# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2017
#######################################################################
#
# 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_saltry-yes_rt
_database_code_depnum_ccdc_archive 'CCDC 1555567'
_audit_update_record
;
2017-06-12 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_audit_creation_date 2016-05-31
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C28 H26 N2 O'
_chemical_formula_sum 'C28 H26 N2 O'
_chemical_formula_weight 406.51
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 8.6959(4)
_cell_length_b 9.22240(10)
_cell_length_c 14.9699(9)
_cell_angle_alpha 75.676(12)
_cell_angle_beta 85.233(15)
_cell_angle_gamma 67.950(12)
_cell_volume 1078.07(13)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 2748
_cell_measurement_temperature 200
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 3.1
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.076
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.889
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Blessing 1995'
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear yellowish yellow'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier yellowish
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.252
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 432
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.1
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0390
_diffrn_reflns_av_unetI/netI 0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 11613
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.479
_diffrn_reflns_theta_min 3.097
_diffrn_ambient_temperature 200
_diffrn_detector CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
scan:
Number of images: 629
Slice: -69.0000 - 119.7000
Image width: 0.3000
Exp time: 8.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 54.0000
Phi: 0.0000
XTD: 49.8600
2theta: 29.8900
scan:
Number of images: 629
Slice: -69.0000 - 119.7000
Image width: 0.3000
Exp time: 8.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 54.0000
Phi: 120.0000
XTD: 49.8600
2theta: 29.8900
scan:
Number of images: 629
Slice: -69.0000 - 119.7000
Image width: 0.3000
Exp time: 8.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 54.0000
Phi: 240.0000
XTD: 49.8600
2theta: 29.8900
;
_diffrn_measurement_device
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type
;
Rigaku Mercury375R (2x2 bin mode)
;
_diffrn_measurement_method 'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type d*Trek
_diffrn_orient_matrix_UB_11 -0.005023
_diffrn_orient_matrix_UB_12 0.020552
_diffrn_orient_matrix_UB_13 -0.122262
_diffrn_orient_matrix_UB_21 -0.109779
_diffrn_orient_matrix_UB_22 -0.000701
_diffrn_orient_matrix_UB_23 0.049273
_diffrn_orient_matrix_UB_31 0.021434
_diffrn_orient_matrix_UB_32 0.064874
_diffrn_orient_matrix_UB_33 0.009262
_diffrn_radiation_monochromator 'Graphite Monochromator'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71075
_diffrn_source 'Sealed Tube'
_diffrn_source_current 12.0
_diffrn_source_power 0.6
_diffrn_source_voltage 50.0
_diffrn_special_details
;
?
;
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 3842
_reflns_number_total 4904
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.249
_refine_diff_density_min -0.193
_refine_diff_density_rms 0.044
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.077
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 284
_refine_ls_number_reflns 4904
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0626
_refine_ls_R_factor_gt 0.0487
_refine_ls_restrained_S_all 1.077
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+0.1659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1204
_refine_ls_wR_factor_ref 0.1323
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H) groups
At 1.5 times of:
All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
C8(H8A,H8B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
C1(H1A), C4(H4), C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14),
C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
C25(H25), C26(H26), C27(H27), C28(H28)
2.c Idealised tetrahedral OH refined as rotating group:
O1(H1)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
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
O1 O 0.18145(15) 0.98185(14) 0.61227(7) 0.0532(3) Uani 1 1 d . . . . .
H1 H 0.2668 0.9004 0.6100 0.080 Uiso 1 1 calc GR . . . .
N1 N 0.43575(14) 0.79241(14) 0.53503(8) 0.0356(3) Uani 1 1 d . . . . .
N2 N 0.50583(14) 0.48747(13) 0.67314(7) 0.0296(2) Uani 1 1 d . . . . .
H2 H 0.4017(19) 0.5703(19) 0.6517(10) 0.036 Uiso 1 1 d R . . . .
C1 C 0.39330(17) 0.89887(17) 0.46006(9) 0.0333(3) Uani 1 1 d . . . . .
H1A H 0.4617 0.8835 0.4077 0.040 Uiso 1 1 calc R . . . .
C2 C 0.24392(17) 1.04387(16) 0.45084(9) 0.0328(3) Uani 1 1 d . . . . .
C3 C 0.14472(18) 1.07936(18) 0.52725(10) 0.0374(3) Uani 1 1 d . . . . .
C4 C 0.00559(19) 1.2203(2) 0.51606(11) 0.0461(4) Uani 1 1 d . . . . .
H4 H -0.0616 1.2450 0.5677 0.055 Uiso 1 1 calc R . . . .
C5 C -0.0359(2) 1.32473(19) 0.43067(12) 0.0467(4) Uani 1 1 d . . . . .
H5 H -0.1314 1.4208 0.4240 0.056 Uiso 1 1 calc R . . . .
C6 C 0.06022(19) 1.29107(19) 0.35427(11) 0.0433(4) Uani 1 1 d . . . . .
H6 H 0.0308 1.3628 0.2954 0.052 Uiso 1 1 calc R . . . .
C7 C 0.19949(19) 1.15152(17) 0.36533(10) 0.0373(3) Uani 1 1 d . . . . .
H7 H 0.2665 1.1285 0.3134 0.045 Uiso 1 1 calc R . . . .
C8 C 0.58954(17) 0.65172(16) 0.53868(9) 0.0335(3) Uani 1 1 d . . . . .
H8A H 0.6814 0.6870 0.5122 0.040 Uiso 1 1 calc R . . . .
H8B H 0.5761 0.5818 0.5017 0.040 Uiso 1 1 calc R . . . .
C9 C 0.63058(16) 0.55847(17) 0.63762(9) 0.0325(3) Uani 1 1 d . . . . .
H9A H 0.7417 0.4723 0.6411 0.039 Uiso 1 1 calc R . . . .
H9B H 0.6328 0.6313 0.6758 0.039 Uiso 1 1 calc R . . . .
C10 C 0.49730(15) 0.43637(15) 0.77551(8) 0.0267(3) Uani 1 1 d . . . . .
C11 C 0.33947(15) 0.39604(15) 0.79658(9) 0.0276(3) Uani 1 1 d . . . . .
C12 C 0.24988(17) 0.41691(17) 0.87674(10) 0.0347(3) Uani 1 1 d . . . . .
H12 H 0.2802 0.4657 0.9178 0.042 Uiso 1 1 calc R . . . .
C13 C 0.11632(18) 0.36687(18) 0.89730(11) 0.0395(3) Uani 1 1 d . . . . .
H13 H 0.0566 0.3807 0.9526 0.047 Uiso 1 1 calc R . . . .
C14 C 0.06976(17) 0.29717(17) 0.83791(11) 0.0386(3) Uani 1 1 d . . . . .
H14 H -0.0217 0.2631 0.8523 0.046 Uiso 1 1 calc R . . . .
C15 C 0.15649(17) 0.27715(16) 0.75767(11) 0.0362(3) Uani 1 1 d . . . . .
H15 H 0.1240 0.2306 0.7162 0.043 Uiso 1 1 calc R . . . .
C16 C 0.29122(16) 0.32513(15) 0.73763(9) 0.0311(3) Uani 1 1 d . . . . .
H16 H 0.3516 0.3093 0.6827 0.037 Uiso 1 1 calc R . . . .
C17 C 0.49289(15) 0.57439(15) 0.81753(9) 0.0282(3) Uani 1 1 d . . . . .
C18 C 0.35318(17) 0.71563(16) 0.80260(10) 0.0346(3) Uani 1 1 d . . . . .
H18 H 0.2558 0.7177 0.7770 0.041 Uiso 1 1 calc R . . . .
C19 C 0.3529(2) 0.85339(18) 0.82421(10) 0.0412(3) Uani 1 1 d . . . . .
H19 H 0.2556 0.9480 0.8141 0.049 Uiso 1 1 calc R . . . .
C20 C 0.4941(2) 0.85334(18) 0.86049(10) 0.0421(4) Uani 1 1 d . . . . .
H20 H 0.4949 0.9481 0.8745 0.051 Uiso 1 1 calc R . . . .
C21 C 0.63366(19) 0.71453(19) 0.87617(10) 0.0394(3) Uani 1 1 d . . . . .
H21 H 0.7308 0.7134 0.9015 0.047 Uiso 1 1 calc R . . . .
C22 C 0.63303(17) 0.57597(17) 0.85510(9) 0.0345(3) Uani 1 1 d . . . . .
H22 H 0.7299 0.4809 0.8666 0.041 Uiso 1 1 calc R . . . .
C23 C 0.64117(15) 0.27739(15) 0.81231(9) 0.0276(3) Uani 1 1 d . . . . .
C24 C 0.66438(16) 0.21323(16) 0.90743(9) 0.0333(3) Uani 1 1 d . . . . .
H24 H 0.5951 0.2722 0.9489 0.040 Uiso 1 1 calc R . . . .
C25 C 0.78675(17) 0.06506(17) 0.94209(10) 0.0378(3) Uani 1 1 d . . . . .
H25 H 0.7997 0.0227 1.0068 0.045 Uiso 1 1 calc R . . . .
C26 C 0.89064(17) -0.02175(17) 0.88251(11) 0.0385(3) Uani 1 1 d . . . . .
H26 H 0.9760 -0.1224 0.9063 0.046 Uiso 1 1 calc R . . . .
C27 C 0.86906(17) 0.03893(17) 0.78889(10) 0.0368(3) Uani 1 1 d . . . . .
H27 H 0.9400 -0.0200 0.7479 0.044 Uiso 1 1 calc R . . . .
C28 C 0.74375(16) 0.18637(16) 0.75380(9) 0.0313(3) Uani 1 1 d . . . . .
H28 H 0.7281 0.2254 0.6890 0.038 Uiso 1 1 calc 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
O1 0.0531(7) 0.0517(7) 0.0350(6) -0.0009(5) 0.0104(5) -0.0049(6)
N1 0.0358(6) 0.0350(6) 0.0333(6) -0.0053(5) 0.0050(5) -0.0126(5)
N2 0.0279(6) 0.0319(6) 0.0292(6) -0.0040(4) 0.0005(4) -0.0132(5)
C1 0.0388(7) 0.0369(7) 0.0287(7) -0.0093(5) 0.0038(5) -0.0186(6)
C2 0.0344(7) 0.0342(7) 0.0330(7) -0.0073(5) 0.0001(5) -0.0166(6)
C3 0.0372(7) 0.0392(8) 0.0339(7) -0.0052(6) 0.0028(6) -0.0147(6)
C4 0.0386(8) 0.0483(9) 0.0456(9) -0.0108(7) 0.0073(7) -0.0110(7)
C5 0.0375(8) 0.0407(8) 0.0542(10) -0.0055(7) -0.0038(7) -0.0083(7)
C6 0.0462(9) 0.0419(8) 0.0406(8) -0.0012(6) -0.0089(7) -0.0182(7)
C7 0.0426(8) 0.0403(8) 0.0323(7) -0.0081(6) 0.0006(6) -0.0192(7)
C8 0.0344(7) 0.0330(7) 0.0340(7) -0.0096(6) 0.0074(5) -0.0137(6)
C9 0.0289(7) 0.0358(7) 0.0345(7) -0.0074(6) 0.0039(5) -0.0152(6)
C10 0.0241(6) 0.0286(6) 0.0279(6) -0.0064(5) 0.0004(5) -0.0104(5)
C11 0.0225(6) 0.0258(6) 0.0320(7) -0.0038(5) -0.0010(5) -0.0079(5)
C12 0.0314(7) 0.0399(7) 0.0357(7) -0.0108(6) 0.0021(5) -0.0154(6)
C13 0.0331(7) 0.0427(8) 0.0423(8) -0.0083(6) 0.0099(6) -0.0166(6)
C14 0.0268(7) 0.0323(7) 0.0560(9) -0.0044(6) -0.0011(6) -0.0136(6)
C15 0.0315(7) 0.0300(7) 0.0488(8) -0.0086(6) -0.0067(6) -0.0123(6)
C16 0.0284(6) 0.0296(6) 0.0357(7) -0.0094(5) 0.0001(5) -0.0099(5)
C17 0.0282(6) 0.0298(6) 0.0277(6) -0.0066(5) 0.0035(5) -0.0126(5)
C18 0.0306(7) 0.0334(7) 0.0385(7) -0.0090(6) 0.0004(6) -0.0101(6)
C19 0.0455(8) 0.0308(7) 0.0432(8) -0.0100(6) 0.0037(6) -0.0094(6)
C20 0.0586(10) 0.0375(8) 0.0383(8) -0.0143(6) 0.0067(7) -0.0245(7)
C21 0.0451(8) 0.0482(8) 0.0354(8) -0.0130(6) 0.0002(6) -0.0266(7)
C22 0.0318(7) 0.0370(7) 0.0367(7) -0.0101(6) 0.0003(5) -0.0138(6)
C23 0.0227(6) 0.0273(6) 0.0342(7) -0.0067(5) 0.0005(5) -0.0112(5)
C24 0.0291(7) 0.0338(7) 0.0347(7) -0.0072(5) 0.0029(5) -0.0101(6)
C25 0.0344(7) 0.0359(7) 0.0383(8) -0.0013(6) -0.0029(6) -0.0113(6)
C26 0.0284(7) 0.0288(7) 0.0539(9) -0.0052(6) -0.0050(6) -0.0072(6)
C27 0.0290(7) 0.0342(7) 0.0494(9) -0.0172(6) 0.0038(6) -0.0101(6)
C28 0.0282(6) 0.0339(7) 0.0346(7) -0.0106(5) 0.0015(5) -0.0130(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
O1 H1 0.8400 . ?
O1 C3 1.3477(17) . ?
N1 C1 1.2693(18) . ?
N1 C8 1.4660(18) . ?
N2 H2 0.956(15) . ?
N2 C9 1.4675(16) . ?
N2 C10 1.4920(16) . ?
C1 H1A 0.9500 . ?
C1 C2 1.4590(19) . ?
C2 C3 1.403(2) . ?
C2 C7 1.3924(19) . ?
C3 C4 1.388(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.378(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.388(2) . ?
C6 H6 0.9500 . ?
C6 C7 1.381(2) . ?
C7 H7 0.9500 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.5126(19) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.5411(16) . ?
C10 C17 1.5404(17) . ?
C10 C23 1.5350(17) . ?
C11 C12 1.3893(18) . ?
C11 C16 1.3912(18) . ?
C12 H12 0.9500 . ?
C12 C13 1.3890(19) . ?
C13 H13 0.9500 . ?
C13 C14 1.380(2) . ?
C14 H14 0.9500 . ?
C14 C15 1.379(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.3870(18) . ?
C16 H16 0.9500 . ?
C17 C18 1.3912(18) . ?
C17 C22 1.3903(18) . ?
C18 H18 0.9500 . ?
C18 C19 1.386(2) . ?
C19 H19 0.9500 . ?
C19 C20 1.383(2) . ?
C20 H20 0.9500 . ?
C20 C21 1.378(2) . ?
C21 H21 0.9500 . ?
C21 C22 1.392(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.3998(18) . ?
C23 C28 1.3926(18) . ?
C24 H24 0.9500 . ?
C24 C25 1.3849(19) . ?
C25 H25 0.9500 . ?
C25 C26 1.389(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.374(2) . ?
C27 H27 0.9500 . ?
C27 C28 1.3933(19) . ?
C28 H28 0.9500 . ?
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
C3 O1 H1 109.5 . . ?
C1 N1 C8 119.24(12) . . ?
C9 N2 H2 105.0(9) . . ?
C9 N2 C10 116.08(10) . . ?
C10 N2 H2 107.6(9) . . ?
