# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_cu95
_database_code_depnum_ccdc_archive 'CCDC 1493331'
_audit_update_record
;
2016-07-14 deposited with the CCDC.
2016-10-25 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014/6
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C10 H14 Cu N6 O S2'
_chemical_formula_sum 'C10 H14 Cu N6 O S2'
_chemical_formula_weight 361.93
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'
S S 0.1246 0.1234 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_H-M_alt 'C 2/c'
_space_group_name_Hall '-C 2yc'
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 18.855(2)
_cell_length_b 5.6220(4)
_cell_length_c 16.886(2)
_cell_angle_alpha 90
_cell_angle_beta 121.342(17)
_cell_angle_gamma 90
_cell_volume 1528.8(4)
_cell_formula_units_Z 4
_cell_measurement_temperature 295(2)
_cell_measurement_reflns_used 1245
_cell_measurement_theta_min 3.4738
_cell_measurement_theta_max 29.2421
_exptl_crystal_description plate
_exptl_crystal_colour green
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.573
_exptl_crystal_F_000 740
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.07
_exptl_crystal_size_min 0.03
_exptl_absorpt_coefficient_mu 1.705
_shelx_estimated_absorpt_T_min ?
_shelx_estimated_absorpt_T_max ?
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.35357
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_process_details 'Blessing, Acta Cryst. A51 (1995) 33-38'
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 295(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_source ?
_diffrn_measurement_device_type 'Oxford Diffraction Gemini A Ultra'
_diffrn_measurement_method ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 3669
_diffrn_reflns_av_unetI/netI 0.0451
_diffrn_reflns_av_R_equivalents 0.0368
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_theta_min 3.839
_diffrn_reflns_theta_max 25.049
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.970
_reflns_number_total 1344
_reflns_number_gt 1140
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_cell_refinement 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_reduction 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics 'Mercury(Macrae, J.Appl.Cryst.41(2008)466-470'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_refine_special_details ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0417P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens mixed
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_coef 0.0078(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns 1344
_refine_ls_number_parameters 96
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0440
_refine_ls_R_factor_gt 0.0348
_refine_ls_wR_factor_ref 0.0837
_refine_ls_wR_factor_gt 0.0794
_refine_ls_goodness_of_fit_ref 1.066
_refine_ls_restrained_S_all 1.066
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.0000 0.5000 0.0000 0.0269(2) Uani 1 2 d S . P . .
N1 N 0.08667(14) 0.5436(4) 0.13521(16) 0.0301(6) Uani 1 1 d . . . . .
N2 N 0.09658(14) 0.3936(4) 0.20285(15) 0.0311(6) Uani 1 1 d . . . . .
H2A H 0.0659 0.2709 0.1933 0.037 Uiso 1 1 calc R U . . .
C1 C 0.14603(17) 0.7046(5) 0.1784(2) 0.0365(7) Uani 1 1 d . . . . .
H1 H 0.1550 0.8315 0.1494 0.044 Uiso 1 1 calc R U . . .
C2 C 0.19312(18) 0.6584(6) 0.2729(2) 0.0381(7) Uani 1 1 d . . . . .
H2 H 0.2380 0.7460 0.3177 0.046 Uiso 1 1 calc R U . . .
C3 C 0.16006(18) 0.4588(5) 0.2867(2) 0.0308(7) Uani 1 1 d . . . . .
C4 C 0.1835(2) 0.3203(6) 0.3720(2) 0.0458(8) Uani 1 1 d . . . . .
H4A H 0.2330 0.3867 0.4235 0.069 Uiso 1 1 calc R U . . .
H4B H 0.1935 0.1578 0.3633 0.069 Uiso 1 1 calc R U . . .
H4C H 0.1392 0.3272 0.3842 0.069 Uiso 1 1 calc R U . . .
C99 C -0.07261(17) 0.0394(5) 0.03069(19) 0.0238(6) Uani 1 1 d . . . . .
N99 N -0.04195(14) 0.2173(4) 0.03049(16) 0.0318(6) Uani 1 1 d . . . . .
S99 S -0.11602(5) -0.20931(13) 0.03227(5) 0.0370(3) Uani 1 1 d . . . . .
O1 O 0.0000 0.0184(6) 0.2500 0.0617(11) Uani 1 2 d S T P . .
H1O H -0.0303 -0.1190 0.2013 0.20(3) Uiso 1 1 d R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0331(3) 0.0221(3) 0.0212(3) 0.00072(19) 0.0111(2) -0.00596(19)
N1 0.0335(14) 0.0298(13) 0.0246(14) 0.0027(10) 0.0134(12) -0.0041(10)
N2 0.0323(13) 0.0305(13) 0.0252(13) 0.0024(11) 0.0111(11) -0.0057(11)
C1 0.0354(17) 0.0338(17) 0.0316(18) 0.0027(14) 0.0113(15) -0.0097(13)
C2 0.0340(16) 0.0428(18) 0.0252(16) -0.0034(14) 0.0067(14) -0.0098(14)
C3 0.0318(15) 0.0356(16) 0.0223(16) -0.0005(13) 0.0121(14) 0.0013(13)
C4 0.0497(19) 0.054(2) 0.0276(17) 0.0056(15) 0.0156(15) -0.0036(16)
C99 0.0267(14) 0.0254(15) 0.0176(15) 0.0007(11) 0.0102(12) 0.0042(12)
N99 0.0428(14) 0.0253(13) 0.0291(13) -0.0028(11) 0.0199(12) -0.0067(11)
S99 0.0407(4) 0.0265(4) 0.0451(5) -0.0003(3) 0.0232(4) -0.0077(3)
O1 0.068(3) 0.060(2) 0.035(2) 0.000 0.0104(19) 0.000
_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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N99 1.960(2) . ?
Cu1 N99 1.960(2) 5_565 ?
Cu1 N1 2.015(2) 5_565 ?
Cu1 N1 2.015(2) . ?
N1 C1 1.324(4) . ?
N1 N2 1.352(3) . ?
N2 C3 1.345(4) . ?
C1 C2 1.389(4) . ?
C2 C3 1.361(4) . ?
C3 C4 1.488(4) . ?
C99 N99 1.156(3) . ?
C99 S99 1.628(3) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N99 Cu1 N99 180.0 . 5_565 ?
N99 Cu1 N1 89.92(9) . 5_565 ?
N99 Cu1 N1 90.08(9) 5_565 5_565 ?
N99 Cu1 N1 90.08(9) . . ?
N99 Cu1 N1 89.92(9) 5_565 . ?
N1 Cu1 N1 180.0 5_565 . ?
C1 N1 N2 104.8(2) . . ?
C1 N1 Cu1 131.5(2) . . ?
N2 N1 Cu1 123.73(17) . . ?
C3 N2 N1 112.1(2) . . ?
N1 C1 C2 110.9(3) . . ?
C3 C2 C1 105.9(3) . . ?
N2 C3 C2 106.3(2) . . ?
N2 C3 C4 122.0(3) . . ?
C2 C3 C4 131.7(3) . . ?
N99 C99 S99 179.1(3) . . ?
C99 N99 Cu1 166.7(2) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1O S99 1.05 2.49 3.4022(17) 143.9 .
N2 H2A O1 0.86 2.39 3.148(3) 147.2 .
N2 H2A N99 0.86 2.44 2.893(3) 113.2 .
_refine_diff_density_max 0.469
_refine_diff_density_min -0.449
_refine_diff_density_rms 0.088
_shelxl_version_number 2014/6
_shelx_res_file
;
TITL Cu95 in C2/c #15
CELL 0.71073 18.855 5.6220 16.886 90 121.342 90
ZERR 4 0.002 0.0004 0.002 0 0.017 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H N S Cu O
UNIT 40 56 24 8 4 4
L.S. 10
PLAN 20
REM reset to C2/c #15
BOND
fmap 2
ACTA
OMIT 0 50.1
HTAB O1 S99
HTAB N2 O1
HTAB N2 N99
WGHT 0.041700
EXTI 0.007806
FVAR 3.93266
CU1 5 0.000000 0.500000 0.000000 10.50000 0.03307 0.02207 =
0.02124 0.00072 0.01109 -0.00596
N1 3 0.086671 0.543637 0.135208 11.00000 0.03350 0.02977 =
0.02457 0.00271 0.01336 -0.00405
N2 3 0.096584 0.393586 0.202850 11.00000 0.03232 0.03048 =
0.02516 0.00239 0.01114 -0.00574
AFIX 43
H2A 2 0.065913 0.270875 0.193350 11.00000 -1.20000
AFIX 0
C1 1 0.146028 0.704555 0.178419 11.00000 0.03535 0.03375 =
0.03165 0.00270 0.01132 -0.00968
AFIX 43
H1 2 0.154984 0.831490 0.149353 11.00000 -1.20000
AFIX 0
C2 1 0.193116 0.658426 0.272942 11.00000 0.03398 0.04285 =
0.02521 -0.00336 0.00669 -0.00980
AFIX 43
H2 2 0.238047 0.746003 0.317667 11.00000 -1.20000
AFIX 0
C3 1 0.160060 0.458821 0.286741 11.00000 0.03176 0.03560 =
0.02232 -0.00046 0.01215 0.00132
C4 1 0.183524 0.320347 0.372024 11.00000 0.04972 0.05356 =
0.02759 0.00560 0.01560 -0.00360
AFIX 137
H4A 2 0.232975 0.386736 0.423537 11.00000 -1.50000
H4B 2 0.193528 0.157752 0.363322 11.00000 -1.50000
H4C 2 0.139211 0.327190 0.384249 11.00000 -1.50000
AFIX 0
C99 1 -0.072606 0.039444 0.030687 11.00000 0.02669 0.02536 =
0.01760 0.00073 0.01022 0.00422
N99 3 -0.041954 0.217272 0.030485 11.00000 0.04279 0.02526 =
0.02906 -0.00278 0.01990 -0.00669
S99 4 -0.116015 -0.209311 0.032271 11.00000 0.04065 0.02653 =
0.04511 -0.00032 0.02318 -0.00774
O1 6 0.000000 0.018432 0.250000 10.50000 0.06764 0.06005 =
0.03452 0.00000 0.01043 0.00000
AFIX 3
H1O 2 -0.030300 -0.118972 0.201300 11.00000 0.19667
AFIX 0
HKLF 4
REM Cu95 in C2/c #15
REM R1 = 0.0348 for 1140 Fo > 4sig(Fo) and 0.0440 for all 1344 data
REM 96 parameters refined using 0 restraints
END
WGHT 0.0417 0.0000
REM Highest difference peak 0.469, deepest hole -0.449, 1-sigma level 0.088
Q1 1 0.0215 0.5023 0.0886 11.00000 0.05 0.47
Q2 1 0.0731 0.5066 0.0750 11.00000 0.05 0.33
Q3 1 0.1702 0.4189 0.3330 11.00000 0.05 0.31
Q4 1 -0.0915 -0.1752 0.1221 11.00000 0.05 0.29
Q5 1 -0.1411 -0.1920 -0.0570 11.00000 0.05 0.27
Q6 1 0.1211 0.6071 0.1367 11.00000 0.05 0.27
Q7 1 0.0183 -0.0193 0.2295 11.00000 0.05 0.25
Q8 1 0.1521 0.1414 0.3602 11.00000 0.05 0.24
Q9 1 0.0944 0.3196 0.0987 11.00000 0.05 0.24
Q10 1 0.1107 0.0654 0.3667 11.00000 0.05 0.24
Q11 1 -0.0506 0.0249 0.1843 11.00000 0.05 0.23
Q12 1 -0.0089 0.3342 0.0337 11.00000 0.05 0.22
Q13 1 0.1931 0.5049 0.2796 11.00000 0.05 0.22
Q14 1 0.2787 0.5277 0.4139 11.00000 0.05 0.21
Q15 1 -0.0713 -0.2050 0.0810 11.00000 0.05 0.21
Q16 1 0.1514 0.8783 0.0789 11.00000 0.05 0.20
Q17 1 -0.2047 -0.1783 -0.0605 11.00000 0.05 0.20
Q18 1 0.1606 0.5900 0.2837 11.00000 0.05 0.20
Q19 1 0.2503 0.2189 0.4158 11.00000 0.05 0.20
Q20 1 -0.1441 -0.1460 0.0455 11.00000 0.05 0.19
;
_shelx_res_checksum 62159
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_cu141
_database_code_depnum_ccdc_archive 'CCDC 1493332'
_audit_update_record
;
2016-07-14 deposited with the CCDC.
