# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015
#######################################################################
#
# 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_vn1
_database_code_depnum_ccdc_archive 'CCDC 1412576'
_audit_update_record
;
2015-07-13 deposited with the CCDC.
2015-08-28 downloaded from the CCDC.
;
_audit_creation_date 2014-09-14
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_shelxl_version_number 2013-4
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C27 H34 N2 O4'
_chemical_formula_sum 'C27 H34 N2 O4'
_chemical_formula_weight 450.56
_chemical_melting_point ?
_chemical_oxdiff_formula 'C20 H20 N2 O2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 15.0493(5)
_cell_length_b 6.6839(2)
_cell_length_c 24.3241(10)
_cell_angle_alpha 90
_cell_angle_beta 100.495(4)
_cell_angle_gamma 90
_cell_volume 2405.77(16)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 1555
_cell_measurement_temperature 180(2)
_cell_measurement_theta_max 76.7400
_cell_measurement_theta_min 3.7820
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.667
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.96420
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.244
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 968
_exptl_crystal_size_max 0.14
_exptl_crystal_size_mid 0.04
_exptl_crystal_size_min 0.04
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0515
_diffrn_reflns_av_unetI/netI 0.0780
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_k_min -4
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_limit_l_min -30
_diffrn_reflns_number 8764
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 78.079
_diffrn_reflns_theta_min 3.788
_diffrn_ambient_temperature 180(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 5.1417
_diffrn_detector_type Ruby
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -66.00 -33.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- -41.7109 57.0000 90.0000 33
#__ type_ start__ end____ width___ exp.time_
2 omega -50.00 32.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- -41.7109 38.0000 -150.0000 82
#__ type_ start__ end____ width___ exp.time_
3 omega 6.00 31.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- -41.7109 57.0000 90.0000 25
#__ type_ start__ end____ width___ exp.time_
4 omega -47.00 33.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- -41.7109 38.0000 -30.0000 80
#__ type_ start__ end____ width___ exp.time_
5 omega -45.00 -19.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- -41.7109 38.0000 -60.0000 26
#__ type_ start__ end____ width___ exp.time_
6 omega 41.00 78.00 1.0000 82.5000
omega____ theta____ kappa____ phi______ frames
- 114.0000 -45.0000 -90.0000 37
#__ type_ start__ end____ width___ exp.time_
7 omega 48.00 96.00 1.0000 82.5000
omega____ theta____ kappa____ phi______ frames
- 114.0000 -45.0000 120.0000 48
#__ type_ start__ end____ width___ exp.time_
8 omega 38.00 70.00 1.0000 82.5000
omega____ theta____ kappa____ phi______ frames
- 114.0000 -30.0000 90.0000 32
#__ type_ start__ end____ width___ exp.time_
9 omega 109.00 178.00 1.0000 82.5000
omega____ theta____ kappa____ phi______ frames
- 114.0000 45.0000 -180.0000 69
#__ type_ start__ end____ width___ exp.time_
10 omega 88.00 178.00 1.0000 82.5000
omega____ theta____ kappa____ phi______ frames
- 114.0000 45.0000 -120.0000 90
#__ type_ start__ end____ width___ exp.time_
11 omega 62.00 93.00 1.0000 82.5000
omega____ theta____ kappa____ phi______ frames
- 114.0000 -45.0000 -60.0000 31
#__ type_ start__ end____ width___ exp.time_
12 omega 85.00 178.00 1.0000 82.5000
omega____ theta____ kappa____ phi______ frames
- 114.0000 61.0000 120.0000 93
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 0.0389974000
_diffrn_orient_matrix_UB_12 0.1635886000
_diffrn_orient_matrix_UB_13 -0.0334208000
_diffrn_orient_matrix_UB_21 -0.0925397000
_diffrn_orient_matrix_UB_22 0.0211217000
_diffrn_orient_matrix_UB_23 -0.0388812000
_diffrn_orient_matrix_UB_31 -0.0275443000
_diffrn_orient_matrix_UB_32 0.1608767000
_diffrn_orient_matrix_UB_33 0.0390019000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 3321
_reflns_number_total 4971
_reflns_odcompleteness_completeness 99.08
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 72.42
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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 'XS (Sheldrick, 2008)'
_refine_diff_density_max 0.219
_refine_diff_density_min -0.167
_refine_diff_density_rms 0.043
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.015
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 306
_refine_ls_number_reflns 4971
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0841
_refine_ls_R_factor_gt 0.0503
_refine_ls_restrained_S_all 1.015
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0291P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1049
_refine_ls_wR_factor_ref 0.1218
_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 C(H,H,H) groups, All C(H,H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
C8(H8A,H8B), C9(H9A,H9B), C19(H19A,H19B), C20(H20A,H20B)
2.b Aromatic/amide H refined with riding coordinates:
C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C23(H23), C24(H24),
C25(H25), C26(H26), C27(H27)
2.c Idealised Me refined as rotating group:
C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C29(H29A,H29B,H29C),
C30(H30A,H30B,H30C)
;
_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
C1 C 0.03970(16) 0.4391(4) 0.32492(11) 0.0475(6) Uani 1 1 d . . . . .
H1A H 0.0345 0.2949 0.3177 0.071 Uiso 1 1 calc GR . . . .
H1B H 0.0011 0.5114 0.2945 0.071 Uiso 1 1 calc GR . . . .
H1C H 0.0205 0.4694 0.3604 0.071 Uiso 1 1 calc GR . . . .
C2 C 0.13727(16) 0.5037(4) 0.32813(10) 0.0400(5) Uani 1 1 d . . . . .
C3 C 0.1682(2) 0.4630(5) 0.27290(11) 0.0565(7) Uani 1 1 d . . . . .
H3A H 0.1307 0.5397 0.2430 0.085 Uiso 1 1 calc GR . . . .
H3B H 0.1622 0.3199 0.2642 0.085 Uiso 1 1 calc GR . . . .
H3C H 0.2315 0.5032 0.2759 0.085 Uiso 1 1 calc GR . . . .
C4 C 0.1517(2) 0.7218(4) 0.34522(13) 0.0574(7) Uani 1 1 d . . . . .
H4A H 0.1332 0.7429 0.3814 0.086 Uiso 1 1 calc GR . . . .
H4B H 0.1155 0.8073 0.3169 0.086 Uiso 1 1 calc GR . . . .
H4C H 0.2158 0.7558 0.3484 0.086 Uiso 1 1 calc GR . . . .
O5 O 0.19778(10) 0.3752(3) 0.36723(7) 0.0387(4) Uani 1 1 d . . . . .
C6 C 0.18622(14) 0.3580(3) 0.42128(9) 0.0316(4) Uani 1 1 d . . . . .
O6 O 0.13425(10) 0.4546(2) 0.44316(7) 0.0377(4) Uani 1 1 d . . . . .
N7 N 0.23967(13) 0.2078(3) 0.44545(8) 0.0336(4) Uani 1 1 d . . . . .
C8 C 0.31520(15) 0.1018(3) 0.42836(10) 0.0348(5) Uani 1 1 d . . . . .
H8A H 0.3651 0.1903 0.4219 0.042 Uiso 1 1 calc R . . . .
H8B H 0.2970 0.0090 0.3966 0.042 Uiso 1 1 calc R . . . .
C9 C 0.33201(15) -0.0011(3) 0.48607(9) 0.0342(5) Uani 1 1 d . . . . .
H9A H 0.3946 0.0131 0.5069 0.041 Uiso 1 1 calc R . . . .
H9B H 0.3120 -0.1423 0.4852 0.041 Uiso 1 1 calc R . . . .
C10 C 0.26337(14) 0.1499(3) 0.50472(9) 0.0302(4) Uani 1 1 d . . . . .
C11 C 0.18495(14) 0.0733(3) 0.53010(9) 0.0311(4) Uani 1 1 d . . . . .
C12 C 0.15826(15) -0.1268(3) 0.52611(10) 0.0380(5) Uani 1 1 d . . . . .
H12 H 0.1918 -0.2214 0.5091 0.046 Uiso 1 1 calc R . . . .
C13 C 0.08257(16) -0.1879(4) 0.54713(11) 0.0449(6) Uani 1 1 d . . . . .
H13 H 0.0646 -0.3242 0.5441 0.054 Uiso 1 1 calc R . . . .
C14 C 0.03348(16) -0.0527(4) 0.57224(11) 0.0457(6) Uani 1 1 d . . . . .
H14 H -0.0180 -0.0956 0.5866 0.055 Uiso 1 1 calc R . . . .
C15 C 0.05979(16) 0.1469(4) 0.57639(11) 0.0444(6) Uani 1 1 d . . . . .
H15 H 0.0261 0.2411 0.5935 0.053 Uiso 1 1 calc R . . . .
C16 C 0.13507(15) 0.2081(3) 0.55564(10) 0.0381(5) Uani 1 1 d . . . . .
H16 H 0.1530 0.3445 0.5589 0.046 Uiso 1 1 calc R . . . .
C17 C 0.31681(13) 0.3189(3) 0.53952(9) 0.0279(4) Uani 1 1 d . . . . .
O17 O 0.32764(10) 0.4840(2) 0.51880(6) 0.0321(3) Uani 1 1 d . . . . .
N18 N 0.35373(11) 0.2675(2) 0.59184(7) 0.0275(3) Uani 1 1 d . . . . .
C19 C 0.35601(16) 0.0757(3) 0.62228(10) 0.0352(5) Uani 1 1 d . . . . .
H19A H 0.3698 -0.0415 0.6004 0.042 Uiso 1 1 calc R . . . .
H19B H 0.3019 0.0511 0.6391 0.042 Uiso 1 1 calc R . . . .
C20 C 0.43788(15) 0.1552(3) 0.66395(10) 0.0356(5) Uani 1 1 d . . . . .
H20A H 0.4962 0.0956 0.6592 0.043 Uiso 1 1 calc R . . . .
H20B H 0.4302 0.1491 0.7035 0.043 Uiso 1 1 calc R . . . .
C21 C 0.41982(13) 0.3671(3) 0.63684(9) 0.0278(4) Uani 1 1 d . . . . .
C22 C 0.37250(14) 0.5034(3) 0.67250(9) 0.0291(4) Uani 1 1 d . . . . .
C23 C 0.40833(16) 0.5281(3) 0.72923(10) 0.0381(5) Uani 1 1 d . . . . .
H23 H 0.4629 0.4621 0.7450 0.046 Uiso 1 1 calc R . . . .
C24 C 0.36512(18) 0.6479(4) 0.76285(10) 0.0437(5) Uani 1 1 d . . . . .
H24 H 0.3910 0.6652 0.8012 0.052 Uiso 1 1 calc R . . . .
C25 C 0.28498(18) 0.7420(3) 0.74106(11) 0.0427(6) Uani 1 1 d . . . . .
H25 H 0.2552 0.8226 0.7643 0.051 Uiso 1 1 calc R . . . .
C26 C 0.24824(16) 0.7178(3) 0.68496(10) 0.0379(5) Uani 1 1 d . . . . .
H26 H 0.1930 0.7822 0.6697 0.046 Uiso 1 1 calc R . . . .
C27 C 0.29177(14) 0.5998(3) 0.65082(9) 0.0309(4) Uani 1 1 d . . . . .
H27 H 0.2661 0.5849 0.6124 0.037 Uiso 1 1 calc R . . . .
C28 C 0.50017(14) 0.4712(3) 0.61569(9) 0.0331(4) Uani 1 1 d . . . . .
O28 O 0.47062(10) 0.6568(2) 0.58929(7) 0.0343(3) Uani 1 1 d . . . . .
C29 C 0.53870(16) 0.3392(4) 0.57410(11) 0.0447(6) Uani 1 1 d . . . . .
H29A H 0.4923 0.3173 0.5408 0.067 Uiso 1 1 calc GR . . . .
H29B H 0.5574 0.2102 0.5916 0.067 Uiso 1 1 calc GR . . . .
H29C H 0.5910 0.4058 0.5634 0.067 Uiso 1 1 calc GR . . . .
C30 C 0.57414(15) 0.5248(4) 0.66505(11) 0.0478(6) Uani 1 1 d . . . . .
H30A H 0.5901 0.4062 0.6884 0.072 Uiso 1 1 calc GR . . . .
H30B H 0.5523 0.6302 0.6872 0.072 Uiso 1 1 calc GR . . . .
H30C H 0.6276 0.5726 0.6512 0.072 Uiso 1 1 calc GR . . . .
H28 H 0.425(2) 0.629(5) 0.5617(14) 0.072 Uiso 1 1 d R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0372(11) 0.0544(14) 0.0458(14) -0.0050(12) -0.0062(11) 0.0039(11)
C2 0.0412(12) 0.0403(12) 0.0350(12) 0.0035(10) -0.0028(10) 0.0019(10)
C3 0.0581(16) 0.0747(19) 0.0338(13) 0.0051(14) 0.0004(12) 0.0013(15)
C4 0.0690(18) 0.0389(13) 0.0606(18) 0.0049(13) 0.0019(15) -0.0095(13)
O5 0.0362(8) 0.0467(9) 0.0325(8) 0.0018(7) 0.0045(7) 0.0079(7)
C6 0.0295(9) 0.0326(10) 0.0315(11) -0.0043(9) 0.0023(8) -0.0021(9)
O6 0.0360(7) 0.0389(8) 0.0382(8) -0.0031(7) 0.0072(7) 0.0086(7)
N7 0.0392(9) 0.0336(9) 0.0286(9) -0.0023(8) 0.0076(7) 0.0068(8)
C8 0.0341(10) 0.0346(10) 0.0368(12) -0.0057(9) 0.0098(9) 0.0023(9)
C9 0.0384(10) 0.0280(10) 0.0377(12) -0.0050(9) 0.0106(9) 0.0060(9)
C10 0.0323(9) 0.0265(9) 0.0311(11) -0.0024(8) 0.0041(8) 0.0057(8)
C11 0.0314(10) 0.0302(10) 0.0305(11) -0.0017(8) 0.0025(8) -0.0009(8)
C12 0.0366(11) 0.0313(10) 0.0430(13) 0.0001(10) -0.0008(10) 0.0024(9)
C13 0.0377(11) 0.0376(12) 0.0557(15) 0.0079(11) -0.0009(11) -0.0089(10)
C14 0.0341(11) 0.0564(14) 0.0456(14) 0.0097(12) 0.0050(10) -0.0115(11)
C15 0.0361(11) 0.0543(14) 0.0448(14) -0.0079(12) 0.0126(10) -0.0040(11)
C16 0.0357(10) 0.0375(11) 0.0426(13) -0.0085(10) 0.0114(10) -0.0038(9)
C17 0.0273(9) 0.0262(9) 0.0319(10) 0.0007(8) 0.0103(8) 0.0049(8)
O17 0.0347(7) 0.0273(7) 0.0342(8) 0.0069(6) 0.0062(6) 0.0016(6)
N18 0.0295(8) 0.0220(7) 0.0312(9) 0.0006(7) 0.0063(7) 0.0007(6)
C19 0.0467(12) 0.0239(9) 0.0358(11) 0.0056(9) 0.0093(10) 0.0013(9)
C20 0.0401(11) 0.0288(10) 0.0375(12) 0.0070(9) 0.0065(9) 0.0056(9)
C21 0.0258(8) 0.0275(9) 0.0297(10) 0.0017(8) 0.0042(8) 0.0025(8)
C22 0.0327(9) 0.0248(9) 0.0320(10) 0.0010(8) 0.0119(8) -0.0036(8)
C23 0.0411(11) 0.0367(11) 0.0359(12) -0.0002(10) 0.0054(10) -0.0044(10)
C24 0.0602(14) 0.0407(12) 0.0313(12) -0.0042(10) 0.0112(11) -0.0089(11)
C25 0.0610(15) 0.0283(10) 0.0458(14) -0.0058(10) 0.0279(12) -0.0041(10)
C26 0.0463(12) 0.0260(9) 0.0462(14) 0.0029(9) 0.0208(11) 0.0034(9)
C27 0.0355(10) 0.0245(9) 0.0344(11) 0.0021(8) 0.0109(9) -0.0002(8)
C28 0.0283(9) 0.0343(10) 0.0379(12) 0.0066(9) 0.0095(9) 0.0037(8)
O28 0.0333(7) 0.0298(7) 0.0408(9) 0.0059(7) 0.0093(7) -0.0007(6)
C29 0.0371(11) 0.0452(12) 0.0573(15) 0.0051(12) 0.0230(11) 0.0128(10)
C30 0.0322(11) 0.0586(15) 0.0513(15) 0.0104(13) 0.0041(11) -0.0077(11)
_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
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.519(3) . ?
C2 C3 1.524(4) . ?
C2 C4 1.521(3) . ?
C2 O5 1.468(3) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
O5 C6 1.362(3) . ?
C6 O6 1.210(3) . ?
C6 N7 1.352(3) . ?
N7 C8 1.462(3) . ?
N7 C10 1.473(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.542(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.569(3) . ?
C10 C11 1.517(3) . ?
C10 C17 1.546(3) . ?
C11 C12 1.395(3) . ?
C11 C16 1.390(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.392(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.378(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.390(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.383(3) . ?
C16 H16 0.9500 . ?
C17 O17 1.236(3) . ?
C17 N18 1.337(3) . ?
N18 C19 1.478(3) . ?
N18 C21 1.495(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.540(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.565(3) . ?
C21 C22 1.521(3) . ?
C21 C28 1.561(3) . ?
C22 C23 1.397(3) . ?
C22 C27 1.391(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.388(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.378(4) . ?
C25 H25 0.9500 . ?
C25 C26 1.385(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.393(3) . ?
C27 H27 0.9500 . ?
C28 O28 1.430(3) . ?
C28 C29 1.533(3) . ?
C28 C30 1.524(3) . ?
O28 H28 0.88(3) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C1 C2 C3 110.6(2) . . ?
C1 C2 C4 112.0(2) . . ?
