data_c2
_audit_creation_date 2011-05-15
_audit_creation_method
;
Olex2 1.1
(compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C40 H35 Cu N8 O5 S4'
_chemical_formula_sum 'C40 H35 Cu N8 O5 S4'
_chemical_formula_weight 899.32
_chemical_absolute_configuration unk
_chemical_melting_point ?
_chemical_oxdiff_formula 'c20 h18 n4 s2 o4 cu1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cu' 'Cu' -1.9646 0.5888
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system 'monoclinic'
_space_group_IT_number 9
_space_group_name_H-M_alt 'C 1 c 1'
_space_group_name_Hall 'C -2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 'x, -y, z+1/2'
3 'x+1/2, y+1/2, z'
4 'x+1/2, -y+1/2, z+1/2'
_cell_length_a 15.0977(3)
_cell_length_b 21.7903(4)
_cell_length_c 13.1399(2)
_cell_angle_alpha 90.00
_cell_angle_beta 103.3750(17)
_cell_angle_gamma 90.00
_cell_volume 4205.57(12)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 5248
_cell_measurement_temperature 150.0
_cell_measurement_theta_max 74.6098
_cell_measurement_theta_min 3.4545
_exptl_absorpt_coefficient_mu 3.049
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.76076
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.10 (release 06-04-2011 CrysAlis171 .NET)
(compiled Apr 6 2011,09:17:13)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour green
_exptl_crystal_density_diffrn 1.468
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description ''
_exptl_crystal_F_000 1928
_exptl_crystal_size_max 0.371
_exptl_crystal_size_mid 0.1481
_exptl_crystal_size_min 0.076
_exptl_special_details
;
?
;
_diffrn_reflns_av_R_equivalents 0.0312
_diffrn_reflns_av_unetI/netI 0.0448
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 8243
_diffrn_reflns_theta_full 67.68
_diffrn_reflns_theta_max 74.78
_diffrn_reflns_theta_min 3.46
_diffrn_ambient_temperature 150.0
_diffrn_detector_area_resol_mean 5.1734
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -25.00 26.00 1.0000 2.4200
omega____ theta____ kappa____ phi______frames
- -38.5000 38.0000 -60.0000 51
#__ type_ start__ end____ width___ exp.time_
2 omega -49.00 -17.00 1.0000 2.4200
omega____ theta____ kappa____ phi______frames
- -38.5000 38.0000 -90.0000 32
#__ type_ start__ end____ width___ exp.time_
3 omega -110.00 -28.00 1.0000 2.4200
omega____ theta____ kappa____ phi______frames
- -38.5000 -38.0000 120.0000 82
#__ type_ start__ end____ width___ exp.time_
4 omega 30.00 85.00 1.0000 2.4200
omega____ theta____ kappa____ phi______frames
- 43.7028 -125.0000 0.0000 55
#__ type_ start__ end____ width___ exp.time_
5 omega 78.00 172.00 1.0000 2.4200
omega____ theta____ kappa____ phi______frames
- 106.4053 77.0000 -30.0000 94
#__ type_ start__ end____ width___ exp.time_
6 omega 37.00 92.00 1.0000 2.4200
omega____ theta____ kappa____ phi______frames
- 106.4053 -45.0000 30.0000 55
#__ type_ start__ end____ width___ exp.time_
7 omega 62.00 87.00 1.0000 2.4200
omega____ theta____ kappa____ phi______frames
- 106.4053 -45.0000 60.0000 25
#__ type_ start__ end____ width___ exp.time_
8 omega 35.00 133.00 1.0000 2.4200
omega____ theta____ kappa____ phi______frames
- 106.4053 -77.0000 -150.0000 98
#__ type_ start__ end____ width___ exp.time_
9 omega 86.00 167.00 1.0000 2.4200
omega____ theta____ kappa____ phi______frames
- 106.4053 45.0000 -60.0000 81
#__ type_ start__ end____ width___ exp.time_
10 omega 69.00 94.00 1.0000 2.4200
omega____ theta____ kappa____ phi______frames
- 106.4053 -45.0000 -180.0000 25
;
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 -0.0120145000
_diffrn_orient_matrix_UB_12 -0.0036034000
_diffrn_orient_matrix_UB_13 0.1131185000
_diffrn_orient_matrix_UB_21 -0.0242503000
_diffrn_orient_matrix_UB_22 -0.0685837000
_diffrn_orient_matrix_UB_23 -0.0154473000
_diffrn_orient_matrix_UB_31 0.1013051000
_diffrn_orient_matrix_UB_32 -0.0168339000
_diffrn_orient_matrix_UB_33 0.0387025000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.5418
_diffrn_source 'SuperNova (Cu) X-ray Source'
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_reflns_number_gt 4908
_reflns_number_total 5127
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.49
_reflns_threshold_expression >2sigma(I)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.10 (release 06-04-2011 CrysAlis171 .NET)
(compiled Apr 6 2011,09:17:13)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.10 (release 06-04-2011 CrysAlis171 .NET)
(compiled Apr 6 2011,09:17:13)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.10 (release 06-04-2011 CrysAlis171 .NET)
(compiled Apr 6 2011,09:17:13)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)'
_refine_diff_density_max 0.482
_refine_diff_density_min -0.377
_refine_diff_density_rms 0.058
_refine_ls_abs_structure_details 'Flack H D (1983), ActaCryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.0(8)
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.019
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 552
_refine_ls_number_reflns 5127
_refine_ls_number_restraints 6
_refine_ls_R_factor_all 0.0360
_refine_ls_R_factor_gt 0.0339
_refine_ls_restrained_S_all 1.019
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+2.1551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0846
_refine_ls_wR_factor_ref 0.0868
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
> The Following Model ALERTS were generated - (Acta-Mode) <
#======
Format: alert-number_ALERT_alert-type_alert-level text
915_ALERT_3_B Low Friedel Pair Coverage ...... 22 Perc.