2016-10-25 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014/6
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C38 H56 Cu3 N18 O2 S6'
_chemical_formula_sum 'C38 H56 Cu3 N18 O2 S6'
_chemical_formula_weight 1179.98
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'
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'
S S 0.1246 0.1234 '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'
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.8235(5)
_cell_length_b 10.5552(6)
_cell_length_c 15.0423(6)
_cell_angle_alpha 77.423(4)
_cell_angle_beta 79.796(4)
_cell_angle_gamma 63.616(6)
_cell_volume 1357.95(13)
_cell_formula_units_Z 1
_cell_measurement_temperature 295(2)
_cell_measurement_reflns_used 4126
_cell_measurement_theta_min 3.7880
_cell_measurement_theta_max 28.1120
_exptl_crystal_description plate
_exptl_crystal_colour green
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.443
_exptl_crystal_F_000 609
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.14
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.04
_exptl_absorpt_coefficient_mu 1.445
_shelx_estimated_absorpt_T_min ?
_shelx_estimated_absorpt_T_max ?
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.65544
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_process_details 'Blessing, Acta Cryst. A51 (1995) 33-38'
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 295(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_source ?
_diffrn_measurement_device_type 'Oxford Diffraction Gemini A Ultra'
_diffrn_measurement_method ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 11700
_diffrn_reflns_av_unetI/netI 0.0513
_diffrn_reflns_av_R_equivalents 0.0384
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_theta_min 3.462
_diffrn_reflns_theta_max 25.050
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total 4806
_reflns_number_gt 3526
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_cell_refinement 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_reduction 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics
'Mercury (Macrae, J.Appl.Cryst. 41 (2008) 466-470'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_refine_special_details ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0420P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 4806
_refine_ls_number_parameters 312
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0568
_refine_ls_R_factor_gt 0.0344
_refine_ls_wR_factor_ref 0.0835
_refine_ls_wR_factor_gt 0.0778
_refine_ls_goodness_of_fit_ref 0.951
_refine_ls_restrained_S_all 0.951
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.14436(4) 0.90566(3) 0.14443(2) 0.03613(12) Uani 1 1 d . . . . .
Cu2 Cu 0.5000 0.5000 0.5000 0.04116(15) Uani 1 2 d S . P . .
N1 N -0.0254(3) 0.9109(2) 0.23791(15) 0.0404(6) Uani 1 1 d . . . . .
N2 N -0.0204(3) 0.7931(3) 0.29822(15) 0.0456(6) Uani 1 1 d . . . . .
H2 H 0.0510 0.7085 0.2955 0.055 Uiso 1 1 calc R U . . .
N3 N 0.3165(3) 0.8885(2) 0.04905(14) 0.0389(6) Uani 1 1 d . . . . .
N4 N 0.4603(3) 0.7873(2) 0.06110(15) 0.0423(6) Uani 1 1 d . . . . .
H4 H 0.4866 0.7288 0.1112 0.051 Uiso 1 1 calc R U . . .
N5 N 0.2983(3) 0.6069(3) 0.56773(15) 0.0441(6) Uani 1 1 d . . . . .
N6 N 0.2639(3) 0.5739(3) 0.65770(16) 0.0503(7) Uani 1 1 d . . . . .
H6A H 0.3260 0.5043 0.6929 0.060 Uiso 1 1 calc R U . . .
C1 C -0.1386(4) 0.8230(3) 0.36238(19) 0.0441(8) Uani 1 1 d . . . . .
C2 C -0.2275(4) 0.9687(3) 0.34406(19) 0.0451(8) Uani 1 1 d . . . . .
C3 C -0.1515(4) 1.0171(3) 0.26595(19) 0.0445(8) Uani 1 1 d . . . . .
H3 H -0.1853 1.1119 0.2374 0.053 Uiso 1 1 calc R U . . .
C4 C -0.3722(4) 1.0573(4) 0.3955(2) 0.0711(11) Uani 1 1 d . . . . .
H4A H -0.4456 1.0189 0.3994 0.107 Uiso 1 1 calc R U . . .
H4B H -0.4119 1.1542 0.3640 0.107 Uiso 1 1 calc R U . . .
H4C H -0.3519 1.0557 0.4559 0.107 Uiso 1 1 calc R U . . .
C5 C -0.1574(5) 0.7085(4) 0.4337(2) 0.0656(10) Uani 1 1 d . . . . .
H5A H -0.1590 0.6365 0.4049 0.098 Uiso 1 1 calc R U . . .
H5B H -0.2515 0.7490 0.4709 0.098 Uiso 1 1 calc R U . . .
H5C H -0.0737 0.6661 0.4712 0.098 Uiso 1 1 calc R U . . .
C6 C 0.3267(4) 0.9545(3) -0.03680(17) 0.0420(7) Uani 1 1 d . . . . .
H6 H 0.2450 1.0302 -0.0650 0.050 Uiso 1 1 calc R U . . .
C7 C 0.4731(4) 0.8969(3) -0.07853(18) 0.0407(7) Uani 1 1 d . . . . .
C8 C 0.5572(4) 0.7886(3) -0.0138(2) 0.0432(8) Uani 1 1 d . . . . .
C9 C 0.5310(5) 0.9406(4) -0.1737(2) 0.0661(11) Uani 1 1 d . . . . .
H9A H 0.4523 1.0264 -0.2016 0.099 Uiso 1 1 calc R U . . .
H9B H 0.5597 0.8655 -0.2089 0.099 Uiso 1 1 calc R U . . .
H9C H 0.6183 0.9580 -0.1714 0.099 Uiso 1 1 calc R U . . .
C10 C 0.7211(4) 0.6890(4) -0.0168(2) 0.0673(10) Uani 1 1 d . . . . .
H10A H 0.7502 0.6508 0.0444 0.101 Uiso 1 1 calc R U . . .
H10B H 0.7806 0.7394 -0.0487 0.101 Uiso 1 1 calc R U . . .
H10C H 0.7389 0.6121 -0.0481 0.101 Uiso 1 1 calc R U . . .
C11 C 0.1733(4) 0.7192(3) 0.5405(2) 0.0482(8) Uani 1 1 d . . . . .
H11 H 0.1625 0.7665 0.4805 0.058 Uiso 1 1 calc R U . . .
C12 C 0.0608(4) 0.7577(3) 0.6118(2) 0.0490(8) Uani 1 1 d . . . . .
C13 C 0.1226(4) 0.6612(4) 0.6864(2) 0.0476(8) Uani 1 1 d . . . . .
C14 C -0.0952(4) 0.8812(4) 0.6090(3) 0.0798(12) Uani 1 1 d . . . . .
H14A H -0.0974 0.9545 0.6382 0.120 Uiso 1 1 calc R U . . .
H14B H -0.1703 0.8483 0.6405 0.120 Uiso 1 1 calc R U . . .
H14C H -0.1171 0.9193 0.5465 0.120 Uiso 1 1 calc R U . . .
C15 C 0.0572(5) 0.6398(5) 0.7831(2) 0.0752(12) Uani 1 1 d . . . . .
H15A H 0.0649 0.5439 0.7995 0.113 Uiso 1 1 calc R U . . .
H15B H -0.0481 0.7067 0.7889 0.113 Uiso 1 1 calc R U . . .
H15C H 0.1129 0.6552 0.8229 0.113 Uiso 1 1 calc R U . . .
C16 C 0.5674(5) 0.4100(4) 0.1313(3) 0.0862(13) Uani 1 1 d . . . . .
H16A H 0.6602 0.3964 0.0925 0.129 Uiso 1 1 calc R U . . .
H16B H 0.4856 0.4377 0.0942 0.129 Uiso 1 1 calc R U . . .
H16C H 0.5799 0.3223 0.1715 0.129 Uiso 1 1 calc R U . . .
C97 C 0.3237(3) 0.4550(3) 0.36770(18) 0.0360(7) Uani 1 1 d . . . . .
C98 C 0.3633(3) 0.7867(3) 0.29481(17) 0.0337(6) Uani 1 1 d . . . . .
C99 C 0.0384(3) 0.8229(3) -0.01446(19) 0.0358(7) Uani 1 1 d . . . . .
N97 N 0.3944(3) 0.4617(3) 0.41805(16) 0.0457(6) Uani 1 1 d . . . . .
N98 N 0.2878(3) 0.7998(3) 0.23999(15) 0.0424(6) Uani 1 1 d . . . . .
N99 N -0.0124(3) 0.9097(2) -0.07641(15) 0.0425(6) Uani 1 1 d . . . . .
S97 S 0.22727(12) 0.44495(9) 0.29406(6) 0.0604(3) Uani 1 1 d . . . . .
S98 S 0.47225(11) 0.76557(8) 0.37131(5) 0.0504(2) Uani 1 1 d . . . . .
S99 S 0.10702(11) 0.70154(8) 0.07348(5) 0.0502(2) Uani 1 1 d . . . . .
O1 O 0.5335(3) 0.5174(2) 0.18286(14) 0.0579(6) Uani 1 1 d . . . . .
H1 H 0.4509 0.5336 0.2128 0.087 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0320(2) 0.0412(2) 0.02711(18) -0.00021(14) -0.00314(14) -0.01054(17)
Cu2 0.0292(3) 0.0503(3) 0.0402(3) -0.0151(2) -0.0031(2) -0.0099(3)
N1 0.0367(17) 0.0394(13) 0.0367(12) 0.0008(11) -0.0010(11) -0.0125(13)
N2 0.0386(18) 0.0409(14) 0.0428(14) 0.0029(11) 0.0002(12) -0.0096(13)
N3 0.0376(17) 0.0423(13) 0.0299(12) 0.0034(10) -0.0039(11) -0.0144(13)
N4 0.0355(17) 0.0418(14) 0.0364(13) 0.0029(11) -0.0009(12) -0.0094(13)
N5 0.0339(17) 0.0494(15) 0.0383(14) -0.0092(11) -0.0033(12) -0.0069(13)
N6 0.0362(18) 0.0608(17) 0.0372(14) -0.0013(12) -0.0060(12) -0.0075(14)
C1 0.039(2) 0.057(2) 0.0359(16) -0.0022(14) -0.0040(14) -0.0218(17)
C2 0.037(2) 0.058(2) 0.0380(16) -0.0116(14) 0.0011(14) -0.0189(17)
C3 0.038(2) 0.0435(17) 0.0458(17) -0.0101(14) -0.0004(15) -0.0116(16)
C4 0.054(3) 0.086(3) 0.061(2) -0.025(2) 0.0198(19) -0.022(2)
C5 0.065(3) 0.081(2) 0.0504(19) 0.0078(18) 0.0001(18) -0.040(2)
C6 0.047(2) 0.0448(17) 0.0318(15) 0.0011(13) -0.0051(14) -0.0196(16)
C7 0.052(2) 0.0450(17) 0.0323(15) -0.0092(13) 0.0076(14) -0.0297(16)
C8 0.039(2) 0.0447(17) 0.0474(17) -0.0138(14) 0.0093(15) -0.0214(16)
C9 0.081(3) 0.080(2) 0.0415(18) -0.0034(17) 0.0133(18) -0.047(2)
C10 0.043(2) 0.064(2) 0.080(2) -0.0109(19) 0.0164(19) -0.018(2)
C11 0.036(2) 0.0461(18) 0.0471(18) -0.0013(14) -0.0065(15) -0.0056(16)
C12 0.031(2) 0.0458(18) 0.066(2) -0.0207(16) -0.0005(16) -0.0089(16)
C13 0.036(2) 0.063(2) 0.0470(17) -0.0222(16) 0.0015(15) -0.0198(17)
C14 0.047(3) 0.065(2) 0.099(3) -0.023(2) 0.000(2) 0.004(2)
C15 0.061(3) 0.115(3) 0.052(2) -0.030(2) 0.0122(19) -0.039(3)
C16 0.083(4) 0.075(3) 0.096(3) -0.033(2) 0.002(3) -0.024(3)
C97 0.0343(19) 0.0304(15) 0.0373(15) -0.0037(12) 0.0004(13) -0.0103(14)
C98 0.0312(18) 0.0300(14) 0.0313(14) 0.0008(12) 0.0022(13) -0.0096(13)
C99 0.0340(19) 0.0318(15) 0.0399(16) -0.0127(13) 0.0006(13) -0.0106(14)
N97 0.0405(17) 0.0491(15) 0.0456(14) -0.0096(12) -0.0082(13) -0.0148(13)
N98 0.0367(17) 0.0536(15) 0.0318(13) -0.0008(11) -0.0058(12) -0.0161(13)
N99 0.0443(18) 0.0381(13) 0.0373(13) -0.0009(11) -0.0083(12) -0.0110(12)
S97 0.0666(7) 0.0552(5) 0.0673(5) -0.0094(4) -0.0284(5) -0.0250(5)
S98 0.0588(6) 0.0482(5) 0.0478(4) 0.0048(4) -0.0245(4) -0.0241(4)
S99 0.0641(6) 0.0358(4) 0.0421(4) 0.0034(3) -0.0147(4) -0.0140(4)
O1 0.0603(18) 0.0530(13) 0.0515(13) -0.0042(11) 0.0002(12) -0.0198(13)
_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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N99 1.970(2) 2_575 ?