C4 C2 C3 111.1(2) . . ?
O5 C2 C1 110.3(2) . . ?
O5 C2 C3 102.3(2) . . ?
O5 C2 C4 110.1(2) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 O5 C2 120.08(18) . . ?
O6 C6 O5 125.9(2) . . ?
O6 C6 N7 125.9(2) . . ?
N7 C6 O5 108.17(18) . . ?
C6 N7 C8 131.88(19) . . ?
C6 N7 C10 129.76(19) . . ?
C8 N7 C10 95.10(16) . . ?
N7 C8 H8A 114.0 . . ?
N7 C8 H8B 114.0 . . ?
N7 C8 C9 87.96(16) . . ?
H8A C8 H8B 111.2 . . ?
C9 C8 H8A 114.0 . . ?
C9 C8 H8B 114.0 . . ?
C8 C9 H9A 114.0 . . ?
C8 C9 H9B 114.0 . . ?
C8 C9 C10 88.21(15) . . ?
H9A C9 H9B 111.2 . . ?
C10 C9 H9A 114.0 . . ?
C10 C9 H9B 114.0 . . ?
N7 C10 C9 86.60(15) . . ?
N7 C10 C11 114.79(17) . . ?
N7 C10 C17 110.69(17) . . ?
C11 C10 C9 120.16(17) . . ?
C11 C10 C17 112.92(17) . . ?
C17 C10 C9 108.90(16) . . ?
C12 C11 C10 122.1(2) . . ?
C16 C11 C10 119.14(19) . . ?
C16 C11 C12 118.7(2) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 C11 120.0(2) . . ?
C13 C12 H12 120.0 . . ?
C12 C13 H13 119.6 . . ?
C14 C13 C12 120.7(2) . . ?
C14 C13 H13 119.6 . . ?
C13 C14 H14 120.2 . . ?
C13 C14 C15 119.5(2) . . ?
C15 C14 H14 120.2 . . ?
C14 C15 H15 120.0 . . ?
C16 C15 C14 119.9(2) . . ?
C16 C15 H15 120.0 . . ?
C11 C16 H16 119.5 . . ?
C15 C16 C11 121.1(2) . . ?
C15 C16 H16 119.5 . . ?
O17 C17 C10 121.53(19) . . ?
O17 C17 N18 123.7(2) . . ?
N18 C17 C10 114.71(17) . . ?
C17 N18 C19 131.84(18) . . ?
C17 N18 C21 133.51(17) . . ?
C19 N18 C21 93.88(15) . . ?
N18 C19 H19A 113.9 . . ?
N18 C19 H19B 113.9 . . ?
N18 C19 C20 88.46(16) . . ?
H19A C19 H19B 111.1 . . ?
C20 C19 H19A 113.9 . . ?
C20 C19 H19B 113.9 . . ?
C19 C20 H20A 113.9 . . ?
C19 C20 H20B 113.9 . . ?
C19 C20 C21 88.76(15) . . ?
H20A C20 H20B 111.1 . . ?
C21 C20 H20A 113.9 . . ?
C21 C20 H20B 113.9 . . ?
N18 C21 C20 86.95(15) . . ?
N18 C21 C22 111.48(16) . . ?
N18 C21 C28 114.14(17) . . ?
C22 C21 C20 111.42(17) . . ?
C22 C21 C28 113.10(17) . . ?
C28 C21 C20 117.16(17) . . ?
C23 C22 C21 119.83(19) . . ?
C27 C22 C21 121.89(19) . . ?
C27 C22 C23 118.2(2) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 C22 120.8(2) . . ?
C24 C23 H23 119.6 . . ?
C23 C24 H24 119.7 . . ?
C25 C24 C23 120.5(2) . . ?
C25 C24 H24 119.7 . . ?
C24 C25 H25 120.3 . . ?
C24 C25 C26 119.4(2) . . ?
C26 C25 H25 120.3 . . ?
C25 C26 H26 119.8 . . ?
C25 C26 C27 120.5(2) . . ?
C27 C26 H26 119.8 . . ?
C22 C27 C26 120.6(2) . . ?
C22 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
O28 C28 C21 109.77(16) . . ?
O28 C28 C29 109.08(18) . . ?
O28 C28 C30 105.82(19) . . ?
C29 C28 C21 111.70(19) . . ?
C30 C28 C21 110.10(18) . . ?
C30 C28 C29 110.21(19) . . ?
C28 O28 H28 107(2) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O28 H28 O17 0.88(3) 1.91(3) 2.750(2) 159(3) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 O5 C6 -57.1(3) . . . . ?
C2 O5 C6 O6 -7.2(3) . . . . ?
C2 O5 C6 N7 169.86(18) . . . . ?
C3 C2 O5 C6 -174.8(2) . . . . ?
C4 C2 O5 C6 67.0(3) . . . . ?
O5 C6 N7 C8 14.7(3) . . . . ?
O5 C6 N7 C10 169.0(2) . . . . ?
C6 N7 C8 C9 171.9(2) . . . . ?
C6 N7 C10 C9 -172.4(2) . . . . ?
C6 N7 C10 C11 65.8(3) . . . . ?
C6 N7 C10 C17 -63.4(3) . . . . ?
O6 C6 N7 C8 -168.2(2) . . . . ?
O6 C6 N7 C10 -13.9(4) . . . . ?
N7 C8 C9 C10 -10.71(16) . . . . ?
N7 C10 C11 C12 86.0(3) . . . . ?
N7 C10 C11 C16 -90.7(2) . . . . ?
N7 C10 C17 O17 6.7(3) . . . . ?
N7 C10 C17 N18 -169.66(16) . . . . ?
C8 N7 C10 C9 -11.28(16) . . . . ?
C8 N7 C10 C11 -133.08(18) . . . . ?
C8 N7 C10 C17 97.65(18) . . . . ?
C8 C9 C10 N7 10.65(16) . . . . ?
C8 C9 C10 C11 127.5(2) . . . . ?
C8 C9 C10 C17 -100.06(18) . . . . ?
C9 C10 C11 C12 -15.1(3) . . . . ?
C9 C10 C11 C16 168.2(2) . . . . ?
C9 C10 C17 O17 100.3(2) . . . . ?
C9 C10 C17 N18 -76.1(2) . . . . ?
C10 N7 C8 C9 11.47(17) . . . . ?
C10 C11 C12 C13 -176.2(2) . . . . ?
C10 C11 C16 C15 176.1(2) . . . . ?
C10 C17 N18 C19 2.7(3) . . . . ?
C10 C17 N18 C21 169.96(18) . . . . ?
C11 C10 C17 O17 -123.5(2) . . . . ?
C11 C10 C17 N18 60.1(2) . . . . ?
C11 C12 C13 C14 -0.3(4) . . . . ?
C12 C11 C16 C15 -0.6(4) . . . . ?
C12 C13 C14 C15 0.2(4) . . . . ?
C13 C14 C15 C16 -0.3(4) . . . . ?
C14 C15 C16 C11 0.5(4) . . . . ?
C16 C11 C12 C13 0.5(3) . . . . ?
C17 C10 C11 C12 -145.9(2) . . . . ?
C17 C10 C11 C16 37.5(3) . . . . ?
C17 N18 C19 C20 159.9(2) . . . . ?
C17 N18 C21 C20 -159.8(2) . . . . ?
C17 N18 C21 C22 88.3(3) . . . . ?
C17 N18 C21 C28 -41.3(3) . . . . ?
O17 C17 N18 C19 -173.6(2) . . . . ?
O17 C17 N18 C21 -6.4(3) . . . . ?
N18 C19 C20 C21 10.34(16) . . . . ?
N18 C21 C22 C23 147.35(18) . . . . ?
N18 C21 C22 C27 -30.1(3) . . . . ?
N18 C21 C28 O28 77.1(2) . . . . ?
N18 C21 C28 C29 -44.0(2) . . . . ?
N18 C21 C28 C30 -166.82(18) . . . . ?
C19 N18 C21 C20 10.69(16) . . . . ?
C19 N18 C21 C22 -101.15(18) . . . . ?
C19 N18 C21 C28 129.18(18) . . . . ?
C19 C20 C21 N18 -10.23(16) . . . . ?
C19 C20 C21 C22 101.66(19) . . . . ?
C19 C20 C21 C28 -125.89(19) . . . . ?
C20 C21 C22 C23 52.0(2) . . . . ?
C20 C21 C22 C27 -125.4(2) . . . . ?
C20 C21 C28 O28 176.54(17) . . . . ?
C20 C21 C28 C29 55.4(3) . . . . ?
C20 C21 C28 C30 -67.4(2) . . . . ?
C21 N18 C19 C20 -10.85(16) . . . . ?
C21 C22 C23 C24 -178.5(2) . . . . ?
C21 C22 C27 C26 177.62(19) . . . . ?
C22 C21 C28 O28 -51.8(2) . . . . ?
C22 C21 C28 C29 -172.88(18) . . . . ?
C22 C21 C28 C30 64.3(2) . . . . ?
C22 C23 C24 C25 1.2(4) . . . . ?
C23 C22 C27 C26 0.1(3) . . . . ?
C23 C24 C25 C26 -0.7(4) . . . . ?
C24 C25 C26 C27 0.0(3) . . . . ?
C25 C26 C27 C22 0.4(3) . . . . ?
C27 C22 C23 C24 -0.9(3) . . . . ?
C28 C21 C22 C23 -82.4(2) . . . . ?
C28 C21 C22 C27 100.1(2) . . . . ?
_iucr_refine_instructions_details
;
TITL vn1 in P21/n #14
CELL 1.54184 15.049271 6.683886 24.324143 90 100.4955 90
ZERR 4 0.000542 0.000212 0.001026 0 0.0042 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N O
UNIT 108 136 8 16
L.S. 4 0 0
PLAN 20
TEMP -93(2)
HTAB O28 O17
REM reset to P21/n #14 colourless 0.04 0.10 0.40
BOND $H
fmap 2 53
acta
MORE -1
CONF
OMIT 0 0 2
REM /Users/guy/Desktop/XrayWork/Shipman/vn1/vn1.hkl
WGHT 0.029100
FVAR 1.95955
C1 1 0.039695 0.439108 0.324921 11.00000 0.03718 0.05445 =
0.04581 -0.00504 -0.00624 0.00391
AFIX 137
H1A 2 0.034529 0.294918 0.317743 11.00000 -1.50000
H1B 2 0.001099 0.511356 0.294536 11.00000 -1.50000
H1C 2 0.020502 0.469367 0.360411 11.00000 -1.50000
AFIX 0
C2 1 0.137268 0.503714 0.328133 11.00000 0.04118 0.04029 =
0.03498 0.00350 -0.00284 0.00187
C3 1 0.168175 0.463008 0.272904 11.00000 0.05811 0.07470 =
0.03382 0.00507 0.00045 0.00125
AFIX 137
H3A 2 0.130657 0.539700 0.243020 11.00000 -1.50000
H3B 2 0.162238 0.319907 0.264238 11.00000 -1.50000
H3C 2 0.231502 0.503243 0.275940 11.00000 -1.50000
AFIX 0
C4 1 0.151719 0.721806 0.345223 11.00000 0.06901 0.03888 =
0.06058 0.00490 0.00193 -0.00951
AFIX 137
H4A 2 0.133172 0.742906 0.381373 11.00000 -1.50000
H4B 2 0.115503 0.807280 0.316930 11.00000 -1.50000
H4C 2 0.215796 0.755793 0.348380 11.00000 -1.50000
AFIX 0
O5 4 0.197777 0.375173 0.367226 11.00000 0.03625 0.04668 =
0.03247 0.00181 0.00454 0.00792
C6 1 0.186224 0.357996 0.421280 11.00000 0.02945 0.03256 =
0.03154 -0.00427 0.00228 -0.00211
O6 4 0.134249 0.454643 0.443163 11.00000 0.03600 0.03894 =
0.03819 -0.00308 0.00719 0.00862
N7 3 0.239666 0.207771 0.445446 11.00000 0.03921 0.03363 =
0.02861 -0.00232 0.00764 0.00676
C8 1 0.315199 0.101843 0.428356 11.00000 0.03411 0.03457 =
0.03684 -0.00575 0.00977 0.00234
AFIX 23
H8A 2 0.365075 0.190308 0.421937 11.00000 -1.20000
H8B 2 0.297004 0.008951 0.396599 11.00000 -1.20000
AFIX 0
C9 1 0.332012 -0.001106 0.486073 11.00000 0.03838 0.02804 =
0.03772 -0.00499 0.01063 0.00598
AFIX 23
H9A 2 0.394645 0.013097 0.506897 11.00000 -1.20000
H9B 2 0.311965 -0.142334 0.485151 11.00000 -1.20000
AFIX 0
C10 1 0.263374 0.149909 0.504723 11.00000 0.03233 0.02647 =
0.03110 -0.00236 0.00407 0.00567
C11 1 0.184947 0.073327 0.530097 11.00000 0.03144 0.03024 =
0.03046 -0.00170 0.00253 -0.00088
C12 1 0.158263 -0.126791 0.526114 11.00000 0.03663 0.03131 =
0.04303 0.00008 -0.00080 0.00239
AFIX 43
H12 2 0.191753 -0.221424 0.509054 11.00000 -1.20000
AFIX 0
C13 1 0.082573 -0.187874 0.547130 11.00000 0.03773 0.03763 =
0.05566 0.00787 -0.00093 -0.00886
AFIX 43
H13 2 0.064554 -0.324249 0.544133 11.00000 -1.20000
AFIX 0
C14 1 0.033476 -0.052684 0.572242 11.00000 0.03410 0.05641 =
0.04561 0.00970 0.00500 -0.01146
AFIX 43
H14 2 -0.017973 -0.095605 0.586608 11.00000 -1.20000
AFIX 0
C15 1 0.059789 0.146869 0.576390 11.00000 0.03614 0.05428 =
0.04481 -0.00786 0.01257 -0.00397
AFIX 43
H15 2 0.026121 0.241122 0.593454 11.00000 -1.20000
AFIX 0
C16 1 0.135067 0.208105 0.555644 11.00000 0.03569 0.03750 =
0.04261 -0.00855 0.01142 -0.00375
AFIX 43
H16 2 0.152954 0.344533 0.558915 11.00000 -1.20000
AFIX 0
C17 1 0.316809 0.318861 0.539516 11.00000 0.02734 0.02620 =
0.03192 0.00065 0.01027 0.00492
O17 4 0.327638 0.483990 0.518797 11.00000 0.03466 0.02727 =
0.03425 0.00687 0.00625 0.00161
N18 3 0.353733 0.267534 0.591837 11.00000 0.02949 0.02200 =
0.03125 0.00062 0.00631 0.00069
C19 1 0.356014 0.075665 0.622284 11.00000 0.04668 0.02388 =
0.03584 0.00563 0.00933 0.00135
AFIX 23
H19A 2 0.369841 -0.041530 0.600419 11.00000 -1.20000
H19B 2 0.301861 0.051101 0.639109 11.00000 -1.20000
AFIX 0
C20 1 0.437878 0.155166 0.663947 11.00000 0.04014 0.02883 =
0.03753 0.00699 0.00646 0.00562
AFIX 23
H20A 2 0.496226 0.095589 0.659184 11.00000 -1.20000
H20B 2 0.430237 0.149065 0.703485 11.00000 -1.20000
AFIX 0
C21 1 0.419816 0.367122 0.636845 11.00000 0.02579 0.02748 =
0.02973 0.00170 0.00417 0.00246
C22 1 0.372497 0.503393 0.672496 11.00000 0.03275 0.02483 =
0.03202 0.00095 0.01190 -0.00363
C23 1 0.408330 0.528090 0.729233 11.00000 0.04115 0.03666 =
0.03586 -0.00024 0.00538 -0.00445
AFIX 43
H23 2 0.462940 0.462060 0.745002 11.00000 -1.20000
AFIX 0
C24 1 0.365116 0.647932 0.762852 11.00000 0.06016 0.04072 =
0.03129 -0.00422 0.01123 -0.00886
AFIX 43
H24 2 0.391010 0.665230 0.801191 11.00000 -1.20000
AFIX 0
C25 1 0.284982 0.741968 0.741057 11.00000 0.06097 0.02828 =
0.04584 -0.00581 0.02790 -0.00412
AFIX 43
H25 2 0.255202 0.822612 0.764273 11.00000 -1.20000
AFIX 0
C26 1 0.248244 0.717804 0.684962 11.00000 0.04632 0.02597 =
0.04618 0.00286 0.02079 0.00342
AFIX 43
H26 2 0.192979 0.782192 0.669677 11.00000 -1.20000
AFIX 0
C27 1 0.291768 0.599767 0.650817 11.00000 0.03553 0.02448 =
0.03438 0.00208 0.01091 -0.00024
AFIX 43
H27 2 0.266093 0.584915 0.612360 11.00000 -1.20000
AFIX 0
C28 1 0.500175 0.471191 0.615690 11.00000 0.02833 0.03430 =
0.03786 0.00663 0.00948 0.00366
O28 4 0.470615 0.656809 0.589286 11.00000 0.03334 0.02982 =
0.04076 0.00587 0.00926 -0.00068
C29 1 0.538696 0.339212 0.574100 11.00000 0.03713 0.04517 =
0.05733 0.00508 0.02299 0.01276
AFIX 137
H29A 2 0.492268 0.317327 0.540773 11.00000 -1.50000
H29B 2 0.557450 0.210207 0.591591 11.00000 -1.50000
H29C 2 0.590991 0.405754 0.563356 11.00000 -1.50000
AFIX 0
C30 1 0.574144 0.524824 0.665047 11.00000 0.03215 0.05861 =
0.05135 0.01039 0.00409 -0.00771
AFIX 137
H30A 2 0.590095 0.406154 0.688425 11.00000 -1.50000
H30B 2 0.552330 0.630233 0.687250 11.00000 -1.50000
H30C 2 0.627575 0.572577 0.651208 11.00000 -1.50000
AFIX 0
H28 2 0.425257 0.629268 0.561748 11.00000 -1.50000
HKLF 4
REM vn1 in P21/n #14
REM R1 = 0.0503 for 3321 Fo > 4sig(Fo) and 0.0841 for all 4971 data
REM 306 parameters refined using 0 restraints
END
WGHT 0.0291 0.0000
REM Highest difference peak 0.219, deepest hole -0.167, 1-sigma level 0.043
Q1 1 0.2963 0.2220 0.5199 11.00000 0.05 0.22
Q2 1 0.2233 0.1021 0.5175 11.00000 0.05 0.20
Q3 1 0.1497 0.6120 0.3387 11.00000 0.05 0.18
Q4 1 0.3920 0.4277 0.6595 11.00000 0.05 0.17
Q5 1 0.3224 -0.0633 0.5980 11.00000 0.05 0.17
Q6 1 0.3564 0.5557 0.5409 11.00000 0.05 0.16
Q7 1 0.3647 0.2661 0.5625 11.00000 0.05 0.16
Q8 1 0.1203 0.7264 0.2241 11.00000 0.05 0.16
Q9 1 0.4575 0.4087 0.6217 11.00000 0.05 0.15
Q10 1 0.4332 0.2607 0.5019 11.00000 0.05 0.15
Q11 1 0.6200 0.1445 0.6596 11.00000 0.05 0.15
Q12 1 0.1053 -0.1602 0.5209 11.00000 0.05 0.15
Q13 1 0.3411 0.5920 0.6589 11.00000 0.05 0.15
Q14 1 0.4127 -0.0086 0.4825 11.00000 0.05 0.14
Q15 1 0.2822 0.6465 0.6737 11.00000 0.05 0.14
Q16 1 0.2919 0.5387 0.5025 11.00000 0.05 0.13
Q17 1 0.2945 0.0778 0.5014 11.00000 0.05 0.13
Q18 1 0.0392 0.2262 0.3594 11.00000 0.05 0.13
Q19 1 0.5014 -0.0775 0.6819 11.00000 0.05 0.13
Q20 1 0.3435 0.7394 0.7426 11.00000 0.05 0.13
REM The information below was added by Olex2.