032_ALERT_4_G Std. Uncertainty on Flack Parameter Value High . 0.80
850_ALERT_4_G Check Flack Parameter Exact Value 0.00 and su .. 0.80
Absolute structure was of no interest for this sample
927_ALERT_1_B Reported and Calculated wR2 * 100.0 Differ by . -1.01
420_ALERT_2_C D-H Without Acceptor N10 - H10 ... ?
732_ALERT_1_C Angle Calc 108(6), Rep 108(2) ...... 3.00 su-Ra
HA -O -HB 1.555 1.555 1.555 # ` 160
911_ALERT_3_C Missing # FCF Refl Between THminSTh/L= 0.600 7
912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 132
926_ALERT_1_C Reported and Calculated R1 * 100.0 Differ by . -0.34
928_ALERT_1_C Reported and Calculated S value Differ by . -0.12
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite 4
069_ALERT_1_G Atom Label without Numerical Part ...... N
069_ALERT_1_G Atom Label without Numerical Part ...... C
069_ALERT_1_G Atom Label without Numerical Part ...... O
720_ALERT_4_G Number of Unusual/Non-Standard Labels ...... 38
760_ALERT_1_G CIF Contains no Torsion Angles ...... ?
794_ALERT_5_G Note: Tentative Bond Valency for Cu1 (II) 2.12
795_ALERT_4_G C-Atom in CIF Coordinate List out of Sequence .. C
796_ALERT_4_G O-Atom in CIF Coordinate List out of Sequence .. O
797_ALERT_4_G N-Atom in CIF Coordinate List out of Sequence .. N
860_ALERT_3_G Note: Number of Least-Squares Restraints ...... 6
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.28894(4) 0.01846(2) 0.04215(4) 0.02339(13) Uani 1 1 d . . .
S2 S 0.05160(6) -0.10641(4) 0.05125(7) 0.02606(19) Uani 1 1 d . . .
S3 S 0.52740(6) 0.13816(4) 0.00693(7) 0.02437(18) Uani 1 1 d . . .
S4 S 0.43959(6) 0.21173(4) 0.17209(7) 0.02456(18) Uani 1 1 d . . .
S5 S 0.13824(6) -0.16036(4) -0.13549(7) 0.02645(19) Uani 1 1 d . . .
N1 N 0.2130(2) 0.09052(15) -0.0257(2) 0.0281(7) Uani 1 1 d . . .
N2 N 0.3592(2) -0.06094(15) 0.0746(3) 0.0295(7) Uani 1 1 d . . .
C3 C 0.1422(2) -0.07711(17) 0.0021(3) 0.0230(7) Uani 1 1 d . . .
N4 N 0.4011(2) 0.06255(14) 0.0199(2) 0.0247(6) Uani 1 1 d . . .
O5 O 0.52980(18) 0.22505(13) 0.1575(2) 0.0289(6) Uani 1 1 d . . .
N6 N 0.1769(2) -0.02734(14) 0.0549(2) 0.0250(7) Uani 1 1 d . . .
N7 N 0.1343(2) -0.00921(14) 0.1322(2) 0.0261(7) Uani 1 1 d . . .
O8 O 0.42464(19) 0.22129(13) 0.2747(2) 0.0321(6) Uani 1 1 d . . .
N9 N 0.4402(2) 0.03940(15) -0.0573(2) 0.0267(7) Uani 1 1 d . . .
N10 N 0.1744(2) -0.09813(14) -0.0772(2) 0.0263(7) Uani 1 1 d . . .
H10 H 0.2168 -0.0771 -0.0980 0.032 Uiso 1 1 calc R . .
N N 0.4085(2) 0.14309(15) 0.1388(2) 0.0263(7) Uani 1 1 d D . .
C12 C 0.4375(2) 0.11501(17) 0.0621(3) 0.0226(7) Uani 1 1 d . . .
C15 C 0.5067(3) 0.07337(16) -0.0725(3) 0.0240(7) Uani 1 1 d . . .
O16 O 0.1591(2) -0.15835(13) -0.2366(2) 0.0373(7) Uani 1 1 d . . .
O17 O 0.04485(19) -0.17325(13) -0.1325(2) 0.0334(6) Uani 1 1 d . . .