Cu1 N1 1.971(2) . ?
Cu1 N98 1.980(2) . ?
Cu1 N3 1.983(2) . ?
Cu1 S99 2.7853(9) . ?
Cu2 N97 1.950(3) . ?
Cu2 N97 1.950(3) 2_666 ?
Cu2 N5 2.009(2) 2_666 ?
Cu2 N5 2.009(2) . ?
N1 C3 1.325(4) . ?
N1 N2 1.357(3) . ?
N2 C1 1.338(4) . ?
N2 H2 0.8600 . ?
N3 C6 1.337(3) . ?
N3 N4 1.355(3) . ?
N4 C8 1.342(4) . ?
N4 H4 0.8600 . ?
N5 C11 1.324(4) . ?
N5 N6 1.343(3) . ?
N6 C13 1.336(4) . ?
N6 H6A 0.8600 . ?
C1 C2 1.383(4) . ?
C1 C5 1.486(4) . ?
C2 C3 1.402(4) . ?
C2 C4 1.495(4) . ?
C3 H3 0.9300 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.378(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.378(4) . ?
C7 C9 1.498(4) . ?
C8 C10 1.480(5) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.381(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.363(4) . ?
C12 C14 1.507(5) . ?
C13 C15 1.495(4) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 O1 1.398(4) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C97 N97 1.147(3) . ?
C97 S97 1.627(3) . ?
C98 N98 1.151(3) . ?
C98 S98 1.623(3) . ?
C99 N99 1.159(3) . ?
C99 S99 1.630(3) . ?
N99 Cu1 1.970(2) 2_575 ?
O1 H1 0.8200 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N99 Cu1 N1 91.20(10) 2_575 . ?
N99 Cu1 N98 148.84(10) 2_575 . ?
N1 Cu1 N98 88.93(10) . . ?
N99 Cu1 N3 90.79(10) 2_575 . ?
N1 Cu1 N3 176.34(9) . . ?
N98 Cu1 N3 90.95(10) . . ?
N99 Cu1 S99 104.44(7) 2_575 . ?
N1 Cu1 S99 88.62(7) . . ?
N98 Cu1 S99 106.71(7) . . ?
N3 Cu1 S99 87.92(7) . . ?
N97 Cu2 N97 180.0 . 2_666 ?
N97 Cu2 N5 90.46(10) . 2_666 ?
N97 Cu2 N5 89.54(10) 2_666 2_666 ?
N97 Cu2 N5 89.54(10) . . ?
N97 Cu2 N5 90.46(10) 2_666 . ?
N5 Cu2 N5 180.0 2_666 . ?
C3 N1 N2 104.6(2) . . ?
C3 N1 Cu1 132.8(2) . . ?
N2 N1 Cu1 122.12(19) . . ?
C1 N2 N1 112.6(2) . . ?
C1 N2 H2 123.7 . . ?
N1 N2 H2 123.7 . . ?
C6 N3 N4 104.0(2) . . ?
C6 N3 Cu1 133.8(2) . . ?
N4 N3 Cu1 122.11(16) . . ?
C8 N4 N3 112.4(2) . . ?
C8 N4 H4 123.8 . . ?
N3 N4 H4 123.8 . . ?
C11 N5 N6 104.0(3) . . ?
C11 N5 Cu2 131.9(2) . . ?
N6 N5 Cu2 124.05(19) . . ?
C13 N6 N5 112.5(2) . . ?
C13 N6 H6A 123.7 . . ?
N5 N6 H6A 123.7 . . ?
N2 C1 C2 106.6(2) . . ?
N2 C1 C5 121.3(3) . . ?
C2 C1 C5 132.0(3) . . ?
C1 C2 C3 104.6(3) . . ?
C1 C2 C4 128.4(3) . . ?
C3 C2 C4 126.9(3) . . ?
N1 C3 C2 111.6(3) . . ?
N1 C3 H3 124.2 . . ?
C2 C3 H3 124.2 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C1 C5 H5A 109.5 . . ?
C1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 C7 111.8(3) . . ?
N3 C6 H6 124.1 . . ?
C7 C6 H6 124.1 . . ?
C8 C7 C6 105.3(2) . . ?
C8 C7 C9 126.5(3) . . ?
C6 C7 C9 128.2(3) . . ?
N4 C8 C7 106.4(3) . . ?
N4 C8 C10 122.3(3) . . ?
C7 C8 C10 131.3(3) . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N5 C11 C12 111.9(3) . . ?
N5 C11 H11 124.1 . . ?
C12 C11 H11 124.1 . . ?
C13 C12 C11 104.9(3) . . ?
C13 C12 C14 127.2(3) . . ?
C11 C12 C14 127.9(3) . . ?
N6 C13 C12 106.6(3) . . ?
N6 C13 C15 121.7(3) . . ?
C12 C13 C15 131.6(3) . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O1 C16 H16A 109.5 . . ?
O1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N97 C97 S97 178.4(3) . . ?
N98 C98 S98 178.9(3) . . ?
N99 C99 S99 179.1(3) . . ?
C97 N97 Cu2 172.6(2) . . ?
C98 N98 Cu1 155.9(2) . . ?
C99 N99 Cu1 158.9(2) . 2_575 ?
C99 S99 Cu1 88.38(9) . . ?
C16 O1 H1 109.5 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 S97 0.82 2.75 3.484(3) 149.7 .
N2 H2 S97 0.86 2.54 3.395(3) 170.6 .
N4 H4 O1 0.86 2.14 2.892(3) 146.2 .
N4 H4 N98 0.86 2.47 2.910(3) 112.2 .
N6 H6A O1 0.86 2.43 3.102(3) 135.7 2_666
_refine_diff_density_max 0.320
_refine_diff_density_min -0.290
_refine_diff_density_rms 0.060
_shelxl_version_number 2014/6
_shelx_res_file
;
TITL cu141 in P1 #1 New: P-1
CELL 0.71073 9.823458 10.555232 15.042303 77.4232 79.7962 63.6156
ZERR 1 0.000545 0.000587 0.00057 0.004 0.0039 0.0055
LATT 1
SFAC C H Cu N S O
UNIT 38 56 3 18 6 2
L.S. 10
PLAN 20
BOND $H
fmap 2
acta
OMIT 0 50.1
REM E:/Nix/cu141.hkl
HTAB O1 S97
HTAB N2 S97
HTAB N4 O1
HTAB N4 N98
HTAB N6 O1_$1
EQIV $1 1-x,1-y,1-z
WGHT 0.042000
FVAR 2.43525
CU1 3 0.144361 0.905660 0.144430 11.00000 0.03204 0.04123 =
0.02711 -0.00021 -0.00314 -0.01054
CU2 3 0.500000 0.500000 0.500000 10.50000 0.02917 0.05034 =
0.04019 -0.01514 -0.00307 -0.00988
N1 4 -0.025429 0.910863 0.237911 11.00000 0.03666 0.03936 =
0.03671 0.00083 -0.00100 -0.01253
N2 4 -0.020362 0.793112 0.298222 11.00000 0.03865 0.04087 =
0.04275 0.00285 0.00021 -0.00958
AFIX 43
H2 2 0.051032 0.708547 0.295511 11.00000 -1.20000
AFIX 0
N3 4 0.316470 0.888497 0.049053 11.00000 0.03759 0.04230 =
0.02990 0.00342 -0.00392 -0.01441
N4 4 0.460287 0.787312 0.061100 11.00000 0.03547 0.04183 =
0.03638 0.00289 -0.00087 -0.00942
AFIX 43
H4 2 0.486553 0.728802 0.111154 11.00000 -1.20000
AFIX 0
N5 4 0.298272 0.606948 0.567728 11.00000 0.03389 0.04936 =
0.03832 -0.00919 -0.00330 -0.00692
N6 4 0.263905 0.573906 0.657696 11.00000 0.03618 0.06079 =
0.03718 -0.00130 -0.00600 -0.00750
AFIX 43
H6A 2 0.325961 0.504273 0.692949 11.00000 -1.20000
AFIX 0
C1 1 -0.138594 0.822954 0.362376 11.00000 0.03872 0.05709 =
0.03594 -0.00218 -0.00400 -0.02176
C2 1 -0.227526 0.968727 0.344059 11.00000 0.03742 0.05840 =
0.03795 -0.01165 0.00114 -0.01886
C3 1 -0.151493 1.017068 0.265947 11.00000 0.03808 0.04348 =
0.04577 -0.01014 -0.00040 -0.01164
AFIX 43
H3 2 -0.185347 1.111907 0.237363 11.00000 -1.20000
AFIX 0
C4 1 -0.372190 1.057296 0.395457 11.00000 0.05412 0.08610 =
0.06071 -0.02530 0.01976 -0.02160
AFIX 137
H4A 2 -0.445596 1.018913 0.399416 11.00000 -1.50000
H4B 2 -0.411914 1.154170 0.364022 11.00000 -1.50000
H4C 2 -0.351937 1.055667 0.455929 11.00000 -1.50000
AFIX 0
C5 1 -0.157357 0.708509 0.433658 11.00000 0.06485 0.08084 =
0.05040 0.00780 0.00009 -0.04027
AFIX 137
H5A 2 -0.158972 0.636500 0.404891 11.00000 -1.50000
H5B 2 -0.251487 0.748985 0.470942 11.00000 -1.50000
H5C 2 -0.073737 0.666082 0.471206 11.00000 -1.50000
AFIX 0
C6 1 0.326744 0.954515 -0.036799 11.00000 0.04667 0.04484 =
0.03177 0.00111 -0.00514 -0.01957
AFIX 43
H6 2 0.245031 1.030183 -0.064951 11.00000 -1.20000
AFIX 0
C7 1 0.473066 0.896876 -0.078531 11.00000 0.05216 0.04497 =
0.03226 -0.00923 0.00760 -0.02965
C8 1 0.557222 0.788584 -0.013831 11.00000 0.03940 0.04472 =
0.04742 -0.01375 0.00932 -0.02143
C9 1 0.531038 0.940617 -0.173675 11.00000 0.08114 0.07965 =
0.04148 -0.00343 0.01326 -0.04718
AFIX 137
H9A 2 0.452343 1.026412 -0.201624 11.00000 -1.50000
H9B 2 0.559662 0.865484 -0.208943 11.00000 -1.50000
H9C 2 0.618269 0.957992 -0.171445 11.00000 -1.50000
AFIX 0
C10 1 0.721137 0.688956 -0.016799 11.00000 0.04325 0.06378 =
0.07992 -0.01086 0.01640 -0.01752
AFIX 137
H10A 2 0.750151 0.650752 0.044443 11.00000 -1.50000
H10B 2 0.780636 0.739426 -0.048684 11.00000 -1.50000
H10C 2 0.738940 0.612072 -0.048081 11.00000 -1.50000
AFIX 0
C11 1 0.173294 0.719217 0.540478 11.00000 0.03616 0.04612 =
0.04713 -0.00134 -0.00647 -0.00562
AFIX 43
H11 2 0.162518 0.766479 0.480502 11.00000 -1.20000
AFIX 0
C12 1 0.060843 0.757718 0.611823 11.00000 0.03114 0.04579 =
0.06620 -0.02066 -0.00046 -0.00892
C13 1 0.122625 0.661205 0.686356 11.00000 0.03645 0.06267 =
0.04697 -0.02219 0.00147 -0.01979
C14 1 -0.095160 0.881158 0.609011 11.00000 0.04683 0.06519 =
0.09853 -0.02257 -0.00017 0.00386
AFIX 137
H14A 2 -0.097427 0.954479 0.638209 11.00000 -1.50000
H14B 2 -0.170289 0.848281 0.640494 11.00000 -1.50000
H14C 2 -0.117117 0.919326 0.546540 11.00000 -1.50000
AFIX 0
C15 1 0.057243 0.639844 0.783073 11.00000 0.06103 0.11534 =
0.05197 -0.02991 0.01217 -0.03851
AFIX 137
H15A 2 0.064938 0.543916 0.799460 11.00000 -1.50000