REM
REM R1 = 0.0503 for 3321 Fo > 4sig(Fo) and 0.0841 for all 9314 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.22, deepest hole -0.17
REM Mean Shift 0, Max Shift 0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0841
REM R1_gt = 0.0503
REM wR_ref = 0.1218
REM GOOF = 1.015
REM Shift_max = 0.001
REM Shift_mean = 0
REM Reflections_all = 9314
REM Reflections_gt = 3321
REM Parameters = n/a
REM Hole = -0.17
REM Peak = 0.22
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_meas
_refln_F_squared_sigma
_refln_scale_group_code
0 0 2 11050.9 319.733 4
0 0 3 -12.088 28.5414 4
0 0 4 3389.87 179.571 4
0 0 5 -18.0036 45.7102 4
0 0 -6 1086.05 77.6344 3
0 0 6 1043.95 124.889 4
0 0 -7 26.4714 25.836 3
0 0 7 -27.7508 58.1578 5
0 0 7 18.2813 57.0019 4
0 0 8 8100.72 406.35 5
0 0 -8 8690.22 288.159 3
0 0 9 -3.06736 62.6676 5
0 0 -9 48.4136 32.2147 3
0 0 10 24226.3 874.879 5
0 0 11 -17.0303 68.0734 5
0 0 12 17280.6 765.825 5
0 0 13 17.6818 61.5397 5
0 0 14 147.679 97.476 2
0 0 14 147.9 95.3115 5
0 0 15 -129.466 105.038 2
0 0 15 -81.0784 93.0832 5
0 0 16 232.34 106.528 2
0 0 16 181.612 128.785 5
0 0 17 12.721 67.3429 2
0 0 17 -46.9059 100.292 5
0 0 18 127.851 112.705 5
0 0 19 -44.4579 53.3704 7
0 0 20 3976.72 233.036 7
0 0 21 3.9336 47.2607 7
0 0 22 232.794 77.2353 7
0 0 23 3.61941 49.283 7
0 0 24 20.9973 51.1264 7
0 0 -25 16.1931 41.6688 10
0 0 -26 92.2289 45.7042 10
0 0 -27 -5.75686 36.2661 10
0 0 -28 539.155 62.1468 10
0 1 0 14.8707 33.3515 1
0 1 1 9059.44 319.84 1
0 1 2 20.6371 30.4976 4
0 1 2 -2.27683 40.747 1
0 1 3 106557 2395.37 1
0 1 3 101273 2371.19 4
0 -1 3 101848 2384.32 5
0 1 4 54.9634 17.2371 2
0 1 4 84.3951 50.724 4
0 -1 4 66.089 48.4139 5
0 -1 5 1478.66 142.985 5
0 1 5 1701.75 90.6539 2
0 1 5 1686.28 138.566 4
0 1 6 4422.82 182.496 2
0 -1 6 3870.2 254.4 5
0 1 6 4151.54 241.757 4
0 1 7 135.899 42.1524 2
0 1 7 203.785 76.6347 4
0 -1 7 117.073 70.2473 5
0 -1 8 488.728 107.792 5
0 1 8 255.723 57.5146 2
0 1 8 372.068 93.2733 4
0 -1 9 3302.82 264.48 5
0 1 9 3738.49 218.117 2
0 1 9 3208.83 260.982 4
0 1 10 1172.16 165.673 5
0 1 10 982.5 156.55 4
0 1 10 1176.63 126.764 2
0 -1 10 1213.5 181.59 5
0 1 11 1146.72 176.134 4
0 -1 11 912.815 169.456 5
0 1 11 1004.24 124.617 2
0 1 11 942.358 162.815 5
0 -1 12 259.18 121.694 5
0 1 12 216.967 105.976 4
0 1 12 278.696 106.82 5
0 1 12 401.907 86.4326 2
0 -1 13 546.527 154.333 5
0 1 13 647.683 149.14 5
0 1 13 620.478 107.666 2
0 -1 14 1130.73 212.989 5
0 1 14 1113.62 199.777 5
0 -1 15 2355.23 307.428 5
0 1 15 2697.75 325.053 5
0 1 16 75.5703 89.5119 5
0 -1 16 186.077 108.771 2
0 1 17 726.797 200.924 5
0 -1 17 740.47 181.982 2
0 -1 18 743.604 99.5123 7
0 -1 18 400.582 135.811 2
0 1 18 577.453 183.23 5
0 1 19 -19.864 60.7036 7
0 -1 19 21.2143 46.3566 7
0 1 19 -100.237 102.67 5
0 -1 20 346.334 73.8191 7
0 1 20 304.703 72.9171 7
0 -1 21 86.1934 55.0661 7
0 1 21 16.6352 52.3479 7
0 -1 22 -1.73197 49.0895 7
0 1 22 64.4118 49.4224 7
0 1 23 687.13 97.0441 7
0 -1 23 753.951 106.317 7
0 -1 24 163.992 62.6915 7
0 -1 25 676.184 96.4372 7
0 1 -25 646.961 95.3345 10
0 1 -26 123.749 52.9637 10
0 1 -27 174.878 47.1317 10
0 1 -28 45.1269 36.3847 10
0 1 -29 11.7396 26.3204 10
0 2 0 6041.64 326.762 1
0 2 -1 33323.5 1004.01 1
0 2 1 33232 1004.86 1
0 2 -2 1271.37 153.282 1
0 2 2 1253.43 150.735 1
0 2 2 1345.29 117.632 4
0 2 3 1007.44 138.349 1
0 2 3 1044.09 110.408 4
0 2 -3 1011.24 139.655 1
0 2 4 838.32 104.356 4
0 2 4 892.389 130.282 1
0 2 5 8760.86 379.167 4
0 2 5 8825.28 414.741 1
0 2 6 18186 635.288 4
0 2 7 1475.64 157.947 4
0 2 8 5535.81 336.74 4
0 2 9 15.9071 51.3626 4
0 2 10 716.872 141.127 4
0 2 -10 880.92 137.823 1
0 2 11 938.318 166.78 4
0 2 -11 1167.91 153.305 1
0 2 11 1030.51 166.154 5
0 2 12 -53.6015 80.8159 4
0 2 12 -47.5363 69.649 5
0 2 13 838.075 173.103 4
0 2 13 914.215 183.409 5
0 2 14 29.6217 75.2416 5
0 2 15 282.935 119.333 5
0 -2 16 78.7114 92.2889 2
0 2 16 -55.5069 96.1868 5
0 -2 17 -91.3167 121.48 2
0 -2 17 18.2166 60.4455 7
0 2 17 -88.6679 79.5251 5
0 2 18 1291.7 263.387 5
0 -2 18 1869.16 153.709 7
0 -2 18 1528.43 306.454 2
0 -2 19 178.455 154.614 2
0 -2 19 182.001 63.0351 7
0 -2 20 6117.06 299.734 7
0 -2 21 243.585 71.2265 7
0 -2 22 1057.8 121.264 7
0 -2 23 -11.6381 48.6106 7
0 2 -24 171.489 56.1402 10
0 -2 24 353.488 74.2469 7
0 2 -25 131.76 56.4619 10
0 2 -26 101.152 50.1599 10
0 2 -27 367.257 62.714 10
0 2 -28 -47.0979 36.5215 10
0 2 -29 133.863 33.0422 10
0 3 0 -26.1013 70.3726 1
0 3 1 3224.9 291.163 1
0 3 -1 3183.31 284.777 1
0 3 1 3229.77 227.782 4
0 3 2 10375.7 543.032 1
0 3 -2 9348.3 524.31 1
0 3 2 10474.7 443.38 4
0 3 -3 -17.4438 73.9081 1
0 3 3 20.6908 80.0739 1
0 3 3 23.8969 41.9729 4
0 3 -4 1673.04 212.319 1
0 3 4 1693.85 211.136 1
0 3 4 1948.24 178.243 4
0 3 5 23126 914.902 1
0 3 -5 22773.1 926.221 1
0 3 5 25590.3 824.193 4
0 3 -6 101.789 79.5001 1
0 3 6 42.085 49.772 4
0 3 7 17.4597 39.5564 4
0 3 -7 87.0573 78.058 1
0 3 8 414.478 99.9639 4
0 3 -8 253.187 97.1811 1
0 3 9 2126.55 231.44 4
0 3 -9 2443.01 265.622 1
0 3 10 5855.79 401.119 4
0 3 -10 6096.87 433.131 1
0 3 -11 483.823 135.107 1
0 3 11 478.389 125.22 4
0 3 12 3007.74 313.782 4
0 -3 15 2148.54 336.304 2
0 3 -15 2520.1 176.697 9
0 3 -16 262.771 70.7948 9
0 -3 16 185.104 120.626 2
0 -3 16 325.076 70.8016 7
0 -3 17 9331.88 368.738 7
0 3 -17 8626.04 368.407 9
0 -3 17 8560.99 708.789 2
0 3 -18 459.501 83.0154 9
0 -3 18 391.877 79.3557 7
0 3 -19 1348.39 134.013 9
0 -3 19 1310.56 130.462 7
0 -3 20 51.7077 54.4961 7
0 3 -20 -38.8851 52.965 9
0 3 -21 744.91 95.0578 9
0 -3 21 688.569 96.3256 7
0 3 -22 90.3628 49.1306 9
0 -3 22 82.9126 53.9998 7
0 3 -23 272.672 69.6912 10
0 3 -24 164.441 58.2883 10
0 3 -25 36.4127 41.1685 10
0 3 -26 105.116 40.5361 10
0 3 -27 417.782 55.7181 10
0 3 -28 63.1802 26.6644 10
0 4 0 377.742 141.973 1
0 4 1 684.108 155.273 1
0 4 -1 531.368 159.314 1
0 4 -2 1622.75 252.031 1
0 -4 2 1949.44 217.559 2
0 4 2 1636.65 250.792 1
0 4 -3 782.958 175.246 1
0 4 3 586.511 173.794 1
0 4 -4 3652.79 375.29 1
0 4 4 3702.8 365.69 1
0 4 -5 200.256 105.095 1
0 4 -6 1192.94 210.478 1
0 4 -7 2561.91 315.843 1
0 4 -8 253.535 121.917 1
0 4 -9 4291.42 426.229 1
0 4 -10 149.838 110.456 1
0 4 -11 -144.869 133.675 1
0 -4 11 -9.59988 89.2248 2
0 -4 12 100.528 86.6581 2
0 4 -12 123.859 51.5755 9
0 -4 13 1685.82 306.144 2
0 4 -13 1539.59 142.199 9
0 -4 14 4491.04 497.765 2
0 4 -14 4532.11 253.279 9
0 4 -15 477.178 84.2638 9
0 4 -16 32.5888 59.0083 9
0 4 -17 2089.13 166.354 9
0 4 -18 3203.88 206.74 9
0 4 -19 90.0155 50.6941 10
0 4 -19 36.0875 42.6239 9
0 4 -20 -22.5333 43.9317 10
0 4 -20 74.4146 49.4411 9
0 4 -21 211.728 57.4992 10
0 4 -21 213.439 59.152 9
0 4 -22 -8.93838 39.2246 9
0 4 -22 38.8679 42.7017 10
0 4 -23 72.0289 38.9633 9
0 4 -23 134.785 47.0518 10
0 4 -24 320.63 50.8904 9
0 4 -24 311.899 58.0657 10
0 4 -25 34.4783 33.2617 10
0 4 -26 537.361 50.9896 10
0 5 0 -116.2 122.236 1
0 5 -1 1043.04 227.528 1
0 5 1 1636.35 287.811 1
0 5 -2 124.843 132.724 1
0 5 -3 455.264 160.395 1
0 5 -4 2318.39 172.846 6
0 5 -4 2407.93 174.905 12
0 5 -5 768.538 103.942 12
0 5 -5 735.133 198.387 1
0 5 -6 3412.97 203.972 9
0 5 -6 3227.32 402.32 1
0 5 6 3768.8 215.209 6
0 5 -6 3511.64 214.019 12
0 5 -7 118.148 57.6125 9
0 5 -7 74.8111 110.325 1
0 5 -7 68.1077 52.205 12
0 5 -8 -87.9567 155.39 1
0 5 -8 111.387 58.0351 12
0 5 -8 5.49137 48.3932 9
0 5 -9 18.1365 51.9837 11
0 5 -9 54.8709 49.9111 12
0 5 -9 53.6555 55.2034 9
0 5 -10 891.963 110.948 11
0 5 -10 640.624 97.0887 12
0 5 -10 763.954 230.865 1
0 5 -10 645.346 98.7169 9
0 5 -11 1200.73 130.282 11
0 5 -11 1116.9 124.268 9
0 5 -12 3445.25 220.902 9
0 5 -12 3482.36 216.837 11
0 5 -13 -42.8844 51.4174 11
0 5 -13 51.9242 51.6409 9
0 5 -14 110.583 58.4262 11
0 5 -14 15.0697 51.9961 9
0 5 -15 2406.67 168.106 11
0 5 -15 2155.24 171.068 9
0 5 -16 1309.49 131.571 9
0 5 -17 -17.5553 46.1232 9
0 5 -18 883.638 101.635 9
0 5 -19 1068.37 108.028 9
0 5 -20 7.02057 39.8743 9
0 5 -21 1027.15 93.1866 9
0 5 -22 268.671 51.869 9
0 5 -23 -10.6116 27.6186 9
0 6 0 2771.87 194.342 6
0 6 0 2562.13 195.598 12
0 6 -1 40.9732 43.308 12
0 6 1 -28.0509 47.8265 12
0 6 -1 136.025 61.8389 6
0 6 1 33.0311 49.1804 6
0 6 -2 717.608 108.241 12
0 6 2 787.474 106.734 6
0 6 2 684.139 105.637 12
0 6 3 1377.48 142.371 12
0 6 3 1705.79 150.136 6
0 6 -3 1332.52 140.997 12
0 6 4 765.367 105.631 6
0 6 -4 765.279 111.115 12
0 6 4 649.735 103.62 12
0 6 -5 -13.9232 46.6956 9
0 6 -5 70.3088 45.8876 12
0 6 5 -53.6714 60.2492 6
0 6 -6 337.914 77.2663 12
0 6 6 434.274 85.6565 6
0 6 -6 362.297 79.0272 9
0 6 -7 383.125 84.5765 11
0 6 -7 338.293 73.6784 9
0 6 7 535.234 87.7494 6
0 6 -8 105.734 55.3619 9
0 6 -8 141.587 69.7986 11
0 6 8 191.694 65.1328 6
0 6 -9 -79.2232 54.6118 11
0 6 -9 51.194 54.871 9
0 6 -10 277.336 70.2338 9
0 6 -10 113.155 49.3638 11
0 6 -11 20.0236 50.5937 11
0 6 -11 164.254 62.5798 9
0 6 -12 730.721 96.4931 9
0 6 -12 778.912 99.6874 11
0 6 -13 -12.0965 49.0864 9
0 6 -13 26.3421 47.597 11
0 6 -14 -73.3111 42.9076 11
0 6 -14 45.8177 40.9382 9
0 6 -15 630.417 81.2346 11
0 6 -15 473.48 75.6567 9
0 6 -16 15.7287 42.9831 9
0 6 -17 -19.2531 36.9568 9
0 6 -18 247.127 52.1998 9
0 6 -19 144.892 40.3996 9
0 6 -20 215.447 41.6043 9
0 6 -21 36.7481 24.1002 9
0 7 0 -87.0351 47.8073 11
0 7 -1 574.157 83.9963 11
0 7 1 568.252 91.4275 11
0 7 -2 16.506 50.1535 11
0 7 2 -20.0424 46.474 11
0 7 3 -26.49 51.1068 11
0 7 -3 1.55602 52.0056 11
0 7 4 -11.5273 43.5034 11
0 7 -4 -47.0992 51.5972 11
0 7 5 1162.26 109.569 11
0 7 -5 831.938 104.32 11
0 7 6 145.452 56.3234 11
0 7 -6 72.0307 50.6154 11
0 7 -7 151.014 56.1247 11
0 7 -8 341.729 70.2491 11
0 7 -8 424.614 65.9121 9
0 7 -9 272.681 66.1725 11
0 7 -9 163.176 46.6865 9
0 7 -10 250.158 59.9168 9
0 7 -10 239.92 57.3086 11
0 7 -11 614.543 78.5122 11
0 7 -11 453.232 63.2666 9
0 7 -12 86.1754 39.6923 9
0 7 -12 45.7083 35.5706 11
0 7 -13 248.11 52.9098 11
0 7 -13 198.287 46.6396 9
0 7 -14 15.5791 33.464 9
0 7 -15 69.4018 32.3208 9
0 7 -16 76.7796 26.3924 9
0 8 0 611.672 68.8273 11
0 8 -1 124.511 42.9762 11
0 8 1 107.041 39.5115 11
0 8 -2 159.332 43.989 11
0 8 2 159.701 42.8749 11
0 8 3 -29.9987 33.0199 11
0 8 -3 25.9973 33.6404 11
0 8 -4 25.936 32.0597 11
0 8 4 35.3686 27.3519 11
0 8 -5 259.606 47.2535 11
0 8 -6 286.256 47.3452 11
0 8 -7 60.2477 31.6492 11
0 8 -8 606.613 57.9696 11
1 0 -29 20.6655 24.2933 10
1 0 -28 -6.46807 34.0431 10
1 0 -27 176.948 51.3022 10
1 0 -26 -7.02586 44.9072 10
-1 0 26 67.0952 53.871 7
-1 0 25 564.9 88.9334 7
-1 0 24 0.93446 51.5968 7
-1 0 23 287.007 70.6321 7
-1 0 22 -79.2756 58.7342 7
-1 0 21 56.8918 50.4083 7
-1 0 20 -33.3665 47.6664 7
-1 0 19 2389.51 176.347 7
-1 0 18 24.9453 86.9194 2
-1 0 17 880.841 192.968 2
-1 0 16 -25.567 85.3178 2
-1 0 16 42.1524 95.7369 5
-1 0 15 1787.87 239.63 2
-1 0 15 1704.12 255.491 5
-1 0 14 -73.1455 88.9351 5
-1 0 14 -90.9773 98.6951 2
-1 0 13 10392 562.645 2
-1 0 13 10410.6 588.396 5
-1 0 12 -35.8856 70.3803 2
-1 0 12 -19.2204 67.8131 5
-1 0 11 652.451 143.169 5
-1 0 11 819.632 143.833 2
-1 0 10 -14.9634 53.5412 2
-1 0 10 -10.534 71.2001 5
-1 0 9 155.285 79.9565 5
-1 0 9 252.884 84.7815 2
-1 0 8 -94.7752 59.2048 2
-1 0 8 -63.2458 70.5399 5
-1 0 7 7122.75 322.257 2
-1 0 7 5200.81 305.188 5
-1 0 6 -21.7813 53.2912 5
-1 0 6 -32.2756 47.49 2
-1 0 5 23782.9 713.886 5
-1 0 5 25784.1 715.675 2