C C 0.0102(3) -0.03666(17) 0.2146(3) 0.0244(7) Uani 1 1 d . . .
C23 C 0.5595(2) 0.06048(17) -0.1507(3) 0.0240(7) Uani 1 1 d . . .
O O 0.3096(2) 0.05298(13) 0.2127(2) 0.0346(6) Uani 1 1 d D . .
C26 C 0.0686(2) -0.04653(17) 0.1400(3) 0.0243(7) Uani 1 1 d . . .
C32 C 0.1557(3) 0.1197(2) 0.0206(4) 0.0361(10) Uani 1 1 d . . .
H32 H 0.1479 0.1049 0.0859 0.043 Uiso 1 1 calc R . .
C33 C -0.0895(3) -0.07500(19) 0.3188(3) 0.0336(9) Uani 1 1 d . . .
H33 H -0.1201 -0.1085 0.3420 0.040 Uiso 1 1 calc R . .
C36 C -0.0370(3) -0.08507(18) 0.2464(3) 0.0310(9) Uani 1 1 d . . .
H36 H -0.0333 -0.1250 0.2186 0.037 Uiso 1 1 calc R . .
C41 C 0.3621(4) -0.0877(2) 0.1668(4) 0.0439(11) Uani 1 1 d . . .
H41 H 0.3355 -0.0672 0.2160 0.053 Uiso 1 1 calc R . .
C44 C 0.3978(3) -0.0892(2) 0.0061(4) 0.0404(10) Uani 1 1 d . . .
H44 H 0.3956 -0.0702 -0.0594 0.048 Uiso 1 1 calc R . .
C52 C 0.1071(3) 0.1709(2) -0.0226(5) 0.0529(13) Uani 1 1 d . . .
H52 H 0.0672 0.1908 0.0132 0.063 Uiso 1 1 calc R . .
C0AA C 0.2052(3) -0.21896(17) -0.0636(3) 0.0243(7) Uani 1 1 d . . .
C1AA C 0.0012(3) 0.02210(17) 0.2523(3) 0.0263(8) Uani 1 1 d . . .
H1A H 0.0324 0.0555 0.2300 0.032 Uiso 1 1 calc R . .
C3AA C 0.2815(3) -0.24006(18) -0.0951(3) 0.0287(8) Uani 1 1 d . . .
H3A H 0.2959 -0.2242 -0.1567 0.034 Uiso 1 1 calc R . .
C4 C 0.1842(3) -0.24285(18) 0.0262(3) 0.0271(8) Uani 1 1 d . . .
H4 H 0.1315 -0.2291 0.0475 0.033 Uiso 1 1 calc R . .
C1CA C 0.5420(3) 0.00775(18) -0.2113(3) 0.0307(9) Uani 1 1 d . . .
H1C H 0.4969 -0.0204 -0.2010 0.037 Uiso 1 1 calc R . .
C8 C -0.0978(3) -0.01645(19) 0.3577(3) 0.0301(8) Uani 1 1 d . . .
C2CA C 0.2222(3) 0.1123(2) -0.1178(3) 0.0418(11) Uani 1 1 d . . .
H2C H 0.2630 0.0922 -0.1522 0.050 Uiso 1 1 calc R . .
C4AA C 0.6710(3) 0.09052(19) -0.2461(3) 0.0323(9) Uani 1 1 d . . .
H4A H 0.7142 0.1196 -0.2584 0.039 Uiso 1 1 calc R . .
C5AA C 0.2404(3) -0.28673(19) 0.0845(3) 0.0338(9) Uani 1 1 d . . .
H5A H 0.2263 -0.3027 0.1462 0.041 Uiso 1 1 calc R . .
C6AA C 0.3366(3) -0.28441(19) -0.0362(4) 0.0345(9) Uani 1 1 d . . .
H6A H 0.3885 -0.2989 -0.0583 0.041 Uiso 1 1 calc R . .
C7AA C 0.6244(3) 0.10168(17) -0.1690(3) 0.0284(8) Uani 1 1 d . . .
H7A H 0.6368 0.1379 -0.1281 0.034 Uiso 1 1 calc R . .
C5 C 0.6553(3) 0.0371(2) -0.3059(3) 0.0309(8) Uani 1 1 d . . .
C8AA C -0.0531(3) 0.03198(18) 0.3221(3) 0.0288(8) Uani 1 1 d . . .
H8A H -0.0600 0.0724 0.3462 0.035 Uiso 1 1 calc R . .
C9 C 0.5905(3) -0.0037(2) -0.2866(3) 0.0324(9) Uani 1 1 d . . .
H9 H 0.5791 -0.0405 -0.3262 0.039 Uiso 1 1 calc R . .
C10 C 0.3176(3) -0.30781(18) 0.0535(3) 0.0335(9) Uani 1 1 d . . .
C2AA C 0.3628(3) 0.25904(17) 0.0845(3) 0.0281(8) Uani 1 1 d . . .
C9AA C 0.3845(3) 0.27843(18) -0.0073(3) 0.0344(9) Uani 1 1 d . . .