N1 C1 H1A 118.6 . . ?
N1 C1 C2 122.82(13) . . ?
C2 C1 H1A 118.6 . . ?
C3 C2 C1 121.22(12) . . ?
C7 C2 C1 119.92(12) . . ?
C7 C2 C3 118.84(13) . . ?
O1 C3 C2 122.07(13) . . ?
O1 C3 C4 118.41(13) . . ?
C4 C3 C2 119.51(13) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 C3 120.54(14) . . ?
C5 C4 H4 119.7 . . ?
C4 C5 H5 119.6 . . ?
C4 C5 C6 120.72(15) . . ?
C6 C5 H5 119.6 . . ?
C5 C6 H6 120.6 . . ?
C7 C6 C5 118.87(14) . . ?
C7 C6 H6 120.6 . . ?
C2 C7 H7 119.2 . . ?
C6 C7 C2 121.52(14) . . ?
C6 C7 H7 119.2 . . ?
N1 C8 H8A 109.7 . . ?
N1 C8 H8B 109.7 . . ?
N1 C8 C9 109.70(11) . . ?
H8A C8 H8B 108.2 . . ?
C9 C8 H8A 109.7 . . ?
C9 C8 H8B 109.7 . . ?
N2 C9 C8 109.89(11) . . ?
N2 C9 H9A 109.7 . . ?
N2 C9 H9B 109.7 . . ?
C8 C9 H9A 109.7 . . ?
C8 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
N2 C10 C11 106.67(10) . . ?
N2 C10 C17 108.75(10) . . ?
N2 C10 C23 110.39(10) . . ?
C17 C10 C11 112.39(10) . . ?
C23 C10 C11 105.00(10) . . ?
C23 C10 C17 113.42(10) . . ?
C12 C11 C10 121.96(11) . . ?
C12 C11 C16 118.35(12) . . ?
C16 C11 C10 119.51(11) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.46(13) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 119.8 . . ?
C14 C13 C12 120.45(13) . . ?
C14 C13 H13 119.8 . . ?
C13 C14 H14 120.1 . . ?
C15 C14 C13 119.73(12) . . ?
C15 C14 H14 120.1 . . ?
C14 C15 H15 120.1 . . ?
C14 C15 C16 119.89(13) . . ?
C16 C15 H15 120.1 . . ?
C11 C16 H16 119.4 . . ?
C15 C16 C11 121.11(13) . . ?
C15 C16 H16 119.4 . . ?
C18 C17 C10 118.85(11) . . ?
C22 C17 C10 122.44(11) . . ?
C22 C17 C18 117.63(12) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 C17 121.46(13) . . ?
C19 C18 H18 119.3 . . ?
C18 C19 H19 119.9 . . ?
C20 C19 C18 120.11(14) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 120.3 . . ?
C21 C20 C19 119.36(13) . . ?
C21 C20 H20 120.3 . . ?
C20 C21 H21 119.8 . . ?
C20 C21 C22 120.36(13) . . ?
C22 C21 H21 119.8 . . ?
C17 C22 C21 121.06(13) . . ?
C17 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C24 C23 C10 120.05(11) . . ?
C28 C23 C10 121.98(12) . . ?
C28 C23 C24 117.79(12) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 C23 121.04(13) . . ?
C25 C24 H24 119.5 . . ?
C24 C25 H25 119.9 . . ?
C24 C25 C26 120.22(13) . . ?
C26 C25 H25 119.9 . . ?
C25 C26 H26 120.2 . . ?
C27 C26 C25 119.55(13) . . ?
C27 C26 H26 120.2 . . ?
C26 C27 H27 119.8 . . ?
C26 C27 C28 120.36(13) . . ?
C28 C27 H27 119.8 . . ?
C23 C28 C27 121.01(13) . . ?
C23 C28 H28 119.5 . . ?
C27 C28 H28 119.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C3 C4 C5 179.25(15) . . . . ?
N1 C1 C2 C3 4.9(2) . . . . ?
N1 C1 C2 C7 -176.40(13) . . . . ?
N1 C8 C9 N2 66.99(14) . . . . ?
N2 C10 C11 C12 -149.41(12) . . . . ?
N2 C10 C11 C16 35.62(15) . . . . ?
N2 C10 C17 C18 68.07(14) . . . . ?
N2 C10 C17 C22 -99.81(14) . . . . ?
N2 C10 C23 C24 175.31(11) . . . . ?
N2 C10 C23 C28 -9.84(15) . . . . ?
C1 N1 C8 C9 169.65(12) . . . . ?
C1 C2 C3 O1 -0.3(2) . . . . ?
C1 C2 C3 C4 178.57(13) . . . . ?
C1 C2 C7 C6 -179.11(13) . . . . ?
C2 C3 C4 C5 0.3(2) . . . . ?
C3 C2 C7 C6 -0.4(2) . . . . ?
C3 C4 C5 C6 0.1(2) . . . . ?
C4 C5 C6 C7 -0.6(2) . . . . ?
C5 C6 C7 C2 0.7(2) . . . . ?
C7 C2 C3 O1 -179.07(13) . . . . ?
C7 C2 C3 C4 -0.2(2) . . . . ?
C8 N1 C1 C2 -178.89(12) . . . . ?
C9 N2 C10 C11 169.75(10) . . . . ?
C9 N2 C10 C17 48.32(14) . . . . ?
C9 N2 C10 C23 -76.71(13) . . . . ?
C10 N2 C9 C8 -161.68(11) . . . . ?
C10 C11 C12 C13 -174.59(12) . . . . ?
C10 C11 C16 C15 175.57(12) . . . . ?
C10 C17 C18 C19 -168.43(12) . . . . ?
C10 C17 C22 C21 167.44(12) . . . . ?
C10 C23 C24 C25 175.87(12) . . . . ?
C10 C23 C28 C27 -177.15(11) . . . . ?
C11 C10 C17 C18 -49.79(15) . . . . ?
C11 C10 C17 C22 142.33(12) . . . . ?
C11 C10 C23 C24 -70.09(14) . . . . ?
C11 C10 C23 C28 104.76(13) . . . . ?
C11 C12 C13 C14 -0.6(2) . . . . ?
C12 C11 C16 C15 0.41(19) . . . . ?
C12 C13 C14 C15 0.0(2) . . . . ?
C13 C14 C15 C16 0.8(2) . . . . ?
C14 C15 C16 C11 -1.1(2) . . . . ?
C16 C11 C12 C13 0.4(2) . . . . ?
C17 C10 C11 C12 -30.31(16) . . . . ?
C17 C10 C11 C16 154.71(11) . . . . ?
C17 C10 C23 C24 52.99(15) . . . . ?
C17 C10 C23 C28 -132.17(12) . . . . ?
C17 C18 C19 C20 0.8(2) . . . . ?
C18 C17 C22 C21 -0.58(19) . . . . ?
C18 C19 C20 C21 -1.0(2) . . . . ?
C19 C20 C21 C22 0.5(2) . . . . ?
C20 C21 C22 C17 0.3(2) . . . . ?
C22 C17 C18 C19 0.0(2) . . . . ?
C23 C10 C11 C12 93.42(14) . . . . ?
C23 C10 C11 C16 -81.56(14) . . . . ?
C23 C10 C17 C18 -168.71(11) . . . . ?
C23 C10 C17 C22 23.41(17) . . . . ?
C23 C24 C25 C26 0.9(2) . . . . ?
C24 C23 C28 C27 -2.20(18) . . . . ?
C24 C25 C26 C27 -1.3(2) . . . . ?
C25 C26 C27 C28 -0.1(2) . . . . ?
C26 C27 C28 C23 1.9(2) . . . . ?
C28 C23 C24 C25 0.81(19) . . . . ?
_shelx_SHELXL_version_number 2014/7
_iucr_refine_instructions_details
;
saltry-yes_200k.res created by SHELXL-2014/7
TITL saltry-yes_200k_a.res in P-1
REM Old TITL SALTRY-YES_200K in P-1 #2
REM SHELXT solution in P-1
REM R1 0.140, Rweak 0.005, Alpha 0.031, Orientation as input
REM Formula found by SHELXT: C28 N2 O
CELL 0.71075 8.6959 9.2224 14.9699 75.676 85.233 67.95
ZERR 2 0.0004 0.0001 0.0009 0.012 0.015 0.012
LATT 1
SFAC C H N O
UNIT 56 52 4 2
L.S. 10
PLAN 20
TEMP -73.15
BOND $H
LIST 4
MORE -1
CONF
fmap 2
acta
REM
REM
REM
WGHT 0.063000 0.165900
FVAR 0.64486
O1 4 0.181451 0.981848 0.612272 11.00000 0.05308 0.05168 =
0.03498 -0.00093 0.01035 -0.00494
AFIX 147
H1 2 0.266755 0.900410 0.610009 11.00000 -1.50000
AFIX 0
N1 3 0.435752 0.792415 0.535027 11.00000 0.03579 0.03498 =
0.03327 -0.00535 0.00500 -0.01262
N2 3 0.505835 0.487474 0.673140 11.00000 0.02787 0.03187 =
0.02923 -0.00403 0.00053 -0.01324
H2 2 0.401749 0.570337 0.651740 11.00000 -1.20000
C1 1 0.393299 0.898871 0.460058 11.00000 0.03882 0.03689 =
0.02871 -0.00929 0.00385 -0.01864
AFIX 43
H1A 2 0.461723 0.883472 0.407707 11.00000 -1.20000
AFIX 0
C2 1 0.243924 1.043870 0.450835 11.00000 0.03436 0.03421 =
0.03301 -0.00734 0.00011 -0.01657
C3 1 0.144720 1.079365 0.527250 11.00000 0.03719 0.03917 =
0.03395 -0.00522 0.00285 -0.01470
C4 1 0.005592 1.220304 0.516061 11.00000 0.03863 0.04827 =
0.04562 -0.01081 0.00732 -0.01101
AFIX 43
H4 2 -0.061558 1.244966 0.567699 11.00000 -1.20000
AFIX 0
C5 1 -0.035919 1.324732 0.430669 11.00000 0.03750 0.04066 =
0.05424 -0.00552 -0.00384 -0.00831
AFIX 43
H5 2 -0.131409 1.420838 0.424028 11.00000 -1.20000
AFIX 0
C6 1 0.060217 1.291067 0.354267 11.00000 0.04624 0.04192 =
0.04056 -0.00122 -0.00887 -0.01821
AFIX 43
H6 2 0.030755 1.362767 0.295352 11.00000 -1.20000
AFIX 0
C7 1 0.199491 1.151522 0.365332 11.00000 0.04257 0.04031 =
0.03234 -0.00810 0.00061 -0.01916
AFIX 43
H7 2 0.266506 1.128468 0.313407 11.00000 -1.20000
AFIX 0
C8 1 0.589541 0.651716 0.538679 11.00000 0.03441 0.03300 =
0.03403 -0.00959 0.00740 -0.01370
AFIX 23
H8A 2 0.681427 0.687008 0.512226 11.00000 -1.20000
H8B 2 0.576066 0.581814 0.501689 11.00000 -1.20000
AFIX 0
C9 1 0.630584 0.558473 0.637623 11.00000 0.02887 0.03582 =
0.03451 -0.00736 0.00393 -0.01516
AFIX 23
H9A 2 0.741745 0.472271 0.641058 11.00000 -1.20000
H9B 2 0.632790 0.631269 0.675848 11.00000 -1.20000
AFIX 0
C10 1 0.497296 0.436374 0.775506 11.00000 0.02405 0.02863 =
0.02788 -0.00636 0.00037 -0.01041
C11 1 0.339468 0.396038 0.796584 11.00000 0.02252 0.02584 =
0.03198 -0.00383 -0.00099 -0.00786
C12 1 0.249877 0.416911 0.876741 11.00000 0.03137 0.03989 =
0.03567 -0.01078 0.00213 -0.01544
AFIX 43
H12 2 0.280173 0.465748 0.917776 11.00000 -1.20000
AFIX 0
C13 1 0.116315 0.366867 0.897301 11.00000 0.03313 0.04270 =
0.04233 -0.00826 0.00994 -0.01663
AFIX 43
H13 2 0.056604 0.380700 0.952611 11.00000 -1.20000
AFIX 0
C14 1 0.069760 0.297167 0.837907 11.00000 0.02684 0.03230 =
0.05599 -0.00444 -0.00111 -0.01359
AFIX 43
H14 2 -0.021675 0.263135 0.852270 11.00000 -1.20000
AFIX 0
C15 1 0.156490 0.277149 0.757668 11.00000 0.03154 0.02999 =
0.04883 -0.00863 -0.00665 -0.01225
AFIX 43
H15 2 0.124031 0.230566 0.716165 11.00000 -1.20000
AFIX 0
C16 1 0.291222 0.325135 0.737632 11.00000 0.02845 0.02962 =
0.03569 -0.00937 0.00008 -0.00992
AFIX 43
H16 2 0.351581 0.309318 0.682725 11.00000 -1.20000
AFIX 0
C17 1 0.492886 0.574391 0.817530 11.00000 0.02816 0.02977 =
0.02774 -0.00663 0.00347 -0.01258
C18 1 0.353177 0.715625 0.802601 11.00000 0.03061 0.03343 =
0.03849 -0.00897 0.00044 -0.01006
AFIX 43
H18 2 0.255794 0.717659 0.777024 11.00000 -1.20000
AFIX 0
C19 1 0.352911 0.853392 0.824206 11.00000 0.04548 0.03079 =
0.04323 -0.01004 0.00373 -0.00941
AFIX 43
H19 2 0.255576 0.948046 0.814079 11.00000 -1.20000
AFIX 0
C20 1 0.494110 0.853342 0.860492 11.00000 0.05863 0.03749 =
0.03827 -0.01432 0.00671 -0.02446
AFIX 43
H20 2 0.494876 0.948092 0.874472 11.00000 -1.20000
AFIX 0
C21 1 0.633663 0.714535 0.876169 11.00000 0.04506 0.04816 =
0.03543 -0.01300 0.00023 -0.02661
AFIX 43
H21 2 0.730835 0.713400 0.901493 11.00000 -1.20000
AFIX 0
C22 1 0.633026 0.575966 0.855099 11.00000 0.03179 0.03697 =
0.03667 -0.01012 0.00025 -0.01382
AFIX 43
H22 2 0.729912 0.480944 0.866576 11.00000 -1.20000
AFIX 0
C23 1 0.641167 0.277395 0.812315 11.00000 0.02270 0.02732 =
0.03422 -0.00668 0.00048 -0.01122
C24 1 0.664376 0.213227 0.907429 11.00000 0.02906 0.03379 =
0.03473 -0.00721 0.00292 -0.01015
AFIX 43
H24 2 0.595091 0.272242 0.948855 11.00000 -1.20000
AFIX 0
C25 1 0.786752 0.065063 0.942093 11.00000 0.03440 0.03588 =
0.03830 -0.00135 -0.00293 -0.01133
AFIX 43
H25 2 0.799682 0.022668 1.006837 11.00000 -1.20000
AFIX 0
C26 1 0.890642 -0.021751 0.882508 11.00000 0.02845 0.02875 =
0.05390 -0.00519 -0.00499 -0.00724
AFIX 43
H26 2 0.976034 -0.122383 0.906294 11.00000 -1.20000
AFIX 0
C27 1 0.869056 0.038933 0.788895 11.00000 0.02895 0.03424 =
0.04943 -0.01720 0.00380 -0.01014
AFIX 43
H27 2 0.939953 -0.019967 0.747894 11.00000 -1.20000
AFIX 0
C28 1 0.743752 0.186373 0.753804 11.00000 0.02819 0.03393 =
0.03457 -0.01061 0.00145 -0.01296
AFIX 43
H28 2 0.728059 0.225407 0.688968 11.00000 -1.20000
AFIX 0
HKLF 4
REM saltry-yes_200k_a.res in P-1
REM R1 = 0.0487 for 3842 Fo > 4sig(Fo) and 0.0626 for all 4904 data
REM 284 parameters refined using 0 restraints
END
WGHT 0.0614 0.1600
REM Highest difference peak 0.249, deepest hole -0.193, 1-sigma level 0.044
Q1 1 0.4227 0.4213 0.7832 11.00000 0.05 0.21
Q2 1 0.5543 0.5819 0.8231 11.00000 0.05 0.20
Q3 1 0.4926 0.5112 0.8067 11.00000 0.05 0.19
Q4 1 0.5645 0.3660 0.7920 11.00000 0.05 0.18
Q5 1 0.6990 0.2273 0.7788 11.00000 0.05 0.17
Q6 1 0.3268 0.3407 0.7725 11.00000 0.05 0.17
Q7 1 0.3062 1.0031 0.4540 11.00000 0.05 0.16
Q8 1 0.4345 0.6362 0.8038 11.00000 0.05 0.16
Q9 1 0.1907 1.0631 0.4837 11.00000 0.05 0.16
Q10 1 0.8113 0.0227 1.0330 11.00000 0.05 0.16
Q11 1 0.8056 0.0980 0.7765 11.00000 0.05 0.15
Q12 1 0.7735 0.3163 0.7912 11.00000 0.05 0.14
Q13 1 0.4970 0.4023 0.6373 11.00000 0.05 0.14
Q14 1 0.5030 0.9263 0.3978 11.00000 0.05 0.14
Q15 1 0.5198 0.1552 0.9197 11.00000 0.05 0.14
Q16 1 0.6184 0.5990 0.5822 11.00000 0.05 0.14
Q17 1 0.5228 0.9234 0.7735 11.00000 0.05 0.14
Q18 1 -0.0408 1.2454 0.6390 11.00000 0.05 0.13
Q19 1 0.2769 0.4359 0.8178 11.00000 0.05 0.13
Q20 1 0.6851 0.6209 0.7073 11.00000 0.05 0.13
REM The information below was added by Olex2.