H15B 2 -0.048054 0.706679 0.788933 11.00000 -1.50000
H15C 2 0.112856 0.655219 0.822935 11.00000 -1.50000
AFIX 0
C16 1 0.567448 0.410038 0.131256 11.00000 0.08329 0.07500 =
0.09555 -0.03318 0.00209 -0.02416
AFIX 137
H16A 2 0.660183 0.396370 0.092545 11.00000 -1.50000
H16B 2 0.485560 0.437739 0.094228 11.00000 -1.50000
H16C 2 0.579888 0.322272 0.171549 11.00000 -1.50000
AFIX 0
C97 1 0.323713 0.454974 0.367698 11.00000 0.03429 0.03037 =
0.03733 -0.00366 0.00041 -0.01031
C98 1 0.363256 0.786716 0.294812 11.00000 0.03115 0.03000 =
0.03134 0.00077 0.00222 -0.00964
C99 1 0.038414 0.822896 -0.014459 11.00000 0.03398 0.03179 =
0.03993 -0.01266 0.00063 -0.01064
N97 4 0.394432 0.461704 0.418054 11.00000 0.04047 0.04914 =
0.04562 -0.00957 -0.00824 -0.01478
N98 4 0.287850 0.799787 0.239988 11.00000 0.03670 0.05356 =
0.03177 -0.00077 -0.00579 -0.01607
N99 4 -0.012397 0.909732 -0.076412 11.00000 0.04426 0.03811 =
0.03728 -0.00095 -0.00828 -0.01097
S97 5 0.227267 0.444946 0.294058 11.00000 0.06663 0.05521 =
0.06732 -0.00941 -0.02841 -0.02495
S98 5 0.472251 0.765568 0.371308 11.00000 0.05878 0.04817 =
0.04783 0.00476 -0.02452 -0.02411
S99 5 0.107018 0.701545 0.073485 11.00000 0.06407 0.03578 =
0.04211 0.00337 -0.01470 -0.01400
O1 6 0.533546 0.517385 0.182861 11.00000 0.06033 0.05299 =
0.05149 -0.00418 0.00018 -0.01981
AFIX 147
H1 2 0.450858 0.533629 0.212813 11.00000 -1.50000
AFIX 0
HKLF 4
REM cu141 in P1 #1 New: P-1
REM R1 = 0.0344 for 3526 Fo > 4sig(Fo) and 0.0568 for all 4806 data
REM 312 parameters refined using 0 restraints
END
WGHT 0.0420 0.0000
REM Highest difference peak 0.320, deepest hole -0.290, 1-sigma level 0.060
Q1 1 0.2607 1.2863 -0.2051 11.00000 0.05 0.32
Q2 1 -0.1804 0.8885 0.3583 11.00000 0.05 0.29
Q3 1 -0.0150 0.8577 0.2652 11.00000 0.05 0.29
Q4 1 -0.2136 0.9993 0.3039 11.00000 0.05 0.29
Q5 1 0.5182 0.7712 0.3097 11.00000 0.05 0.28
Q6 1 0.4632 0.4590 0.4611 11.00000 0.05 0.28
Q7 1 0.4135 0.7160 0.0951 11.00000 0.05 0.27
Q8 1 0.1247 0.9407 0.2238 11.00000 0.05 0.27
Q9 1 0.1007 0.8462 0.1232 11.00000 0.05 0.27
Q10 1 0.1351 0.7441 0.0169 11.00000 0.05 0.26
Q11 1 0.2444 0.6847 0.5677 11.00000 0.05 0.25
Q12 1 0.1576 0.8745 0.0705 11.00000 0.05 0.25
Q13 1 0.5209 0.8540 -0.0407 11.00000 0.05 0.24
Q14 1 0.0757 0.6457 0.0592 11.00000 0.05 0.24
Q15 1 -0.1274 0.8962 0.6700 11.00000 0.05 0.23
Q16 1 -0.3635 1.1437 0.4173 11.00000 0.05 0.23
Q17 1 0.1961 0.4532 0.3575 11.00000 0.05 0.23
Q18 1 0.3195 0.9149 0.0024 11.00000 0.05 0.23
Q19 1 0.3919 0.5306 0.4273 11.00000 0.05 0.22
Q20 1 -0.3909 1.0190 0.4349 11.00000 0.05 0.22
;
_shelx_res_checksum 26861
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_cu100
_database_code_depnum_ccdc_archive 'CCDC 1493333'
_audit_update_record
;
2016-07-14 deposited with the CCDC.
2016-10-25 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014/6
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C25 H32 Cu2 N11 S3'
_chemical_formula_sum 'C25 H32 Cu2 N11 S3'
_chemical_formula_weight 709.87
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'
S S 0.1246 0.1234 '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'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 21/c'
_space_group_name_Hall '-P 2ybc'
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 20.3583(15)
_cell_length_b 7.8165(4)
_cell_length_c 21.6675(17)
_cell_angle_alpha 90
_cell_angle_beta 116.100(9)
_cell_angle_gamma 90
_cell_volume 3096.4(4)
_cell_formula_units_Z 4
_cell_measurement_temperature 295(2)
_cell_measurement_reflns_used 4230
_cell_measurement_theta_min 3.3366
_cell_measurement_theta_max 29.1931
_exptl_crystal_description needle
_exptl_crystal_colour brown
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.523
_exptl_crystal_F_000 1460
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.10
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.04
_exptl_absorpt_coefficient_mu 1.612
_shelx_estimated_absorpt_T_min ?
_shelx_estimated_absorpt_T_max ?
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.78268
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_process_details 'Blessing, Acta Cryst. A51 (1995) 33-38'
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 295(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_source ?
_diffrn_measurement_device_type 'Oxford Diffraction Gemini A Ultra'
_diffrn_measurement_method ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 13725
_diffrn_reflns_av_unetI/netI 0.0673
_diffrn_reflns_av_R_equivalents 0.0523
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 24
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_theta_min 3.343
_diffrn_reflns_theta_max 25.050
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.962
_reflns_number_total 5391
_reflns_number_gt 3686
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_cell_refinement 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_reduction 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics
'Mercury (Macrae, J.Appl.Cryst. 41 (2008) 466-470'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_refine_special_details ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0661P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 5391
_refine_ls_number_parameters 378
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0853
_refine_ls_R_factor_gt 0.0503
_refine_ls_wR_factor_ref 0.1293
_refine_ls_wR_factor_gt 0.1147
_refine_ls_goodness_of_fit_ref 0.983
_refine_ls_restrained_S_all 0.983
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.14764(3) 0.35878(6) 0.39946(3) 0.03736(18) Uani 1 1 d . . . . .
Cu2 Cu 0.37362(3) -0.18503(7) 0.57227(3) 0.0520(2) Uani 1 1 d . . . . .
N1 N 0.09824(19) 0.2486(5) 0.45388(18) 0.0416(9) Uani 1 1 d . . . . .
N2 N 0.02375(19) 0.2515(5) 0.4287(2) 0.0435(9) Uani 1 1 d . . . . .
N3 N 0.05595(18) 0.5122(4) 0.35423(19) 0.0422(9) Uani 1 1 d . . . . .
N4 N -0.01265(19) 0.4507(4) 0.33744(19) 0.0402(9) Uani 1 1 d . . . . .
N5 N 0.4468(2) -0.3748(4) 0.57265(18) 0.0426(9) Uani 1 1 d . . . . .
N6 N 0.5163(2) -0.3222(5) 0.58537(19) 0.0446(9) Uani 1 1 d . . . . .
N7 N 0.4581(2) -0.0471(4) 0.64494(19) 0.0452(10) Uani 1 1 d . . . . .
N8 N 0.5257(2) -0.0620(5) 0.6463(2) 0.0474(10) Uani 1 1 d . . . . .
C1 C 0.1233(3) 0.2267(5) 0.5218(3) 0.0458(12) Uani 1 1 d . . . . .
C2 C 0.0648(3) 0.2184(6) 0.5388(3) 0.0548(13) Uani 1 1 d . . . . .
H2 H 0.0678 0.2037 0.5826 0.066 Uiso 1 1 calc R U . . .
C3 C 0.0022(3) 0.2358(6) 0.4792(3) 0.0481(12) Uani 1 1 d . . . . .
C4 C -0.0181(2) 0.2751(5) 0.3558(2) 0.0437(11) Uani 1 1 d . . . . .
H4A H -0.0689 0.2466 0.3425 0.052 Uiso 1 1 calc R U . . .
H4B H 0.0002 0.1992 0.3315 0.052 Uiso 1 1 calc R U . . .
C5 C -0.0646(3) 0.5722(6) 0.3082(2) 0.0469(12) Uani 1 1 d . . . . .
C6 C -0.0279(3) 0.7164(6) 0.3062(3) 0.0524(13) Uani 1 1 d . . . . .
H6 H -0.0487 0.8220 0.2885 0.063 Uiso 1 1 calc R U . . .
C7 C 0.0466(3) 0.6770(6) 0.3356(2) 0.0445(11) Uani 1 1 d . . . . .
C8 C 0.2032(3) 0.2129(7) 0.5700(3) 0.0614(14) Uani 1 1 d . . . . .
H8A H 0.2188 0.3147 0.5974 0.092 Uiso 1 1 calc R U . . .
H8B H 0.2308 0.1996 0.5440 0.092 Uiso 1 1 calc R U . . .
H8C H 0.2111 0.1154 0.5994 0.092 Uiso 1 1 calc R U . . .
C9 C -0.0764(3) 0.2433(7) 0.4665(3) 0.0672(15) Uani 1 1 d . . . . .
H9A H -0.0800 0.2140 0.5079 0.101 Uiso 1 1 calc R U . . .
H9B H -0.1046 0.1638 0.4309 0.101 Uiso 1 1 calc R U . . .
H9C H -0.0949 0.3570 0.4526 0.101 Uiso 1 1 calc R U . . .
C10 C 0.1081(3) 0.7947(6) 0.3474(3) 0.0600(14) Uani 1 1 d . . . . .