H9A H 0.4416 0.2679 -0.0214 0.041 Uiso 1 1 calc R . .
C8BA C -0.1551(3) -0.0049(2) 0.4361(4) 0.0439(11) Uani 1 1 d . . .
H8BA H -0.2080 -0.0323 0.4214 0.066 Uiso 1 1 calc R . .
H8BB H -0.1758 0.0379 0.4307 0.066 Uiso 1 1 calc R . .
H8BC H -0.1186 -0.0127 0.5068 0.066 Uiso 1 1 calc R . .
C9BA C 0.7079(3) 0.0232(2) -0.3883(4) 0.0442(11) Uani 1 1 d . . .
H9BA H 0.7295 0.0616 -0.4129 0.066 Uiso 1 1 calc R . .
H9BB H 0.6681 0.0019 -0.4473 0.066 Uiso 1 1 calc R . .
H9BC H 0.7601 -0.0030 -0.3582 0.066 Uiso 1 1 calc R . .
C6 C 0.2387(3) 0.3297(2) -0.0591(4) 0.0452(12) Uani 1 1 d . . .
C7 C 0.2190(3) 0.3104(2) 0.0328(4) 0.0445(11) Uani 1 1 d . . .
H7 H 0.1625 0.3218 0.0473 0.053 Uiso 1 1 calc R . .
C3BA C 0.4413(3) -0.1459(2) 0.0273(5) 0.0562(15) Uani 1 1 d . . .
H3B H 0.4684 -0.1654 -0.0226 0.067 Uiso 1 1 calc R . .
C1BA C 0.1743(4) 0.1634(3) -0.1653(4) 0.0567(15) Uani 1 1 d . . .
H1B H 0.1820 0.1775 -0.2311 0.068 Uiso 1 1 calc R . .
C0BA C 0.2794(3) 0.2747(2) 0.1053(4) 0.0372(10) Uani 1 1 d . . .
H0B H 0.2640 0.2613 0.1678 0.045 Uiso 1 1 calc R . .
C2BA C 0.4028(4) -0.1446(2) 0.1932(4) 0.0581(15) Uani 1 1 d . . .
H2B H 0.4021 -0.1634 0.2582 0.070 Uiso 1 1 calc R . .
C4BA C 0.3224(3) 0.3133(2) -0.0783(4) 0.0413(10) Uani 1 1 d . . .
H4B H 0.3373 0.3262 -0.1413 0.050 Uiso 1 1 calc R . .
C5BA C 0.1166(4) 0.1926(2) -0.1164(5) 0.0605(16) Uani 1 1 d . . .
H5B H 0.0834 0.2276 -0.1472 0.073 Uiso 1 1 calc R . .
C6BA C 0.4436(4) -0.1726(2) 0.1231(5) 0.0666(18) Uani 1 1 d . . .
H6B H 0.4739 -0.2107 0.1405 0.080 Uiso 1 1 calc R . .
HA H 0.331(4) 0.0896(12) 0.207(5) 0.093 Uiso 1 1 d D . .
HB H 0.2532(16) 0.057(3) 0.217(6) 0.093 Uiso 1 1 d 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 0.0234(3) 0.0218(2) 0.0281(3) -0.0016(2) 0.0125(2) -0.0045(2)
S2 0.0241(4) 0.0258(4) 0.0309(4) -0.0056(4) 0.0117(3) -0.0063(3)
S3 0.0250(4) 0.0229(4) 0.0293(4) -0.0036(3) 0.0146(4) -0.0053(3)
S4 0.0251(4) 0.0257(4) 0.0258(4) -0.0051(3) 0.0119(3) -0.0046(3)
S5 0.0268(5) 0.0298(5) 0.0236(4) -0.0022(4) 0.0074(3) 0.0017(4)
N1 0.0260(17) 0.0287(16) 0.0292(16) 0.0045(13) 0.0056(13) -0.0058(13)
N2 0.0236(17) 0.0236(16) 0.0390(18) -0.0020(14) 0.0028(14) -0.0081(13)
C3 0.0198(18) 0.0246(17) 0.0260(17) 0.0053(14) 0.0079(14) 0.0008(14)
N4 0.0215(16) 0.0257(16) 0.0292(15) -0.0026(13) 0.0103(12) -0.0052(12)
O5 0.0259(14) 0.0322(14) 0.0323(14) -0.0048(11) 0.0141(11) -0.0053(11)
N6 0.0269(16) 0.0235(15) 0.0287(16) -0.0027(13) 0.0150(13) -0.0041(13)
N7 0.0263(17) 0.0238(16) 0.0328(17) -0.0032(13) 0.0163(14) -0.0054(12)
O8 0.0332(16) 0.0394(16) 0.0282(14) -0.0056(12) 0.0165(12) -0.0043(12)
N9 0.0276(17) 0.0252(16) 0.0304(16) -0.0031(13) 0.0128(13) -0.0034(13)
N10 0.0250(17) 0.0278(16) 0.0288(16) -0.0008(13) 0.0114(13) -0.0034(13)
N 0.0255(17) 0.0269(16) 0.0311(16) 0.0002(13) 0.0157(13) -0.0033(13)
C12 0.0183(17) 0.0252(17) 0.0261(17) -0.0002(15) 0.0086(14) -0.0054(14)
