 -18 7.90 2.10
-2 8 -18 8.80 2.10
-2 8 -18 16.60 3.00
-3 -8 -18 1.30 1.90
3 -9 -18 0.80 1.70
2 -9 -18 18.40 2.70
2 -9 -18 18.20 2.40
2 9 -18 21.90 4.00
1 -9 -18 18.00 2.50
1 9 -18 15.50 2.40
1 9 -18 15.30 2.40
0 -9 -18 32.70 3.00
0 -9 -18 32.60 3.00
0 9 -18 28.50 3.00
0 9 -18 32.80 3.20
-1 -9 -18 4.40 1.70
-1 -9 -18 3.10 2.00
-1 9 -18 5.90 2.20
-1 9 -18 4.80 2.30
2 -10 -18 9.10 2.80
1 -10 -18 4.90 2.40
1 10 -18 6.80 2.30
4 0 -19 -0.70 1.60
3 0 -19 2.70 1.80
3 0 -19 1.80 2.00
3 0 -19 5.10 2.00
2 0 -19 0.70 1.70
2 0 -19 -0.80 1.70
1 0 -19 0.20 1.60
1 0 -19 1.90 1.80
0 0 -19 -2.30 1.40
0 0 -19 0.50 1.70
-1 0 -19 1.00 1.70
-1 0 -19 1.30 1.70
-1 0 -19 -0.60 1.50
-2 0 -19 -0.30 1.50
-2 0 -19 0.10 1.60
-2 0 -19 1.50 2.00
4 -1 -19 13.00 2.20
4 1 -19 8.60 3.10
4 1 -19 10.60 2.30
3 -1 -19 6.50 1.90
3 -1 -19 0.80 1.80
3 -1 -19 6.80 2.00
3 1 -19 3.00 1.80
3 1 -19 2.80 1.90
3 1 -19 4.70 2.00
2 -1 -19 28.90 3.00
2 -1 -19 27.00 2.90
2 1 -19 27.00 2.80
2 1 -19 29.10 3.00
1 -1 -19 2.20 1.80
1 -1 -19 1.30 1.80
1 1 -19 1.80 1.70
1 1 -19 2.80 1.80
0 -1 -19 17.60 2.50
0 -1 -19 19.90 2.50
0 1 -19 21.80 2.80
0 1 -19 16.90 2.40
-1 -1 -19 2.30 1.80
-1 -1 -19 3.10 1.80
-1 1 -19 2.70 1.90
-1 1 -19 1.20 1.60
-1 1 -19 2.20 1.80
-2 -1 -19 11.70 2.40
-2 -1 -19 12.30 2.70
-2 -1 -19 15.70 2.50
-2 1 -19 14.10 3.20
-2 1 -19 7.70 2.10
-2 1 -19 12.70 2.30
4 -2 -19 13.50 2.20
4 2 -19 9.60 3.00
4 2 -19 7.30 3.00
3 -2 -19 -0.80 1.60
3 -2 -19 -0.40 1.80
3 -2 -19 -2.00 1.70
3 2 -19 0.50 1.50
3 2 -19 1.20 1.80
2 -2 -19 16.90 2.50
2 -2 -19 17.30 2.50
2 2 -19 19.80 2.70
2 2 -19 13.90 2.40
1 -2 -19 0.70 1.70
1 -2 -19 -0.60 1.60
1 2 -19 1.80 1.80
1 2 -19 -0.40 1.50
0 -2 -19 16.00 2.50
0 -2 -19 17.40 2.50
0 2 -19 17.90 2.60
0 2 -19 22.10 2.60
-1 -2 -19 1.60 1.80
-1 -2 -19 0.30 1.80
-1 2 -19 2.40 1.80
-1 2 -19 0.80 1.70
-1 2 -19 1.80 1.80
-2 -2 -19 25.30 3.80
-2 -2 -19 16.50 2.50
-2 2 -19 21.50 2.70
-2 2 -19 17.30 2.50
4 3 -19 3.10 2.70
3 -3 -19 8.30 3.20
3 -3 -19 9.40 2.10
3 -3 -19 5.10 2.80
3 3 -19 7.10 2.30
3 3 -19 8.50 2.20
2 -3 -19 0.80 1.70
2 -3 -19 2.50 1.90
2 3 -19 3.00 1.90
2 3 -19 1.70 1.80
1 -3 -19 0.60 1.70
1 -3 -19 -1.50 1.70
1 3 -19 0.90 1.80
1 3 -19 1.00 1.80
0 -3 -19 -1.50 1.60
0 -3 -19 0.80 1.70
0 3 -19 1.40 1.70
0 3 -19 1.40 1.80