H10A H 0.0892 0.8999 0.3231 0.090 Uiso 1 1 calc R U . . .
H10B H 0.1402 0.7427 0.3311 0.090 Uiso 1 1 calc R U . . .
H10C H 0.1346 0.8179 0.3957 0.090 Uiso 1 1 calc R U . . .
C11 C -0.1442(3) 0.5418(6) 0.2867(3) 0.0633(15) Uani 1 1 d . . . . .
H11A H -0.1694 0.6496 0.2782 0.095 Uiso 1 1 calc R U . . .
H11B H -0.1503 0.4823 0.3226 0.095 Uiso 1 1 calc R U . . .
H11C H -0.1642 0.4742 0.2455 0.095 Uiso 1 1 calc R U . . .
C12 C 0.4492(3) -0.5458(6) 0.5757(2) 0.0465(12) Uani 1 1 d . . . . .
C13 C 0.5202(3) -0.6016(7) 0.5898(3) 0.0572(14) Uani 1 1 d . . . . .
H13 H 0.5362 -0.7144 0.5944 0.069 Uiso 1 1 calc R U . . .
C14 C 0.5613(3) -0.4580(7) 0.5956(3) 0.0544(13) Uani 1 1 d . . . . .
C15 C 0.5298(3) -0.1423(6) 0.5882(2) 0.0494(12) Uani 1 1 d . . . . .
H15A H 0.4942 -0.0896 0.5463 0.059 Uiso 1 1 calc R U . . .
H15B H 0.5780 -0.1228 0.5908 0.059 Uiso 1 1 calc R U . . .
C16 C 0.5789(3) -0.0010(6) 0.7062(3) 0.0572(14) Uani 1 1 d . . . . .
C17 C 0.5442(3) 0.0542(7) 0.7435(3) 0.0644(16) Uani 1 1 d . . . . .
H17 H 0.5662 0.1036 0.7869 0.077 Uiso 1 1 calc R U . . .
C18 C 0.4694(3) 0.0235(6) 0.7050(3) 0.0524(13) Uani 1 1 d . . . . .
C19 C 0.3843(3) -0.6458(6) 0.5669(3) 0.0608(15) Uani 1 1 d . . . . .
H19A H 0.3927 -0.7647 0.5621 0.091 Uiso 1 1 calc R U . . .
H19B H 0.3426 -0.6073 0.5265 0.091 Uiso 1 1 calc R U . . .
H19C H 0.3751 -0.6303 0.6064 0.091 Uiso 1 1 calc R U . . .
C20 C 0.6400(3) -0.4414(8) 0.6117(3) 0.0777(18) Uani 1 1 d . . . . .
H20A H 0.6677 -0.4132 0.6594 0.116 Uiso 1 1 calc R U . . .
H20B H 0.6459 -0.3526 0.5840 0.116 Uiso 1 1 calc R U . . .
H20C H 0.6574 -0.5477 0.6022 0.116 Uiso 1 1 calc R U . . .
C21 C 0.4081(3) 0.0549(7) 0.7225(3) 0.0729(17) Uani 1 1 d . . . . .
H21A H 0.4242 0.1283 0.7620 0.109 Uiso 1 1 calc R U . . .
H21B H 0.3916 -0.0519 0.7326 0.109 Uiso 1 1 calc R U . . .
H21C H 0.3686 0.1088 0.6844 0.109 Uiso 1 1 calc R U . . .
C22 C 0.6584(3) -0.0015(9) 0.7220(3) 0.088(2) Uani 1 1 d . . . . .
H22A H 0.6861 0.0540 0.7653 0.131 Uiso 1 1 calc R U . . .
H22B H 0.6650 0.0585 0.6865 0.131 Uiso 1 1 calc R U . . .
H22C H 0.6749 -0.1174 0.7243 0.131 Uiso 1 1 calc R U . . .
C97 C 0.2347(2) 0.6266(6) 0.5244(2) 0.0401(11) Uani 1 1 d . . . . .
C98 C 0.1834(2) 0.4780(6) 0.2808(2) 0.0430(11) Uani 1 1 d . . . . .
C99 C 0.2639(3) 0.0641(6) 0.4369(2) 0.0403(11) Uani 1 1 d . . . . .
N97 N 0.2052(2) 0.5425(5) 0.4772(2) 0.0467(10) Uani 1 1 d . . . . .
N98 N 0.1732(2) 0.4273(5) 0.3258(2) 0.0518(10) Uani 1 1 d . . . . .
N99 N 0.2184(2) 0.1669(5) 0.4237(2) 0.0498(10) Uani 1 1 d . . . . .
S97 S 0.27763(7) -0.25515(17) 0.59446(7) 0.0550(3) Uani 1 1 d . . . . .
S98 S 0.19882(8) 0.54885(19) 0.21779(7) 0.0641(4) Uani 1 1 d . . . . .
S99 S 0.32762(7) -0.07967(15) 0.45375(7) 0.0509(3) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0216(3) 0.0480(3) 0.0406(3) 0.0013(2) 0.0119(2) -0.0015(2)
Cu2 0.0309(4) 0.0552(4) 0.0625(4) -0.0069(3) 0.0137(3) -0.0041(3)
N1 0.025(2) 0.057(2) 0.042(2) 0.0101(18) 0.0142(18) -0.0003(17)
N2 0.024(2) 0.051(2) 0.055(2) 0.0056(18) 0.0169(19) -0.0024(16)
N3 0.020(2) 0.054(2) 0.049(2) 0.0076(18) 0.0111(17) -0.0026(16)
N4 0.022(2) 0.045(2) 0.051(2) 0.0009(18) 0.0143(18) 0.0003(16)
N5 0.025(2) 0.053(2) 0.045(2) -0.0018(18) 0.0110(18) -0.0033(16)
N6 0.029(2) 0.056(2) 0.043(2) -0.0003(18) 0.0105(18) -0.0030(18)
N7 0.037(2) 0.046(2) 0.045(2) -0.0015(18) 0.0113(19) -0.0056(17)
N8 0.034(2) 0.058(2) 0.046(2) -0.0044(19) 0.014(2) -0.0136(18)
C1 0.039(3) 0.043(3) 0.054(3) 0.003(2) 0.019(2) -0.002(2)
C2 0.056(4) 0.068(3) 0.044(3) 0.002(2) 0.025(3) -0.009(3)
C3 0.046(3) 0.049(3) 0.063(3) -0.002(2) 0.037(3) -0.005(2)
C4 0.024(2) 0.052(3) 0.052(3) -0.004(2) 0.014(2) -0.0046(19)
C5 0.030(3) 0.055(3) 0.053(3) -0.001(2) 0.016(2) 0.004(2)
C6 0.040(3) 0.053(3) 0.055(3) 0.006(2) 0.012(2) 0.007(2)
C7 0.037(3) 0.049(3) 0.045(3) 0.006(2) 0.016(2) 0.001(2)
C8 0.042(3) 0.082(4) 0.050(3) 0.021(3) 0.012(3) 0.003(3)
C9 0.046(3) 0.092(4) 0.082(4) 0.001(3) 0.044(3) -0.004(3)
C10 0.044(3) 0.055(3) 0.074(4) 0.015(3) 0.019(3) -0.008(2)
C11 0.027(3) 0.067(3) 0.085(4) -0.004(3) 0.015(3) 0.002(2)
C12 0.041(3) 0.047(3) 0.044(3) -0.001(2) 0.012(2) 0.005(2)
C13 0.045(3) 0.060(3) 0.052(3) 0.000(2) 0.009(3) 0.015(3)
C14 0.031(3) 0.078(4) 0.047(3) -0.002(3) 0.010(2) 0.011(3)
C15 0.032(3) 0.073(3) 0.042(3) 0.007(2) 0.015(2) -0.006(2)
C16 0.045(3) 0.060(3) 0.048(3) 0.000(2) 0.004(3) -0.013(2)
C17 0.066(4) 0.063(3) 0.046(3) -0.004(3) 0.008(3) -0.013(3)
C18 0.050(3) 0.052(3) 0.046(3) -0.004(2) 0.012(3) -0.008(2)
C19 0.045(3) 0.053(3) 0.074(4) 0.000(3) 0.016(3) -0.005(2)
C20 0.032(3) 0.117(5) 0.077(4) -0.001(4) 0.017(3) 0.008(3)
C21 0.072(4) 0.084(4) 0.064(4) -0.016(3) 0.031(3) -0.004(3)
C22 0.045(4) 0.132(5) 0.068(4) -0.011(4) 0.009(3) -0.030(4)
C97 0.022(2) 0.051(3) 0.049(3) 0.001(2) 0.017(2) 0.000(2)
C98 0.022(2) 0.058(3) 0.042(3) -0.011(2) 0.008(2) 0.004(2)
C99 0.030(3) 0.053(3) 0.039(3) -0.002(2) 0.017(2) -0.009(2)
N97 0.031(2) 0.055(2) 0.043(2) -0.004(2) 0.0063(19) -0.0080(18)
N98 0.035(2) 0.078(3) 0.048(2) 0.005(2) 0.022(2) 0.004(2)
N99 0.034(2) 0.059(2) 0.055(2) 0.004(2) 0.018(2) 0.002(2)
S97 0.0385(7) 0.0751(8) 0.0524(8) -0.0166(6) 0.0210(6) -0.0092(6)
S98 0.0568(9) 0.0890(10) 0.0534(8) 0.0172(7) 0.0307(7) 0.0156(7)
S99 0.0440(8) 0.0566(7) 0.0551(8) 0.0067(6) 0.0247(6) 0.0122(6)
_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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N98 1.959(4) . ?
Cu1 N99 1.983(4) . ?
Cu1 N1 2.046(4) . ?
Cu1 N3 2.067(3) . ?
Cu1 N97 2.130(4) . ?
Cu2 N7 2.054(4) . ?
Cu2 N5 2.099(4) . ?
Cu2 S97 2.2752(15) . ?
Cu2 S99 2.4564(14) . ?
N1 C1 1.339(6) . ?
N1 N2 1.368(5) . ?
N2 C3 1.351(6) . ?
N2 C4 1.438(6) . ?
N3 C7 1.339(5) . ?
N3 N4 1.366(5) . ?
N4 C5 1.354(5) . ?
N4 C4 1.447(5) . ?
N5 C12 1.338(5) . ?
N5 N6 1.380(5) . ?
N6 C14 1.355(6) . ?
N6 C15 1.429(6) . ?
N7 C18 1.336(6) . ?
N7 N8 1.369(5) . ?
N8 C16 1.360(6) . ?
N8 C15 1.441(6) . ?
C1 C2 1.395(7) . ?
C1 C8 1.501(6) . ?
C2 C3 1.364(7) . ?
C3 C9 1.502(7) . ?
C5 C6 1.363(7) . ?
C5 C11 1.496(7) . ?
C6 C7 1.396(6) . ?
C7 C10 1.482(6) . ?
C12 C13 1.409(7) . ?
C12 C19 1.474(7) . ?
C13 C14 1.372(7) . ?
C14 C20 1.489(7) . ?
C16 C17 1.357(8) . ?
C16 C22 1.500(8) . ?
C17 C18 1.397(7) . ?
C18 C21 1.477(8) . ?
C97 N97 1.139(5) . ?
C97 S97 1.660(5) 1_565 ?
C98 N98 1.153(6) . ?
C98 S98 1.626(6) . ?
C99 N99 1.164(6) . ?
C99 S99 1.631(5) . ?
S97 C97 1.660(5) 1_545 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N98 Cu1 N99 90.03(17) . . ?
N98 Cu1 N1 163.51(16) . . ?
N99 Cu1 N1 90.73(16) . . ?
N98 Cu1 N3 87.88(16) . . ?
N99 Cu1 N3 164.44(15) . . ?
N1 Cu1 N3 86.97(14) . . ?
N98 Cu1 N97 102.05(16) . . ?
N99 Cu1 N97 102.57(15) . . ?