C15 0.0263(19) 0.0208(17) 0.0262(17) -0.0013(14) 0.0091(15) -0.0012(14)
O16 0.0475(18) 0.0433(17) 0.0232(13) -0.0003(13) 0.0123(12) 0.0072(15)
O17 0.0230(14) 0.0367(15) 0.0383(15) -0.0084(13) 0.0024(12) -0.0023(12)
C 0.0218(18) 0.0253(17) 0.0268(18) 0.0041(15) 0.0068(15) 0.0006(14)
C23 0.0220(18) 0.0274(18) 0.0244(17) 0.0018(14) 0.0092(14) -0.0021(14)
O 0.0396(17) 0.0370(15) 0.0280(13) -0.0017(12) 0.0090(12) -0.0100(13)
C26 0.0224(18) 0.0255(18) 0.0258(17) 0.0004(15) 0.0074(14) -0.0011(14)
C32 0.028(2) 0.031(2) 0.049(3) -0.0020(19) 0.0095(19) 0.0008(17)
C33 0.029(2) 0.036(2) 0.041(2) 0.0109(19) 0.0181(18) 0.0036(17)
C36 0.030(2) 0.0266(19) 0.040(2) 0.0038(16) 0.0154(18) -0.0032(16)
C41 0.058(3) 0.032(2) 0.038(2) 0.0011(19) 0.002(2) -0.013(2)
C44 0.032(2) 0.033(2) 0.061(3) -0.005(2) 0.021(2) -0.0072(18)
C52 0.040(3) 0.031(2) 0.082(4) 0.002(3) 0.002(2) 0.005(2)
C0AA 0.0220(19) 0.0262(18) 0.0259(17) -0.0030(15) 0.0079(14) -0.0035(14)
C1AA 0.0250(19) 0.029(2) 0.0268(18) 0.0032(15) 0.0086(15) -0.0047(15)
C3AA 0.032(2) 0.0307(19) 0.0268(18) -0.0058(15) 0.0132(16) -0.0031(16)
C4 0.0257(19) 0.0291(19) 0.0297(19) -0.0020(16) 0.0127(15) -0.0054(15)
C1CA 0.029(2) 0.029(2) 0.037(2) -0.0046(17) 0.0135(17) -0.0032(16)
C8 0.026(2) 0.040(2) 0.0267(19) 0.0051(16) 0.0105(15) -0.0003(17)
C2CA 0.045(3) 0.052(3) 0.026(2) 0.0041(19) 0.0048(19) -0.011(2)
C4AA 0.030(2) 0.034(2) 0.038(2) 0.0021(18) 0.0180(18) -0.0035(17)
C5AA 0.039(2) 0.029(2) 0.033(2) 0.0023(16) 0.0079(18) -0.0096(17)
C6AA 0.026(2) 0.034(2) 0.044(2) -0.0062(18) 0.0094(17) 0.0055(17)
C7AA 0.030(2) 0.0259(18) 0.0307(19) -0.0041(15) 0.0105(16) -0.0030(15)
C5 0.028(2) 0.039(2) 0.0272(18) -0.0017(17) 0.0098(16) 0.0037(17)
C8AA 0.029(2) 0.0284(19) 0.0297(19) -0.0008(16) 0.0089(16) 0.0040(16)
C9 0.038(2) 0.033(2) 0.027(2) -0.0089(17) 0.0080(17) 0.0036(17)
C10 0.032(2) 0.0239(19) 0.042(2) -0.0017(17) 0.0035(18) -0.0028(16)
C2AA 0.033(2) 0.0238(18) 0.0278(18) -0.0071(15) 0.0075(15) -0.0052(15)
C9AA 0.036(2) 0.028(2) 0.040(2) -0.0026(17) 0.0106(18) -0.0058(17)
C8BA 0.040(3) 0.056(3) 0.043(2) 0.001(2) 0.024(2) 0.002(2)
C9BA 0.048(3) 0.053(3) 0.038(2) -0.005(2) 0.023(2) 0.003(2)
C6 0.046(3) 0.028(2) 0.053(3) -0.005(2) -0.007(2) -0.0050(19)
C7 0.030(2) 0.050(3) 0.050(3) -0.011(2) 0.003(2) 0.005(2)
C3BA 0.032(3) 0.031(2) 0.103(5) -0.014(3) 0.010(3) -0.003(2)
C1BA 0.062(4) 0.059(3) 0.037(3) 0.020(2) -0.012(2) -0.022(3)
C0BA 0.030(2) 0.043(2) 0.040(2) -0.007(2) 0.0120(18) 0.0018(19)
C7BA 0.049(3) 0.034(2) 0.057(3) 0.001(2) -0.005(2) 0.006(2)
C2BA 0.082(4) 0.026(2) 0.050(3) 0.003(2) -0.017(3) -0.007(2)
C4BA 0.050(3) 0.033(2) 0.037(2) 0.0009(18) 0.003(2) -0.008(2)
C5BA 0.047(3) 0.039(3) 0.078(4) 0.014(3) -0.020(3) -0.003(2)
C6BA 0.051(3) 0.030(3) 0.096(5) -0.004(3) -0.030(3) 0.004(2)
C0CA 0.065(4) 0.045(3) 0.061(3) 0.005(3) -0.015(3) 0.001(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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 2.025(3) . ?