-1 0 4 6.48863 38.3031 2
-1 0 4 12.9898 44.2728 5
-1 0 3 7481.61 258.694 2
-1 0 3 7283.71 260.232 5
-1 0 2 12.909 21.1053 2
1 0 1 21424.3 543.216 4
1 0 2 80.268 35.2253 4
1 0 3 20208 577.777 4
1 0 4 49.4761 39.6354 4
1 0 5 270.84 76.3676 4
1 0 6 -58.3666 56.5915 4
1 0 7 20695.7 713.581 4
1 0 8 31.1851 69.3521 4
-1 0 -9 53991.9 1367.6 3
1 0 9 51130.8 1531.2 4
1 0 10 7.0051 53.1674 4
-1 0 -10 20.1449 40.7918 3
1 0 11 30329.3 1102.29 5
-1 0 -11 32166 909.624 3
1 0 12 -8.06657 72.2739 5
1 0 13 21358.2 924.03 5
1 0 14 175.256 103.386 5
1 0 15 992.202 204.332 5
1 0 16 -74.9321 110.105 5
1 0 16 -55.0074 90.7691 2
1 0 17 975.184 215.227 5
1 0 18 17.6603 77.4327 5
1 0 18 -78.1323 49.3512 7
1 0 19 1555.82 139.214 7
1 0 19 1701.43 296.71 5
1 0 20 -115.02 61.9065 7
1 0 21 130.783 49.3121 7
1 0 22 13.9765 47.1253 7
-1 0 -23 5.31017 49.0701 10
1 0 23 12.6268 54.5932 7
-1 0 -24 -66.3787 59.4787 10
-1 0 -25 11.0027 39.8296 10
-1 0 -26 23.2311 38.7578 10
-1 0 -27 -51.1333 39.9329 10
-1 0 -28 -53.5481 31.328 10
1 1 -29 19.9189 30.1792 10
1 1 -28 103.654 38.5627 10
1 1 -27 380.381 68.6253 10
-1 -1 26 325.761 70.3909 7
1 1 -26 368.117 76.9824 10
-1 -1 25 232.656 70.4942 7
-1 -1 24 226.705 68.3654 7
-1 1 24 312.292 76.4886 7
-1 -1 23 689.055 100.292 7
-1 1 23 815.553 106.321 7
-1 -1 22 1213.22 130.412 7
-1 1 22 1306.44 129.667 7
-1 1 21 36.1761 54.5012 7
-1 -1 21 -3.72578 54.013 7
-1 -1 20 642.581 98.8136 7
-1 1 20 837.461 103.73 7
-1 -1 20 994.719 247.282 2
-1 -1 19 139.972 119.667 2
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16 0 -8 343.447 76.9517 12
16 0 -7 -50.5226 50.2585 12
16 0 -6 2599.94 178.946 12
16 0 -5 -29.2915 45.4754 12
16 0 -4 54.4562 43.188 12
16 0 -3 67.1329 49.8072 12
-16 0 3 82.2235 44.4798 10
16 0 -2 153.957 51.9791 12
-16 0 2 222.68 59.7125 10
16 0 -1 22.669 46.9325 12
-16 0 1 -54.8415 52.5421 10
16 0 0 549.205 86.2869 12
-16 0 0 486.522 76.6491 10
16 0 1 19.7957 41.9551 12
-16 0 -1 9.66244 39.883 10
-16 0 -2 1332.33 116.46 10
16 0 2 1346.77 121.401 12
16 0 3 -7.33903 41.3236 12
-16 0 -3 61.327 46.4687 10
16 0 4 69.3911 42.2399 12
-16 0 -4 57.8232 41.7848 10
16 0 5 4.74933 37.1754 12
-16 0 -5 59.1971 41.2912 10
16 0 6 426.763 58.2933 12
-16 0 -6 365.061 62.0024 10
-16 0 -7 10.7128 33.8561 10
-16 0 -8 619.224 66.2675 10
-16 0 -9 6.07905 30.2966 10
-16 0 -10 151.935 31.8603 10
-16 -1 20 127.401 34.6098 7
-16 -1 19 321.179 47.1119 7
-16 -1 18 184.772 42.9297 8
-16 -1 17 252.937 52.5285 8
-16 -1 16 282.806 58.7668 8
-16 -1 15 260.131 59.8689 8
-16 1 14 255.549 48.1051 8
-16 -1 14 320.139 66.7546 8
16 1 -14 266.468 50.6396 12
16 -1 -13 11.6425 34.1595 12
-16 1 13 -44.4372 42.7299 8
-16 -1 13 9.27133 43.4453 8
16 1 -13 34.0429 40.6376 12
16 -1 -12 -70.479 44.899 12
-16 1 12 -2.61917 36.4034 8
-16 -1 12 -45.9675 39.1022 8
16 1 -12 -47.5433 37.6263 12
16 -1 -11 718.293 87.9201 12
-16 1 11 899.746 95.3134 8
-16 -1 11 626.647 91.4392 8
16 1 -11 698.394 87.4821 12
16 1 -10 351.638 67.2794 12
16 -1 -10 311.179 65.493 12
16 1 -9 57.3147 54.662 12
16 -1 -9 -24.6644 41.2963 12
16 1 -8 42.4795 49.5993 12
16 -1 -8 -53.6714 49.5829 12
16 1 -7 229.995 64.2074 12
16 -1 -7 277.206 64.1773 12
16 1 -6 121.379 57.8348 12
16 -1 -6 -8.2834 44.6205 12
16 1 -5 -18.7307 51.0768 12
16 -1 -5 47.6726 45.4135 12
16 1 -4 89.7736 53.8443 12
16 -1 -4 153.07 59.8985 12
-16 1 4 115.769 51.4167 10
16 1 -3 -31.0868 46.2754 12
16 -1 -3 27.0479 39.4221 12
-16 1 3 33.4394 38.4677 10
16 1 -2 -41.6304 47.1146 12
16 -1 -2 -31.4162 41.3491 12
-16 1 2 -8.39842 42.9296 10
16 1 -1 -23.878 53.3793 12
16 -1 -1 -43.2826 43.5443 12
-16 1 1 30.6752 47.3209 10
16 1 0 13.3874 41.7013 12
16 -1 0 44.6563 51.2658 12
-16 1 0 125.413 52.7486 10
16 1 1 187.273 57.0081 12
16 -1 1 149.297 56.7686 12
-16 -1 -1 179.935 56.4279 10
-16 1 -1 171.329 49.3858 10
16 1 2 -29.9391 42.4404 12
16 -1 2 44.8008 43.5193 12
-16 -1 -2 39.8657 41.3341 10
-16 1 -2 16.2069 38.5247 10
16 1 3 88.5045 48.9943 12
16 -1 3 69.4786 42.3213 12
-16 -1 -3 21.4923 38.6589 10
-16 1 -3 54.9722 37.9843 10
16 -1 4 292.091 66.7065 12
-16 -1 -4 446.493 68.4055 10
-16 1 -4 337.959 65.805 10
16 1 4 367.478 63.2762 12
16 -1 5 94.9081 43.5841 12
-16 -1 -5 152.212 46.2226 10
-16 1 -5 95.6966 45.1216 10
16 1 5 122.253 44.8427 12
16 -1 6 392.645 57.2408 12
-16 -1 -6 547.239 63.4151 10
-16 1 -6 460.007 66.34 10
-16 -1 -7 52.8558 33.4194 10
-16 1 -7 48.4659 35.2947 10
-16 1 -8 362.43 57.7486 10
-16 1 -9 26.7777 32.2101 10
-16 1 -10 153.294 35.1011 10
-16 1 -11 171.171 29.9942 10
-16 -2 19 159.736 35.056 7
-16 -2 18 -15.9777 29.051 7
-16 -2 18 -4.63144 27.5315 8
-16 -2 17 54.7996 35.3474 8
-16 -2 16 22.7172 36.166 8
-16 -2 15 -24.5457 37.916 8
-16 -2 14 147.154 48.7887 8
16 2 -14 141.896 46.3082 12
-16 -2 13 270.899 58.7172 8
16 2 -13 349.871 58.158 12
16 -2 -12 501.797 66.1984 12
-16 -2 12 455.572 73.3394 8
16 2 -12 436.331 64.9318 12
16 -2 -11 643.58 79.1505 12
-16 -2 11 519.627 79.9402 8
16 2 -11 741.306 86.0514 12
16 -2 -10 -50.3462 43.4879 12
-16 -2 10 -38.2033 45.1026 8
16 2 -10 16.8742 42.4049 12
16 -2 -9 -4.99078 42.4568 12
-16 -2 9 32.5607 42.8142 8
16 2 -9 0.1947 43.808 12
16 2 -8 90.8781 49.8871 12
16 2 -7 257.606 60.5219 12
16 2 -6 302.854 71.3298 12
16 2 -5 -10.7624 41.1921 12
16 2 -4 882.969 102.978 12
-16 2 3 116.196 46.1544 10
16 2 -3 124.268 45.2817 12
-16 2 2 10.3942 37.9789 10
16 2 -2 -14.5685 41.2073 12
-16 2 1 167.033 55.1537 10
16 2 -1 209.471 60.0018 12
-16 2 0 58.2993 42.0477 10
16 2 0 32.3014 46.4541 12
-16 2 -1 -68.7592 47.0125 10
16 2 1 64.4259 43.034 12
-16 2 -2 123.983 52.7165 10
16 2 2 -36.1084 39.8408 12
16 -2 3 205.031 50.5801 12
-16 2 -3 148.065 49.886 10
16 2 3 128.573 43.7558 12
16 -2 4 10.8071 36.3601 12
-16 2 -4 47.0799 36.7508 10
16 2 4 106.493 43.6472 12
16 -2 5 192.369 43.8876 12
-16 2 -5 265.018 52.5357 10
16 2 5 184.59 40.4445 12
16 -2 6 142.734 37.9531 12
-16 2 -6 128.066 41.3028 10
-16 2 -7 92.8474 38.7039 10
-16 2 -8 197.926 40.0897 10
-16 2 -9 60.9368 27.0404 10
-16 2 -10 36.1536 21.5268 10
16 3 -17 672.051 52.569 9
-16 -3 16 106.311 28.9424 7
-16 -3 16 22.1822 22.5055 8
-16 -3 15 82.65 37.3383 8
-16 -3 14 -4.43021 30.4462 8
-16 -3 13 300.363 52.4148 8
16 3 -13 600.089 59.8813 12
-16 -3 12 166.424 47.7928 8
16 3 -12 120.239 37.7151 12
16 -3 -11 559.667 64.0762 12
-16 -3 11 635.84 76.4761 8
16 3 -11 804.762 78.1475 12
16 -3 -10 -24.2718 31.8051 12
-16 -3 10 -14.1212 33.6616 8
16 3 -10 81.8359 40.7749 12
-16 -3 9 118.888 46.3698 8
16 3 -9 67.341 41.2902 12
-16 -3 8 30.7114 38.3548 8
16 3 -8 64.1592 45.3119 12
-16 -3 7 -29.0334 37.1387 8
16 3 -7 -3.11246 43.6959 12
-16 -3 6 39.0384 37.1679 8
16 3 -6 72.6004 43.2619 12
-16 -3 5 113.293 44.6543 8
16 3 -5 206.515 58.8477 12
-16 -3 4 33.7773 39.4238 8
16 3 -4 42.4278 45.7551 12
16 3 -3 14.6626 37.8469 12
16 3 -2 -9.86568 41.3962 12
16 3 -1 1216.21 105.069 12
16 3 0 120.063 43.9474 12
-16 3 -1 80.7357 38.2189 10
16 3 1 -11.5706 33.1174 12
-16 3 -2 529.253 62.8666 10
16 3 2 585.509 69.0495 12
-16 3 -3 725.912 68.2293 10
16 3 3 670.611 66.2752 12
16 -3 4 63.6487 35.2038 12
-16 3 -4 -3.69417 27.8493 10
16 -3 5 161.207 33.0274 12
-16 3 -5 243.431 39.4177 10
-16 3 -6 51.5098 27.3318 10
16 4 -10 126.066 34.7666 12
16 -4 -9 275.598 41.3762 12
16 4 -9 469.435 54.9895 12
16 -4 -8 40.6963 28.2778 12
16 4 -8 85.3523 33.749 12
16 4 -7 432.636 57.0961 12
16 4 -6 102.714 35.1128 12
16 4 -5 84.1099 34.284 12
16 4 -4 90.4713 38.5193 12
16 4 -3 3.43442 29.5259 12
16 4 -2 127.985 37.5238 12
16 4 -1 4.87952 30.2302 12
16 4 0 -2.28499 28.0612 12
16 4 1 372.419 41.5823 12
16 -4 2 109.361 27.7916 12
-17 0 17 916.205 64.8798 7
-17 0 16 40.6935 23.4412 8
-17 0 15 209.747 47.4404 8
-17 0 14 37.8457 31.3392 8
-17 0 13 528.059 68.8429 8
17 0 -13 564.441 62.7369 12
-17 0 12 -28.1771 39.152 8
17 0 -12 -50.4885 36.23 12
17 0 -11 83.8737 40.6092 12
-17 0 11 93.8384 46.5246 8
17 0 -10 -11.6997 36.3406 12
-17 0 10 -36.8762 40.8077 8
17 0 -9 151.104 47.6769 12
17 0 -8 7.83838 36.7883 12
17 0 -7 293.856 63.9007 12
17 0 -6 -6.87841 40.7358 12
17 0 -5 1095.99 107.245 12
17 0 -4 -11.7426 41.2922 12
17 0 -3 370.196 66.7918 12
17 0 -2 75.0647 50.2132 12
17 0 -1 19.3682 42.2849 12
17 0 0 11.4441 40.3527 12
17 0 1 138.966 47.007 12
-17 0 -1 174.091 45.5311 10
17 0 2 31.2067 37.6883 12
-17 0 -2 63.3205 40.1246 10
17 0 3 24.6546 35.0076 12
-17 0 -3 -7.39172 32.9136 10
17 0 4 -14.513 32.3093 12
-17 0 -4 -51.602 34.4266 10
-17 0 -5 571.569 60.6671 10
17 0 5 528.842 54.0379 12
-17 0 -6 63.0395 31.9426 10
-17 -1 18 14.5969 23.8809 7
-17 -1 17 333.793 46.0545 7
-17 -1 17 116.502 31.7226 8
-17 -1 16 3.41919 26.5536 8
-17 -1 15 31.3286 29.2423 8
-17 -1 14 454.468 64.3599 8
-17 -1 13 436.359 65.5157 8
17 1 -13 431.883 54.2655 12
17 -1 -12 655.972 68.3277 12
-17 1 12 571.199 65.1379 8
-17 -1 12 523.123 71.9662 8
17 1 -12 594.339 68.2718 12
17 -1 -11 613.301 71.3409 12
-17 1 11 488.71 63.9787 8
-17 -1 11 645.738 81.4132 8
17 1 -11 682.5 75.8015 12
17 -1 -10 124.175 43.5516 12
-17 1 10 167.256 44.7717 8
-17 -1 10 210.118 53.264 8
17 1 -10 240.819 52.5385 12
17 -1 -9 -35.4019 41.8878 12
17 1 -9 -3.22499 39.5166 12
17 1 -8 269.065 61.0782 12
17 -1 -8 252.374 55.2953 12
17 1 -7 4.92171 39.6991 12
17 -1 -7 -11.2672 44.1052 12
17 1 -6 309.886 68.0411 12
17 -1 -6 143.547 56.0129 12
17 1 -5 130.885 54.1924 12
17 -1 -5 94.6946 46.2895 12
17 1 -4 48.238 38.975 12
17 -1 -4 -36.0151 35.5639 12
17 1 -3 23.913 35.8556 12
17 -1 -3 41.5334 41.723 12
17 1 -2 69.9255 44.7705 12
17 -1 -2 103.506 49.7258 12
17 1 -1 1079.11 105.259 12
17 -1 -1 1020.65 99.4937 12
17 1 0 -30.433 39.2749 12
17 -1 0 -5.9867 38.2573 12
-17 1 0 43.9908 41.623 10
17 -1 1 656.648 78.9808 12
-17 1 -1 692.873 77.7797 10
17 1 1 746.991 81.7221 12
17 -1 2 18.1579 36.1751 12
-17 1 -2 -54.4943 41.7961 10
17 1 2 63.3265 39.4835 12
17 -1 3 176.705 43.977 12
-17 1 -3 193.021 45.2096 10
17 1 3 139.107 42.2284 12
17 -1 4 200.323 44.5253 12
-17 1 -4 187.174 45.9117 10
17 1 4 66.6776 31.0681 12
17 -1 5 137.301 35.7162 12
-17 1 -5 97.0687 34.3348 10
-17 1 -6 45.3569 31.9644 10
-17 1 -7 182.423 36.3211 10
-17 1 -8 -20.849 19.3975 10
-17 -2 16 46.7695 24.4327 8
-17 -2 15 -4.08639 27.0302 8
-17 -2 14 282.725 53.2962 8
-17 -2 13 58.1884 37.0452 8
17 2 -13 32.2409 25.7082 12
17 -2 -12 -20.359 24.5737 12
-17 -2 12 2.39902 30.5059 8
17 2 -12 34.2736 29.3354 12
17 -2 -11 236.294 42.9309 12
-17 -2 11 226.738 52.2982 8
17 2 -11 187.412 43.6582 12
17 -2 -10 197.585 43.8346 12
-17 -2 10 133.747 43.8286 8
17 2 -10 114.709 44.034 12
17 -2 -9 60.5941 38.8191 12
-17 -2 9 27.7289 37.8349 8
17 2 -9 -22.6143 34.5768 12
17 -2 -8 -15.2176 35.4642 12
-17 -2 8 74.2059 40.338 8
17 2 -8 71.8745 42.7884 12
17 -2 -7 96.3137 41.0199 12
-17 -2 7 36.2634 36.214 8
17 2 -7 -10.8244 36.7775 12
17 -2 -6 3.66113 38.8892 12
17 2 -6 -25.3486 41.2389 12
17 -2 -5 61.5864 36.3857 12
17 2 -5 100.961 48.8087 12
17 -2 -4 14.1023 38.3792 12
17 2 -4 72.1053 40.6188 12
17 -2 -3 136.347 47.2137 12
17 2 -3 118.437 44.6619 12
17 -2 -2 119.742 42.2531 12
17 2 -2 196.947 51.4437 12
17 -2 -1 745.475 83.299 12
17 2 -1 703.681 79.345 12
17 -2 0 67.2317 42.8996 12
17 2 0 23.9816 33.081 12
17 -2 1 71.6379 35.6315 12
-17 2 -1 78.4198 33.6079 10
17 2 1 145.04 42.4445 12
17 -2 2 131.106 38.6261 12
-17 2 -2 70.4549 34.545 10
17 2 2 96.0209 35.4128 12