REM
REM R1 = 0.0487 for 3842 Fo > 4sig(Fo) and 0.0626 for all 11613 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.25, deepest hole -0.19
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0626
REM R1_gt = 0.0487
REM wR_ref = 0.1323
REM GOOF = 1.077
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 11613
REM Reflections_gt = 3842
REM Parameters = n/a
REM Hole = -0.19
REM Peak = 0.25
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# 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_saltry-yes_90k
_database_code_depnum_ccdc_archive 'CCDC 1555566'
_audit_update_record
;
2017-06-12 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_audit_creation_date 2016-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C28 H26 N2 O'
_chemical_formula_sum 'C28 H26 N2 O'
_chemical_formula_weight 406.51
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 8.6520(10)
_cell_length_b 9.2161(6)
_cell_length_c 14.815(2)
_cell_angle_alpha 75.93(4)
_cell_angle_beta 85.85(4)
_cell_angle_gamma 68.03(3)
_cell_volume 1062.4(4)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 2943
_cell_measurement_temperature 90
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 3.1
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.077
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.782
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Blessing 1995'
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear yellowish yellow'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier yellowish
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.271
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 432
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.4
_exptl_crystal_size_min 0.3
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0654
_diffrn_reflns_av_unetI/netI 0.0628
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 11174
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.512
_diffrn_reflns_theta_min 3.105
_diffrn_ambient_temperature 90
_diffrn_detector CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
scan:
Number of images: 629
Slice: -69.0000 - 119.7000
Image width: 0.3000
Exp time: 10.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 54.0000
Phi: 120.0000
XTD: 49.8600
2theta: 29.8900
scan:
Number of images: 629
Slice: -69.0000 - 119.7000
Image width: 0.3000
Exp time: 10.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 54.0000
Phi: 0.0000
XTD: 49.8600
2theta: 29.8900
scan:
Number of images: 629
Slice: -69.0000 - 119.7000
Image width: 0.3000
Exp time: 10.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 54.0000
Phi: 240.0000
XTD: 49.8600
2theta: 29.8900
;
_diffrn_measurement_device
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type
;
Rigaku Mercury375R (2x2 bin mode)
;
_diffrn_measurement_method 'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type d*Trek
_diffrn_orient_matrix_UB_11 0.108056
_diffrn_orient_matrix_UB_12 -0.033609
_diffrn_orient_matrix_UB_13 0.052287
_diffrn_orient_matrix_UB_21 -0.078333
_diffrn_orient_matrix_UB_22 0.040218
_diffrn_orient_matrix_UB_23 0.082012
_diffrn_orient_matrix_UB_31 -0.016244
_diffrn_orient_matrix_UB_32 -0.067383
_diffrn_orient_matrix_UB_33 -0.006322
_diffrn_radiation_monochromator 'Graphite Monochromator'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71075
_diffrn_source 'Sealed Tube'
_diffrn_source_current 12.0
_diffrn_source_power 0.6
_diffrn_source_voltage 50.0
_diffrn_special_details
;
?
;
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 3538
_reflns_number_total 4829
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.357
_refine_diff_density_min -0.294
_refine_diff_density_rms 0.062
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.066
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 285
_refine_ls_number_reflns 4829
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0676
_refine_ls_R_factor_gt 0.0528
_refine_ls_restrained_S_all 1.066
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0766P)^2^+0.0629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1333
_refine_ls_wR_factor_ref 0.1519
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
C8(H8A,H8B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
C1(H1A), C4(H4), C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14),
C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
C25(H25), C26(H26), C27(H27), C28(H28)
2.c Idealised tetrahedral OH refined as rotating group:
O1(H1)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
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
O1 O 0.82228(14) 0.02028(14) 0.38775(8) 0.0290(3) Uani 1 1 d . . . . .
H1 H 0.7352 0.1004 0.3899 0.044 Uiso 1 1 calc GR . . . .
N1 N 0.56553(15) 0.20760(15) 0.46562(9) 0.0213(3) Uani 1 1 d . . . . .
N2 N 0.49619(15) 0.51260(15) 0.32763(8) 0.0184(3) Uani 1 1 d . . . . .
H2 H 0.601(2) 0.430(2) 0.3506(12) 0.026(4) Uiso 1 1 d . . . . .
C1 C 0.60643(19) 0.09912(18) 0.54112(10) 0.0206(3) Uani 1 1 d . . . . .
H1A H 0.5365 0.1129 0.5933 0.025 Uiso 1 1 calc R . . . .
C2 C 0.75721(18) -0.04576(18) 0.55013(10) 0.0205(3) Uani 1 1 d . . . . .
C3 C 0.85855(19) -0.07964(18) 0.47319(10) 0.0219(3) Uani 1 1 d . . . . .
C4 C 0.9980(2) -0.22082(19) 0.48355(11) 0.0260(4) Uani 1 1 d . . . . .
H4 H 1.0655 -0.2443 0.4316 0.031 Uiso 1 1 calc R . . . .
C5 C 1.03853(19) -0.32746(19) 0.56987(11) 0.0256(3) Uani 1 1 d . . . . .
H5 H 1.1341 -0.4239 0.5767 0.031 Uiso 1 1 calc R . . . .
C6 C 0.94061(19) -0.29474(19) 0.64691(11) 0.0251(3) Uani 1 1 d . . . . .
H6 H 0.9698 -0.3675 0.7061 0.030 Uiso 1 1 calc R . . . .
C7 C 0.80077(19) -0.15535(18) 0.63598(11) 0.0217(3) Uani 1 1 d . . . . .
H7 H 0.7328 -0.1337 0.6881 0.026 Uiso 1 1 calc R . . . .
C8 C 0.41065(18) 0.34788(18) 0.46235(10) 0.0203(3) Uani 1 1 d . . . . .
H8A H 0.4241 0.4170 0.5006 0.024 Uiso 1 1 calc R . . . .
H8B H 0.3186 0.3121 0.4881 0.024 Uiso 1 1 calc R . . . .
C9 C 0.36940(18) 0.44223(18) 0.36277(10) 0.0197(3) Uani 1 1 d . . . . .
H9A H 0.3659 0.3704 0.3236 0.024 Uiso 1 1 calc R . . . .
H9B H 0.2582 0.5291 0.3592 0.024 Uiso 1 1 calc R . . . .
C10 C 0.50467(17) 0.56353(17) 0.22468(10) 0.0168(3) Uani 1 1 d . . . . .
C11 C 0.66366(17) 0.60383(17) 0.20354(10) 0.0178(3) Uani 1 1 d . . . . .
C12 C 0.71170(18) 0.67593(17) 0.26339(10) 0.0194(3) Uani 1 1 d . . . . .
H12 H 0.6513 0.6920 0.3186 0.023 Uiso 1 1 calc R . . . .
C13 C 0.84701(18) 0.72459(18) 0.24321(11) 0.0220(3) Uani 1 1 d . . . . .
H13 H 0.8794 0.7719 0.2851 0.026 Uiso 1 1 calc R . . . .
C14 C 0.93435(18) 0.70419(18) 0.16234(11) 0.0229(3) Uani 1 1 d . . . . .
H14 H 1.0257 0.7388 0.1481 0.028 Uiso 1 1 calc R . . . .
C15 C 0.88777(19) 0.63288(18) 0.10213(11) 0.0228(3) Uani 1 1 d . . . . .
H15 H 0.9476 0.6183 0.0466 0.027 Uiso 1 1 calc R . . . .
C16 C 0.75324(18) 0.58257(18) 0.12285(10) 0.0210(3) Uani 1 1 d . . . . .
H16 H 0.7225 0.5333 0.0814 0.025 Uiso 1 1 calc R . . . .
C17 C 0.36027(17) 0.72212(17) 0.18756(10) 0.0175(3) Uani 1 1 d . . . . .
C18 C 0.25830(18) 0.81389(18) 0.24644(10) 0.0193(3) Uani 1 1 d . . . . .
H18 H 0.2753 0.7750 0.3119 0.023 Uiso 1 1 calc R . . . .
C19 C 0.13204(18) 0.96140(18) 0.21138(11) 0.0220(3) Uani 1 1 d . . . . .
H19 H 0.0612 1.0200 0.2528 0.026 Uiso 1 1 calc R . . . .
C20 C 0.10972(19) 1.02254(18) 0.11634(11) 0.0231(3) Uani 1 1 d . . . . .
H20 H 0.0242 1.1234 0.0921 0.028 Uiso 1 1 calc R . . . .
C21 C 0.21368(18) 0.93501(18) 0.05632(11) 0.0229(3) Uani 1 1 d . . . . .
H21 H 0.2003 0.9775 -0.0091 0.027 Uiso 1 1 calc R . . . .
C22 C 0.33646(18) 0.78640(18) 0.09140(11) 0.0203(3) Uani 1 1 d . . . . .
H22 H 0.4055 0.7272 0.0497 0.024 Uiso 1 1 calc R . . . .
C23 C 0.50909(18) 0.42525(17) 0.18205(10) 0.0182(3) Uani 1 1 d . . . . .
C24 C 0.36721(18) 0.42344(18) 0.14369(10) 0.0206(3) Uani 1 1 d . . . . .
H24 H 0.2699 0.5186 0.1315 0.025 Uiso 1 1 calc R . . . .
C25 C 0.3662(2) 0.28413(19) 0.12294(10) 0.0233(3) Uani 1 1 d . . . . .
H25 H 0.2683 0.2852 0.0972 0.028 Uiso 1 1 calc R . . . .
C26 C 0.5060(2) 0.14486(19) 0.13953(11) 0.0243(3) Uani 1 1 d . . . . .
H26 H 0.5046 0.0498 0.1259 0.029 Uiso 1 1 calc R . . . .
C27 C 0.6494(2) 0.14516(19) 0.17651(11) 0.0248(3) Uani 1 1 d . . . . .
H27 H 0.7470 0.0503 0.1875 0.030 Uiso 1 1 calc R . . . .
C28 C 0.64961(18) 0.28409(18) 0.19728(10) 0.0212(3) Uani 1 1 d . . . . .
H28 H 0.7482 0.2827 0.2225 0.025 Uiso 1 1 calc 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
O1 0.0286(6) 0.0286(6) 0.0239(6) -0.0019(5) 0.0043(5) -0.0072(5)
N1 0.0214(6) 0.0218(7) 0.0229(7) -0.0042(5) 0.0015(5) -0.0111(5)
N2 0.0172(6) 0.0217(7) 0.0197(6) -0.0032(5) 0.0009(5) -0.0120(5)
C1 0.0228(7) 0.0243(8) 0.0215(7) -0.0081(6) 0.0031(6) -0.0151(6)
C2 0.0209(7) 0.0217(8) 0.0249(8) -0.0066(6) 0.0006(6) -0.0139(6)
C3 0.0235(8) 0.0239(8) 0.0223(8) -0.0049(6) 0.0015(6) -0.0136(6)
C4 0.0234(8) 0.0276(8) 0.0291(9) -0.0077(6) 0.0033(6) -0.0115(7)
C5 0.0211(8) 0.0231(8) 0.0330(9) -0.0045(6) -0.0018(6) -0.0093(6)
C6 0.0270(8) 0.0259(8) 0.0254(8) -0.0011(6) -0.0042(6) -0.0152(7)
C7 0.0235(8) 0.0241(8) 0.0235(8) -0.0062(6) 0.0009(6) -0.0151(6)
C8 0.0201(7) 0.0204(7) 0.0234(8) -0.0059(6) 0.0030(6) -0.0110(6)
C9 0.0175(7) 0.0220(7) 0.0232(8) -0.0052(6) 0.0030(6) -0.0117(6)
C10 0.0156(7) 0.0181(7) 0.0192(7) -0.0042(5) -0.0002(5) -0.0088(6)
C11 0.0165(7) 0.0169(7) 0.0214(7) -0.0027(5) -0.0009(5) -0.0088(5)
C12 0.0174(7) 0.0183(7) 0.0241(8) -0.0062(6) 0.0008(6) -0.0077(6)
C13 0.0209(7) 0.0196(7) 0.0292(8) -0.0061(6) -0.0026(6) -0.0107(6)
C14 0.0175(7) 0.0200(8) 0.0337(9) -0.0033(6) -0.0008(6) -0.0112(6)
C15 0.0217(8) 0.0253(8) 0.0246(8) -0.0056(6) 0.0054(6) -0.0130(6)
C16 0.0201(7) 0.0248(8) 0.0217(7) -0.0061(6) -0.0002(6) -0.0117(6)
C17 0.0146(7) 0.0186(7) 0.0240(7) -0.0048(6) 0.0004(6) -0.0113(6)
C18 0.0184(7) 0.0221(8) 0.0225(7) -0.0062(6) 0.0006(6) -0.0125(6)
C19 0.0169(7) 0.0226(8) 0.0323(8) -0.0120(6) 0.0031(6) -0.0107(6)
C20 0.0187(7) 0.0189(7) 0.0337(9) -0.0039(6) -0.0023(6) -0.0102(6)
C21 0.0218(8) 0.0238(8) 0.0252(8) -0.0025(6) -0.0007(6) -0.0126(6)
C22 0.0179(7) 0.0213(8) 0.0254(8) -0.0075(6) 0.0023(6) -0.0103(6)
C23 0.0192(7) 0.0194(7) 0.0192(7) -0.0039(5) 0.0014(6) -0.0112(6)
C24 0.0192(7) 0.0218(7) 0.0226(7) -0.0051(6) 0.0004(6) -0.0094(6)
C25 0.0267(8) 0.0298(8) 0.0218(8) -0.0074(6) 0.0008(6) -0.0188(7)
C26 0.0339(9) 0.0223(8) 0.0235(8) -0.0080(6) 0.0043(6) -0.0169(7)
C27 0.0273(8) 0.0219(8) 0.0255(8) -0.0053(6) 0.0019(6) -0.0098(6)
C28 0.0195(7) 0.0237(8) 0.0238(8) -0.0060(6) 0.0012(6) -0.0116(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
O1 H1 0.8400 . ?