Cu1 N2 2.023(3) . ?
Cu1 N4 2.026(3) . ?
Cu1 N6 2.004(3) . ?
Cu1 O 2.316(3) . ?
S2 C3 1.762(4) . ?
S2 C26 1.729(4) . ?
S3 C12 1.754(4) . ?
S3 C15 1.740(4) . ?
S4 O5 1.448(3) . ?
S4 O8 1.433(3) . ?
S4 N 1.598(3) . ?
S4 C2AA 1.765(4) . ?
S5 N10 1.591(3) . ?
S5 O16 1.436(3) . ?
S5 O17 1.447(3) . ?
S5 C0AA 1.762(4) . ?
N1 C32 1.330(5) . ?
N1 C2CA 1.336(5) . ?
N2 C41 1.336(6) . ?
N2 C44 1.331(5) . ?
C3 N6 1.328(5) . ?
C3 N10 1.330(5) . ?
N4 N9 1.383(4) . ?
N4 C12 1.332(5) . ?
N6 N7 1.379(4) . ?
N7 C26 1.305(5) . ?
N9 C15 1.299(5) . ?
N10 H10 0.8800 . ?
N C12 1.336(5) . ?
C15 C23 1.465(5) . ?
C C26 1.477(5) . ?
C C36 1.391(5) . ?
C C1AA 1.391(5) . ?
C23 C1CA 1.388(5) . ?
C23 C7AA 1.391(5) . ?
O HA 0.869(10) . ?
O HB 0.871(10) . ?
C32 H32 0.9500 . ?
C32 C52 1.383(6) . ?
C33 H33 0.9500 . ?
C33 C36 1.390(6) . ?
C33 C8 1.391(6) . ?
C36 H36 0.9500 . ?
C41 H41 0.9500 . ?
C41 C2BA 1.390(7) . ?
C44 H44 0.9500 . ?
C44 C3BA 1.396(6) . ?
C52 H52 0.9500 . ?
C52 C5BA 1.358(8) . ?
C0AA C3AA 1.390(5) . ?
C0AA C4 1.392(5) . ?
C1AA H1A 0.9500 . ?
C1AA C8AA 1.381(5) . ?
C3AA H3A 0.9500 . ?
C3AA C6AA 1.388(6) . ?
C4 H4 0.9500 . ?
C4 C5AA 1.386(6) . ?
C1CA H1C 0.9500 . ?
C1CA C9 1.383(5) . ?
C8 C8AA 1.391(5) . ?
C8 C8BA 1.510(6) . ?
C2CA H2C 0.9500 . ?
C2CA C1BA 1.393(7) . ?
C4AA H4A 0.9500 . ?
C4AA C7AA 1.382(5) . ?
C4AA C5 1.395(6) . ?
C5AA H5A 0.9500 . ?
C5AA C10 1.398(6) . ?
C6AA H6A 0.9500 . ?
C6AA C10 1.374(6) . ?
C7AA H7A 0.9500 . ?
C5 C9 1.388(6) . ?
C5 C9BA 1.514(6) . ?
C8AA H8A 0.9500 . ?
C9 H9 0.9500 . ?
C10 C7BA 1.514(6) . ?
C2AA C9AA 1.386(6) . ?
C2AA C0BA 1.391(6) . ?
C9AA H9A 0.9500 . ?
C9AA C4BA 1.386(6) . ?
C8BA H8BA 0.9800 . ?
C8BA H8BB 0.9800 . ?
C8BA H8BC 0.9800 . ?
C9BA H9BA 0.9800 . ?
C9BA H9BB 0.9800 . ?
C9BA H9BC 0.9800 . ?
C6 C7 1.373(7) . ?
C6 C4BA 1.392(7) . ?
C6 C0CA 1.507(7) . ?
C7 H7 0.9500 . ?
C7 C0BA 1.394(6) . ?
C3BA H3B 0.9500 . ?
C3BA C6BA 1.380(9) . ?
C1BA H1B 0.9500 . ?
C1BA C5BA 1.355(9) . ?
C0BA H0B 0.9500 . ?
C7BA H7BA 0.9800 . ?
C7BA H7BB 0.9800 . ?
C7BA H7BC 0.9800 . ?
C2BA H2B 0.9500 . ?
C2BA C6BA 1.365(10) . ?
C4BA H4B 0.9500 . ?
C5BA H5B 0.9500 . ?
C6BA H6B 0.9500 . ?
C0CA H0CA 0.9800 . ?
C0CA H0CB 0.9800 . ?
C0CA H0CC 0.9800 . ?
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
N1 Cu1 N4 88.60(13) . . ?
N1 Cu1 O 96.33(12) . . ?