17 -2 3 136.829 37.6663 12
-17 2 -3 96.9188 35.5467 10
17 2 3 87.4875 29.6159 12
-17 2 -4 1252.54 84.9716 10
17 -2 4 1103.83 75.911 12
-17 2 -5 225.618 40.2242 10
-17 2 -6 196.584 33.2811 10
-17 -3 12 169.646 36.7512 8
-17 -3 11 8.81259 24.9943 8
17 3 -11 23.6053 22.745 12
-17 -3 10 141.65 42.1131 8
17 3 -10 397.598 50.6437 12
17 -3 -9 48.4493 32.0986 12
-17 -3 9 51.482 32.0483 8
17 3 -9 60.626 34.4815 12
17 -3 -8 270.177 45.702 12
-17 -3 8 209.809 44.9912 8
17 3 -8 365.509 52.5483 12
17 -3 -7 20.0464 28.3063 12
-17 -3 7 -21.3035 30.9474 8
17 3 -7 -9.95062 30.4305 12
17 -3 -6 280.112 51.9893 12
-17 -3 6 130.44 37.4496 8
17 3 -6 348.123 55.2617 12
17 -3 -5 69.0319 36.9277 12
-17 -3 5 2.94018 25.0824 8
17 3 -5 79.6885 36.9752 12
17 -3 -4 42.3359 34.4852 12
-17 -3 4 -0.80045 24.7614 8
17 3 -4 30.3339 28.951 12
17 -3 -3 64.3337 37.3321 12
-17 -3 3 16.1711 24.948 8
17 3 -3 24.8373 32.2281 12
17 -3 -2 185.404 45.4262 12
-17 -3 2 84.7842 28.3581 8
17 3 -2 222.037 46.717 12
17 -3 -1 210.999 46.065 12
17 3 -1 291.029 45.9445 12
17 3 0 717.336 62.4991 12
17 -3 0 730.966 67.0438 12
17 -3 1 369.376 47.8917 12
17 3 1 374.815 42.6707 12
17 -3 2 -37.241 24.2428 12
-18 0 13 55.1229 26.0332 8
-18 0 12 -13.5609 24.6719 8
-18 0 11 16.0329 32.3581 8
18 0 -11 5.50432 25.4799 12
-18 0 10 483.9 63.4021 8
18 0 -10 544.097 61.5379 12
-18 0 9 49.2017 31.7923 8
18 0 -9 -6.02182 33.5372 12
18 0 -8 380.918 57.7242 12
-18 0 8 322.096 54.6034 8
18 0 -7 0.13734 35.3515 12
18 0 -6 -10.7111 37.4001 12
18 0 -5 12.6651 33.5291 12
18 0 -4 12.0367 33.4231 12
18 0 -3 8.46721 34.5402 12
18 0 -2 29.3165 34.0083 12
18 0 -1 31.3795 32.8854 12
18 0 0 1777.74 109.375 12
18 0 1 45.5034 29.3956 12
18 0 2 99.0701 32.1207 12
-18 -1 14 33.336 18.4922 8
-18 -1 13 60.9432 26.7328 8
-18 -1 12 76.2546 32.9924 8
-18 -1 11 72.4277 33.903 8
18 -1 -11 61.5499 25.6082 12
18 -1 -10 428.692 54.5137 12
-18 -1 10 216.371 46.53 8
18 1 -10 468.217 56.573 12
18 -1 -9 379.616 52.9557 12
-18 1 9 191.778 39.1568 8
-18 -1 9 223.961 52.3641 8
18 1 -9 361.97 52.6335 12
18 -1 -8 26.4979 30.4787 12
-18 1 8 -17.2424 27.949 8
-18 -1 8 65.3082 35.7576 8
18 1 -8 -6.88784 33.7518 12
18 -1 -7 68.3205 35.597 12
-18 1 7 -5.39321 26.8025 8
18 1 -7 24.9866 32.3713 12
18 -1 -6 255.427 49.6421 12
18 1 -6 202.302 47.4082 12
18 -1 -5 420.838 60.5589 12
18 1 -5 535.506 66.972 12
18 -1 -4 10.7699 33.2213 12
18 1 -4 27.0964 34.8946 12
18 -1 -3 74.4967 39.9414 12
18 1 -3 17.6723 34.238 12
18 -1 -2 15.4833 34.112 12
18 1 -2 17.938 33.4972 12
18 -1 -1 58.5574 34.1241 12
18 1 -1 -23.124 37.3884 12
18 -1 0 45.8313 33.2804 12
18 1 0 24.27 29.2704 12
18 -1 1 147.721 35.6619 12
18 1 1 117.71 34.9153 12
18 -1 2 183.955 33.2557 12
-18 -2 12 76.6361 25.1457 8
-18 -2 11 4.35281 19.7937 8
-18 -2 10 136.089 39.1134 8
18 2 -10 408.266 43.4999 12
18 -2 -9 17.9098 22.1207 12
-18 -2 9 38.9553 27.434 8
18 2 -9 37.9197 27.6806 12
18 -2 -8 204.431 40.6192 12
-18 -2 8 160.117 42.519 8
18 2 -8 299.563 44.9091 12
18 -2 -7 -33.3387 26.2577 12
-18 -2 7 -20.3248 24.2912 8
18 2 -7 28.5435 27.5738 12
18 -2 -6 -35.2733 31.8457 12
-18 -2 6 -14.6582 27.4202 8
18 2 -6 -50.2733 32.6365 12
18 -2 -5 -49.1265 33.705 12
-18 -2 5 34.1502 31.2802 8
18 2 -5 1.66675 28.4702 12
18 -2 -4 16.3234 29.9008 12
-18 -2 4 51.3878 31.1968 8
18 2 -4 -14.354 32.2015 12
18 -2 -3 10.4064 27.6563 12
-18 -2 3 -11.497 23.3444 8
18 2 -3 -62.4816 29.5415 12
18 -2 -2 323.454 47.4867 12
-18 -2 2 214.421 42.3692 8
18 2 -2 418.758 50.5532 12
18 -2 -1 442.873 51.43 12
-18 -2 1 184.899 37.5037 8
18 2 -1 394.187 45.3081 12
18 -2 0 192.079 36.6041 12
18 2 0 170.942 31.2911 12
19 0 -7 682.341 53.8419 12
19 0 -6 27.5973 21.6106 12
19 0 -5 37.3572 20.926 12
19 0 -4 6.73489 22.1841 12
19 0 -3 -28.5663 19.6475 12
#######################################################################
#
# 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_sua1
_database_code_depnum_ccdc_archive 'CCDC 1412577'
_audit_update_record
;
2015-07-13 deposited with the CCDC.
2015-08-28 downloaded from the CCDC.
;
_audit_creation_date 2015-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C27 H34 N2 O4'
_chemical_formula_sum 'C27 H34 N2 O4'
_chemical_formula_weight 450.56
_chemical_melting_point ?
_chemical_oxdiff_formula 'C20 H20 N2 O2 '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 10.0556(2)
_cell_length_b 23.0371(5)
_cell_length_c 10.8204(3)
_cell_angle_alpha 90
_cell_angle_beta 106.221(3)
_cell_angle_gamma 90
_cell_volume 2406.78(10)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 7889
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 78.0570
_cell_measurement_theta_min 3.8160
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.667
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.82476
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.243
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 968
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.09
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0376
_diffrn_reflns_av_unetI/netI 0.0296
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -28
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 19755
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 79.932
_diffrn_reflns_theta_min 3.838
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 150(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.2833
_diffrn_detector_type Ruby
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -107.00 -13.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -38.5000 -57.0000 -120.0000 94
#__ type_ start__ end____ width___ exp.time_
2 omega -64.00 30.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -38.5000 57.0000 30.0000 94
#__ type_ start__ end____ width___ exp.time_
3 omega 35.00 109.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ frames
- 114.0000 -95.0000 0.0000 74
#__ type_ start__ end____ width___ exp.time_
4 omega 41.00 91.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ frames
- 114.0000 -30.0000 -120.0000 50
#__ type_ start__ end____ width___ exp.time_
5 omega 41.00 91.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ frames
- 114.0000 -30.0000 -30.0000 50
#__ type_ start__ end____ width___ exp.time_
6 omega 41.00 91.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ frames
- 114.0000 -30.0000 120.0000 50
#__ type_ start__ end____ width___ exp.time_
7 omega 100.00 178.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ frames
- 114.0000 111.0000 0.0000 78
#__ type_ start__ end____ width___ exp.time_
8 omega 93.00 178.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ frames
- 114.0000 30.0000 90.0000 85
#__ type_ start__ end____ width___ exp.time_
9 omega 100.00 178.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ frames
- 114.0000 111.0000 30.0000 78
#__ type_ start__ end____ width___ exp.time_
10 omega 13.00 115.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 43.3790 77.0000 30.0000 102
#__ type_ start__ end____ width___ exp.time_
11 omega -25.00 69.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 43.3790 -57.0000 120.0000 94
#__ type_ start__ end____ width___ exp.time_
12 omega 93.00 173.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ frames
- 114.0000 30.0000 -60.0000 80
#__ type_ start__ end____ width___ exp.time_
13 omega 46.00 98.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ frames
- 114.0000 -45.0000 30.0000 52
#__ type_ start__ end____ width___ exp.time_
14 omega 41.00 116.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ frames
- 114.0000 -111.0000 -180.0000 75
#__ type_ start__ end____ width___ exp.time_
15 omega 93.00 178.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ frames
- 114.0000 30.0000 -180.0000 85
#__ type_ start__ end____ width___ exp.time_
16 omega -50.00 33.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -38.5000 38.0000 -60.0000 83
#__ type_ start__ end____ width___ exp.time_
17 omega 18.00 112.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 43.3790 57.0000 150.0000 94
#__ type_ start__ end____ width___ exp.time_
18 omega 74.00 94.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ frames
- 114.0000 15.0000 30.0000 20
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 0.0857872000
_diffrn_orient_matrix_UB_12 0.0321517000
_diffrn_orient_matrix_UB_13 0.1210362000
_diffrn_orient_matrix_UB_21 -0.1345391000
_diffrn_orient_matrix_UB_22 0.0210321000
_diffrn_orient_matrix_UB_23 0.0273178000
_diffrn_orient_matrix_UB_31 -0.0013005000
_diffrn_orient_matrix_UB_32 -0.0546782000
_diffrn_orient_matrix_UB_33 0.0813154000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4150
_reflns_number_total 5102
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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, 2015)'
_refine_diff_density_max 0.277
_refine_diff_density_min -0.198
_refine_diff_density_rms 0.037
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.037
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 306
_refine_ls_number_reflns 5102
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0515
_refine_ls_R_factor_gt 0.0406
_refine_ls_restrained_S_all 1.037
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+0.4731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1049
_refine_ls_wR_factor_ref 0.1136
_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 C(H,H,H) groups, All C(H,H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
C8(H8A,H8B), C9(H9A,H9B), C19(H19A,H19B), C20(H20A,H20B)
2.b Aromatic/amide H refined with riding coordinates:
C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C23(H23), C24(H24),
C25(H25), C26(H26), C27(H27)
2.c Idealised Me refined as rotating group:
C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C29(H29A,H29B,H29C),
C30(H30A,H30B,H30C)
;
_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
C1 C 0.67027(16) 0.62760(7) -0.00458(17) 0.0433(4) Uani 1 1 d . . . . .
H1A H 0.6129 0.6088 -0.0826 0.065 Uiso 1 1 calc GR . . . .
H1B H 0.7675 0.6267 -0.0051 0.065 Uiso 1 1 calc GR . . . .
H1C H 0.6406 0.6680 -0.0019 0.065 Uiso 1 1 calc GR . . . .
C2 C 0.65435(14) 0.59548(6) 0.11324(15) 0.0349(3) Uani 1 1 d . . . . .
C3 C 0.69536(16) 0.53214(7) 0.11154(16) 0.0397(3) Uani 1 1 d . . . . .
H3A H 0.6847 0.5127 0.1888 0.060 Uiso 1 1 calc GR . . . .
H3B H 0.7921 0.5296 0.1099 0.060 Uiso 1 1 calc GR . . . .
H3C H 0.6357 0.5132 0.0348 0.060 Uiso 1 1 calc GR . . . .
C4 C 0.73130(16) 0.62679(7) 0.23578(17) 0.0435(4) Uani 1 1 d . . . . .
H4A H 0.6881 0.6647 0.2392 0.065 Uiso 1 1 calc GR . . . .
H4B H 0.8282 0.6323 0.2367 0.065 Uiso 1 1 calc GR . . . .
H4C H 0.7272 0.6036 0.3106 0.065 Uiso 1 1 calc GR . . . .
O5 O 0.50283(10) 0.59874(4) 0.09378(10) 0.0350(2) Uani 1 1 d . . . . .
C6 C 0.44514(14) 0.57585(6) 0.18051(13) 0.0316(3) Uani 1 1 d . . . . .
O6 O 0.50425(10) 0.55535(5) 0.28459(10) 0.0380(2) Uani 1 1 d . . . . .
N7 N 0.30446(12) 0.57756(5) 0.13251(11) 0.0309(2) Uani 1 1 d . . . . .
C8 C 0.22062(15) 0.61319(7) 0.02625(14) 0.0358(3) Uani 1 1 d . . . . .
H8A H 0.2013 0.5944 -0.0592 0.043 Uiso 1 1 calc R . . . .
H8B H 0.2562 0.6531 0.0239 0.043 Uiso 1 1 calc R . . . .
C9 C 0.10071(14) 0.60876(6) 0.08845(14) 0.0340(3) Uani 1 1 d . . . . .
H9A H 0.0258 0.5821 0.0432 0.041 Uiso 1 1 calc R . . . .
H9B H 0.0629 0.6468 0.1047 0.041 Uiso 1 1 calc R . . . .