-1 -3 -19 8.30 2.20
-1 -3 -19 3.70 2.00
-1 3 -19 8.20 2.10
-1 3 -19 6.60 2.10
-1 3 -19 6.10 1.90
-2 -3 -19 4.20 1.90
-2 3 -19 3.00 1.90
-2 3 -19 1.10 1.80
3 -4 -19 1.20 1.70
3 4 -19 0.10 2.20
2 -4 -19 2.90 1.70
2 -4 -19 1.60 2.10
2 4 -19 -1.70 1.70
2 4 -19 0.80 2.10
1 -4 -19 -0.30 1.80
1 -4 -19 2.60 1.80
1 4 -19 0.60 1.60
1 4 -19 2.50 1.80
0 -4 -19 0.70 1.70
0 -4 -19 0.00 1.70
0 4 -19 1.50 1.70
0 4 -19 0.70 1.70
0 4 -19 0.20 1.70
-1 -4 -19 -0.50 1.90
-1 4 -19 0.20 1.60
-1 4 -19 2.40 1.80
-1 4 -19 1.20 2.40
-2 4 -19 22.40 3.00
-2 4 -19 16.30 3.70
2 -5 -19 6.70 1.90
2 5 -19 3.40 1.90
1 -5 -19 55.59 3.70
1 -5 -19 59.09 4.30
1 5 -19 54.19 3.70
0 -5 -19 1.20 1.80
0 -5 -19 -1.50 2.30
0 5 -19 1.50 1.70
0 5 -19 1.60 1.80
-1 -5 -19 34.00 5.00
-1 5 -19 31.30 3.10
-1 5 -19 28.60 2.90
2 6 -19 10.20 3.00
1 -6 -19 -1.00 1.60
1 6 -19 2.10 1.80
0 -6 -19 9.10 3.10
0 6 -19 11.10 2.20
0 6 -19 8.50 2.20
1 -7 -19 7.00 2.90
_computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)'
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_shelx_hkl_checksum 50979
_shelx_res_file
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JLG2_0m_a.res created by SHELXL-2014/7
TITL JLG2_0m_a.res in P2(1)/n
REM Old TITL JLG2_0m in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.129, Rweak 0.005, Alpha 0.024, Orientation as input
REM Formula found by SHELXT: C17 N2 O Cl2 Cu
CELL 0.71073 8.9387 15.0607 11.9235 90.000 92.949 90.000
ZERR 4.000 0.0002 0.0004 0.0003 0.000 0.001 0.000
LATT 1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC C H N O CL CU
UNIT 32 80 16 32 8 4
TEMP -100.000
SIZE 0.18 0.21 0.23
L.S. 4
BOND $H
LIST 6
FMAP 2
SADI N1 H1 N2 H2 N3 H3 N4 H4
BIND Cu1 O1
PLAN 20
ACTA
CONF
HTAB
WGHT 0.035700 0.452600
EXTI 0.002475
FVAR 0.44444
C1 1 0.428549 0.415949 0.838060 11.00000 0.02649 0.03898 =
0.02775 0.00946 -0.00999 -0.00224
AFIX 23
H1A 2 0.524018 0.427739 0.881281 11.00000 -1.20000
H1B 2 0.404270 0.352111 0.844961 11.00000 -1.20000
AFIX 0
C2 1 0.304391 0.472111 0.882384 11.00000 0.03678 0.04654 =
0.01841 -0.00147 -0.00378 -0.00370
AFIX 23
H2A 2 0.284988 0.453974 0.960109 11.00000 -1.20000
H2B 2 0.334387 0.535395 0.883464 11.00000 -1.20000
AFIX 0
C3 1 0.072185 0.384025 0.839217 11.00000 0.02961 0.03276 =