N2 Cu1 N1 166.35(14) . . ?
N2 Cu1 N4 91.20(13) . . ?
N2 Cu1 O 97.31(12) . . ?
N4 Cu1 O 93.19(12) . . ?
N6 Cu1 N1 91.16(13) . . ?
N6 Cu1 N2 88.17(13) . . ?
N6 Cu1 N4 176.36(13) . . ?
N6 Cu1 O 90.45(12) . . ?
C26 S2 C3 88.12(17) . . ?
C15 S3 C12 88.05(17) . . ?
O5 S4 N 112.16(16) . . ?
O5 S4 C2AA 106.99(18) . . ?
O8 S4 O5 116.95(17) . . ?
O8 S4 N 107.08(17) . . ?
O8 S4 C2AA 107.84(18) . . ?
N S4 C2AA 105.13(17) . . ?
N10 S5 C0AA 105.61(17) . . ?
O16 S5 N10 107.16(17) . . ?
O16 S5 O17 117.07(18) . . ?
O16 S5 C0AA 107.27(17) . . ?
O17 S5 N10 112.38(17) . . ?
O17 S5 C0AA 106.65(17) . . ?
C32 N1 Cu1 122.1(3) . . ?
C32 N1 C2CA 117.4(4) . . ?
C2CA N1 Cu1 120.5(3) . . ?
C41 N2 Cu1 118.1(3) . . ?
C44 N2 Cu1 123.0(3) . . ?
C44 N2 C41 118.8(4) . . ?
N6 C3 S2 110.5(3) . . ?
N6 C3 N10 121.3(3) . . ?
N10 C3 S2 128.2(3) . . ?
N9 N4 Cu1 116.5(2) . . ?
C12 N4 Cu1 128.7(2) . . ?
C12 N4 N9 114.4(3) . . ?
C3 N6 Cu1 127.0(2) . . ?
C3 N6 N7 115.1(3) . . ?
N7 N6 Cu1 117.7(2) . . ?
C26 N7 N6 111.8(3) . . ?
C15 N9 N4 112.4(3) . . ?
S5 N10 H10 119.2 . . ?
C3 N10 S5 121.6(3) . . ?
C3 N10 H10 119.2 . . ?
C12 N S4 120.5(3) . . ?
N4 C12 S3 111.1(3) . . ?
N4 C12 N 122.0(3) . . ?
N C12 S3 126.9(3) . . ?
N9 C15 S3 114.1(3) . . ?
N9 C15 C23 124.2(3) . . ?
C23 C15 S3 121.7(3) . . ?
C36 C C26 121.0(3) . . ?
C36 C C1AA 119.4(4) . . ?
C1AA C C26 119.6(3) . . ?
C1CA C23 C15 119.9(3) . . ?
C1CA C23 C7AA 118.9(3) . . ?
C7AA C23 C15 121.1(3) . . ?
Cu1 O HA 101(5) . . ?
Cu1 O HB 101(5) . . ?
HA O HB 108(2) . . ?
N7 C26 S2 114.4(3) . . ?
N7 C26 C 122.9(3) . . ?
C C26 S2 122.6(3) . . ?
N1 C32 H32 118.7 . . ?
N1 C32 C52 122.5(5) . . ?
C52 C32 H32 118.7 . . ?
C36 C33 H33 119.7 . . ?
C36 C33 C8 120.7(4) . . ?
C8 C33 H33 119.7 . . ?
C C36 H36 120.0 . . ?
C33 C36 C 120.0(4) . . ?
C33 C36 H36 120.0 . . ?
N2 C41 H41 118.8 . . ?
N2 C41 C2BA 122.4(5) . . ?
C2BA C41 H41 118.8 . . ?
N2 C44 H44 118.8 . . ?
N2 C44 C3BA 122.3(5) . . ?
C3BA C44 H44 118.8 . . ?
C32 C52 H52 120.1 . . ?
C5BA C52 C32 119.7(5) . . ?
C5BA C52 H52 120.1 . . ?
C3AA C0AA S5 119.5(3) . . ?
C3AA C0AA C4 119.8(4) . . ?
C4 C0AA S5 120.7(3) . . ?
C C1AA H1A 119.9 . . ?
C8AA C1AA C 120.2(3) . . ?
C8AA C1AA H1A 119.9 . . ?
C0AA C3AA H3A 120.2 . . ?
C6AA C3AA C0AA 119.6(4) . . ?
C6AA C3AA H3A 120.2 . . ?
C0AA C4 H4 120.1 . . ?
C5AA C4 C0AA 119.8(4) . . ?
C5AA C4 H4 120.1 . . ?
C23 C1CA H1C 120.1 . . ?
C9 C1CA C23 119.9(4) . . ?
C9 C1CA H1C 120.1 . . ?
C33 C8 C8AA 118.7(4) . . ?
C33 C8 C8BA 121.2(4) . . ?
C8AA C8 C8BA 120.1(4) . . ?
N1 C2CA H2C 118.8 . . ?
N1 C2CA C1BA 122.5(5) . . ?