C10 C 0.20559(13) 0.58142(6) 0.21042(13) 0.0290(3) Uani 1 1 d . . . . .
C11 C 0.15791(13) 0.52473(6) 0.25320(13) 0.0302(3) Uani 1 1 d . . . . .
C12 C 0.21293(15) 0.47187(6) 0.23092(15) 0.0373(3) Uani 1 1 d . . . . .
H12 H 0.2854 0.4708 0.1904 0.045 Uiso 1 1 calc R . . . .
C13 C 0.16260(18) 0.42039(7) 0.26765(17) 0.0453(4) Uani 1 1 d . . . . .
H13 H 0.2005 0.3843 0.2516 0.054 Uiso 1 1 calc R . . . .
C14 C 0.05757(17) 0.42140(7) 0.32749(17) 0.0452(4) Uani 1 1 d . . . . .
H14 H 0.0249 0.3863 0.3545 0.054 Uiso 1 1 calc R . . . .
C15 C 0.00076(16) 0.47387(7) 0.34763(16) 0.0421(3) Uani 1 1 d . . . . .
H15 H -0.0726 0.4747 0.3871 0.051 Uiso 1 1 calc R . . . .
C16 C 0.04988(14) 0.52536(7) 0.31080(14) 0.0359(3) Uani 1 1 d . . . . .
H16 H 0.0098 0.5612 0.3248 0.043 Uiso 1 1 calc R . . . .
C17 C 0.25522(13) 0.62832(6) 0.31562(13) 0.0286(3) Uani 1 1 d . . . . .
O17 O 0.25852(10) 0.67917(4) 0.27901(9) 0.0331(2) Uani 1 1 d . . . . .
N18 N 0.28941(11) 0.61381(5) 0.44023(11) 0.0284(2) Uani 1 1 d . . . . .
C19 C 0.33914(14) 0.55939(6) 0.51145(13) 0.0319(3) Uani 1 1 d . . . . .
H19A H 0.4138 0.5398 0.4841 0.038 Uiso 1 1 calc R . . . .
H19B H 0.2641 0.5319 0.5133 0.038 Uiso 1 1 calc R . . . .
C20 C 0.39141(15) 0.59540(6) 0.63542(13) 0.0331(3) Uani 1 1 d . . . . .
H20A H 0.4933 0.5947 0.6718 0.040 Uiso 1 1 calc R . . . .
H20B H 0.3445 0.5861 0.7021 0.040 Uiso 1 1 calc R . . . .
C21 C 0.33592(14) 0.65172(6) 0.55774(13) 0.0299(3) Uani 1 1 d . . . . .
C22 C 0.21343(14) 0.67964(6) 0.59235(13) 0.0309(3) Uani 1 1 d . . . . .
C23 C 0.09703(15) 0.69863(6) 0.49831(14) 0.0352(3) Uani 1 1 d . . . . .
H23 H 0.0921 0.6934 0.4101 0.042 Uiso 1 1 calc R . . . .
C24 C -0.01234(17) 0.72523(7) 0.53157(16) 0.0409(3) Uani 1 1 d . . . . .
H24 H -0.0913 0.7378 0.4660 0.049 Uiso 1 1 calc R . . . .
C25 C -0.00690(17) 0.73349(7) 0.65951(17) 0.0428(4) Uani 1 1 d . . . . .
H25 H -0.0810 0.7522 0.6821 0.051 Uiso 1 1 calc R . . . .
C26 C 0.10774(18) 0.71417(7) 0.75432(16) 0.0416(3) Uani 1 1 d . . . . .
H26 H 0.1119 0.7194 0.8424 0.050 Uiso 1 1 calc R . . . .
C27 C 0.21646(16) 0.68729(6) 0.72128(14) 0.0369(3) Uani 1 1 d . . . . .
H27 H 0.2941 0.6739 0.7872 0.044 Uiso 1 1 calc R . . . .
O28 O 0.39188(11) 0.74732(4) 0.48198(11) 0.0381(2) Uani 1 1 d . . . . .
C28 C 0.45105(14) 0.69731(6) 0.55445(14) 0.0339(3) Uani 1 1 d . . . . .
C29 C 0.55991(15) 0.67076(7) 0.49670(16) 0.0411(3) Uani 1 1 d . . . . .
H29A H 0.5179 0.6626 0.4052 0.062 Uiso 1 1 calc GR . . . .
H29B H 0.5948 0.6346 0.5418 0.062 Uiso 1 1 calc GR . . . .
H29C H 0.6367 0.6981 0.5061 0.062 Uiso 1 1 calc GR . . . .
C30 C 0.51855(17) 0.71977(7) 0.68928(16) 0.0441(4) Uani 1 1 d . . . . .
H30A H 0.5922 0.7473 0.6869 0.066 Uiso 1 1 calc GR . . . .
H30B H 0.5581 0.6872 0.7458 0.066 Uiso 1 1 calc GR . . . .
H30C H 0.4489 0.7394 0.7222 0.066 Uiso 1 1 calc GR . . . .
H28 H 0.341(2) 0.7326(10) 0.406(2) 0.066 Uiso 1 1 d R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0417(8) 0.0427(8) 0.0512(9) 0.0042(7) 0.0225(7) 0.0016(6)
C2 0.0296(6) 0.0353(7) 0.0424(8) -0.0016(6) 0.0142(6) 0.0010(5)
C3 0.0372(7) 0.0373(8) 0.0460(8) -0.0045(6) 0.0138(6) 0.0019(6)
C4 0.0376(7) 0.0425(8) 0.0512(9) -0.0099(7) 0.0136(7) -0.0009(6)
O5 0.0307(5) 0.0397(5) 0.0368(5) 0.0029(4) 0.0129(4) 0.0020(4)
C6 0.0340(6) 0.0293(7) 0.0330(7) -0.0034(5) 0.0119(5) 0.0011(5)
O6 0.0344(5) 0.0454(6) 0.0340(5) 0.0041(4) 0.0092(4) 0.0036(4)
N7 0.0319(5) 0.0329(6) 0.0288(6) 0.0001(4) 0.0100(4) 0.0011(4)
C8 0.0386(7) 0.0401(8) 0.0274(7) 0.0024(6) 0.0071(6) 0.0009(6)
C9 0.0306(6) 0.0369(7) 0.0319(7) 0.0015(6) 0.0046(5) 0.0015(5)
C10 0.0270(6) 0.0308(6) 0.0292(6) -0.0004(5) 0.0076(5) 0.0021(5)
C11 0.0282(6) 0.0323(7) 0.0281(6) -0.0017(5) 0.0045(5) -0.0011(5)
C12 0.0397(7) 0.0341(7) 0.0393(8) -0.0022(6) 0.0131(6) 0.0005(6)
C13 0.0530(9) 0.0318(8) 0.0512(9) 0.0004(7) 0.0145(7) 0.0002(7)
C14 0.0497(9) 0.0385(8) 0.0467(9) 0.0033(7) 0.0121(7) -0.0116(7)
C15 0.0375(7) 0.0477(9) 0.0420(8) -0.0017(7) 0.0124(6) -0.0100(6)
C16 0.0314(6) 0.0383(8) 0.0380(8) -0.0036(6) 0.0099(6) -0.0017(6)
C17 0.0269(6) 0.0284(6) 0.0318(7) 0.0017(5) 0.0102(5) 0.0026(5)
O17 0.0395(5) 0.0283(5) 0.0316(5) 0.0032(4) 0.0100(4) 0.0013(4)
N18 0.0310(5) 0.0251(5) 0.0284(6) 0.0001(4) 0.0071(4) 0.0005(4)
C19 0.0354(6) 0.0264(6) 0.0326(7) 0.0040(5) 0.0076(5) 0.0020(5)
C20 0.0369(7) 0.0296(7) 0.0308(7) 0.0041(5) 0.0062(5) 0.0000(5)
C21 0.0345(6) 0.0273(6) 0.0268(6) 0.0001(5) 0.0067(5) -0.0017(5)
C22 0.0377(7) 0.0240(6) 0.0325(7) -0.0003(5) 0.0124(5) -0.0043(5)
C23 0.0423(7) 0.0305(7) 0.0355(7) 0.0025(5) 0.0154(6) 0.0014(6)
C24 0.0443(8) 0.0353(8) 0.0464(9) 0.0062(6) 0.0181(7) 0.0066(6)
C25 0.0518(9) 0.0318(7) 0.0528(9) -0.0015(6) 0.0279(7) 0.0033(6)
C26 0.0569(9) 0.0346(7) 0.0390(8) -0.0067(6) 0.0226(7) -0.0044(7)
C27 0.0446(8) 0.0324(7) 0.0352(7) -0.0032(6) 0.0134(6) -0.0050(6)
O28 0.0452(6) 0.0290(5) 0.0396(6) 0.0033(4) 0.0111(5) -0.0042(4)
C28 0.0361(7) 0.0307(7) 0.0337(7) 0.0022(5) 0.0080(6) -0.0038(5)
C29 0.0348(7) 0.0419(8) 0.0470(9) 0.0030(7) 0.0121(6) -0.0046(6)
C30 0.0485(8) 0.0404(8) 0.0396(8) -0.0018(6) 0.0063(7) -0.0142(7)
_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
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.521(2) . ?
C2 C3 1.518(2) . ?
C2 C4 1.518(2) . ?
C2 O5 1.4806(15) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
O5 C6 1.3415(17) . ?
C6 O6 1.2127(18) . ?
C6 N7 1.3645(17) . ?
N7 C8 1.4714(18) . ?
N7 C10 1.4750(17) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.540(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.5726(18) . ?
C10 C11 1.5078(19) . ?
C10 C17 1.5475(18) . ?
C11 C12 1.386(2) . ?
C11 C16 1.3953(19) . ?
C12 H12 0.9500 . ?
C12 C13 1.390(2) . ?
C13 H13 0.9500 . ?
C13 C14 1.385(2) . ?
C14 H14 0.9500 . ?
C14 C15 1.380(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.386(2) . ?
C16 H16 0.9500 . ?
C17 O17 1.2400(17) . ?
C17 N18 1.3375(17) . ?
N18 C19 1.4834(17) . ?
N18 C21 1.5053(17) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.5394(19) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.5619(18) . ?
C21 C22 1.5260(19) . ?
C21 C28 1.5708(19) . ?
C22 C23 1.390(2) . ?
C22 C27 1.398(2) . ?
C23 H23 0.9500 . ?
C23 C24 1.391(2) . ?
C24 H24 0.9500 . ?
C24 C25 1.383(2) . ?
C25 H25 0.9500 . ?
C25 C26 1.385(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.387(2) . ?
C27 H27 0.9500 . ?
O28 C28 1.4267(17) . ?
O28 H28 0.91(2) . ?
C28 C29 1.531(2) . ?
C28 C30 1.518(2) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C3 C2 C1 111.41(13) . . ?
C3 C2 C4 113.18(13) . . ?
C4 C2 C1 110.71(13) . . ?
O5 C2 C1 101.61(11) . . ?
O5 C2 C3 108.63(11) . . ?
O5 C2 C4 110.69(11) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 O5 C2 120.63(11) . . ?
O5 C6 N7 109.11(12) . . ?
O6 C6 O5 127.38(13) . . ?
O6 C6 N7 123.49(13) . . ?
C6 N7 C8 128.34(12) . . ?
C6 N7 C10 125.23(11) . . ?
C8 N7 C10 94.73(10) . . ?
N7 C8 H8A 113.9 . . ?
N7 C8 H8B 113.9 . . ?
N7 C8 C9 88.23(10) . . ?
H8A C8 H8B 111.1 . . ?
C9 C8 H8A 113.9 . . ?
C9 C8 H8B 113.9 . . ?
C8 C9 H9A 113.9 . . ?
C8 C9 H9B 113.9 . . ?
C8 C9 C10 88.28(10) . . ?
H9A C9 H9B 111.1 . . ?
C10 C9 H9A 113.9 . . ?
C10 C9 H9B 113.9 . . ?
N7 C10 C9 86.88(10) . . ?
N7 C10 C11 116.50(11) . . ?
N7 C10 C17 109.40(10) . . ?
C11 C10 C9 114.10(11) . . ?
C11 C10 C17 116.34(11) . . ?
C17 C10 C9 109.91(11) . . ?
C12 C11 C10 122.07(12) . . ?
C12 C11 C16 119.02(13) . . ?
C16 C11 C10 118.82(12) . . ?
C11 C12 H12 119.8 . . ?
C11 C12 C13 120.32(14) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 119.8 . . ?
C14 C13 C12 120.35(15) . . ?
C14 C13 H13 119.8 . . ?
C13 C14 H14 120.3 . . ?
C15 C14 C13 119.48(15) . . ?
C15 C14 H14 120.3 . . ?
C14 C15 H15 119.7 . . ?
C14 C15 C16 120.53(15) . . ?
C16 C15 H15 119.7 . . ?
C11 C16 H16 119.9 . . ?
C15 C16 C11 120.27(14) . . ?
C15 C16 H16 119.9 . . ?
O17 C17 C10 117.16(12) . . ?
O17 C17 N18 122.40(12) . . ?
N18 C17 C10 120.42(11) . . ?
C17 N18 C19 133.58(11) . . ?
C17 N18 C21 129.66(11) . . ?
C19 N18 C21 94.10(10) . . ?
N18 C19 H19A 113.8 . . ?
N18 C19 H19B 113.8 . . ?
N18 C19 C20 88.90(10) . . ?
H19A C19 H19B 111.1 . . ?
C20 C19 H19A 113.8 . . ?
C20 C19 H19B 113.8 . . ?
C19 C20 H20A 113.7 . . ?
C19 C20 H20B 113.7 . . ?
C19 C20 C21 89.71(10) . . ?
H20A C20 H20B 110.9 . . ?
C21 C20 H20A 113.7 . . ?
C21 C20 H20B 113.7 . . ?
N18 C21 C20 87.28(10) . . ?
N18 C21 C22 111.73(10) . . ?
N18 C21 C28 115.20(11) . . ?
C20 C21 C28 114.38(11) . . ?
C22 C21 C20 114.17(11) . . ?
C22 C21 C28 111.98(11) . . ?
C23 C22 C21 121.69(12) . . ?
C23 C22 C27 118.04(13) . . ?
C27 C22 C21 120.26(13) . . ?
C22 C23 H23 119.5 . . ?
C22 C23 C24 120.94(14) . . ?
C24 C23 H23 119.5 . . ?
C23 C24 H24 119.8 . . ?
C25 C24 C23 120.42(15) . . ?
C25 C24 H24 119.8 . . ?
C24 C25 H25 120.4 . . ?
C24 C25 C26 119.29(14) . . ?
C26 C25 H25 120.4 . . ?
C25 C26 H26 119.8 . . ?
C25 C26 C27 120.34(15) . . ?
C27 C26 H26 119.8 . . ?
C22 C27 H27 119.5 . . ?
C26 C27 C22 120.95(15) . . ?
C26 C27 H27 119.5 . . ?
C28 O28 H28 103.9(15) . . ?
O28 C28 C21 110.82(11) . . ?
O28 C28 C29 109.52(12) . . ?
O28 C28 C30 105.00(12) . . ?
C29 C28 C21 110.95(12) . . ?
C30 C28 C21 109.92(12) . . ?
C30 C28 C29 110.47(13) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O28 H28 O17 0.91(2) 1.86(2) 2.7279(15) 160(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
C1 C2 O5 C6 -178.65(12) . . . . ?
C2 O5 C6 O6 6.6(2) . . . . ?
C2 O5 C6 N7 -171.95(11) . . . . ?
C3 C2 O5 C6 63.80(16) . . . . ?
C4 C2 O5 C6 -61.04(17) . . . . ?
O5 C6 N7 C8 -18.31(19) . . . . ?
O5 C6 N7 C10 -151.71(12) . . . . ?
C6 N7 C8 C9 -154.23(14) . . . . ?
C6 N7 C10 C9 155.68(13) . . . . ?
C6 N7 C10 C11 -88.86(16) . . . . ?
C6 N7 C10 C17 45.66(17) . . . . ?
O6 C6 N7 C8 163.09(14) . . . . ?
O6 C6 N7 C10 29.7(2) . . . . ?
N7 C8 C9 C10 10.07(10) . . . . ?
N7 C10 C11 C12 5.66(18) . . . . ?
N7 C10 C11 C16 -170.82(12) . . . . ?
N7 C10 C17 O17 64.62(15) . . . . ?
N7 C10 C17 N18 -116.94(13) . . . . ?
C8 N7 C10 C9 10.56(11) . . . . ?
C8 N7 C10 C11 126.01(12) . . . . ?
C8 N7 C10 C17 -99.46(12) . . . . ?
C8 C9 C10 N7 -10.05(10) . . . . ?
C8 C9 C10 C11 -127.77(12) . . . . ?
C8 C9 C10 C17 99.46(12) . . . . ?
C9 C10 C11 C12 104.66(15) . . . . ?
C9 C10 C11 C16 -71.82(16) . . . . ?
C9 C10 C17 O17 -29.17(16) . . . . ?
C9 C10 C17 N18 149.27(12) . . . . ?
C10 N7 C8 C9 -10.78(11) . . . . ?
C10 C11 C12 C13 -177.62(14) . . . . ?
C10 C11 C16 C15 178.02(13) . . . . ?
C10 C17 N18 C19 25.4(2) . . . . ?
C10 C17 N18 C21 -178.11(11) . . . . ?
C11 C10 C17 O17 -160.78(11) . . . . ?
C11 C10 C17 N18 17.66(17) . . . . ?
C11 C12 C13 C14 -0.4(2) . . . . ?
C12 C11 C16 C15 1.4(2) . . . . ?
C12 C13 C14 C15 1.6(3) . . . . ?
C13 C14 C15 C16 -1.3(2) . . . . ?
C14 C15 C16 C11 -0.2(2) . . . . ?
C16 C11 C12 C13 -1.1(2) . . . . ?