N1 Cu1 N97 93.85(15) . . ?
N3 Cu1 N97 92.94(15) . . ?
N7 Cu2 N5 90.85(14) . . ?
N7 Cu2 S97 118.15(13) . . ?
N5 Cu2 S97 120.18(11) . . ?
N7 Cu2 S99 115.54(11) . . ?
N5 Cu2 S99 100.63(11) . . ?
S97 Cu2 S99 109.50(5) . . ?
C1 N1 N2 105.1(4) . . ?
C1 N1 Cu1 129.8(3) . . ?
N2 N1 Cu1 120.2(3) . . ?
C3 N2 N1 111.9(4) . . ?
C3 N2 C4 130.9(4) . . ?
N1 N2 C4 117.2(4) . . ?
C7 N3 N4 105.4(3) . . ?
C7 N3 Cu1 132.9(3) . . ?
N4 N3 Cu1 121.7(3) . . ?
C5 N4 N3 112.0(3) . . ?
C5 N4 C4 131.0(4) . . ?
N3 N4 C4 116.9(3) . . ?
C12 N5 N6 105.9(4) . . ?
C12 N5 Cu2 135.8(3) . . ?
N6 N5 Cu2 117.0(3) . . ?
C14 N6 N5 111.1(4) . . ?
C14 N6 C15 131.3(4) . . ?
N5 N6 C15 117.6(4) . . ?
C18 N7 N8 105.8(4) . . ?
C18 N7 Cu2 133.7(4) . . ?
N8 N7 Cu2 117.8(3) . . ?
C16 N8 N7 111.2(4) . . ?
C16 N8 C15 131.2(5) . . ?
N7 N8 C15 117.5(4) . . ?
N1 C1 C2 109.8(4) . . ?
N1 C1 C8 123.1(4) . . ?
C2 C1 C8 127.1(5) . . ?
C3 C2 C1 107.2(4) . . ?
N2 C3 C2 106.0(4) . . ?
N2 C3 C9 123.2(5) . . ?
C2 C3 C9 130.8(5) . . ?
N2 C4 N4 110.1(3) . . ?
N4 C5 C6 105.5(4) . . ?
N4 C5 C11 123.4(4) . . ?
C6 C5 C11 131.0(4) . . ?
C5 C6 C7 107.7(4) . . ?
N3 C7 C6 109.3(4) . . ?
N3 C7 C10 123.3(4) . . ?
C6 C7 C10 127.4(4) . . ?
N5 C12 C13 109.4(4) . . ?
N5 C12 C19 120.7(4) . . ?
C13 C12 C19 129.8(4) . . ?
C14 C13 C12 107.0(4) . . ?
N6 C14 C13 106.5(4) . . ?
N6 C14 C20 123.4(5) . . ?
C13 C14 C20 130.0(5) . . ?
N6 C15 N8 112.5(4) . . ?
C17 C16 N8 106.0(5) . . ?
C17 C16 C22 131.1(5) . . ?
N8 C16 C22 122.9(6) . . ?
C16 C17 C18 107.8(5) . . ?
N7 C18 C17 109.2(5) . . ?
N7 C18 C21 121.0(5) . . ?
C17 C18 C21 129.8(5) . . ?
N97 C97 S97 178.5(4) . 1_565 ?
N98 C98 S98 179.3(4) . . ?
N99 C99 S99 178.8(4) . . ?
C97 N97 Cu1 171.1(4) . . ?
C98 N98 Cu1 174.0(4) . . ?
C99 N99 Cu1 174.1(4) . . ?
C97 S97 Cu2 95.55(17) 1_545 . ?
C99 S99 Cu2 111.40(17) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C4 H4A S98 0.97 2.84 3.748(4) 156.7 2_545
C8 H8B N99 0.96 2.52 3.336(7) 143.2 .
C10 H10B N98 0.96 2.57 3.282(7) 131.0 .
_refine_diff_density_max 0.818
_refine_diff_density_min -0.576
_refine_diff_density_rms 0.081
_shelxl_version_number 2014/6
_shelx_res_file
;
TITL Cu100 in P21/c #14
CELL 0.71073 20.3583 7.8165 21.6675 90 116.100 90
ZERR 4 0.0015 0.0004 0.0017 0 0.009 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N S Cu
UNIT 100 128 44 12 8
L.S. 20
PLAN 20
REM reset to P21/c #14
BOND
fmap 2
ACTA
EQIV $1 -x,-1/2+y,1/2-z
HTAB C4 S98_$1
HTAB C8 N99
HTAB C10 N98
OMIT 0 50.1
REM C:/XcaliburData/Cu100/struct/olex2_Cu100/Cu100.hkl
WGHT 0.066100
FVAR 0.93444
CU1 5 0.147635 0.358776 0.399464 11.00000 0.02163 0.04797 =
0.04059 0.00132 0.01195 -0.00148
CU2 5 0.373617 -0.185033 0.572269 11.00000 0.03093 0.05521 =
0.06248 -0.00693 0.01372 -0.00413
N1 3 0.098239 0.248600 0.453880 11.00000 0.02541 0.05707 =
0.04178 0.01005 0.01420 -0.00035
N2 3 0.023746 0.251528 0.428716 11.00000 0.02409 0.05133 =
0.05464 0.00564 0.01685 -0.00235
N3 3 0.055945 0.512216 0.354235 11.00000 0.01978 0.05371 =
0.04873 0.00762 0.01107 -0.00263
N4 3 -0.012651 0.450718 0.337441 11.00000 0.02186 0.04534 =
0.05132 0.00086 0.01432 0.00027
N5 3 0.446757 -0.374776 0.572650 11.00000 0.02522 0.05271 =
0.04514 -0.00182 0.01101 -0.00326
N6 3 0.516272 -0.322235 0.585366 11.00000 0.02907 0.05642 =
0.04258 -0.00033 0.01050 -0.00298
N7 3 0.458080 -0.047058 0.644944 11.00000 0.03694 0.04644 =
0.04496 -0.00148 0.01132 -0.00563
N8 3 0.525707 -0.062026 0.646291 11.00000 0.03351 0.05849 =
0.04627 -0.00440 0.01386 -0.01357
C1 1 0.123308 0.226701 0.521788 11.00000 0.03907 0.04258 =
0.05363 0.00253 0.01850 -0.00230
C2 1 0.064762 0.218392 0.538795 11.00000 0.05574 0.06767 =
0.04447 0.00236 0.02523 -0.00865
AFIX 43
H2 2 0.067805 0.203730 0.582569 11.00000 -1.20000
AFIX 0
C3 1 0.002239 0.235803 0.479189 11.00000 0.04650 0.04907 =
0.06287 -0.00151 0.03705 -0.00517
C4 1 -0.018055 0.275068 0.355848 11.00000 0.02357 0.05245 =
0.05246 -0.00366 0.01428 -0.00463
AFIX 23
H4A 2 -0.068888 0.246595 0.342515 11.00000 -1.20000
H4B 2 0.000191 0.199218 0.331478 11.00000 -1.20000
AFIX 0
C5 1 -0.064611 0.572216 0.308159 11.00000 0.02955 0.05543 =
0.05318 -0.00071 0.01580 0.00357
C6 1 -0.027867 0.716375 0.306222 11.00000 0.04025 0.05258 =
0.05486 0.00577 0.01230 0.00713
AFIX 43
H6 2 -0.048678 0.821982 0.288537 11.00000 -1.20000
AFIX 0
C7 1 0.046611 0.677036 0.335552 11.00000 0.03718 0.04878 =
0.04518 0.00620 0.01603 0.00125
C8 1 0.203215 0.212850 0.570007 11.00000 0.04249 0.08248 =
0.05030 0.02112 0.01224 0.00293
AFIX 137
H8A 2 0.218830 0.314681 0.597437 11.00000 -1.50000
H8B 2 0.230771 0.199569 0.543988 11.00000 -1.50000
H8C 2 0.211137 0.115445 0.599428 11.00000 -1.50000
AFIX 0
C9 1 -0.076430 0.243332 0.466495 11.00000 0.04573 0.09164 =
0.08194 0.00090 0.04430 -0.00360
AFIX 137
H9A 2 -0.080033 0.214017 0.507923 11.00000 -1.50000
H9B 2 -0.104595 0.163836 0.430856 11.00000 -1.50000
H9C 2 -0.094937 0.356954 0.452593 11.00000 -1.50000
AFIX 0
C10 1 0.108077 0.794711 0.347402 11.00000 0.04415 0.05482 =
0.07388 0.01498 0.01947 -0.00792
AFIX 137
H10A 2 0.089250 0.899851 0.323126 11.00000 -1.50000
H10B 2 0.140195 0.742671 0.331079 11.00000 -1.50000
H10C 2 0.134612 0.817859 0.395680 11.00000 -1.50000
AFIX 0
C11 1 -0.144240 0.541832 0.286685 11.00000 0.02739 0.06715 =
0.08463 -0.00371 0.01491 0.00198
AFIX 137
H11A 2 -0.169359 0.649560 0.278178 11.00000 -1.50000
H11B 2 -0.150318 0.482267 0.322579 11.00000 -1.50000
H11C 2 -0.164152 0.474168 0.245516 11.00000 -1.50000
AFIX 0
C12 1 0.449195 -0.545818 0.575661 11.00000 0.04053 0.04723 =
0.04450 -0.00136 0.01204 0.00548
C13 1 0.520205 -0.601593 0.589811 11.00000 0.04546 0.06012 =
0.05233 -0.00028 0.00887 0.01499
AFIX 43
H13 2 0.536207 -0.714387 0.594363 11.00000 -1.20000
AFIX 0
C14 1 0.561305 -0.458023 0.595607 11.00000 0.03055 0.07798 =
0.04680 -0.00219 0.00971 0.01073
C15 1 0.529794 -0.142277 0.588229 11.00000 0.03215 0.07257 =
0.04237 0.00750 0.01534 -0.00647
AFIX 23
H15A 2 0.494235 -0.089564 0.546285 11.00000 -1.20000
H15B 2 0.577992 -0.122841 0.590802 11.00000 -1.20000
AFIX 0
C16 1 0.578883 -0.001047 0.706236 11.00000 0.04536 0.05983 =
0.04831 0.00037 0.00392 -0.01298
C17 1 0.544159 0.054185 0.743505 11.00000 0.06583 0.06317 =
0.04582 -0.00422 0.00764 -0.01342
AFIX 43
H17 2 0.566175 0.103649 0.786939 11.00000 -1.20000
AFIX 0
C18 1 0.469430 0.023493 0.704990 11.00000 0.04968 0.05200 =
0.04553 -0.00354 0.01186 -0.00812
C19 1 0.384254 -0.645753 0.566907 11.00000 0.04469 0.05282 =
0.07440 -0.00033 0.01647 -0.00528
AFIX 137
H19A 2 0.392739 -0.764745 0.562101 11.00000 -1.50000
H19B 2 0.342633 -0.607292 0.526525 11.00000 -1.50000
H19C 2 0.375103 -0.630297 0.606394 11.00000 -1.50000
AFIX 0
C20 1 0.640049 -0.441389 0.611749 11.00000 0.03199 0.11684 =
0.07704 -0.00121 0.01749 0.00848
AFIX 137
H20A 2 0.667674 -0.413161 0.659445 11.00000 -1.50000
H20B 2 0.645880 -0.352550 0.583964 11.00000 -1.50000
H20C 2 0.657376 -0.547727 0.602248 11.00000 -1.50000
AFIX 0
C21 1 0.408098 0.054913 0.722517 11.00000 0.07238 0.08372 =
0.06409 -0.01634 0.03137 -0.00449
AFIX 137
H21A 2 0.424172 0.128253 0.762011 11.00000 -1.50000
H21B 2 0.391603 -0.051906 0.732562 11.00000 -1.50000
H21C 2 0.368649 0.108818 0.684372 11.00000 -1.50000
AFIX 0
C22 1 0.658373 -0.001511 0.722010 11.00000 0.04545 0.13194 =
0.06793 -0.01109 0.00883 -0.02971
AFIX 137
H22A 2 0.686107 0.054026 0.765318 11.00000 -1.50000
H22B 2 0.664952 0.058518 0.686477 11.00000 -1.50000
H22C 2 0.674945 -0.117373 0.724333 11.00000 -1.50000
AFIX 0
C97 1 0.234675 0.626559 0.524383 11.00000 0.02235 0.05111 =
0.04875 0.00135 0.01726 0.00031
C98 1 0.183370 0.477996 0.280755 11.00000 0.02215 0.05772 =
0.04228 -0.01080 0.00779 0.00384
C99 1 0.263913 0.064060 0.436892 11.00000 0.03035 0.05305 =
0.03925 -0.00188 0.01680 -0.00919
N97 3 0.205173 0.542548 0.477167 11.00000 0.03114 0.05540 =
0.04260 -0.00438 0.00625 -0.00795
N98 3 0.173192 0.427349 0.325780 11.00000 0.03470 0.07773 =
0.04759 0.00523 0.02227 0.00354
N99 3 0.218400 0.166942 0.423734 11.00000 0.03427 0.05880 =
0.05488 0.00394 0.01816 0.00237
S97 4 0.277635 -0.255146 0.594458 11.00000 0.03846 0.07514 =