C1BA C2CA H2C 118.8 . . ?
C7AA C4AA H4A 119.6 . . ?
C7AA C4AA C5 120.7(4) . . ?
C5 C4AA H4A 119.6 . . ?
C4 C5AA H5A 119.6 . . ?
C4 C5AA C10 120.7(4) . . ?
C10 C5AA H5A 119.6 . . ?
C3AA C6AA H6A 119.3 . . ?
C10 C6AA C3AA 121.4(4) . . ?
C10 C6AA H6A 119.3 . . ?
C23 C7AA H7A 119.6 . . ?
C4AA C7AA C23 120.8(4) . . ?
C4AA C7AA H7A 119.6 . . ?
C4AA C5 C9BA 121.4(4) . . ?
C9 C5 C4AA 117.8(4) . . ?
C9 C5 C9BA 120.8(4) . . ?
C1AA C8AA C8 120.9(4) . . ?
C1AA C8AA H8A 119.5 . . ?
C8 C8AA H8A 119.5 . . ?
C1CA C9 C5 121.9(4) . . ?
C1CA C9 H9 119.1 . . ?
C5 C9 H9 119.1 . . ?
C5AA C10 C7BA 119.7(4) . . ?
C6AA C10 C5AA 118.8(4) . . ?
C6AA C10 C7BA 121.5(4) . . ?
C9AA C2AA S4 119.6(3) . . ?
C9AA C2AA C0BA 120.2(4) . . ?
C0BA C2AA S4 120.1(3) . . ?
C2AA C9AA H9A 120.2 . . ?
C2AA C9AA C4BA 119.6(4) . . ?
C4BA C9AA H9A 120.2 . . ?
C8 C8BA H8BA 109.5 . . ?
C8 C8BA H8BB 109.5 . . ?
C8 C8BA H8BC 109.5 . . ?
H8BA C8BA H8BB 109.5 . . ?
H8BA C8BA H8BC 109.5 . . ?
H8BB C8BA H8BC 109.5 . . ?
C5 C9BA H9BA 109.5 . . ?
C5 C9BA H9BB 109.5 . . ?
C5 C9BA H9BC 109.5 . . ?
H9BA C9BA H9BB 109.5 . . ?
H9BA C9BA H9BC 109.5 . . ?
H9BB C9BA H9BC 109.5 . . ?
C7 C6 C4BA 118.1(4) . . ?
C7 C6 C0CA 121.3(5) . . ?
C4BA C6 C0CA 120.6(5) . . ?
C6 C7 H7 118.9 . . ?
C6 C7 C0BA 122.1(4) . . ?
C0BA C7 H7 118.9 . . ?
C44 C3BA H3B 121.1 . . ?
C6BA C3BA C44 117.7(5) . . ?
C6BA C3BA H3B 121.1 . . ?
C2CA C1BA H1B 120.4 . . ?
C5BA C1BA C2CA 119.2(5) . . ?
C5BA C1BA H1B 120.4 . . ?
C2AA C0BA C7 118.7(4) . . ?
C2AA C0BA H0B 120.6 . . ?
C7 C0BA H0B 120.6 . . ?
C10 C7BA H7BA 109.5 . . ?
C10 C7BA H7BB 109.5 . . ?
C10 C7BA H7BC 109.5 . . ?
H7BA C7BA H7BB 109.5 . . ?
H7BA C7BA H7BC 109.5 . . ?
H7BB C7BA H7BC 109.5 . . ?
C41 C2BA H2B 120.9 . . ?
C6BA C2BA C41 118.2(5) . . ?
C6BA C2BA H2B 120.9 . . ?
C9AA C4BA C6 121.3(4) . . ?
C9AA C4BA H4B 119.3 . . ?
C6 C4BA H4B 119.3 . . ?
C52 C5BA H5B 120.7 . . ?
C1BA C5BA C52 118.7(5) . . ?
C1BA C5BA H5B 120.7 . . ?
C3BA C6BA H6B 119.8 . . ?
C2BA C6BA C3BA 120.5(5) . . ?
C2BA C6BA H6B 119.8 . . ?
C6 C0CA H0CA 109.5 . . ?
C6 C0CA H0CB 109.5 . . ?
C6 C0CA H0CC 109.5 . . ?
H0CA C0CA H0CB 109.5 . . ?
H0CA C0CA H0CC 109.5 . . ?
H0CB C0CA H0CC 109.5 . . ?
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-2 -14 0 0.0395 -2.0000 -14.0000 0.0000 0.0745 1.0087 0.0331
2 14 0 0.0365 2.0000 14.0000 -0.0000 -0.0745 -1.0087 -0.0331
1 -5 -8 0.1551 1.0000 -5.0001 -8.0000 -0.8989 0.4423 -0.1241
-1 5 8 0.1551 -1.0000 5.0001 8.0000 0.8989 -0.4423 0.1241
9 -4 0 0.0740 9.0000 -4.0000 0.0000 -0.0937 0.0561 0.9791
-9 4 0 0.0740 -9.0000 4.0000 -0.0000 0.0937 -0.0561 -0.9791