0.03749 0.00772 0.01102 0.00041
AFIX 23
H3A 2 0.019824 0.397668 0.908332 11.00000 -1.20000
H3B 2 0.135274 0.330756 0.853300 11.00000 -1.20000
AFIX 0
C4 1 -0.040500 0.367168 0.742536 11.00000 0.01755 0.02852 =
0.06004 0.00486 0.00489 -0.00054
AFIX 23
H4A 2 -0.094533 0.310989 0.755356 11.00000 -1.20000
H4B 2 -0.114780 0.415958 0.737850 11.00000 -1.20000
AFIX 0
C5 1 0.087857 0.270943 0.606319 11.00000 0.02994 0.01910 =
0.03858 0.00517 -0.01165 -0.00493
AFIX 23
H5A 2 0.000582 0.233377 0.583643 11.00000 -1.20000
H5B 2 0.141516 0.243101 0.671975 11.00000 -1.20000
AFIX 0
C6 1 0.191066 0.279469 0.510353 11.00000 0.05225 0.02370 =
0.02662 -0.00217 -0.00643 -0.00874
AFIX 23
H6A 2 0.235590 0.220939 0.494262 11.00000 -1.20000
H6B 2 0.133505 0.299793 0.441969 11.00000 -1.20000
AFIX 0
C7 1 0.444859 0.305414 0.602257 11.00000 0.03065 0.02064 =
0.04018 0.00129 0.00987 0.00076
AFIX 23
H7A 2 0.504563 0.270705 0.550027 11.00000 -1.20000
H7B 2 0.412564 0.265109 0.661983 11.00000 -1.20000
AFIX 0
C8 1 0.538666 0.380476 0.653557 11.00000 0.01987 0.02521 =
0.05013 0.00141 0.00814 -0.00062
AFIX 23
H8A 2 0.620081 0.355840 0.703709 11.00000 -1.20000
H8B 2 0.584710 0.414738 0.593424 11.00000 -1.20000
AFIX 0
H1 2 0.473428 0.493747 0.717165 11.00000 -1.20000
H2 2 0.114643 0.509651 0.806345 11.00000 -1.20000
H3 2 -0.015516 0.380231 0.578100 11.00000 -1.20000
H4 2 0.338928 0.371862 0.482008 11.00000 -1.20000
N1 3 0.442048 0.439933 0.718713 11.00000 0.01901 0.02175 =
0.02818 0.00332 -0.00213 -0.00229
N2 3 0.166145 0.460121 0.808491 11.00000 0.02415 0.02798 =
0.02591 0.00129 0.00301 0.00112
N3 3 0.037460 0.361457 0.635462 11.00000 0.02364 0.02083 =
0.03997 0.00647 -0.01341 -0.00218
N4 3 0.312075 0.344443 0.540870 11.00000 0.04026 0.02076 =
0.02237 0.00181 0.00324 -0.00401
O1 4 0.191812 0.555827 0.556946 11.00000 0.03609 0.01549 =
0.02270 -0.00121 -0.00910 -0.00254
O2 4 0.406953 0.631968 0.629227 11.00000 0.02132 0.03479 =
0.04657 0.00800 -0.00948 -0.00190
O3 4 0.179274 0.648427 0.714880 11.00000 0.05417 0.04517 =
0.04080 -0.02159 0.01924 -0.01358
O4 4 0.210836 0.710208 0.536087 11.00000 0.04196 0.01811 =
0.05382 0.00838 -0.02188 -0.00160
O5 4 0.245468 0.443525 0.316347 11.00000 0.06135 0.02808 =
0.02223 -0.00584 -0.00539 0.00537