0.05235 -0.01655 0.02096 -0.00915
S98 4 0.198823 0.548853 0.217794 11.00000 0.05682 0.08899 =
0.05340 0.01721 0.03065 0.01564
S99 4 0.327615 -0.079666 0.453749 11.00000 0.04401 0.05656 =
0.05515 0.00665 0.02468 0.01224
HKLF 4
REM Cu100 in P21/c #14
REM R1 = 0.0503 for 3686 Fo > 4sig(Fo) and 0.0853 for all 5391 data
REM 378 parameters refined using 0 restraints
END
WGHT 0.0661 0.0000
REM Highest difference peak 0.818, deepest hole -0.576, 1-sigma level 0.081
Q1 1 0.5574 -0.7530 0.5895 11.00000 0.05 0.82
Q2 1 0.3005 -0.0522 0.4082 11.00000 0.05 0.48
Q3 1 0.2515 -0.1766 0.5506 11.00000 0.05 0.46
Q4 1 0.3677 -0.0650 0.5747 11.00000 0.05 0.44
Q5 1 0.1423 0.4825 0.4079 11.00000 0.05 0.43
Q6 1 0.3695 -0.3426 0.5604 11.00000 0.05 0.40
Q7 1 0.2047 0.4223 0.2259 11.00000 0.05 0.37
Q8 1 -0.1674 0.4277 0.2803 11.00000 0.05 0.36
Q9 1 0.1397 0.4059 0.3319 11.00000 0.05 0.34
Q10 1 0.3632 -0.5118 0.5714 11.00000 0.05 0.33
Q11 1 0.1437 0.2490 0.4092 11.00000 0.05 0.33
Q12 1 0.2114 0.2015 0.6197 11.00000 0.05 0.32
Q13 1 0.1041 0.8921 0.3594 11.00000 0.05 0.30
Q14 1 0.1218 0.7993 0.2893 11.00000 0.05 0.30
Q15 1 0.1523 0.7510 0.3742 11.00000 0.05 0.28
Q16 1 -0.0223 0.3654 0.3299 11.00000 0.05 0.28
Q17 1 0.3703 -0.2583 0.6112 11.00000 0.05 0.28
Q18 1 -0.0425 0.6167 0.2821 11.00000 0.05 0.27
Q19 1 0.3903 -0.3062 0.6064 11.00000 0.05 0.27
Q20 1 0.1785 0.3857 0.4394 11.00000 0.05 0.27
;
_shelx_res_checksum 16611
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_cu115a
_database_code_depnum_ccdc_archive 'CCDC 1493334'
_audit_update_record
;
2016-07-14 deposited with the CCDC.
2016-10-25 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014/6
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C13 H9 Cu N7 S2'
_chemical_formula_sum 'C13 H9 Cu N7 S2'
_chemical_formula_weight 390.93
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
S S 0.1246 0.1234 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 21/c'
_space_group_name_Hall '-P 2ybc'
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 12.7902(7)
_cell_length_b 8.3391(3)
_cell_length_c 15.9931(7)
_cell_angle_alpha 90
_cell_angle_beta 113.001(6)
_cell_angle_gamma 90
_cell_volume 1570.19(14)
_cell_formula_units_Z 4
_cell_measurement_temperature 295(2)
_cell_measurement_reflns_used 3824
_cell_measurement_theta_min 3.4539
_cell_measurement_theta_max 29.2121
_exptl_crystal_description plate
_exptl_crystal_colour green
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.654
_exptl_crystal_F_000 788
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.21
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.10
_exptl_absorpt_coefficient_mu 1.665
_shelx_estimated_absorpt_T_min ?
_shelx_estimated_absorpt_T_max ?
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.81550
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_process_details 'Blessing, Acta Cryst. A51 (1995) 33-38'
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 295(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_source ?
_diffrn_measurement_device_type 'Oxford Diffraction Gemini A Ultra'
_diffrn_measurement_method ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 8050
_diffrn_reflns_av_unetI/netI 0.0320
_diffrn_reflns_av_R_equivalents 0.0295
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 3.461
_diffrn_reflns_theta_max 25.046
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.977
_reflns_number_total 2777
_reflns_number_gt 2281
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_cell_refinement 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_reduction 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics
'Mercury (Macrae, J.Appl.Cryst. 41 (2008) 466-470'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_refine_special_details ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0421P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 2777
_refine_ls_number_parameters 208
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0417
_refine_ls_R_factor_gt 0.0299
_refine_ls_wR_factor_ref 0.0789
_refine_ls_wR_factor_gt 0.0743
_refine_ls_goodness_of_fit_ref 1.040
_refine_ls_restrained_S_all 1.040
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.19739(3) 0.08085(3) 0.04014(2) 0.03549(13) Uani 1 1 d . . . . .
N1 N 0.18168(18) -0.1192(2) 0.10653(12) 0.0365(5) Uani 1 1 d . . . . .
N2 N 0.24092(17) -0.2465(2) 0.09379(12) 0.0368(5) Uani 1 1 d . . . . .
N3 N 0.28297(17) -0.0768(2) 0.00184(12) 0.0338(5) Uani 1 1 d . . . . .
N4 N 0.28990(19) 0.1163(3) -0.09531(13) 0.0421(6) Uani 1 1 d . . . . .
N5 N 0.21147(18) 0.1929(3) -0.07119(13) 0.0424(5) Uani 1 1 d . . . . .
C1 C 0.1264(2) -0.1763(3) 0.15489(17) 0.0462(7) Uani 1 1 d . . . . .
H1 H 0.0788 -0.1158 0.1740 0.055 Uiso 1 1 calc R U . . .
C2 C 0.1488(3) -0.3393(4) 0.17340(19) 0.0549(8) Uani 1 1 d . . . . .
H2 H 0.1203 -0.4057 0.2062 0.066 Uiso 1 1 calc R U . . .
C3 C 0.2214(3) -0.3807(3) 0.13327(18) 0.0493(7) Uani 1 1 d . . . . .
H3 H 0.2519 -0.4819 0.1331 0.059 Uiso 1 1 calc R U . . .
C4 C 0.3012(2) -0.2222(3) 0.03800(15) 0.0375(6) Uani 1 1 d . . . . .
C5 C 0.3667(3) -0.3336(3) 0.01803(18) 0.0531(8) Uani 1 1 d . . . . .
H5 H 0.3801 -0.4345 0.0449 0.064 Uiso 1 1 calc R U . . .
C6 C 0.4117(3) -0.2888(4) -0.0438(2) 0.0635(9) Uani 1 1 d . . . . .
H6 H 0.4576 -0.3608 -0.0582 0.076 Uiso 1 1 calc R U . . .
C7 C 0.3908(3) -0.1402(4) -0.08493(18) 0.0548(8) Uani 1 1 d . . . . .
H7 H 0.4198 -0.1116 -0.1279 0.066 Uiso 1 1 calc R U . . .
C8 C 0.3252(2) -0.0366(3) -0.05953(15) 0.0391(6) Uani 1 1 d . . . . .
C9 C 0.3192(3) 0.2082(4) -0.15280(18) 0.0558(8) Uani 1 1 d . . . . .
H9 H 0.3711 0.1817 -0.1782 0.067 Uiso 1 1 calc R U . . .
C10 C 0.2593(3) 0.3441(4) -0.1659(2) 0.0651(9) Uani 1 1 d . . . . .
H10 H 0.2610 0.4302 -0.2023 0.078 Uiso 1 1 calc R U . . .
C11 C 0.1932(3) 0.3307(4) -0.11396(18) 0.0527(7) Uani 1 1 d . . . . .
H11 H 0.1434 0.4089 -0.1103 0.063 Uiso 1 1 calc R U . . .
C98 C 0.4145(2) 0.2918(3) 0.17406(15) 0.0353(6) Uani 1 1 d . . . . .
C99 C 0.0279(2) 0.2356(3) 0.09932(16) 0.0398(6) Uani 1 1 d . . . . .
N98 N 0.3423(2) 0.2087(3) 0.12985(14) 0.0488(6) Uani 1 1 d . . . . .
N99 N 0.0823(2) 0.2039(3) 0.05889(15) 0.0528(6) Uani 1 1 d . . . . .
S98 S 0.51352(6) 0.41546(8) 0.23624(5) 0.0488(2) Uani 1 1 d . . . . .
S99 S -0.04941(7) 0.27740(11) 0.15566(5) 0.0637(2) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0373(2) 0.0371(2) 0.03828(19) -0.00302(13) 0.02148(15) 0.00379(14)
N1 0.0380(12) 0.0389(12) 0.0388(11) -0.0032(9) 0.0217(10) 0.0004(10)
N2 0.0415(13) 0.0366(12) 0.0375(11) 0.0014(9) 0.0211(9) 0.0034(10)
N3 0.0372(12) 0.0371(12) 0.0319(10) -0.0032(9) 0.0188(9) 0.0027(10)
N4 0.0498(14) 0.0480(14) 0.0373(11) 0.0030(10) 0.0265(10) 0.0059(11)
N5 0.0470(14) 0.0422(14) 0.0434(12) 0.0022(10) 0.0237(10) 0.0080(11)
C1 0.0475(17) 0.0520(19) 0.0495(15) -0.0002(13) 0.0303(13) 0.0009(14)
C2 0.061(2) 0.058(2) 0.0573(17) 0.0111(15) 0.0349(15) -0.0016(16)
C3 0.0569(19) 0.0402(17) 0.0531(16) 0.0083(13) 0.0240(14) 0.0046(14)
C4 0.0394(15) 0.0424(16) 0.0329(12) -0.0025(11) 0.0166(11) 0.0064(12)
C5 0.067(2) 0.0487(18) 0.0553(16) 0.0093(14) 0.0362(15) 0.0243(16)
C6 0.076(2) 0.065(2) 0.0688(19) 0.0099(16) 0.0494(17) 0.0325(18)
C7 0.064(2) 0.065(2) 0.0516(16) 0.0059(15) 0.0410(15) 0.0188(17)
C8 0.0425(16) 0.0467(16) 0.0345(12) -0.0026(12) 0.0220(11) 0.0025(13)
C9 0.062(2) 0.068(2) 0.0493(16) 0.0111(15) 0.0336(14) 0.0006(17)
C10 0.077(2) 0.061(2) 0.0616(19) 0.0223(16) 0.0324(17) 0.0022(19)
C11 0.058(2) 0.0463(18) 0.0534(16) 0.0123(14) 0.0212(14) 0.0116(15)
C98 0.0421(16) 0.0360(14) 0.0343(12) 0.0030(11) 0.0220(11) 0.0101(13)
C99 0.0375(15) 0.0357(15) 0.0434(14) 0.0002(11) 0.0127(12) 0.0046(12)
N98 0.0483(15) 0.0457(14) 0.0489(13) -0.0088(11) 0.0153(11) -0.0005(12)
N99 0.0501(15) 0.0573(16) 0.0594(14) 0.0003(12) 0.0304(12) 0.0170(12)
S98 0.0497(5) 0.0514(5) 0.0467(4) -0.0082(3) 0.0202(3) -0.0131(3)
S99 0.0571(5) 0.0819(6) 0.0677(5) -0.0009(4) 0.0411(4) 0.0117(4)
_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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N99 1.911(2) . ?