O1 C3 1.3503(19) . ?
N1 C1 1.275(2) . ?
N1 C8 1.4670(19) . ?
N2 H2 0.959(18) . ?
N2 C9 1.4766(18) . ?
N2 C10 1.4879(18) . ?
C1 H1A 0.9500 . ?
C1 C2 1.462(2) . ?
C2 C3 1.410(2) . ?
C2 C7 1.393(2) . ?
C3 C4 1.388(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.386(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.396(2) . ?
C6 H6 0.9500 . ?
C6 C7 1.380(2) . ?
C7 H7 0.9500 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.510(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.5464(18) . ?
C10 C17 1.530(2) . ?
C10 C23 1.541(2) . ?
C11 C12 1.395(2) . ?
C11 C16 1.391(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.392(2) . ?
C13 H13 0.9500 . ?
C13 C14 1.383(2) . ?
C14 H14 0.9500 . ?
C14 C15 1.388(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.395(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.394(2) . ?
C17 C22 1.401(2) . ?
C18 H18 0.9500 . ?
C18 C19 1.392(2) . ?
C19 H19 0.9500 . ?
C19 C20 1.382(2) . ?
C20 H20 0.9500 . ?
C20 C21 1.393(2) . ?
C21 H21 0.9500 . ?
C21 C22 1.386(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.397(2) . ?
C23 C28 1.391(2) . ?
C24 H24 0.9500 . ?
C24 C25 1.394(2) . ?
C25 H25 0.9500 . ?
C25 C26 1.378(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.393(2) . ?
C27 H27 0.9500 . ?
C27 C28 1.388(2) . ?
C28 H28 0.9500 . ?
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
C3 O1 H1 109.5 . . ?
C1 N1 C8 118.59(13) . . ?
C9 N2 H2 105.6(10) . . ?
C9 N2 C10 116.07(11) . . ?
C10 N2 H2 108.3(10) . . ?
N1 C1 H1A 118.9 . . ?
N1 C1 C2 122.25(14) . . ?
C2 C1 H1A 118.9 . . ?
C3 C2 C1 121.55(14) . . ?
C7 C2 C1 119.63(14) . . ?
C7 C2 C3 118.80(15) . . ?
O1 C3 C2 121.86(14) . . ?
O1 C3 C4 118.07(14) . . ?
C4 C3 C2 120.05(15) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 C3 119.88(15) . . ?
C5 C4 H4 120.1 . . ?
C4 C5 H5 119.6 . . ?
C4 C5 C6 120.75(15) . . ?
C6 C5 H5 119.6 . . ?
C5 C6 H6 120.4 . . ?
C7 C6 C5 119.16(15) . . ?
C7 C6 H6 120.4 . . ?
C2 C7 H7 119.3 . . ?
C6 C7 C2 121.35(15) . . ?
C6 C7 H7 119.3 . . ?
N1 C8 H8A 109.8 . . ?
N1 C8 H8B 109.8 . . ?
N1 C8 C9 109.40(13) . . ?
H8A C8 H8B 108.2 . . ?
C9 C8 H8A 109.8 . . ?
C9 C8 H8B 109.8 . . ?
N2 C9 C8 110.04(12) . . ?
N2 C9 H9A 109.7 . . ?
N2 C9 H9B 109.7 . . ?
C8 C9 H9A 109.7 . . ?
C8 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
N2 C10 C11 107.13(11) . . ?
N2 C10 C17 110.14(12) . . ?
N2 C10 C23 108.62(11) . . ?
C17 C10 C11 105.00(11) . . ?
C17 C10 C23 113.62(11) . . ?
C23 C10 C11 112.11(12) . . ?
C12 C11 C10 119.09(13) . . ?
C16 C11 C10 122.17(13) . . ?
C16 C11 C12 118.54(13) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 C11 120.81(14) . . ?
C13 C12 H12 119.6 . . ?
C12 C13 H13 119.9 . . ?
C14 C13 C12 120.18(14) . . ?
C14 C13 H13 119.9 . . ?
C13 C14 H14 120.2 . . ?
C13 C14 C15 119.61(13) . . ?
C15 C14 H14 120.2 . . ?
C14 C15 H15 119.9 . . ?
C14 C15 C16 120.19(14) . . ?
C16 C15 H15 119.9 . . ?
C11 C16 C15 120.66(14) . . ?
C11 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C18 C17 C10 122.11(13) . . ?
C18 C17 C22 117.76(14) . . ?
C22 C17 C10 119.89(13) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 C17 121.41(14) . . ?
C19 C18 H18 119.3 . . ?
C18 C19 H19 120.0 . . ?
C20 C19 C18 120.00(14) . . ?
C20 C19 H19 120.0 . . ?
C19 C20 H20 120.3 . . ?
C19 C20 C21 119.46(15) . . ?
C21 C20 H20 120.3 . . ?
C20 C21 H21 119.8 . . ?
C22 C21 C20 120.39(15) . . ?
C22 C21 H21 119.8 . . ?
C17 C22 H22 119.5 . . ?
C21 C22 C17 120.92(14) . . ?
C21 C22 H22 119.5 . . ?
C24 C23 C10 122.33(13) . . ?
C28 C23 C10 118.97(12) . . ?
C28 C23 C24 117.60(13) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 C23 121.00(14) . . ?
C25 C24 H24 119.5 . . ?
C24 C25 H25 119.7 . . ?
C26 C25 C24 120.56(14) . . ?
C26 C25 H25 119.7 . . ?
C25 C26 H26 120.4 . . ?
C25 C26 C27 119.20(14) . . ?
C27 C26 H26 120.4 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 C26 120.01(15) . . ?
C28 C27 H27 120.0 . . ?
C23 C28 H28 119.2 . . ?
C27 C28 C23 121.61(14) . . ?
C27 C28 H28 119.2 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C3 C4 C5 -179.31(14) . . . . ?
N1 C1 C2 C3 -5.4(2) . . . . ?
N1 C1 C2 C7 176.10(13) . . . . ?
N1 C8 C9 N2 -66.28(15) . . . . ?
N2 C10 C11 C12 -36.02(17) . . . . ?
N2 C10 C11 C16 149.26(14) . . . . ?
N2 C10 C17 C18 10.52(17) . . . . ?
N2 C10 C17 C22 -175.20(11) . . . . ?
N2 C10 C23 C24 99.40(16) . . . . ?
N2 C10 C23 C28 -68.36(16) . . . . ?
C1 N1 C8 C9 -168.65(12) . . . . ?
C1 C2 C3 O1 0.5(2) . . . . ?
C1 C2 C3 C4 -177.96(13) . . . . ?
C1 C2 C7 C6 178.93(13) . . . . ?
C2 C3 C4 C5 -0.8(2) . . . . ?
C3 C2 C7 C6 0.3(2) . . . . ?
C3 C4 C5 C6 0.0(2) . . . . ?
C4 C5 C6 C7 0.9(2) . . . . ?
C5 C6 C7 C2 -1.1(2) . . . . ?
C7 C2 C3 O1 179.08(13) . . . . ?
C7 C2 C3 C4 0.6(2) . . . . ?
C8 N1 C1 C2 179.06(12) . . . . ?
C9 N2 C10 C11 -169.99(11) . . . . ?
C9 N2 C10 C17 76.34(14) . . . . ?
C9 N2 C10 C23 -48.69(16) . . . . ?
C10 N2 C9 C8 161.30(12) . . . . ?
C10 C11 C12 C13 -175.34(13) . . . . ?
C10 C11 C16 C15 174.50(13) . . . . ?
C10 C17 C18 C19 177.13(12) . . . . ?
C10 C17 C22 C21 -175.60(12) . . . . ?
C10 C23 C24 C25 -166.88(13) . . . . ?
C10 C23 C28 C27 167.47(13) . . . . ?
C11 C10 C17 C18 -104.51(14) . . . . ?
C11 C10 C17 C22 69.77(15) . . . . ?
C11 C10 C23 C24 -142.41(14) . . . . ?
C11 C10 C23 C28 49.84(17) . . . . ?
C11 C12 C13 C14 1.0(2) . . . . ?
C12 C11 C16 C15 -0.2(2) . . . . ?
C12 C13 C14 C15 -0.9(2) . . . . ?
C13 C14 C15 C16 0.2(2) . . . . ?
C14 C15 C16 C11 0.4(2) . . . . ?
C16 C11 C12 C13 -0.4(2) . . . . ?
C17 C10 C11 C12 81.09(16) . . . . ?
C17 C10 C11 C16 -93.63(16) . . . . ?
C17 C10 C23 C24 -23.55(19) . . . . ?
C17 C10 C23 C28 168.69(12) . . . . ?
C17 C18 C19 C20 -2.4(2) . . . . ?
C18 C17 C22 C21 -1.1(2) . . . . ?
C18 C19 C20 C21 0.4(2) . . . . ?
C19 C20 C21 C22 1.3(2) . . . . ?
C20 C21 C22 C17 -0.9(2) . . . . ?
C22 C17 C18 C19 2.73(19) . . . . ?
C23 C10 C11 C12 -155.09(13) . . . . ?
C23 C10 C11 C16 30.19(19) . . . . ?
C23 C10 C17 C18 132.63(13) . . . . ?
C23 C10 C17 C22 -53.08(17) . . . . ?
C23 C24 C25 C26 -0.3(2) . . . . ?
C24 C23 C28 C27 -0.9(2) . . . . ?
C24 C25 C26 C27 -0.6(2) . . . . ?
C25 C26 C27 C28 0.8(2) . . . . ?
C26 C27 C28 C23 0.0(2) . . . . ?
C28 C23 C24 C25 1.0(2) . . . . ?
_shelx_SHELXL_version_number 2014/7
_iucr_refine_instructions_details
;
saltry-yes_90k.res created by SHELXL-2014/7
TITL saltry-yes_90k_a.res in P-1
REM Old TITL SALTRY-YES_90K in P-1 #2
REM SHELXT solution in P-1
REM R1 0.137, Rweak 0.003, Alpha 0.025, Orientation as input
REM Formula found by SHELXT: C28 N2 O
CELL 0.71075 8.652 9.2161 14.8152 75.93 85.847 68.029
ZERR 2 0.001 0.0006 0.0023 0.04 0.037 0.031
LATT 1
SFAC C H N O
UNIT 56 52 4 2
L.S. 10
PLAN 20
TEMP -183.15
BOND $H
LIST 4
MORE -1
CONF
fmap 2
acta
OMIT 1 0 3
OMIT -6 5 0
OMIT -2 1 4
REM
REM
REM
WGHT 0.076600 0.062900
FVAR 0.61764
O1 4 0.822275 0.020284 0.387746 11.00000 0.02856 0.02858 =
0.02394 -0.00190 0.00432 -0.00719
AFIX 147
H1 2 0.735189 0.100402 0.389897 11.00000 -1.50000
AFIX 0
N1 3 0.565528 0.207596 0.465616 11.00000 0.02137 0.02181 =
0.02290 -0.00420 0.00155 -0.01111
N2 3 0.496186 0.512595 0.327633 11.00000 0.01725 0.02174 =
0.01968 -0.00323 0.00089 -0.01202
H2 2 0.601192 0.430342 0.350566 11.00000 0.02592
C1 1 0.606426 0.099123 0.541119 11.00000 0.02279 0.02428 =
0.02151 -0.00806 0.00313 -0.01514
AFIX 43
H1A 2 0.536540 0.112886 0.593326 11.00000 -1.20000
AFIX 0
C2 1 0.757213 -0.045759 0.550127 11.00000 0.02090 0.02166 =
0.02495 -0.00660 0.00060 -0.01390
C3 1 0.858550 -0.079642 0.473185 11.00000 0.02347 0.02392 =
0.02235 -0.00485 0.00151 -0.01362
C4 1 0.997970 -0.220818 0.483546 11.00000 0.02341 0.02764 =
0.02910 -0.00772 0.00331 -0.01149
AFIX 43
H4 2 1.065464 -0.244291 0.431553 11.00000 -1.20000
AFIX 0
C5 1 1.038533 -0.327464 0.569873 11.00000 0.02114 0.02311 =
0.03296 -0.00450 -0.00175 -0.00932
AFIX 43
H5 2 1.134078 -0.423933 0.576683 11.00000 -1.20000
AFIX 0
C6 1 0.940606 -0.294742 0.646914 11.00000 0.02703 0.02587 =
0.02542 -0.00106 -0.00420 -0.01524
AFIX 43
H6 2 0.969837 -0.367499 0.706132 11.00000 -1.20000
AFIX 0
C7 1 0.800771 -0.155354 0.635982 11.00000 0.02352 0.02408 =
0.02352 -0.00625 0.00095 -0.01507
AFIX 43
H7 2 0.732828 -0.133708 0.688080 11.00000 -1.20000
AFIX 0
C8 1 0.410651 0.347884 0.462350 11.00000 0.02009 0.02045 =
0.02343 -0.00591 0.00301 -0.01102
AFIX 23
H8A 2 0.424131 0.416969 0.500573 11.00000 -1.20000
H8B 2 0.318602 0.312081 0.488101 11.00000 -1.20000
AFIX 0
C9 1 0.369396 0.442233 0.362769 11.00000 0.01745 0.02201 =
0.02322 -0.00520 0.00303 -0.01168
AFIX 23
H9A 2 0.365947 0.370394 0.323599 11.00000 -1.20000
H9B 2 0.258173 0.529096 0.359238 11.00000 -1.20000
AFIX 0
C10 1 0.504671 0.563535 0.224676 11.00000 0.01558 0.01811 =
0.01921 -0.00423 -0.00022 -0.00881
C11 1 0.663657 0.603825 0.203539 11.00000 0.01650 0.01691 =
0.02143 -0.00270 -0.00095 -0.00877
C12 1 0.711700 0.675926 0.263389 11.00000 0.01740 0.01826 =
0.02410 -0.00615 0.00079 -0.00766
AFIX 43
H12 2 0.651338 0.692001 0.318582 11.00000 -1.20000
AFIX 0
C13 1 0.847006 0.724590 0.243206 11.00000 0.02087 0.01956 =
0.02921 -0.00615 -0.00256 -0.01072
AFIX 43
H13 2 0.879447 0.771938 0.285078 11.00000 -1.20000
AFIX 0
C14 1 0.934355 0.704188 0.162339 11.00000 0.01752 0.02002 =
0.03366 -0.00330 -0.00079 -0.01120
AFIX 43
H14 2 1.025696 0.738796 0.148115 11.00000 -1.20000
AFIX 0
C15 1 0.887768 0.632876 0.102126 11.00000 0.02167 0.02528 =
0.02460 -0.00562 0.00543 -0.01304
AFIX 43
H15 2 0.947644 0.618265 0.046627 11.00000 -1.20000
AFIX 0
C16 1 0.753244 0.582569 0.122855 11.00000 0.02006 0.02475 =
0.02167 -0.00607 -0.00021 -0.01172
AFIX 43
H16 2 0.722540 0.533305 0.081439 11.00000 -1.20000
AFIX 0
C17 1 0.360267 0.722117 0.187565 11.00000 0.01457 0.01858 =
0.02399 -0.00482 0.00037 -0.01129
C18 1 0.258304 0.813886 0.246440 11.00000 0.01845 0.02207 =
0.02252 -0.00623 0.00055 -0.01245
AFIX 43
H18 2 0.275327 0.774952 0.311884 11.00000 -1.20000
AFIX 0
C19 1 0.132037 0.961399 0.211380 11.00000 0.01690 0.02265 =
0.03231 -0.01200 0.00311 -0.01069
AFIX 43
H19 2 0.061242 1.020000 0.252796 11.00000 -1.20000
AFIX 0
C20 1 0.109716 1.022542 0.116335 11.00000 0.01870 0.01892 =
0.03374 -0.00393 -0.00228 -0.01017
AFIX 43
H20 2 0.024167 1.123444 0.092126 11.00000 -1.20000
AFIX 0
C21 1 0.213683 0.935012 0.056318 11.00000 0.02184 0.02380 =
0.02520 -0.00254 -0.00074 -0.01264
AFIX 43
H21 2 0.200322 0.977467 -0.009051 11.00000 -1.20000
AFIX 0
C22 1 0.336464 0.786395 0.091400 11.00000 0.01787 0.02135 =
0.02538 -0.00752 0.00228 -0.01032
AFIX 43
H22 2 0.405477 0.727243 0.049682 11.00000 -1.20000
AFIX 0
C23 1 0.509090 0.425248 0.182051 11.00000 0.01921 0.01936 =
0.01918 -0.00387 0.00141 -0.01121
C24 1 0.367213 0.423435 0.143686 11.00000 0.01925 0.02177 =