C17 C10 C11 C12 -125.71(14) . . . . ?
C17 C10 C11 C16 57.80(16) . . . . ?
C17 N18 C19 C20 161.30(14) . . . . ?
C17 N18 C21 C20 -162.40(13) . . . . ?
C17 N18 C21 C22 82.62(16) . . . . ?
C17 N18 C21 C28 -46.65(18) . . . . ?
O17 C17 N18 C19 -156.24(13) . . . . ?
O17 C17 N18 C21 0.2(2) . . . . ?
N18 C19 C20 C21 0.74(10) . . . . ?
N18 C21 C22 C23 -37.19(17) . . . . ?
N18 C21 C22 C27 143.44(12) . . . . ?
N18 C21 C28 O28 81.12(14) . . . . ?
N18 C21 C28 C29 -40.78(16) . . . . ?
N18 C21 C28 C30 -163.26(12) . . . . ?
C19 N18 C21 C20 0.76(10) . . . . ?
C19 N18 C21 C22 -114.23(11) . . . . ?
C19 N18 C21 C28 116.51(12) . . . . ?
C19 C20 C21 N18 -0.73(10) . . . . ?
C19 C20 C21 C22 111.91(12) . . . . ?
C19 C20 C21 C28 -117.25(12) . . . . ?
C20 C21 C22 C23 -134.25(13) . . . . ?
C20 C21 C22 C27 46.38(17) . . . . ?
C20 C21 C28 O28 -179.92(11) . . . . ?
C20 C21 C28 C29 58.18(16) . . . . ?
C20 C21 C28 C30 -64.30(16) . . . . ?
C21 N18 C19 C20 -0.77(10) . . . . ?
C21 C22 C23 C24 -178.47(13) . . . . ?
C21 C22 C27 C26 178.04(13) . . . . ?
C22 C21 C28 O28 -48.02(15) . . . . ?
C22 C21 C28 C29 -169.92(12) . . . . ?
C22 C21 C28 C30 67.60(15) . . . . ?
C22 C23 C24 C25 0.3(2) . . . . ?
C23 C22 C27 C26 -1.4(2) . . . . ?
C23 C24 C25 C26 -1.0(2) . . . . ?
C24 C25 C26 C27 0.6(2) . . . . ?
C25 C26 C27 C22 0.6(2) . . . . ?
C27 C22 C23 C24 0.9(2) . . . . ?
C28 C21 C22 C23 93.74(15) . . . . ?
C28 C21 C22 C27 -85.63(15) . . . . ?
_shelx_SHELXL_version_number 2014/7
_iucr_refine_instructions_details
;
sua1.res created by SHELXL-2014/7
TITL sua1_a.res in P2(1)/n
REM Old TITL SUA1 in P21/n #14
REM SHELXT solution in P2(1)/n
REM R1 0.124, Rweak 0.013, Alpha 0.019, Orientation as input
REM Formula found by SHELXT: C27 N2 O4
CELL 1.54184 10.055584 23.03715 10.820382 90 106.2209 90
ZERR 4 0.000236 0.000491 0.000286 0 0.0026 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N O
UNIT 108 136 8 16
L.S. 4 0 0
PLAN 20
TEMP -123(2)
HTAB O28 O17
HTAB
BOND $H
LIST 6
fmap 2 53
acta
MORE -1
CONF
REM
REM
REM
WGHT 0.055300 0.473100
FVAR 2.87668
C1 1 0.670274 0.627598 -0.004577 11.00000 0.04166 0.04268 =
0.05124 0.00419 0.02252 0.00162
AFIX 137
H1A 2 0.612924 0.608836 -0.082619 11.00000 -1.50000
H1B 2 0.767546 0.626670 -0.005113 11.00000 -1.50000
H1C 2 0.640612 0.667989 -0.001925 11.00000 -1.50000
AFIX 0
C2 1 0.654351 0.595475 0.113242 11.00000 0.02962 0.03533 =
0.04239 -0.00159 0.01419 0.00095
C3 1 0.695363 0.532143 0.111537 11.00000 0.03721 0.03732 =
0.04600 -0.00449 0.01378 0.00185
AFIX 137
H3A 2 0.684728 0.512739 0.188814 11.00000 -1.50000
H3B 2 0.792129 0.529552 0.109885 11.00000 -1.50000
H3C 2 0.635715 0.513243 0.034809 11.00000 -1.50000
AFIX 0
C4 1 0.731300 0.626795 0.235783 11.00000 0.03759 0.04249 =
0.05124 -0.00987 0.01359 -0.00087
AFIX 137
H4A 2 0.688146 0.664680 0.239213 11.00000 -1.50000
H4B 2 0.828198 0.632326 0.236690 11.00000 -1.50000
H4C 2 0.727232 0.603597 0.310560 11.00000 -1.50000
AFIX 0
O5 4 0.502835 0.598739 0.093775 11.00000 0.03067 0.03970 =
0.03685 0.00289 0.01295 0.00198
C6 1 0.445141 0.575853 0.180510 11.00000 0.03404 0.02934 =
0.03295 -0.00340 0.01192 0.00112
O6 4 0.504255 0.555351 0.284586 11.00000 0.03438 0.04535 =
0.03401 0.00413 0.00920 0.00364
N7 3 0.304462 0.577561 0.132509 11.00000 0.03190 0.03287 =
0.02876 0.00011 0.00999 0.00111
C8 1 0.220623 0.613194 0.026252 11.00000 0.03860 0.04013 =
0.02740 0.00236 0.00708 0.00086
AFIX 23
H8A 2 0.201294 0.594389 -0.059207 11.00000 -1.20000
H8B 2 0.256247 0.653122 0.023919 11.00000 -1.20000
AFIX 0
C9 1 0.100709 0.608763 0.088452 11.00000 0.03063 0.03689 =
0.03191 0.00149 0.00455 0.00154
AFIX 23
H9A 2 0.025761 0.582061 0.043177 11.00000 -1.20000
H9B 2 0.062903 0.646780 0.104745 11.00000 -1.20000
AFIX 0
C10 1 0.205586 0.581420 0.210422 11.00000 0.02697 0.03076 =
0.02915 -0.00044 0.00758 0.00213
C11 1 0.157910 0.524733 0.253204 11.00000 0.02820 0.03227 =
0.02808 -0.00167 0.00446 -0.00111
C12 1 0.212928 0.471866 0.230922 11.00000 0.03975 0.03405 =
0.03933 -0.00216 0.01313 0.00049
AFIX 43
H12 2 0.285371 0.470812 0.190358 11.00000 -1.20000
AFIX 0
C13 1 0.162605 0.420386 0.267649 11.00000 0.05298 0.03176 =
0.05115 0.00036 0.01455 0.00020
AFIX 43
H13 2 0.200481 0.384319 0.251604 11.00000 -1.20000
AFIX 0
C14 1 0.057566 0.421400 0.327492 11.00000 0.04966 0.03848 =
0.04665 0.00329 0.01209 -0.01159
AFIX 43
H14 2 0.024868 0.386254 0.354469 11.00000 -1.20000
AFIX 0
C15 1 0.000759 0.473871 0.347633 11.00000 0.03748 0.04772 =
0.04200 -0.00165 0.01239 -0.00997
AFIX 43
H15 2 -0.072606 0.474694 0.387064 11.00000 -1.20000
AFIX 0
C16 1 0.049877 0.525364 0.310799 11.00000 0.03144 0.03827 =
0.03799 -0.00358 0.00992 -0.00169
AFIX 43
H16 2 0.009835 0.561245 0.324817 11.00000 -1.20000
AFIX 0
C17 1 0.255223 0.628321 0.315623 11.00000 0.02691 0.02843 =
0.03177 0.00174 0.01020 0.00264
O17 4 0.258516 0.679168 0.279009 11.00000 0.03949 0.02825 =
0.03161 0.00325 0.00996 0.00134
N18 3 0.289411 0.613813 0.440232 11.00000 0.03105 0.02511 =
0.02844 0.00005 0.00713 0.00052
C19 1 0.339137 0.559393 0.511455 11.00000 0.03543 0.02643 =
0.03264 0.00395 0.00755 0.00197
AFIX 23
H19A 2 0.413790 0.539771 0.484054 11.00000 -1.20000
H19B 2 0.264140 0.531857 0.513333 11.00000 -1.20000
AFIX 0
C20 1 0.391413 0.595401 0.635421 11.00000 0.03691 0.02955 =
0.03084 0.00406 0.00624 -0.00004
AFIX 23
H20A 2 0.493326 0.594722 0.671832 11.00000 -1.20000
H20B 2 0.344509 0.586051 0.702131 11.00000 -1.20000
AFIX 0
C21 1 0.335920 0.651723 0.557737 11.00000 0.03452 0.02734 =
0.02683 0.00011 0.00669 -0.00171
C22 1 0.213428 0.679637 0.592355 11.00000 0.03768 0.02403 =
0.03250 -0.00031 0.01242 -0.00433
C23 1 0.097032 0.698630 0.498306 11.00000 0.04230 0.03052 =
0.03550 0.00249 0.01543 0.00135
AFIX 43
H23 2 0.092079 0.693376 0.410051 11.00000 -1.20000
AFIX 0
C24 1 -0.012336 0.725228 0.531565 11.00000 0.04435 0.03534 =
0.04639 0.00622 0.01809 0.00658
AFIX 43
H24 2 -0.091257 0.737797 0.465990 11.00000 -1.20000
AFIX 0
C25 1 -0.006895 0.733488 0.659505 11.00000 0.05176 0.03178 =
0.05284 -0.00152 0.02786 0.00330
AFIX 43
H25 2 -0.080983 0.752206 0.682101 11.00000 -1.20000
AFIX 0
C26 1 0.107739 0.714174 0.754319 11.00000 0.05689 0.03457 =
0.03904 -0.00666 0.02260 -0.00435
AFIX 43
H26 2 0.111943 0.719364 0.842429 11.00000 -1.20000
AFIX 0
C27 1 0.216458 0.687286 0.721278 11.00000 0.04459 0.03239 =
0.03519 -0.00318 0.01340 -0.00496
AFIX 43
H27 2 0.294076 0.673880 0.787217 11.00000 -1.20000
AFIX 0
O28 4 0.391875 0.747318 0.481982 11.00000 0.04518 0.02903 =
0.03958 0.00335 0.01106 -0.00419
C28 1 0.451047 0.697309 0.554448 11.00000 0.03612 0.03074 =
0.03369 0.00219 0.00798 -0.00384
C29 1 0.559908 0.670763 0.496700 11.00000 0.03484 0.04194 =
0.04704 0.00303 0.01208 -0.00458
AFIX 137
H29A 2 0.517888 0.662588 0.405207 11.00000 -1.50000
H29B 2 0.594785 0.634587 0.541841 11.00000 -1.50000
H29C 2 0.636720 0.698126 0.506096 11.00000 -1.50000
AFIX 0
C30 1 0.518552 0.719773 0.689279 11.00000 0.04852 0.04040 =
0.03960 -0.00179 0.00629 -0.01420
AFIX 137
H30A 2 0.592189 0.747254 0.686901 11.00000 -1.50000
H30B 2 0.558126 0.687178 0.745813 11.00000 -1.50000
H30C 2 0.448926 0.739391 0.722179 11.00000 -1.50000
AFIX 0
H28 2 0.341473 0.732592 0.405527 11.00000 -1.50000
HKLF 4
REM sua1_a.res in P2(1)/n
REM R1 = 0.0406 for 4150 Fo > 4sig(Fo) and 0.0515 for all 5102 data
REM 306 parameters refined using 0 restraints
END
WGHT 0.0553 0.4731
REM Instructions for potential hydrogen bonds
HTAB C3 O6
HTAB C4 O6
HTAB C19 O6
HTAB C29 O17
EQIV $1 x+1/2, -y+3/2, z+1/2
HTAB C30 O17_$1
HTAB O28 O17
REM Highest difference peak 0.277, deepest hole -0.198, 1-sigma level 0.037
Q1 1 0.3884 0.6762 0.5577 11.00000 0.05 0.28
Q2 1 0.1459 0.5967 0.1627 11.00000 0.05 0.24
Q3 1 0.2704 0.6637 0.5786 11.00000 0.05 0.24
Q4 1 0.2284 0.5998 0.2651 11.00000 0.05 0.24
Q5 1 0.1852 0.5536 0.2326 11.00000 0.05 0.23
Q6 1 0.3774 0.5753 0.5791 11.00000 0.05 0.23
Q7 1 0.2880 0.6400 0.4843 11.00000 0.05 0.19
Q8 1 0.2445 0.6184 0.3814 11.00000 0.05 0.19
Q9 1 0.2434 0.6983 0.6557 11.00000 0.05 0.18
Q10 1 0.6790 0.5622 0.1235 11.00000 0.05 0.18
Q11 1 0.1443 0.6186 0.0436 11.00000 0.05 0.18
Q12 1 0.3744 0.6214 0.6172 11.00000 0.05 0.17
Q13 1 0.2924 0.5845 0.4624 11.00000 0.05 0.17
Q14 1 0.6719 0.6135 0.0639 11.00000 0.05 0.17
Q15 1 0.2820 0.5934 0.0814 11.00000 0.05 0.16
Q16 1 0.4973 0.7028 0.6206 11.00000 0.05 0.16
Q17 1 0.2148 0.5001 0.2860 11.00000 0.05 0.16
Q18 1 0.1658 0.5002 0.2131 11.00000 0.05 0.16
Q19 1 0.2635 0.5647 0.1618 11.00000 0.05 0.15
Q20 1 0.1534 0.6804 0.5444 11.00000 0.05 0.15
REM The information below was added by Olex2.