O6 4 0.369781 0.409258 0.153175 11.00000 0.02581 0.05157 =
0.03708 0.00188 0.00326 -0.00208
O7 4 0.213327 0.303424 0.232292 11.00000 0.05365 0.02032 =
0.04929 -0.00147 0.00306 -0.00324
O8 4 0.108642 0.429257 0.142270 11.00000 0.03017 0.05384 =
0.02951 -0.00052 -0.00422 0.01645
CL1 5 0.247756 0.637771 0.610249 11.00000 0.02111 0.01695 =
0.02384 -0.00201 -0.00426 -0.00122
CL2 5 0.233536 0.395875 0.210988 11.00000 0.02481 0.02058 =
0.02081 -0.00166 -0.00149 0.00237
CU1 6 0.231189 0.428019 0.654383 11.00000 0.01806 0.01641 =
0.01824 0.00267 -0.00382 -0.00136
HKLF 4
REM JLG2_0m_a.res in P2(1)/n
REM R1 = 0.0247 for 6655 Fo > 4sig(Fo) and 0.0297 for all 7519 data
REM 221 parameters refined using 6 restraints
END
WGHT 0.0357 0.4526
REM Instructions for potential hydrogen bonds
EQIV $1 x, y, z+1
HTAB C2 O6_$1
EQIV $2 -x+1/2, y-1/2, -z+3/2
HTAB C3 O4_$2
EQIV $3 x-1/2, -y+1/2, z+1/2
HTAB C4 O7_$3
EQIV $4 -x, -y+1, -z+1
HTAB C4 O5_$4
HTAB C5 O4_$4
HTAB C5 O6_$3
HTAB C5 O3_$2
HTAB C6 O7
HTAB C7 O3_$2
EQIV $5 x+1/2, -y+1/2, z+1/2
HTAB C8 O7_$5
HTAB N1 O2
EQIV $6 -x+1, -y+1, -z+1
HTAB N1 O6_$6
HTAB N2 O3
HTAB N2 O8_$4
HTAB N3 O1_$4
HTAB N3 O4_$4
HTAB N4 O5
REM Highest difference peak 0.596, deepest hole -0.438, 1-sigma level 0.061
Q1 1 0.1720 0.4329 0.3181 11.00000 0.05 0.60
Q2 1 0.0312 0.3709 0.7913 11.00000 0.05 0.51
Q3 1 0.1640 0.7082 0.5819 11.00000 0.05 0.46
Q4 1 0.4040 0.4595 0.7680 11.00000 0.05 0.44
Q5 1 0.1076 0.4336 0.7807 11.00000 0.05 0.44
Q6 1 0.2172 0.6335 0.6616 11.00000 0.05 0.43
Q7 1 0.3337 0.4393 0.1741 11.00000 0.05 0.43
Q8 1 0.1610 0.4028 0.1868 11.00000 0.05 0.43
Q9 1 0.2463 0.3972 0.6934 11.00000 0.05 0.42
Q10 1 0.2273 0.6007 0.5819 11.00000 0.05 0.38
Q11 1 0.4015 0.5997 0.5956 11.00000 0.05 0.35
Q12 1 0.0852 0.3449 0.5786 11.00000 0.05 0.35
Q13 1 0.1431 0.2748 0.5593 11.00000 0.05 0.34
Q14 1 0.4023 0.3667 0.5655 11.00000 0.05 0.34
Q15 1 0.2577 0.3103 0.2578 11.00000 0.05 0.33
Q16 1 0.3250 0.6340 0.6223 11.00000 0.05 0.33
Q17 1 0.2200 0.6802 0.5723 11.00000 0.05 0.33
Q18 1 0.3629 0.4444 0.8597 11.00000 0.05 0.33
Q19 1 -0.0421 0.3596 0.6881 11.00000 0.05 0.33
Q20 1 0.4932 0.3408 0.6301 11.00000 0.05 0.32
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_shelx_res_checksum 65629