0.02256 -0.00513 0.00036 -0.00940
AFIX 43
H24 2 0.269944 0.518576 0.131544 11.00000 -1.20000
AFIX 0
C25 1 0.366183 0.284128 0.122944 11.00000 0.02666 0.02979 =
0.02176 -0.00744 0.00083 -0.01885
AFIX 43
H25 2 0.268262 0.285222 0.097152 11.00000 -1.20000
AFIX 0
C26 1 0.505990 0.144859 0.139534 11.00000 0.03386 0.02230 =
0.02353 -0.00804 0.00427 -0.01688
AFIX 43
H26 2 0.504615 0.049794 0.125918 11.00000 -1.20000
AFIX 0
C27 1 0.649356 0.145156 0.176510 11.00000 0.02726 0.02193 =
0.02552 -0.00531 0.00194 -0.00979
AFIX 43
H27 2 0.746977 0.050283 0.187519 11.00000 -1.20000
AFIX 0
C28 1 0.649606 0.284090 0.197279 11.00000 0.01948 0.02374 =
0.02380 -0.00599 0.00125 -0.01157
AFIX 43
H28 2 0.748151 0.282709 0.222506 11.00000 -1.20000
AFIX 0
HKLF 4
REM saltry-yes_90k_a.res in P-1
REM R1 = 0.0528 for 3538 Fo > 4sig(Fo) and 0.0676 for all 4829 data
REM 285 parameters refined using 0 restraints
END
WGHT 0.0763 0.0665
REM Highest difference peak 0.357, deepest hole -0.294, 1-sigma level 0.062
Q1 1 0.5137 0.5218 0.2835 11.00000 0.05 0.27
Q2 1 0.6229 0.1757 0.4147 11.00000 0.05 0.27
Q3 1 0.5020 0.4964 0.1958 11.00000 0.05 0.25
Q4 1 0.8059 -0.0608 0.5136 11.00000 0.05 0.25
Q5 1 0.2937 0.9112 0.0734 11.00000 0.05 0.24
Q6 1 0.3816 0.4085 0.4189 11.00000 0.05 0.24
Q7 1 0.8461 -0.2582 0.6297 11.00000 0.05 0.23
Q8 1 0.1533 0.9922 0.1645 11.00000 0.05 0.23
Q9 1 0.6986 0.2636 0.4194 11.00000 0.05 0.22
Q10 1 0.9982 -0.2094 0.7068 11.00000 0.05 0.21
Q11 1 0.9051 0.6851 0.0270 11.00000 0.05 0.21
Q12 1 0.7315 0.5704 0.1650 11.00000 0.05 0.21
Q13 1 0.9845 -0.3122 0.6078 11.00000 0.05 0.20
Q14 1 0.5759 0.1016 0.3280 11.00000 0.05 0.20
Q15 1 0.8911 0.6184 0.3350 11.00000 0.05 0.20
Q16 1 0.4392 0.6371 0.2026 11.00000 0.05 0.20
Q17 1 0.6529 -0.0088 0.5331 11.00000 0.05 0.20
Q18 1 0.7674 0.8740 0.3321 11.00000 0.05 0.20
Q19 1 0.1827 1.0075 -0.0274 11.00000 0.05 0.20
Q20 1 0.7672 0.2623 0.3024 11.00000 0.05 0.19
REM The information below was added by Olex2.
REM
REM R1 = 0.0528 for 3538 Fo > 4sig(Fo) and 0.0676 for all 11182 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.36, deepest hole -0.29
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0676
REM R1_gt = 0.0528
REM wR_ref = 0.1519
REM GOOF = 1.066
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 11182
REM Reflections_gt = 3538
REM Parameters = n/a
REM Hole = -0.29
REM Peak = 0.36
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# 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_ligand-try
_database_code_depnum_ccdc_archive 'CCDC 1555565'
_audit_update_record
;
2017-06-12 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_audit_creation_date 2015-05-07
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_shelxl_version_number 2014/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety '0.5(C56 H52 N4 O2 Zn)'
_chemical_formula_sum 'C28 H26 Br0 N2 O Zn0.25'
_chemical_formula_weight 422.85
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 13.339(4)
_cell_length_b 13.342(4)
_cell_length_c 15.359(5)
_cell_angle_alpha 95.814(3)
_cell_angle_beta 109.924(7)
_cell_angle_gamma 112.425(9)
_cell_volume 2289.8(12)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 3179
_cell_measurement_temperature 293
_cell_measurement_theta_max 27.4
_cell_measurement_theta_min 3.1
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.328
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.913
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_process_details 'Blessing 1995'
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'metallic yellowish yellow'
_exptl_crystal_colour_lustre metallic
_exptl_crystal_colour_modifier yellowish
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.227
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description Prism
_exptl_crystal_F_000 894
_exptl_crystal_size_max 0.1
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.1
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0908
_diffrn_reflns_av_unetI/netI 0.1280
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 25027
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.488
_diffrn_reflns_theta_min 3.083
_diffrn_ambient_temperature 293
_diffrn_detector CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
scan:
Number of images: 629
Slice: -69.0000 - 119.7000
Image width: 0.3000
Exp time: 15.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 54.0000
Phi: 240.0000
XTD: 49.8600
2theta: 29.8900
scan:
Number of images: 629
Slice: -69.0000 - 119.7000
Image width: 0.3000
Exp time: 15.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 54.0000
Phi: 120.0000
XTD: 49.8600
2theta: 29.8900
scan:
Number of images: 629
Slice: -69.0000 - 119.7000
Image width: 0.3000
Exp time: 15.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 54.0000
Phi: 0.0000
XTD: 49.8600
2theta: 29.8900
;
_diffrn_measurement_device
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type
;
Rigaku Mercury375R (2x2 bin mode)
;
_diffrn_measurement_method 'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type d*Trek
_diffrn_orient_matrix_UB_11 -0.081145
_diffrn_orient_matrix_UB_12 -0.036610
_diffrn_orient_matrix_UB_13 -0.001266
_diffrn_orient_matrix_UB_21 -0.004416
_diffrn_orient_matrix_UB_22 -0.080346
_diffrn_orient_matrix_UB_23 -0.024510
_diffrn_orient_matrix_UB_31 -0.016681
_diffrn_orient_matrix_UB_32 -0.037157
_diffrn_orient_matrix_UB_33 0.059184
_diffrn_radiation_monochromator 'Graphite Monochromator'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71075
_diffrn_source 'Sealed Tube'
_diffrn_source_current 12.0
_diffrn_source_power 0.6
_diffrn_source_voltage 50.0
_diffrn_special_details
;
?
;
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4957
_reflns_number_total 10469
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2008)'
_computing_structure_solution 'ShelXT (Sheldrick, 2008)'
_refine_diff_density_max 0.464
_refine_diff_density_min -0.379
_refine_diff_density_rms 0.067
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.054
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 568
_refine_ls_number_reflns 10469
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1796
_refine_ls_R_factor_gt 0.0853
_refine_ls_restrained_S_all 1.054
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+1.6729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1444
_refine_ls_wR_factor_ref 0.1919
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
N006(H00A,H00B), N007(H00C,H00D), C00A(H00E,H00F), C00J(H00G,H00I), C00N(H00J,
H00K), C00P(H00M,H00N)
2.b Aromatic/amide H refined with riding coordinates:
C008(H008), C00H(H00H), C00L(H00L), C00Q(H00Q), C00S(H00S), C00T(H00T),
C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y), C00Z(H00Z),
C010(H010), C011(H011), C012(H012), C013(H013), C014(H014), C015(H015),
C016(H016), C017(H017), C018(H018), C019(H019), C01A(H01A), C01B(H01B),
C01C(H01C), C01D(H01D), C01E(H01E), C01F(H01F), C01G(H01G), C01H(H01H),
C01I(H01I), C01J(H01J), C01K(H01K), C01L(H01L), C01M(H01M), C01N(H01N),
C01O(H01O), C01P(H01P), C01Q(H01Q), C01R(H01R)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
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
Zn01 Zn 0.55582(5) 0.50388(5) 0.82630(4) 0.0481(2) Uani 1 1 d . . . . .
O002 O 0.7026(3) 0.6216(3) 0.9203(2) 0.0534(9) Uani 1 1 d . . . . .
O003 O 0.4421(3) 0.5607(3) 0.7725(2) 0.0485(8) Uani 1 1 d . . . . .
N004 N 0.4615(3) 0.3977(3) 0.8827(3) 0.0409(9) Uani 1 1 d . . . . .
N005 N 0.6190(3) 0.4582(3) 0.7373(3) 0.0428(9) Uani 1 1 d . . . . .
N006 N 0.5229(3) 0.1489(3) 0.8935(3) 0.0450(10) Uani 1 1 d . . . . .
H00A H 0.4737 0.1042 0.9153 0.054 Uiso 1 1 calc R . . . .
H00B H 0.5904 0.1939 0.9442 0.054 Uiso 1 1 calc R . . . .
N007 N 0.3738(3) 0.3956(3) 0.5827(3) 0.0462(10) Uani 1 1 d . . . . .
H00C H 0.4182 0.4347 0.5547 0.055 Uiso 1 1 calc R . . . .
H00D H 0.3848 0.4439 0.6334 0.055 Uiso 1 1 calc R . . . .
C008 C 0.3719(4) 0.4065(4) 0.8909(3) 0.0432(11) Uani 1 1 d . . . . .
H008 H 0.3343 0.3580 0.9215 0.052 Uiso 1 1 calc R . . . .
C009 C 0.8047(4) 0.6560(4) 0.9130(4) 0.0486(12) Uani 1 1 d . . . . .
C00A C 0.4974(4) 0.3173(4) 0.9252(3) 0.0449(12) Uani 1 1 d . . . . .
H00E H 0.4555 0.2904 0.9650 0.054 Uiso 1 1 calc R . . . .
H00F H 0.5821 0.3547 0.9659 0.054 Uiso 1 1 calc R . . . .
C00B C 0.3229(4) 0.4818(4) 0.8588(3) 0.0435(11) Uani 1 1 d . . . . .
C00C C 0.2472(4) 0.3473(4) 0.5142(3) 0.0444(11) Uani 1 1 d . . . . .
C00D C 0.3597(4) 0.5551(4) 0.8039(3) 0.0441(11) Uani 1 1 d . . . . .
C00E C 0.8217(4) 0.6086(4) 0.8360(4) 0.0482(12) Uani 1 1 d . . . . .
C00F C 0.5959(4) 0.0081(4) 0.8938(4) 0.0438(12) Uani 1 1 d . . . . .
C00G C 0.1705(4) 0.2780(4) 0.5622(3) 0.0473(12) Uani 1 1 d . . . . .
C00H C 0.7295(4) 0.5156(4) 0.7555(4) 0.0490(12) Uani 1 1 d . . . . .
H00H H 0.7534 0.4936 0.7098 0.059 Uiso 1 1 calc R . . . .
C00I C 0.2320(4) 0.2785(4) 0.4207(3) 0.0473(12) Uani 1 1 d . . . . .
C00J C 0.4708(4) 0.2179(4) 0.8486(3) 0.0467(12) Uani 1 1 d . . . . .
H00G H 0.3854 0.1737 0.8137 0.056 Uiso 1 1 calc R . . . .
H00I H 0.5035 0.2448 0.8033 0.056 Uiso 1 1 calc R . . . .
C00K C 0.5494(4) 0.0781(4) 0.8333(3) 0.0465(12) Uani 1 1 d . . . . .
C00L C 0.2315(4) 0.4809(4) 0.8864(4) 0.0535(13) Uani 1 1 d . . . . .
H00L H 0.2058 0.4311 0.9211 0.064 Uiso 1 1 calc R . . . .
C00M C 0.2185(4) 0.4448(4) 0.4921(3) 0.0491(12) Uani 1 1 d . . . . .
C00N C 0.5504(4) 0.3628(4) 0.6507(3) 0.0504(13) Uani 1 1 d . . . . .
H00J H 0.5731 0.3032 0.6637 0.061 Uiso 1 1 calc R . . . .
H00K H 0.5716 0.3868 0.5993 0.061 Uiso 1 1 calc R . . . .
C00O C 0.6546(4) 0.1537(4) 0.8129(4) 0.0498(13) Uani 1 1 d . . . . .
C00P C 0.4179(4) 0.3164(4) 0.6171(3) 0.0474(12) Uani 1 1 d . . . . .
H00M H 0.3796 0.2480 0.5657 0.057 Uiso 1 1 calc R . . . .
H00N H 0.3966 0.2972 0.6696 0.057 Uiso 1 1 calc R . . . .
C00Q C 0.7290(5) 0.2636(4) 0.8667(4) 0.0582(14) Uani 1 1 d . . . . .
H00Q H 0.7132 0.2941 0.9147 0.070 Uiso 1 1 calc R . . . .
C00R C 0.4352(5) 0.0060(4) 0.7427(4) 0.0522(13) Uani 1 1 d . . . . .
C00S C 0.1802(4) 0.5513(4) 0.8634(4) 0.0573(14) Uani 1 1 d . . . . .
H00S H 0.1212 0.5506 0.8830 0.069 Uiso 1 1 calc R . . . .
C00T C 0.6630(4) 0.0525(4) 0.9919(4) 0.0537(13) Uani 1 1 d . . . . .
H00T H 0.6710 0.1210 1.0218 0.064 Uiso 1 1 calc R . . . .
C00U C 0.3048(4) 0.6255(4) 0.7802(4) 0.0551(13) Uani 1 1 d . . . . .
H00U H 0.3271 0.6741 0.7437 0.066 Uiso 1 1 calc R . . . .
C00V C 0.7182(4) -0.0031(5) 1.0461(4) 0.0604(14) Uani 1 1 d . . . . .
H00V H 0.7647 0.0292 1.1116 0.072 Uiso 1 1 calc R . . . .
C00W C 0.3018(5) 0.5546(4) 0.5256(4) 0.0591(14) Uani 1 1 d . . . . .
H00W H 0.3805 0.5724 0.5639 0.071 Uiso 1 1 calc R . . . .