Cu1 N3 1.9562(19) . ?
Cu1 N1 2.029(2) . ?
Cu1 N5 2.080(2) . ?
Cu1 N98 2.134(2) . ?
N1 C1 1.324(3) . ?
N1 N2 1.365(3) . ?
N2 C3 1.355(3) . ?
N2 C4 1.403(3) . ?
N3 C4 1.324(3) . ?
N3 C8 1.335(3) . ?
N4 C9 1.357(3) . ?
N4 N5 1.366(3) . ?
N4 C8 1.399(3) . ?
N5 C11 1.311(3) . ?
C1 C2 1.397(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.363(4) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.370(3) . ?
C5 C6 1.377(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.379(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.372(4) . ?
C7 H7 0.9300 . ?
C9 C10 1.338(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.402(4) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C98 N98 1.150(3) . ?
C98 S98 1.634(3) . ?
C99 N99 1.151(3) . ?
C99 S99 1.614(3) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N99 Cu1 N3 165.78(10) . . ?
N99 Cu1 N1 96.87(9) . . ?
N3 Cu1 N1 78.06(8) . . ?
N99 Cu1 N5 102.87(9) . . ?
N3 Cu1 N5 77.74(8) . . ?
N1 Cu1 N5 151.24(8) . . ?
N99 Cu1 N98 98.40(10) . . ?
N3 Cu1 N98 95.80(9) . . ?
N1 Cu1 N98 107.25(8) . . ?
N5 Cu1 N98 90.47(9) . . ?
C1 N1 N2 105.2(2) . . ?
C1 N1 Cu1 141.84(19) . . ?
N2 N1 Cu1 112.78(14) . . ?
C3 N2 N1 111.0(2) . . ?
C3 N2 C4 131.5(2) . . ?
N1 N2 C4 117.20(19) . . ?
C4 N3 C8 119.9(2) . . ?
C4 N3 Cu1 120.19(15) . . ?
C8 N3 Cu1 119.88(17) . . ?
C9 N4 N5 110.8(2) . . ?
C9 N4 C8 131.4(2) . . ?
N5 N4 C8 117.78(19) . . ?
C11 N5 N4 105.2(2) . . ?
C11 N5 Cu1 141.55(18) . . ?
N4 N5 Cu1 110.54(15) . . ?
N1 C1 C2 111.2(2) . . ?
N1 C1 H1 124.4 . . ?
C2 C1 H1 124.4 . . ?
C3 C2 C1 105.5(2) . . ?
C3 C2 H2 127.2 . . ?
C1 C2 H2 127.2 . . ?
N2 C3 C2 107.1(2) . . ?
N2 C3 H3 126.5 . . ?
C2 C3 H3 126.5 . . ?
N3 C4 C5 122.5(2) . . ?
N3 C4 N2 111.3(2) . . ?
C5 C4 N2 126.0(2) . . ?
C4 C5 C6 116.7(3) . . ?
C4 C5 H5 121.7 . . ?
C6 C5 H5 121.7 . . ?
C5 C6 C7 122.0(3) . . ?
C5 C6 H6 119.0 . . ?
C7 C6 H6 119.0 . . ?
C8 C7 C6 116.8(2) . . ?
C8 C7 H7 121.6 . . ?
C6 C7 H7 121.6 . . ?
N3 C8 C7 122.0(2) . . ?
N3 C8 N4 111.8(2) . . ?
C7 C8 N4 126.2(2) . . ?
C10 C9 N4 106.9(3) . . ?
C10 C9 H9 126.5 . . ?
N4 C9 H9 126.5 . . ?
C9 C10 C11 106.3(3) . . ?
C9 C10 H10 126.9 . . ?
C11 C10 H10 126.9 . . ?
N5 C11 C10 110.7(3) . . ?
N5 C11 H11 124.6 . . ?
C10 C11 H11 124.6 . . ?
N98 C98 S98 177.8(2) . . ?
N99 C99 S99 179.2(3) . . ?
C98 N98 Cu1 172.9(2) . . ?
C99 N99 Cu1 152.0(2) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C9 H9 S98 0.93 2.79 3.720(3) 175.3 4_565
C11 H11 S99 0.93 2.85 3.681(3) 149.2 3_565
_refine_diff_density_max 0.329
_refine_diff_density_min -0.300
_refine_diff_density_rms 0.053
_shelxl_version_number 2014/6
_shelx_res_file
;
TITL Cu115a in P21/c #14
CELL 0.71073 12.7902 8.3391 15.9931 90 113.001 90
ZERR 4 0.0007 0.0003 0.0007 0 0.006 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC H N S Cu C
UNIT 36 28 8 4 52
L.S. 10
BOND $H
ACTA
OMIT 0 50.1
EQIV $1 x,1/2-y,-1/2+z
EQIV $2 -x,1-y,-z
HTAB C9 S98_$1
HTAB C11 S99_$2
WGHT 0.042100
FVAR 3.57707
CU1 4 0.197389 0.080845 0.040136 11.00000 0.03728 0.03709 =
0.03828 -0.00302 0.02148 0.00379
N1 2 0.181679 -0.119202 0.106530 11.00000 0.03801 0.03889 =
0.03879 -0.00323 0.02172 0.00041
N2 2 0.240923 -0.246550 0.093790 11.00000 0.04147 0.03662 =
0.03745 0.00136 0.02113 0.00342
N3 2 0.282972 -0.076850 0.001835 11.00000 0.03722 0.03707 =
0.03191 -0.00323 0.01879 0.00271
N4 2 0.289904 0.116323 -0.095312 11.00000 0.04977 0.04803 =
0.03733 0.00299 0.02653 0.00594
N5 2 0.211471 0.192857 -0.071187 11.00000 0.04700 0.04221 =
0.04344 0.00223 0.02368 0.00803
C1 5 0.126387 -0.176349 0.154886 11.00000 0.04753 0.05200 =
0.04955 -0.00024 0.03034 0.00095
AFIX 43
H1 1 0.078778 -0.115844 0.174035 11.00000 -1.20000
AFIX 0
C2 5 0.148850 -0.339298 0.173401 11.00000 0.06063 0.05782 =
0.05727 0.01106 0.03493 -0.00157
AFIX 43
H2 1 0.120286 -0.405656 0.206214 11.00000 -1.20000
AFIX 0
C3 5 0.221444 -0.380676 0.133274 11.00000 0.05694 0.04024 =
0.05311 0.00831 0.02398 0.00460
AFIX 43
H3 1 0.251854 -0.481899 0.133051 11.00000 -1.20000
AFIX 0
C4 5 0.301153 -0.222204 0.038002 11.00000 0.03941 0.04245 =
0.03291 -0.00249 0.01660 0.00636
C5 5 0.366674 -0.333595 0.018033 11.00000 0.06655 0.04870 =
0.05533 0.00935 0.03621 0.02426
AFIX 43
H5 1 0.380055 -0.434517 0.044914 11.00000 -1.20000
AFIX 0
C6 5 0.411732 -0.288762 -0.043793 11.00000 0.07640 0.06464 =
0.06884 0.00992 0.04942 0.03254
AFIX 43
H6 1 0.457631 -0.360796 -0.058244 11.00000 -1.20000
AFIX 0
C7 5 0.390833 -0.140217 -0.084934 11.00000 0.06436 0.06548 =
0.05160 0.00594 0.04100 0.01876
AFIX 43
H7 1 0.419830 -0.111623 -0.127867 11.00000 -1.20000
AFIX 0
C8 5 0.325240 -0.036624 -0.059527 11.00000 0.04251 0.04673 =
0.03454 -0.00256 0.02201 0.00248
C9 5 0.319214 0.208184 -0.152795 11.00000 0.06155 0.06751 =
0.04928 0.01112 0.03365 0.00061
AFIX 43
H9 1 0.371093 0.181727 -0.178208 11.00000 -1.20000
AFIX 0
C10 5 0.259254 0.344064 -0.165941 11.00000 0.07735 0.06113 =
0.06155 0.02232 0.03238 0.00222
AFIX 43
H10 1 0.261022 0.430186 -0.202311 11.00000 -1.20000
AFIX 0
C11 5 0.193242 0.330714 -0.113960 11.00000 0.05777 0.04630 =
0.05343 0.01226 0.02122 0.01165
AFIX 43
H11 1 0.143355 0.408915 -0.110310 11.00000 -1.20000
AFIX 0
C98 5 0.414537 0.291788 0.174064 11.00000 0.04210 0.03604 =
0.03434 0.00299 0.02200 0.01011
C99 5 0.027854 0.235568 0.099319 11.00000 0.03745 0.03573 =
0.04339 0.00022 0.01267 0.00457
N98 2 0.342337 0.208691 0.129851 11.00000 0.04834 0.04568 =
0.04893 -0.00879 0.01529 -0.00049
N99 2 0.082349 0.203907 0.058890 11.00000 0.05006 0.05727 =
0.05940 0.00032 0.03035 0.01699
S98 3 0.513522 0.415456 0.236239 11.00000 0.04965 0.05144 =
0.04670 -0.00822 0.02018 -0.01306
S99 3 -0.049412 0.277397 0.155660 11.00000 0.05706 0.08189 =
0.06774 -0.00090 0.04113 0.01172
HKLF 4
REM Cu115a in P21/c #14
REM R1 = 0.0299 for 2281 Fo > 4sig(Fo) and 0.0417 for all 2777 data
REM 208 parameters refined using 0 restraints
END
WGHT 0.0421 0.0000
REM Highest difference peak 0.329, deepest hole -0.300, 1-sigma level 0.053
Q1 1 0.0140 0.3214 0.1960 11.00000 0.05 0.33
Q2 1 0.2548 -0.2374 0.0534 11.00000 0.05 0.26
Q3 1 0.1187 -0.2629 0.1450 11.00000 0.05 0.25
Q4 1 0.2025 0.1613 -0.0310 11.00000 0.05 0.24
Q5 1 0.1645 -0.0585 0.0561 11.00000 0.05 0.23
Q6 1 -0.0748 0.3173 0.1081 11.00000 0.05 0.23
Q7 1 0.2972 -0.0586 -0.0250 11.00000 0.05 0.22
Q8 1 -0.0382 0.1885 0.1503 11.00000 0.05 0.21
Q9 1 0.1637 -0.3576 0.1258 11.00000 0.05 0.21
Q10 1 0.1989 -0.1775 0.0924 11.00000 0.05 0.21
Q11 1 0.2013 -0.5584 0.0345 11.00000 0.05 0.21
Q12 1 0.1280 -0.1626 0.0996 11.00000 0.05 0.20
Q13 1 0.2773 -0.1575 0.0126 11.00000 0.05 0.20
Q14 1 0.1796 -0.1360 0.1421 11.00000 0.05 0.20
Q15 1 0.2801 0.0322 -0.1051 11.00000 0.05 0.19
Q16 1 0.2618 -0.2918 0.1285 11.00000 0.05 0.19
Q17 1 0.3048 -0.2814 0.0132 11.00000 0.05 0.18
Q18 1 0.3791 0.1859 0.1657 11.00000 0.05 0.18
Q19 1 0.2882 0.1419 -0.1358 11.00000 0.05 0.18
Q20 1 0.3333 -0.0854 -0.0925 11.00000 0.05 0.18
;
_shelx_res_checksum 3928