C00X C 0.7050(5) -0.1056(5) 1.0038(5) 0.0650(16) Uani 1 1 d . . . . .
H00X H 0.7422 -0.1428 1.0405 0.078 Uiso 1 1 calc R . . . .
C00Y C 0.1317(4) 0.3285(5) 0.6188(4) 0.0558(14) Uani 1 1 d . . . . .
H00Y H 0.1450 0.4027 0.6223 0.067 Uiso 1 1 calc R . . . .
C00Z C 0.5831(5) -0.0959(4) 0.8532(4) 0.0604(14) Uani 1 1 d . . . . .
H00Z H 0.5373 -0.1283 0.7876 0.072 Uiso 1 1 calc R . . . .
C010 C 0.1235(5) 0.1902(4) 0.3572(4) 0.0632(15) Uani 1 1 d . . . . .
H010 H 0.0581 0.1700 0.3727 0.076 Uiso 1 1 calc R . . . .
C011 C 0.1494(5) 0.1677(5) 0.5608(4) 0.0603(14) Uani 1 1 d . . . . .
H011 H 0.1745 0.1314 0.5239 0.072 Uiso 1 1 calc R . . . .
C012 C 0.3255(5) 0.3076(5) 0.3920(4) 0.0604(14) Uani 1 1 d . . . . .
H012 H 0.3981 0.3684 0.4315 0.073 Uiso 1 1 calc R . . . .
C013 C 0.3439(5) -0.0815(4) 0.7500(4) 0.0630(15) Uani 1 1 d . . . . .
H013 H 0.3568 -0.1019 0.8075 0.076 Uiso 1 1 calc R . . . .
C014 C 0.9066(5) 0.7455(5) 0.9873(4) 0.0645(15) Uani 1 1 d . . . . .
H014 H 0.8994 0.7790 1.0395 0.077 Uiso 1 1 calc R . . . .
C015 C 0.2175(5) 0.6235(5) 0.8105(4) 0.0626(15) Uani 1 1 d . . . . .
H015 H 0.1833 0.6720 0.7949 0.075 Uiso 1 1 calc R . . . .
C016 C 0.6363(5) -0.1531(5) 0.9069(5) 0.0685(17) Uani 1 1 d . . . . .
H016 H 0.6258 -0.2231 0.8778 0.082 Uiso 1 1 calc R . . . .
C017 C 0.1033(5) 0.4231(5) 0.4346(4) 0.0712(17) Uani 1 1 d . . . . .
H017 H 0.0451 0.3488 0.4094 0.085 Uiso 1 1 calc R . . . .
C018 C 0.0735(5) 0.2696(6) 0.6699(4) 0.0708(17) Uani 1 1 d . . . . .
H018 H 0.0474 0.3049 0.7065 0.085 Uiso 1 1 calc R . . . .
C019 C 1.0310(5) 0.7357(5) 0.9082(5) 0.0760(18) Uani 1 1 d . . . . .
H019 H 1.1060 0.7618 0.9074 0.091 Uiso 1 1 calc R . . . .
C01A C 1.0155(5) 0.7836(5) 0.9837(5) 0.0745(18) Uani 1 1 d . . . . .
H01A H 1.0807 0.8431 1.0332 0.089 Uiso 1 1 calc R . . . .
C01B C 0.3138(6) 0.2497(5) 0.3073(4) 0.0713(17) Uani 1 1 d . . . . .
H01B H 0.3784 0.2706 0.2907 0.086 Uiso 1 1 calc R . . . .
C01C C 0.9347(5) 0.6494(5) 0.8349(4) 0.0668(16) Uani 1 1 d . . . . .
H01C H 0.9443 0.6173 0.7835 0.080 Uiso 1 1 calc R . . . .
C01D C 0.4118(5) 0.0342(5) 0.6561(4) 0.0708(17) Uani 1 1 d . . . . .
H01D H 0.4712 0.0935 0.6490 0.085 Uiso 1 1 calc R . . . .
C01E C 0.2713(6) 0.6403(5) 0.5036(5) 0.0773(18) Uani 1 1 d . . . . .
H01E H 0.3297 0.7145 0.5271 0.093 Uiso 1 1 calc R . . . .
C01F C 0.8266(5) 0.3295(5) 0.8509(5) 0.0775(18) Uani 1 1 d . . . . .
H01F H 0.8753 0.4037 0.8876 0.093 Uiso 1 1 calc R . . . .
C01G C 0.1116(6) 0.1323(5) 0.2718(4) 0.0764(18) Uani 1 1 d . . . . .
H01G H 0.0383 0.0735 0.2306 0.092 Uiso 1 1 calc R . . . .
C01H C 0.1580(7) 0.6173(6) 0.4488(5) 0.0811(19) Uani 1 1 d . . . . .
H01H H 0.1382 0.6753 0.4350 0.097 Uiso 1 1 calc R . . . .
C01I C 0.2322(6) -0.1402(5) 0.6732(6) 0.091(2) Uani 1 1 d . . . . .
H01I H 0.1720 -0.1993 0.6798 0.110 Uiso 1 1 calc R . . . .
C01J C 0.0917(5) 0.1103(5) 0.6129(5) 0.0755(18) Uani 1 1 d . . . . .
H01J H 0.0788 0.0363 0.6106 0.091 Uiso 1 1 calc R . . . .
C01K C 0.3000(7) -0.0254(6) 0.5790(5) 0.092(2) Uani 1 1 d . . . . .
H01K H 0.2866 -0.0063 0.5209 0.110 Uiso 1 1 calc R . . . .
C01L C 0.2061(7) 0.1601(6) 0.2465(4) 0.0810(19) Uani 1 1 d . . . . .
H01L H 0.1978 0.1194 0.1895 0.097 Uiso 1 1 calc R . . . .
C01M C 0.0534(5) 0.1608(6) 0.6677(5) 0.0800(19) Uani 1 1 d . . . . .
H01M H 0.0147 0.1222 0.7027 0.096 Uiso 1 1 calc R . . . .
C01N C 0.0718(6) 0.5074(6) 0.4134(5) 0.085(2) Uani 1 1 d . . . . .
H01N H -0.0068 0.4904 0.3756 0.102 Uiso 1 1 calc R . . . .
C01O C 0.8511(7) 0.2853(7) 0.7812(6) 0.098(2) Uani 1 1 d . . . . .
H01O H 0.9157 0.3298 0.7693 0.118 Uiso 1 1 calc R . . . .
C01P C 0.2112(7) -0.1109(6) 0.5882(6) 0.098(3) Uani 1 1 d . . . . .
H01P H 0.1367 -0.1493 0.5372 0.118 Uiso 1 1 calc R . . . .
C01Q C 0.7815(7) 0.1765(7) 0.7291(6) 0.105(3) Uani 1 1 d . . . . .
H01Q H 0.7997 0.1466 0.6825 0.126 Uiso 1 1 calc R . . . .
C01R C 0.6836(6) 0.1088(6) 0.7444(4) 0.0804(19) Uani 1 1 d . . . . .
H01R H 0.6376 0.0340 0.7090 0.096 Uiso 1 1 calc 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
Zn01 0.0463(3) 0.0480(4) 0.0551(4) 0.0142(3) 0.0247(3) 0.0224(3)
O002 0.049(2) 0.054(2) 0.054(2) 0.0085(17) 0.0227(17) 0.0195(18)
O003 0.055(2) 0.051(2) 0.054(2) 0.0213(17) 0.0293(17) 0.0295(18)
N004 0.047(2) 0.033(2) 0.046(2) 0.0098(18) 0.0196(19) 0.0210(19)
N005 0.040(2) 0.043(2) 0.047(2) 0.0140(19) 0.0161(19) 0.021(2)
N006 0.040(2) 0.042(2) 0.047(2) 0.0115(19) 0.0131(19) 0.016(2)
N007 0.048(2) 0.043(2) 0.049(2) 0.0125(19) 0.025(2) 0.016(2)
C008 0.045(3) 0.037(3) 0.043(3) 0.005(2) 0.018(2) 0.016(2)
C009 0.046(3) 0.045(3) 0.058(3) 0.023(3) 0.022(3) 0.020(3)
C00A 0.052(3) 0.039(3) 0.045(3) 0.012(2) 0.016(2) 0.024(2)
C00B 0.043(3) 0.037(3) 0.048(3) 0.006(2) 0.018(2) 0.017(2)
C00C 0.037(3) 0.046(3) 0.046(3) 0.009(2) 0.016(2) 0.016(2)
C00D 0.043(3) 0.044(3) 0.042(3) 0.005(2) 0.014(2) 0.020(2)
C00E 0.039(3) 0.048(3) 0.051(3) 0.016(3) 0.013(2) 0.016(3)
C00F 0.040(3) 0.034(3) 0.057(3) 0.012(2) 0.022(2) 0.015(2)
C00G 0.039(3) 0.046(3) 0.051(3) 0.008(2) 0.018(2) 0.015(2)
C00H 0.055(3) 0.053(3) 0.054(3) 0.023(3) 0.030(3) 0.030(3)
C00I 0.058(3) 0.045(3) 0.042(3) 0.009(2) 0.020(3) 0.027(3)
C00J 0.049(3) 0.041(3) 0.052(3) 0.014(2) 0.018(2) 0.024(3)
C00K 0.049(3) 0.041(3) 0.050(3) 0.009(2) 0.020(2) 0.021(3)
C00L 0.044(3) 0.058(3) 0.052(3) 0.008(3) 0.016(3) 0.021(3)
C00M 0.048(3) 0.055(3) 0.046(3) 0.010(3) 0.018(2) 0.026(3)
C00N 0.050(3) 0.053(3) 0.051(3) 0.010(3) 0.020(3) 0.027(3)
C00O 0.060(3) 0.055(3) 0.056(3) 0.026(3) 0.031(3) 0.037(3)
C00P 0.048(3) 0.039(3) 0.049(3) 0.011(2) 0.014(2) 0.018(2)
C00Q 0.053(3) 0.048(3) 0.074(4) 0.022(3) 0.028(3) 0.021(3)
C00R 0.057(3) 0.035(3) 0.055(3) -0.002(2) 0.018(3) 0.019(3)
C00S 0.051(3) 0.063(4) 0.062(4) 0.008(3) 0.024(3) 0.032(3)
C00T 0.044(3) 0.044(3) 0.067(4) 0.014(3) 0.016(3) 0.019(3)
C00U 0.059(3) 0.052(3) 0.063(3) 0.018(3) 0.026(3) 0.031(3)
C00V 0.054(3) 0.060(4) 0.069(4) 0.026(3) 0.021(3) 0.029(3)
C00W 0.060(3) 0.056(4) 0.072(4) 0.027(3) 0.030(3) 0.031(3)
C00X 0.065(4) 0.064(4) 0.094(5) 0.047(4) 0.043(4) 0.042(3)
C00Y 0.047(3) 0.056(3) 0.053(3) -0.001(3) 0.020(3) 0.017(3)
C00Z 0.074(4) 0.046(3) 0.069(4) 0.013(3) 0.034(3) 0.031(3)
C010 0.067(4) 0.056(3) 0.059(4) 0.010(3) 0.023(3) 0.024(3)
C011 0.064(4) 0.056(4) 0.063(4) 0.013(3) 0.035(3) 0.022(3)
C012 0.064(4) 0.067(4) 0.058(4) 0.016(3) 0.032(3) 0.031(3)
C013 0.054(3) 0.050(3) 0.064(4) 0.004(3) 0.008(3) 0.019(3)
C014 0.057(4) 0.058(4) 0.072(4) 0.014(3) 0.021(3) 0.024(3)
C015 0.061(4) 0.067(4) 0.072(4) 0.015(3) 0.023(3) 0.045(3)
C016 0.091(4) 0.060(4) 0.094(5) 0.036(4) 0.055(4) 0.054(4)
C017 0.070(4) 0.072(4) 0.056(4) 0.007(3) 0.002(3) 0.041(4)
C018 0.061(4) 0.089(5) 0.060(4) 0.009(4) 0.036(3) 0.025(4)
C019 0.039(3) 0.067(4) 0.109(5) 0.016(4) 0.031(4) 0.013(3)
C01A 0.042(3) 0.062(4) 0.090(5) 0.007(3) 0.012(3) 0.012(3)
C01B 0.088(5) 0.080(4) 0.064(4) 0.016(3) 0.042(4) 0.046(4)
C01C 0.044(3) 0.067(4) 0.091(4) 0.020(3) 0.036(3) 0.021(3)
C01D 0.082(4) 0.055(4) 0.063(4) 0.007(3) 0.016(3) 0.032(3)
C01E 0.086(5) 0.058(4) 0.091(5) 0.024(4) 0.032(4) 0.037(4)
C01F 0.062(4) 0.073(4) 0.108(5) 0.043(4) 0.045(4) 0.028(4)
C01G 0.097(5) 0.063(4) 0.053(4) 0.003(3) 0.025(4) 0.029(4)
C01H 0.118(6) 0.083(5) 0.073(5) 0.032(4) 0.043(4) 0.069(5)
C01I 0.059(4) 0.063(4) 0.105(6) -0.006(4) 0.002(4) 0.017(4)
C01J 0.074(4) 0.056(4) 0.094(5) 0.027(4) 0.041(4) 0.020(3)
C01K 0.125(6) 0.084(5) 0.054(4) 0.009(4) 0.010(4) 0.061(5)
C01L 0.116(6) 0.077(5) 0.060(4) 0.013(4) 0.041(4) 0.050(5)
C01M 0.070(4) 0.091(5) 0.075(4) 0.029(4) 0.040(4) 0.020(4)
C01N 0.080(5) 0.103(6) 0.073(4) 0.017(4) 0.012(4) 0.061(5)
C01O 0.089(5) 0.109(6) 0.128(7) 0.063(6) 0.074(5) 0.041(5)
C01P 0.094(6) 0.074(5) 0.081(5) -0.012(4) -0.015(4) 0.045(5)
C01Q 0.121(7) 0.116(7) 0.119(6) 0.037(5) 0.093(6) 0.053(6)
C01R 0.090(5) 0.087(5) 0.085(5) 0.027(4) 0.056(4) 0.042(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
Zn01 O002 1.911(3) . ?
Zn01 O003 1.926(3) . ?
Zn01 N004 1.993(4) . ?
Zn01 N005 1.989(4) . ?
O002 C009 1.309(5) . ?
O003 C00D 1.324(5) . ?
N004 C008 1.292(5) . ?
N004 C00A 1.457(5) . ?
N005 C00H 1.284(5) . ?
N005 C00N 1.472(6) . ?
N006 H00A 0.8900 . ?
N006 H00B 0.8900 . ?
N006 C00J 1.449(5) . ?
N006 C00K 1.473(5) . ?
N007 H00C 0.8900 . ?
N007 H00D 0.8900 . ?
N007 C00C 1.482(5) . ?
N007 C00P 1.454(5) . ?
C008 H008 0.9300 . ?
C008 C00B 1.435(6) . ?
C009 C00E 1.411(7) . ?
C009 C014 1.417(7) . ?
C00A H00E 0.9700 . ?
C00A H00F 0.9700 . ?
C00A C00J 1.519(6) . ?
C00B C00D 1.411(6) . ?
C00B C00L 1.416(6) . ?
C00C C00G 1.541(6) . ?
C00C C00I 1.530(6) . ?
C00C C00M 1.527(6) . ?
C00D C00U 1.402(6) . ?
C00E C00H 1.439(7) . ?
C00E C01C 1.401(6) . ?
C00F C00K 1.531(6) . ?
C00F C00T 1.384(6) . ?
C00F C00Z 1.385(6) . ?
C00G C00Y 1.389(6) . ?
C00G C011 1.385(7) . ?
C00H H00H 0.9300 . ?
C00I C010 1.392(7) . ?
C00I C012 1.393(7) . ?
C00J H00G 0.9700 . ?
C00J H00I 0.9700 . ?
C00K C00O 1.539(7) . ?
C00K C00R 1.532(7) . ?
C00L H00L 0.9300 . ?
C00L C00S 1.368(6) . ?
C00M C00W 1.364(7) . ?
C00M C017 1.382(7) . ?
C00N H00J 0.9700 . ?
C00N H00K 0.9700 . ?
C00N C00P 1.500(6) . ?
C00O C00Q 1.379(7) . ?
C00O C01R 1.394(7) . ?
C00P H00M 0.9700 . ?
C00P H00N 0.9700 . ?
C00Q H00Q 0.9300 . ?
C00Q C01F 1.383(7) . ?
C00R C013 1.376(7) . ?
C00R C01D 1.385(7) . ?
C00S H00S 0.9300 . ?
C00S C015 1.379(7) . ?
C00T H00T 0.9300 . ?
C00T C00V 1.383(6) . ?
C00U H00U 0.9300 . ?
C00U C015 1.386(7) . ?
C00V H00V 0.9300 . ?
C00V C00X 1.370(7) . ?
C00W H00W 0.9300 . ?
C00W C01E 1.389(7) . ?
C00X H00X 0.9300 . ?
C00X C016 1.376(8) . ?
C00Y H00Y 0.9300 . ?
C00Y C018 1.382(7) . ?
C00Z H00Z 0.9300 . ?
C00Z C016 1.381(7) . ?
C010 H010 0.9300 . ?
C010 C01G 1.379(7) . ?
C011 H011 0.9300 . ?
C011 C01J 1.384(7) . ?
C012 H012 0.9300 . ?
C012 C01B 1.372(7) . ?
C013 H013 0.9300 . ?
C013 C01I 1.396(7) . ?
C014 H014 0.9300 . ?
C014 C01A 1.367(7) . ?
C015 H015 0.9300 . ?
C016 H016 0.9300 . ?
C017 H017 0.9300 . ?
C017 C01N 1.375(8) . ?
C018 H018 0.9300 . ?
C018 C01M 1.366(8) . ?
C019 H019 0.9300 . ?
C019 C01A 1.382(8) . ?
C019 C01C 1.367(7) . ?
C01A H01A 0.9300 . ?
C01B H01B 0.9300 . ?
C01B C01L 1.384(8) . ?
C01C H01C 0.9300 . ?
C01D H01D 0.9300 . ?
C01D C01K 1.399(8) . ?
C01E H01E 0.9300 . ?
C01E C01H 1.346(8) . ?
C01F H01F 0.9300 . ?
C01F C01O 1.363(9) . ?
C01G H01G 0.9300 . ?
C01G C01L 1.372(8) . ?
C01H H01H 0.9300 . ?
C01H C01N 1.377(8) . ?
C01I H01I 0.9300 . ?
C01I C01P 1.369(10) . ?
C01J H01J 0.9300 . ?
C01J C01M 1.364(8) . ?
C01K H01K 0.9300 . ?
C01K C01P 1.357(10) . ?
C01L H01L 0.9300 . ?
C01M H01M 0.9300 . ?
C01N H01N 0.9300 . ?
C01O H01O 0.9300 . ?
C01O C01Q 1.357(9) . ?
C01P H01P 0.9300 . ?
C01Q H01Q 0.9300 . ?
C01Q C01R 1.388(8) . ?
C01R H01R 0.9300 . ?
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
O002 Zn01 O003 110.90(14) . . ?
O002 Zn01 N004 113.45(15) . . ?
O002 Zn01 N005 97.92(15) . . ?
O003 Zn01 N004 96.43(14) . . ?
O003 Zn01 N005 115.07(14) . . ?
N005 Zn01 N004 123.61(15) . . ?
C009 O002 Zn01 124.7(3) . . ?
C00D O003 Zn01 122.8(3) . . ?
C008 N004 Zn01 119.6(3) . . ?
C008 N004 C00A 117.8(4) . . ?
C00A N004 Zn01 122.3(3) . . ?
C00H N005 Zn01 118.5(3) . . ?
C00H N005 C00N 115.6(4) . . ?
C00N N005 Zn01 125.9(3) . . ?
H00A N006 H00B 107.3 . . ?
C00J N006 H00A 108.0 . . ?
C00J N006 H00B 108.0 . . ?
C00J N006 C00K 117.0(4) . . ?
C00K N006 H00A 108.0 . . ?
C00K N006 H00B 108.0 . . ?
H00C N007 H00D 107.3 . . ?
C00C N007 H00C 108.1 . . ?
C00C N007 H00D 108.1 . . ?
C00P N007 H00C 108.1 . . ?
C00P N007 H00D 108.1 . . ?
C00P N007 C00C 116.7(4) . . ?
N004 C008 H008 115.9 . . ?
N004 C008 C00B 128.2(4) . . ?
C00B C008 H008 115.9 . . ?
O002 C009 C00E 124.4(5) . . ?
O002 C009 C014 118.9(5) . . ?
C00E C009 C014 116.6(5) . . ?
N004 C00A H00E 109.3 . . ?
N004 C00A H00F 109.3 . . ?
N004 C00A C00J 111.5(4) . . ?
H00E C00A H00F 108.0 . . ?
C00J C00A H00E 109.3 . . ?
C00J C00A H00F 109.3 . . ?
C00D C00B C008 125.0(4) . . ?
C00D C00B C00L 119.2(4) . . ?
C00L C00B C008 115.8(4) . . ?
N007 C00C C00G 108.1(4) . . ?
N007 C00C C00I 108.3(4) . . ?
N007 C00C C00M 107.8(4) . . ?
C00I C00C C00G 113.7(4) . . ?
C00M C00C C00G 110.9(4) . . ?
C00M C00C C00I 107.8(4) . . ?
O003 C00D C00B 124.1(4) . . ?
O003 C00D C00U 117.9(4) . . ?
C00U C00D C00B 118.0(4) . . ?
C009 C00E C00H 124.5(4) . . ?
C01C C00E C009 120.7(5) . . ?
C01C C00E C00H 114.8(5) . . ?
C00T C00F C00K 120.2(4) . . ?
C00T C00F C00Z 117.2(5) . . ?
C00Z C00F C00K 122.4(5) . . ?
C00Y C00G C00C 120.7(5) . . ?
C011 C00G C00C 121.9(4) . . ?
C011 C00G C00Y 116.9(5) . . ?
N005 C00H C00E 129.8(5) . . ?
N005 C00H H00H 115.1 . . ?
C00E C00H H00H 115.1 . . ?
C010 C00I C00C 122.3(5) . . ?
C010 C00I C012 116.8(5) . . ?
C012 C00I C00C 120.7(5) . . ?
N006 C00J C00A 109.5(4) . . ?
N006 C00J H00G 109.8 . . ?
N006 C00J H00I 109.8 . . ?
C00A C00J H00G 109.8 . . ?
C00A C00J H00I 109.8 . . ?
H00G C00J H00I 108.2 . . ?
N006 C00K C00F 107.5(4) . . ?
N006 C00K C00O 109.2(4) . . ?
N006 C00K C00R 108.1(4) . . ?
C00F C00K C00O 104.8(4) . . ?
C00F C00K C00R 113.1(4) . . ?
C00R C00K C00O 113.9(4) . . ?
C00B C00L H00L 119.1 . . ?
C00S C00L C00B 121.8(5) . . ?
C00S C00L H00L 119.1 . . ?
C00W C00M C00C 123.4(4) . . ?
C00W C00M C017 117.0(5) . . ?
C017 C00M C00C 119.7(5) . . ?
N005 C00N H00J 108.7 . . ?
N005 C00N H00K 108.7 . . ?
N005 C00N C00P 114.3(4) . . ?
H00J C00N H00K 107.6 . . ?
C00P C00N H00J 108.7 . . ?
C00P C00N H00K 108.7 . . ?
C00Q C00O C00K 121.8(5) . . ?
C00Q C00O C01R 117.8(5) . . ?
C01R C00O C00K 120.0(5) . . ?
N007 C00P C00N 112.4(4) . . ?
N007 C00P H00M 109.1 . . ?
N007 C00P H00N 109.1 . . ?
C00N C00P H00M 109.1 . . ?
C00N C00P H00N 109.1 . . ?
H00M C00P H00N 107.9 . . ?
C00O C00Q H00Q 119.2 . . ?
C00O C00Q C01F 121.6(6) . . ?
C01F C00Q H00Q 119.2 . . ?
C013 C00R C00K 119.1(5) . . ?
C013 C00R C01D 117.3(5) . . ?
C01D C00R C00K 123.0(5) . . ?
C00L C00S H00S 120.7 . . ?
C00L C00S C015 118.7(5) . . ?
C015 C00S H00S 120.7 . . ?
C00F C00T H00T 119.4 . . ?
C00V C00T C00F 121.2(5) . . ?
C00V C00T H00T 119.4 . . ?
C00D C00U H00U 119.6 . . ?
C015 C00U C00D 120.8(5) . . ?
C015 C00U H00U 119.6 . . ?
C00T C00V H00V 119.8 . . ?
C00X C00V C00T 120.4(5) . . ?
C00X C00V H00V 119.8 . . ?
C00M C00W H00W 119.4 . . ?
C00M C00W C01E 121.2(5) . . ?
C01E C00W H00W 119.4 . . ?
C00V C00X H00X 120.2 . . ?
C00V C00X C016 119.7(5) . . ?
C016 C00X H00X 120.2 . . ?
C00G C00Y H00Y 119.6 . . ?
C018 C00Y C00G 120.8(5) . . ?
C018 C00Y H00Y 119.6 . . ?
C00F C00Z H00Z 119.0 . . ?
C016 C00Z C00F 122.1(5) . . ?
C016 C00Z H00Z 119.0 . . ?
C00I C010 H010 119.5 . . ?
C01G C010 C00I 121.0(6) . . ?
C01G C010 H010 119.5 . . ?
C00G C011 H011 119.3 . . ?
C01J C011 C00G 121.5(5) . . ?
C01J C011 H011 119.3 . . ?
C00I C012 H012 118.9 . . ?
C01B C012 C00I 122.2(5) . . ?
C01B C012 H012 118.9 . . ?
C00R C013 H013 119.2 . . ?
C00R C013 C01I 121.6(6) . . ?
C01I C013 H013 119.2 . . ?
C009 C014 H014 119.4 . . ?
C01A C014 C009 121.1(6) . . ?
C01A C014 H014 119.4 . . ?
C00S C015 C00U 121.5(5) . . ?
C00S C015 H015 119.2 . . ?
C00U C015 H015 119.2 . . ?
C00X C016 C00Z 119.5(5) . . ?
C00X C016 H016 120.3 . . ?
C00Z C016 H016 120.3 . . ?
C00M C017 H017 118.9 . . ?
C01N C017 C00M 122.3(6) . . ?
C01N C017 H017 118.9 . . ?
C00Y C018 H018 119.3 . . ?
C01M C018 C00Y 121.5(6) . . ?
C01M C018 H018 119.3 . . ?
C01A C019 H019 120.5 . . ?
C01C C019 H019 120.5 . . ?
C01C C019 C01A 119.1(5) . . ?
C014 C01A C019 121.6(6) . . ?
C014 C01A H01A 119.2 . . ?
C019 C01A H01A 119.2 . . ?
C012 C01B H01B 120.0 . . ?
C012 C01B C01L 120.0(6) . . ?
C01L C01B H01B 120.0 . . ?
C00E C01C H01C 119.5 . . ?
C019 C01C C00E 120.9(6) . . ?
C019 C01C H01C 119.5 . . ?
C00R C01D H01D 119.5 . . ?
C00R C01D C01K 121.0(6) . . ?
C01K C01D H01D 119.5 . . ?
C00W C01E H01E 119.6 . . ?
C01H C01E C00W 120.8(6) . . ?
C01H C01E H01E 119.6 . . ?
C00Q C01F H01F 120.2 . . ?
C01O C01F C00Q 119.6(6) . . ?
C01O C01F H01F 120.2 . . ?
C010 C01G H01G 119.4 . . ?
C01L C01G C010 121.1(6) . . ?
C01L C01G H01G 119.4 . . ?
C01E C01H H01H 120.2 . . ?
C01E C01H C01N 119.6(6) . . ?
C01N C01H H01H 120.2 . . ?
C013 C01I H01I 120.0 . . ?
C01P C01I C013 120.0(7) . . ?
C01P C01I H01I 120.0 . . ?
C011 C01J H01J 119.5 . . ?
C01M C01J C011 120.9(6) . . ?
C01M C01J H01J 119.5 . . ?
C01D C01K H01K 119.7 . . ?
C01P C01K C01D 120.5(7) . . ?
C01P C01K H01K 119.7 . . ?
C01B C01L H01L 120.6 . . ?
C01G C01L C01B 118.8(6) . . ?
C01G C01L H01L 120.6 . . ?
C018 C01M H01M 120.8 . . ?
C01J C01M C018 118.4(6) . . ?
C01J C01M H01M 120.8 . . ?
C017 C01N C01H 119.2(6) . . ?
C017 C01N H01N 120.4 . . ?
C01H C01N H01N 120.4 . . ?
C01F C01O H01O 120.0 . . ?
C01Q C01O C01F 120.1(7) . . ?
C01Q C01O H01O 120.0 . . ?
C01I C01P H01P 120.2 . . ?
C01K C01P C01I 119.5(7) . . ?
C01K C01P H01P 120.2 . . ?
C01O C01Q H01Q 119.5 . . ?
C01O C01Q C01R 121.1(7) . . ?
C01R C01Q H01Q 119.5 . . ?
C00O C01R H01R 120.1 . . ?
C01Q C01R C00O 119.7(6) . . ?
C01Q C01R H01R 120.1 . . ?
_shelx_res_file
;
TITL ligand-try_a.res in P-1
CELL 0.71075 13.3391 13.3419 15.3591 95.814 109.924 112.425
ZERR 4 0.0042 0.0039 0.0046 0.003 0.007 0.009
LATT 1
SFAC C H N O Br Zn
UNIT 112 104 8 4 0 1
L.S. 10
PLAN 20
REM Old TITL Ligand-Try in P-1 #2
BOND $H
LIST 6
fmap 2 53
ACTA
REM D:/ARCLab/INAMUR/Ligand-Try_100K/structure/Ligand-Try.hkl
WGHT 0.049200 1.672900
FVAR 1.16779
ZN01 6 0.555817 0.503885 0.826304 11.00000 0.04628 0.04797 =
0.05512 0.01423 0.02473 0.02236
O002 4 0.702602 0.621578 0.920255 11.00000 0.04858 0.05404 =
0.05407 0.00853 0.02270 0.01951
O003 4 0.442054 0.560657 0.772485 11.00000 0.05459 0.05139 =
0.05355 0.02126 0.02925 0.02952
N004 3 0.461536 0.397654 0.882746 11.00000 0.04710 0.03337 =
0.04570 0.00984 0.01958 0.02102
N005 3 0.619035 0.458226 0.737347 11.00000 0.04038 0.04258 =
0.04703 0.01403 0.01611 0.02124
N006 3 0.522932 0.148859 0.893483 11.00000 0.03999 0.04182 =
0.04697 0.01147 0.01307 0.01640
AFIX 23
H00A 2 0.473672 0.104162 0.915345 11.00000 -1.20000
H00B 2 0.590378 0.193945 0.944162 11.00000 -1.20000
AFIX 0
N007 3 0.373838 0.395595 0.582693 11.00000 0.04795 0.04273 =
0.04860 0.01250 0.02489 0.01631
AFIX 23
H00C 2 0.418249 0.434703 0.554660 11.00000 -1.20000
H00D 2 0.384843 0.443918 0.633409 11.00000 -1.20000
AFIX 0
C008 1 0.371863 0.406517 0.890944 11.00000 0.04542 0.03732 =
0.04323 0.00548 0.01806 0.01625
AFIX 43
H008 2 0.334288 0.357994 0.921500 11.00000 -1.20000
AFIX 0
C009 1 0.804654 0.655983 0.912988 11.00000 0.04580 0.04473 =
0.05759 0.02262 0.02154 0.02013
C00A 1 0.497429 0.317333 0.925153 11.00000 0.05185 0.03921 =
0.04454 0.01177 0.01627 0.02416
AFIX 23
H00E 2 0.455530 0.290420 0.965019 11.00000 -1.20000
H00F 2 0.582076 0.354672 0.965914 11.00000 -1.20000
AFIX 0
C00B 1 0.322873 0.481802 0.858849 11.00000 0.04299 0.03749 =
0.04786 0.00593 0.01825 0.01743
C00C 1 0.247201 0.347318 0.514229 11.00000 0.03710 0.04595 =
0.04630 0.00860 0.01643 0.01617
C00D 1 0.359691 0.555054 0.803913 11.00000 0.04263 0.04373 =
0.04185 0.00474 0.01384 0.02003
C00E 1 0.821668 0.608610 0.835998 11.00000 0.03858 0.04831 =
0.05110 0.01612 0.01342 0.01644
C00F 1 0.595921 0.008123 0.893831 11.00000 0.04034 0.03376 =
0.05685 0.01230 0.02173 0.01450
C00G 1 0.170470 0.278046 0.562192 11.00000 0.03909 0.04627 =
0.05125 0.00843 0.01813 0.01528
C00H 1 0.729455 0.515560 0.755526 11.00000 0.05458 0.05302 =
0.05395 0.02342 0.02955 0.02978
AFIX 43
H00H 2 0.753424 0.493616 0.709761 11.00000 -1.20000
AFIX 0
C00I 1 0.232024 0.278516 0.420705 11.00000 0.05785 0.04535 =
0.04193 0.00920 0.01987 0.02742
C00J 1 0.470810 0.217947 0.848568 11.00000 0.04858 0.04121 =
0.05209 0.01411 0.01763 0.02418
AFIX 23
H00G 2 0.385380 0.173658 0.813652 11.00000 -1.20000
H00I 2 0.503527 0.244753 0.803263 11.00000 -1.20000
AFIX 0
C00K 1 0.549392 0.078054 0.833334 11.00000 0.04867 0.04059 =
0.05013 0.00905 0.02017 0.02079
C00L 1 0.231536 0.480935 0.886402 11.00000 0.04353 0.05811 =
0.05230 0.00784 0.01614 0.02106
AFIX 43
H00L 2 0.205800 0.431149 0.921072 11.00000 -1.20000
AFIX 0
C00M 1 0.218516 0.444776 0.492095 11.00000 0.04758 0.05506 =
0.04570 0.00963 0.01827 0.02564
C00N 1 0.550381 0.362838 0.650693 11.00000 0.04964 0.05302 =
0.05142 0.01024 0.02039 0.02682
AFIX 23
H00J 2 0.573106 0.303151 0.663666 11.00000 -1.20000
H00K 2 0.571610 0.386789 0.599261 11.00000 -1.20000
AFIX 0
C00O 1 0.654585 0.153678 0.812920 11.00000 0.05999 0.05494 =
0.05571 0.02646 0.03145 0.03703
C00P 1 0.417906 0.316421 0.617050 11.00000 0.04809 0.03864 =
0.04897 0.01056 0.01429 0.01814
AFIX 23
H00M 2 0.379642 0.247954 0.565703 11.00000 -1.20000
H00N 2 0.396630 0.297235 0.669630 11.00000 -1.20000
AFIX 0
C00Q 1 0.729008 0.263579 0.866660 11.00000 0.05328 0.04820 =
0.07417 0.02152 0.02763 0.02107
AFIX 43
H00Q 2 0.713171 0.294069 0.914673 11.00000 -1.20000
AFIX 0
C00R 1 0.435161 0.006036 0.742738 11.00000 0.05696 0.03504 =
0.05507 -0.00229 0.01803 0.01909
C00S 1 0.180150 0.551345 0.863398 11.00000 0.05061 0.06348 =
0.06217 0.00824 0.02357 0.03153
AFIX 43
H00S 2 0.121204 0.550579 0.883004 11.00000 -1.20000
AFIX 0
C00T 1 0.662963 0.052506 0.991865 11.00000 0.04370 0.04400 =
0.06692 0.01408 0.01589 0.01941
AFIX 43
H00T 2 0.670986 0.120997 1.021829 11.00000 -1.20000
AFIX 0
C00U 1 0.304766 0.625483 0.780196 11.00000 0.05854 0.05229 =
0.06273 0.01797 0.02563 0.03145
AFIX 43
H00U 2 0.327138 0.674112 0.743667 11.00000 -1.20000
AFIX 0
C00V 1 0.718232 -0.003108 1.046073 11.00000 0.05367 0.05984 =
0.06919 0.02598 0.02074 0.02862
AFIX 43
H00V 2 0.764663 0.029178 1.111559 11.00000 -1.20000
AFIX 0
C00W 1 0.301809 0.554590 0.525617 11.00000 0.05977 0.05628 =
0.07158 0.02706 0.02977 0.03115
AFIX 43
H00W 2 0.380497 0.572353 0.563890 11.00000 -1.20000
AFIX 0
C00X 1 0.704965 -0.105553 1.003826 11.00000 0.06542 0.06396 =
0.09418 0.04684 0.04323 0.04153
AFIX 43
H00X 2 0.742198 -0.142789 1.040491 11.00000 -1.20000
AFIX 0
C00Y 1 0.131682 0.328451 0.618761 11.00000 0.04733 0.05613 =
0.05342 -0.00143 0.02004 0.01736
AFIX 43
H00Y 2 0.145041 0.402744 0.622308 11.00000 -1.20000
AFIX 0
C00Z 1 0.583127 -0.095934 0.853173 11.00000 0.07376 0.04607 =
0.06895 0.01295 0.03371 0.03100
AFIX 43
H00Z 2 0.537285 -0.128344 0.787627 11.00000 -1.20000
AFIX 0
C010 1 0.123522 0.190240 0.357244 11.00000 0.06720 0.05616 =
0.05874 0.00972 0.02253 0.02438
AFIX 43
H010 2 0.058098 0.169989 0.372681 11.00000 -1.20000
AFIX 0
C011 1 0.149351 0.167722 0.560777 11.00000 0.06380 0.05622 =
0.06259 0.01311 0.03463 0.02152
AFIX 43
H011 2 0.174497 0.131413 0.523949 11.00000 -1.20000
AFIX 0
C012 1 0.325460 0.307638 0.391970 11.00000 0.06356 0.06681 =
0.05846 0.01568 0.03192 0.03066
AFIX 43
H012 2 0.398128 0.368381 0.431507 11.00000 -1.20000
AFIX 0
C013 1 0.343858 -0.081455 0.750018 11.00000 0.05428 0.04968 =
0.06367 0.00406 0.00821 0.01900
AFIX 43
H013 2 0.356831 -0.101937 0.807499 11.00000 -1.20000
AFIX 0
C014 1 0.906623 0.745536 0.987339 11.00000 0.05714 0.05752 =
0.07188 0.01386 0.02117 0.02412
AFIX 43
H014 2 0.899375 0.779019 1.039539 11.00000 -1.20000
AFIX 0
C015 1 0.217498 0.623507 0.810543 11.00000 0.06120 0.06672 =
0.07156 0.01497 0.02289 0.04482
AFIX 43
H015 2 0.183346 0.671967 0.794897 11.00000 -1.20000
AFIX 0
C016 1 0.636289 -0.153072 0.906889 11.00000 0.09135 0.05970 =
0.09378 0.03609 0.05509 0.05358
AFIX 43
H016 2 0.625779 -0.223099 0.877808 11.00000 -1.20000
AFIX 0
C017 1 0.103314 0.423060 0.434598 11.00000 0.07028 0.07174 =
0.05645 0.00686 0.00188 0.04051
AFIX 43
H017 2 0.045057 0.348819 0.409363 11.00000 -1.20000
AFIX 0
C018 1 0.073480 0.269615 0.669857 11.00000 0.06117 0.08948 =
0.06049 0.00890 0.03632 0.02516
AFIX 43
H018 2 0.047362 0.304852 0.706539 11.00000 -1.20000
AFIX 0
C019 1 1.031022 0.735671 0.908224 11.00000 0.03925 0.06700 =
0.10870 0.01584 0.03079 0.01253
AFIX 43
H019 2 1.105956 0.761759 0.907367 11.00000 -1.20000
AFIX 0
C01A 1 1.015502 0.783588 0.983682 11.00000 0.04245 0.06206 =
0.09031 0.00722 0.01202 0.01168
AFIX 43
H01A 2 1.080670 0.843140 1.033158 11.00000 -1.20000
AFIX 0
C01B 1 0.313845 0.249680 0.307265 11.00000 0.08786 0.07962 =
0.06400 0.01597 0.04174 0.04611
AFIX 43
H01B 2 0.378404 0.270594 0.290680 11.00000 -1.20000
AFIX 0
C01C 1 0.934684 0.649392 0.834867 11.00000 0.04446 0.06727 =
0.09122 0.01956 0.03602 0.02070
AFIX 43
H01C 2 0.944280 0.617301 0.783477 11.00000 -1.20000
AFIX 0
C01D 1 0.411771 0.034150 0.656080 11.00000 0.08162 0.05517 =
0.06263 0.00701 0.01557 0.03223
AFIX 43
H01D 2 0.471213 0.093528 0.649014 11.00000 -1.20000
AFIX 0
C01E 1 0.271266 0.640349 0.503644 11.00000 0.08587 0.05756 =
0.09073 0.02436 0.03234 0.03654
AFIX 43
H01E 2 0.329736 0.714527 0.527069 11.00000 -1.20000
AFIX 0
C01F 1 0.826633 0.329536 0.850858 11.00000 0.06236 0.07325 =
0.10847 0.04337 0.04520 0.02794
AFIX 43
H01F 2 0.875275 0.403654 0.887564 11.00000 -1.20000
AFIX 0
C01G 1 0.111588 0.132344 0.271792 11.00000 0.09703 0.06291 =
0.05345 0.00334 0.02476 0.02860
AFIX 43
H01G 2 0.038264 0.073499 0.230623 11.00000 -1.20000
AFIX 0
C01H 1 0.158043 0.617348 0.448850 11.00000 0.11806 0.08318 =
0.07297 0.03238 0.04348 0.06881
AFIX 43
H01H 2 0.138197 0.675335 0.435033 11.00000 -1.20000
AFIX 0
C01I 1 0.232211 -0.140225 0.673199 11.00000 0.05942 0.06337 =
0.10451 -0.00585 0.00156 0.01689
AFIX 43
H01I 2 0.172043 -0.199347 0.679772 11.00000 -1.20000
AFIX 0
C01J 1 0.091668 0.110345 0.612949 11.00000 0.07423 0.05601 =
0.09433 0.02729 0.04075 0.02000
AFIX 43
H01J 2 0.078792 0.036346 0.610648 11.00000 -1.20000
AFIX 0
C01K 1 0.300048 -0.025424 0.578972 11.00000 0.12465 0.08429 =
0.05440 0.00912 0.00993 0.06136
AFIX 43
H01K 2 0.286558 -0.006275 0.520906 11.00000 -1.20000
AFIX 0
C01L 1 0.206078 0.160105 0.246502 11.00000 0.11616 0.07687 =
0.05989 0.01275 0.04050 0.05028
AFIX 43
H01L 2 0.197826 0.119430 0.189529 11.00000 -1.20000
AFIX 0
C01M 1 0.053444 0.160838 0.667696 11.00000 0.06951 0.09073 =
0.07471 0.02922 0.04028 0.01958
AFIX 43
H01M 2 0.014681 0.122166 0.702707 11.00000 -1.20000
AFIX 0
C01N 1 0.071791 0.507402 0.413385 11.00000 0.07976 0.10305 =
0.07337 0.01657 0.01210 0.06148
AFIX 43
H01N 2 -0.006810 0.490385 0.375554 11.00000 -1.20000
AFIX 0
C01O 1 0.851144 0.285292 0.781187 11.00000 0.08933 0.10889 =
0.12770 0.06285 0.07405 0.04140
AFIX 43
H01O 2 0.915660 0.329762 0.769333 11.00000 -1.20000
AFIX 0
C01P 1 0.211244 -0.110891 0.588220 11.00000 0.09449 0.07377 =
0.08101 -0.01172 -0.01518 0.04545
AFIX 43
H01P 2 0.136661 -0.149267 0.537185 11.00000 -1.20000
AFIX 0
C01Q 1 0.781510 0.176450 0.729128 11.00000 0.12095 0.11599 =
0.11857 0.03705 0.09276 0.05320
AFIX 43
H01Q 2 0.799676 0.146643 0.682455 11.00000 -1.20000
AFIX 0
C01R 1 0.683602 0.108842 0.744369 11.00000 0.09037 0.08717 =
0.08461 0.02730 0.05574 0.04176
AFIX 43
H01R 2 0.637564 0.033961 0.709003 11.00000 -1.20000
AFIX 0
HKLF 4
REM ligand-try_a.res in P-1
REM R1 = 0.0853 for 4957 Fo > 4sig(Fo) and 0.1796 for all 10469 data
REM 568 parameters refined using 0 restraints
END
WGHT 0.0492 1.6733
REM Highest difference peak 0.464, deepest hole -0.379, 1-sigma level 0.067
Q1 1 0.3249 0.4849 0.5167 11.00000 0.05 0.46
Q2 1 0.4117 0.5228 0.6880 11.00000 0.05 0.30
Q3 1 0.6249 0.4551 0.7949 11.00000 0.05 0.29
Q4 1 0.5182 0.3422 1.0197 11.00000 0.05 0.27
Q5 1 0.7359 0.1252 0.7617 11.00000 0.05 0.26
Q6 1 0.6117 0.3116 0.5865 11.00000 0.05 0.25
Q7 1 0.5033 0.4153 0.5433 11.00000 0.05 0.25
Q8 1 0.0657 0.3805 0.4971 11.00000 0.05 0.25
Q9 1 -0.0533 0.4564 0.3590 11.00000 0.05 0.25
Q10 1 0.3249 -0.0819 0.5191 11.00000 0.05 0.25
Q11 1 0.2011 0.2673 0.3610 11.00000 0.05 0.24
Q12 1 0.4644 0.7376 0.6381 11.00000 0.05 0.24
Q13 1 0.7799 0.5969 0.8005 11.00000 0.05 0.24
Q14 1 0.2210 0.4431 0.6757 11.00000 0.05 0.23
Q15 1 0.7386 -0.0417 1.0221 11.00000 0.05 0.23
Q16 1 0.1588 0.4804 0.6003 11.00000 0.05 0.23
Q17 1 0.2289 0.2351 0.4362 11.00000 0.05 0.23
Q18 1 0.3819 -0.0321 0.8383 11.00000 0.05 0.23
Q19 1 0.3887 0.5128 0.7408 11.00000 0.05 0.23
Q20 1 0.6371 0.6818 0.9174 11.00000 0.05 0.23
;
_shelx_res_checksum 40447
_olex2_submission_special_instructions 'No special instructions were received'