REM
REM R1 = 0.0406 for 4150 Fo > 4sig(Fo) and 0.0515 for all 20062 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.28, deepest hole -0.20
REM Mean Shift 0, Max Shift -0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0515
REM R1_gt = 0.0406
REM wR_ref = 0.1136
REM GOOF = 1.037
REM Shift_max = -0.001
REM Shift_mean = 0
REM Reflections_all = 20062
REM Reflections_gt = 4150
REM Parameters = n/a
REM Hole = -0.20
REM Peak = 0.28
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_meas
_refln_F_squared_sigma
_refln_scale_group_code
0 0 1 27.6496 17.4951 2
0 0 2 16648.6 420.461 2
0 0 -2 15313.4 277.748 11
0 0 3 103.898 59.4373 2
0 0 -4 86596.3 1771.15 10
0 0 4 88022.6 1765.57 2
0 0 5 -62.2343 68.0801 2
0 0 -5 26.9357 73.263 10
0 0 6 74.289 63.4585 2
0 0 -6 -13.2713 96.423 10
0 0 7 -32.8899 71.6201 2
0 0 -7 -15.2322 92.4294 10
0 0 -8 2445.96 331.772 10
0 0 8 2685.48 156.241 3
0 0 8 2672.8 313.423 2
0 0 -9 5.83801 138.699 10
0 0 9 -29.5935 40.336 3
0 0 10 1482.22 118.935 3
0 0 11 -39.3195 40.389 3
0 0 12 156.788 41.1152 5
0 1 1 2728.24 113.111 1
0 -1 -1 2706.5 103.987 16
0 -1 1 2723.94 107.536 2
0 -1 -1 2768.45 93.7702 11
0 -1 -2 140242 2233.24 11
0 1 2 142234 2353.61 2
0 -1 2 140425 2346.7 2
0 1 3 2369.87 168.637 2
0 -1 -3 2317.22 170.74 10
0 -1 -3 2148.02 98.6721 11
0 -1 3 2157.74 165.345 2
0 -1 4 1064.94 138.132 2
0 1 4 908.465 122.602 2
0 -1 -4 785.726 123.092 10
0 1 -4 837.027 126.646 10
0 -1 5 36988.1 1002.82 2
0 1 -5 35405.1 1024.86 10
0 1 5 35017.6 1000.12 2
0 -1 -5 32775.9 997.43 10
0 1 6 613.601 138.03 2
0 -1 6 628.057 137.077 2
0 -1 -6 385.993 126.278 10
0 1 -6 520.304 137.739 10
0 -1 7 236.48 94.3399 2
0 1 -7 140.835 84.3309 10
0 -1 -7 307.383 127.456 10
0 1 7 227.702 95.7787 2
0 1 8 -75.5749 103.415 2
0 -1 8 40.8966 42.961 3
0 1 -8 42.7072 80.9024 10
0 -1 8 -94.481 81.3429 2
0 -1 -8 -134.245 114.337 10
0 -1 9 2067.88 144.417 3
0 1 -9 2392.16 350.447 10
0 -1 -9 1938.87 303.959 10
0 1 9 2219.9 147.195 3
0 1 9 2157.95 137.685 15
0 -1 10 83.631 43.9763 3
0 1 10 9.77136 34.93 15
0 -1 11 213.767 51.0029 3
0 1 11 162.844 45.3651 3
0 -1 12 -18.0658 26.0977 5
0 1 12 20.7202 28.1111 5
0 -1 12 -15.3554 25.2091 3
0 2 0 4193.05 121.71 1
0 -2 0 4157.8 125.499 16
0 -2 1 52736.3 971.316 2
0 2 1 53096 980.935 1
0 -2 1 56583.6 905.12 16
0 -2 -1 55371.7 984.79 16
0 -2 2 81552.4 1400.5 2
0 2 2 80407.6 1422.84 1
0 -2 -2 78578 1334.22 11
0 2 3 2022.6 158.691 2
0 -2 -3 1844.66 113.692 11
0 -2 -3 1860.36 154.714 10
0 -2 3 2065.2 158.962 2
0 2 4 29570.7 803.033 2
0 -2 4 29138.2 798.568 2
0 2 -4 29644.1 817.011 10
0 2 -5 717.159 150.157 10
0 -2 5 875.113 145.718 2
0 2 5 696.489 126.68 2
0 -2 -5 649.246 127.623 10
0 2 6 1066.69 168.854 2
0 2 -6 1002.25 179.219 10
0 -2 -6 1017.31 177.525 10
0 -2 6 1077 170.322 2
0 -2 7 1110.64 189.001 2
0 -2 -7 938.629 180.496 10
0 2 -7 1093.03 206.523 10
0 2 7 1254 200.063 2
0 2 -8 182.53 145.833 10
0 -2 8 66.2667 81.4123 2
0 -2 8 274.365 62.7033 3
0 2 8 258.538 54.2557 15
0 2 8 399.752 143.65 2
0 -2 -8 259.937 140.933 10
0 -2 9 1845.37 136.294 3
0 2 -9 2106.96 330.72 10
0 -2 -9 2235.21 329.947 10
0 2 9 2084.81 137.566 15
0 2 9 2206.05 143.196 3
0 2 10 -8.58834 38.5286 15
0 -2 10 -56.9959 44.0913 3
0 2 10 21.5431 30.9232 3
0 2 11 1670.44 105.332 15
0 -2 11 1487.11 113.765 3
0 -2 12 79.2683 28.6415 3
0 -2 12 50.6071 26.8173 5
0 2 12 27.5396 32.5445 5
0 2 13 28.0381 12.3224 5
0 -3 0 107.874 30.2593 16
0 3 0 90.5217 28.4578 1
0 3 0 115.498 21.2596 17
0 -3 1 57009.3 937.436 11
0 -3 -1 51973.2 984.32 16
0 3 1 52470.9 971.798 1
0 -3 1 52381.9 956.948 2
0 -3 1 55749.8 906.269 16
0 -3 -1 53114.8 954.847 10
0 3 1 51038.5 963.088 17
0 -3 2 82218 1321.67 11
0 -3 2 83042.9 1313.4 16
0 -3 -2 82703.3 1464.73 10
0 -3 -2 77259.9 1433.35 11
0 3 2 81036.7 1489.45 1
0 -3 2 80261.1 1458.9 2
0 3 3 4.24899 52.4632 2
0 -3 3 16.3463 14.4905 16
0 -3 3 57.1391 49.6445 2
0 -3 -3 21.2023 32.9001 11
0 -3 -3 53.2588 56.8025 10
0 -3 4 3624.79 126.578 16
0 -3 4 4164.22 263.456 2
0 3 4 3855.38 266.077 2
0 -3 -4 4089.89 266.842 10
0 -3 -4 3942.99 195.339 11
0 3 -4 4016.07 274.958 10
0 -3 -5 267.887 93.5163 10
0 3 -5 196.366 81.7244 10
0 -3 5 155.339 85.006 2
0 3 5 204.131 89.7951 2
0 3 6 12007.6 590.719 2
0 -3 -6 12674.2 613.922 10
0 -3 6 13352.4 601.375 2
0 3 -6 11814 620.492 10
0 3 7 4170.35 371.257 2
0 -3 7 4784.59 391.613 2
0 -3 -7 4285.51 385.199 10
0 3 -7 4261.48 401.894 10
0 -3 8 97.5316 75.7125 2
0 3 -8 -24.7643 102.111 10
0 -3 8 20.1783 33.1447 3
0 -3 -8 -87.9901 110.021 10
0 3 8 -5.55176 39.9363 15
0 3 8 119.256 101.309 2
0 -3 -9 34.2321 86.1974 10
0 -3 9 50.4797 45.7694 3
0 3 9 6.12408 31.7565 15
0 3 -9 111.543 135.529 10
0 -3 10 2369.57 156.951 3
0 3 10 2569.96 151.547 15
0 3 11 326.633 53.1711 15
0 -3 11 250.135 53.5229 3
0 -3 12 513.146 56.2032 3
0 -3 12 344.438 42.4919 5
0 3 12 432.435 57.3624 5
0 3 13 -0.13436 12.6617 5
0 -4 0 39600.9 756.792 16
0 4 0 38185 678.134 17
0 4 0 38335.2 729.847 1
0 -4 1 106714 1767.97 2
0 -4 1 109937 1743.89 16
0 -4 1 110866 1786.87 11
0 4 1 104118 1802.7 1
0 -4 -1 106541 1833.91 16
0 -4 -1 106600 1790.64 10
0 4 2 21007 562.456 1
0 -4 2 22623.3 460.589 11
0 -4 2 21487.6 530.088 2
0 4 2 20058.9 544.909 17
0 -4 -2 21304.7 540.532 11
0 -4 -2 21502.7 565.823 16
0 -4 -2 21095.3 532.333 10
0 -4 2 22537 430.929 16
0 -4 3 17121.1 352.162 16
0 -4 3 17870.9 533.702 2
0 -4 -3 17905.7 496.99 11
0 4 3 18042.2 557.163 17
0 -4 -3 17963.9 529.573 10
0 4 3 18793 565.599 1
0 -4 -4 7042.86 292.485 11
0 -4 4 7506.56 364.961 2
0 -4 -4 7055.01 355.115 10
0 4 4 7270.13 397.83 2
0 4 5 4458.91 320.905 2
0 -4 -5 4833.18 333.884 10
0 4 -5 4808.58 347.173 10
0 -4 5 5230.95 328.867 2
0 4 6 7121.05 451.618 2
0 -4 6 7387.22 440.853 2
0 4 -6 7026.85 470.56 10
0 -4 -6 7043.03 452.89 10
0 4 7 171.876 101.733 2
0 -4 7 70.4615 61.5184 2
0 4 -7 136.31 111.937 10
0 -4 -7 185.781 134.365 10
0 4 8 833.209 89.0944 15
0 -4 8 932.089 205.549 2
0 -4 -8 1141.11 234.315 10
0 4 8 919.349 201.827 2
0 4 -8 618.43 171.363 10
0 -4 8 815.313 90.9706 3
0 4 -9 1643.9 297.62 10
0 -4 -9 2046 318.488 10
0 -4 9 1743.95 137.355 3
0 4 9 1964.06 136.271 15
0 4 10 395.853 65.4814 15
0 -4 10 254.321 63.9786 3
0 -4 11 163.017 45.8723 3
0 4 11 183.797 43.0578 15
0 -4 11 174.854 45.3944 5
0 -4 12 73.6817 30.1521 3
0 4 12 41.1627 30.7461 5
0 4 13 9.80367 13.6954 5
0 5 0 65.7897 29.729 17
0 5 0 46.7938 36.378 1
0 -5 0 43.108 41.6357 16
0 -5 1 195496 3072.94 2
0 -5 1 195396 3117.8 11
0 -5 -1 194884 3102.38 10
0 5 1 195009 3121.34 1
0 -5 -1 192751 3163.5 16
0 -5 1 195184 3065.16 16
0 -5 2 29081.9 600.732 11
0 -5 -2 27186.7 678.47 11
0 -5 2 28830.8 652.568 2
0 -5 -2 25930.7 685.805 16
0 5 2 26174.3 677.678 1
0 -5 2 27830.4 551.352 16
0 5 2 26991.1 668.081 17
0 5 3 1364.26 147.726 17
0 -5 -3 1470.02 140.827 10
0 5 3 1431.39 153.242 1
0 -5 -3 1470.92 140.145 11
0 -5 3 1406.47 75.79 16
0 -5 3 1448.56 141.541 2
0 -5 -4 14741.7 495.253 11
0 -5 -4 14830.7 541.628 10
0 -5 4 15595.7 542.159 2
0 5 4 14753.7 556.826 2
0 -5 5 1760.01 198.83 2
0 -5 -5 1442.73 182.862 10
0 5 5 1690.58 203.44 2
0 5 -5 1681.86 205.918 10
0 -5 -6 4074.99 340.569 10
0 5 -6 3834.01 350.327 10
0 -5 6 4310.25 334.162 2
0 5 6 3977.87 342.551 2
0 -5 7 398.031 113.781 2
0 -5 -7 386.064 117.669 10
0 5 7 542.786 157.318 2
0 5 -7 557.077 169.797 10
0 5 8 1993.57 135.968 15
0 5 8 2069.9 285.96 2
0 5 -8 2080.47 332.558 10
0 -5 -8 2100.5 307.002 10
0 -5 8 2075.25 276.896 2
0 -5 8 2021.45 142.197 3
0 -5 9 3689.41 197.773 3
0 5 -9 3695.7 439.585 10
0 5 9 3694.46 190.456 15
0 -5 -9 3619.57 409.339 10
0 5 10 223.06 55.91 15
0 -5 10 234.694 56.403 3
0 -5 11 996.122 93.1567 3
0 5 11 958.16 85.5022 15
0 5 12 240.797 44.7335 5
0 -5 12 339.339 47.0761 3
0 5 12 309.334 39.4892 15
0 5 13 16.0441 13.093 5
0 6 0 96670.3 1603.01 17
0 6 0 96913.2 1695.37 1
0 -6 0 95119.3 1721.29 16
0 -6 1 39423 789.357 2
0 -6 -1 40091.1 815.151 10
0 6 -1 37750.8 817.334 1
0 -6 1 39630.9 795.717 16
0 6 -1 38719.6 722.32 17
0 -6 -1 37584.4 864.198 16
0 6 1 39235.8 831.49 1
0 6 1 35780.3 778.836 17
0 -6 2 17.751 25.3092 16
0 -6 2 53.2905 41.0635 2
0 -6 -2 30.9977 59.0318 11
0 -6 -2 -5.89768 67.2443 16
0 -6 2 5.55522 40.4059 11
0 6 2 -17.5847 44.3797 17
0 -6 3 6015.33 291.012 2
0 6 3 5638.91 302.597 17
0 -6 -3 5561.09 289.776 10
0 -6 -3 5780.27 299.185 11
0 6 3 5830.78 315.184 1
0 -6 3 6009.54 190.184 16
0 6 4 13651.7 541.974 2
0 -6 -4 13780.8 528.745 10
0 -6 4 13610.4 512.705 2
0 -6 -4 13485 498.461 11
0 6 -5 7505.78 449.075 10
0 -6 5 7905.74 419.472 2
0 -6 -5 7728.57 427.097 10
0 6 5 7550.27 433.498 2
0 6 -6 6139.82 448.716 10
0 -6 -6 5796.83 412.436 10
0 6 6 5816.35 414.377 2
0 -6 6 6165.42 414.534 2
0 -6 7 702.874 166.882 2
0 6 -7 1069.22 221.859 10
0 6 7 857.186 177.445 2
0 -6 -7 685.709 174.947 10
0 -6 8 -3.33787 40.1348 3
0 -6 -8 -87.2188 121.558 10
0 -6 8 28.4537 85.2077 2
0 6 8 17.7295 35.3116 15
0 6 -8 31.4508 96.1223 10
0 6 8 -39.4986 91.2033 2
0 -6 9 75.3249 33.7313 3
0 -6 -9 138.324 178.5 10
0 6 9 90.6497 41.9724 15
0 -6 10 129.256 53.4938 3
0 6 10 168.695 47.8996 15
0 6 11 330.539 56.1082 15
0 -6 11 250.65 53.5768 3
0 6 12 118.141 30.9151 15
0 -6 12 103.304 30.4074 3
0 6 12 80.6803 33.6319 5
0 -7 0 4.98867 42.2497 16
0 -7 0 55.0258 62.0902 11
0 7 0 24.3666 29.6029 17
0 7 0 24.8906 40.07 1
0 -7 -1 14743.9 489.627 11
0 7 1 13843.3 404.587 17
0 7 1 14463.2 444.883 1
0 7 -1 14129.6 350.737 17
0 -7 1 14903.4 430.207 16
0 -7 1 14657.1 460.272 11
0 7 -1 14833.8 446.959 1
0 -7 -1 14489.1 481.53 16
0 -7 2 14318.5 437.704 2
0 -7 -2 14039.7 510.468 16
0 -7 -2 14626 459.537 10
0 7 2 14378.6 485.14 1
0 7 2 13537.4 449.328 17
0 -7 -2 13205.1 493.733 11
0 -7 2 14185.9 394.096 16
0 -7 3 10748.6 408.939 2
0 -7 -3 10705.5 442.598 11
0 -7 -3 10028.7 410.03 10
0 7 3 10108.9 430.954 17
0 -7 3 10549.6 295.978 16
0 7 3 10464.2 448.102 1
0 7 4 33032.7 941.255 2
0 -7 -4 34013.2 926.834 11
0 -7 4 35141.9 927.133 2
0 -7 -4 34169 934.84 10
0 -7 -5 22007.3 781.304 10
0 -7 -5 22618.4 740.404 11
0 7 5 20822 778.808 2
0 -7 5 22914.4 772.302 2
0 -7 -6 266.646 94.1074 10
0 7 6 194.24 93.3709 2
0 7 -6 131.923 85.3773 10
0 -7 6 184.054 99.2533 2
0 -7 -7 255.938 110.045 10
0 7 -7 137.607 89.001 10
0 7 7 166.962 100.263 2
0 -7 7 497.777 143.268 2
0 7 -8 3941.05 435.671 10
0 -7 8 4360.36 212.625 3
0 -7 8 3932.51 370.848 2
0 7 8 4696.31 438.444 2
0 7 8 4001.58 201.997 15
0 -7 -8 4040.32 416.796 10
0 -7 9 1547.63 131.221 3
0 7 9 1744.71 130.429 15
0 -7 10 1185.75 108.92 3
0 7 10 1228.92 106.076 15
0 7 11 2.47623 31.8528 15
0 -7 11 -8.05593 32.9657 3
0 7 12 15.3766 22.5575 15
0 7 12 18.824 24.8989 5
0 -7 12 10.616 25.2278 3
0 -8 0 3177.64 211.943 16
0 8 0 3224.34 154.646 17
0 8 0 3288.22 200.859 1
0 -8 0 3196.8 224.816 11
0 8 1 15323.3 443.598 17
0 8 -1 15384 476.7 1
0 8 1 15970.2 489.504 1
0 -8 1 14989.3 465.695 16
0 8 -1 14943.5 371.696 17
0 -8 -1 15094 528.251 11
0 -8 -1 15565.3 531.836 16
0 -8 1 15107 504.552 11
0 -8 -1 15550.3 474.57 10
0 -8 2 30033.6 745.196 11
0 8 2 29009.7 747.176 17
0 8 -2 28773.5 753.449 1
0 8 2 29185.9 784.883 1
0 -8 -2 28454.8 813.935 11
0 -8 -2 28925.9 745.65 10
0 -8 2 29078.2 682.216 16
0 -8 2 30144.8 725.11 2
0 -8 -2 28950.3 826.41 16
0 -8 3 51673.6 965.862 16
0 -8 3 49398.7 1119.28 2
0 -8 -3 47829.9 1130.99 10
0 8 3 46916.5 1177.51 1
0 -8 -3 47350 1188.83 11
0 8 3 48681.8 1159.13 17
0 -8 4 1877.88 195.776 2
0 8 4 1624.35 189.715 2
0 -8 -4 1788.17 204.312 11
0 8 4 2039.81 217.929 1
0 -8 -4 1920.11 196.806 10
0 8 5 -33.0626 72.7111 2
0 -8 -5 -21.8933 54.3509 10
0 -8 -5 -27.4299 58.8279 11
0 -8 5 23.3307 49.0491 2
0 -8 6 523.44 132.004 2
0 8 6 535.409 129.393 2
0 -8 -6 353.33 90.8916 10
0 8 -6 428.543 137.055 10
0 8 -7 275.823 99.0249 10
0 -8 7 403.887 128.091 2
0 8 7 282.007 56.631 15
0 -8 7 299.072 58.0637 3
0 -8 -7 293.291 112.905 10
0 8 7 441.131 144.567 2
0 8 8 257.703 141.647 2
0 8 8 408.103 67.9074 15
0 8 -8 311.144 133.256 10
0 -8 8 400.672 69.1926 3
0 -8 -8 383.439 135.192 10
0 -8 8 490.823 153.289 2
0 -8 9 979.883 103.302 3
0 8 9 947.194 98.862 15
0 8 10 927.01 94.5801 15
0 -8 10 1011.94 101.185 3
0 8 11 9.80385 31.3081 15
0 -8 11 34.2466 37.3692 3
0 -8 12 366.178 45.1229 3
0 8 12 224.022 41.3262 5
0 8 12 320.266 38.1952 15
0 9 0 37.3655 33.4674 17
0 -9 0 93.2534 71.263 11
0 -9 0 52.5573 53.1114 16
0 9 0 0.66813 47.1031 1
0 -9 -1 11210.5 472.848 11
0 9 1 11345.9 379.294 17
0 9 -1 12013.9 425.452 1
0 -9 1 11219.3 446.329 11
0 9 1 11261.8 424.357 1
0 -9 1 11316.1 416.86 16
0 -9 -1 11092.4 464.646 16
0 9 -1 11476.4 315.829 17
0 9 -2 36074.1 904.811 1
0 9 2 34600.8 866.371 17
0 -9 -2 36064.4 884.481 10
0 -9 2 37091.6 857.298 2
0 -9 2 35868.8 891.663 11
0 9 -2 35661.6 749.354 17
0 -9 2 36110.2 829.375 16
0 9 2 35673.9 928.243 1
0 -9 -2 33446.1 959.685 11
0 -9 -2 34298.5 970.035 16
0 -9 -3 6674.82 386.867 11
0 9 3 6529.08 370.783 1
0 -9 3 6941.1 273.238 16
0 9 3 6450.1 355.486 17
0 -9 3 7137.33 344.737 2
0 -9 -3 6626.15 348.849 10
0 9 4 3178.6 279.056 1
0 -9 -4 3076.92 270.421 11
0 -9 4 3401.77 257.911 2
0 -9 -4 2972.86 248.707 10
0 9 4 3100.99 264.204 2
0 -9 -5 -12.0605 72.1888 11
0 9 5 9.37563 68.1748 2
0 -9 -5 178.419 105.753 10
0 -9 5 110.012 57.9872 2
0 -9 -6 3371.23 327.654 10
0 -9 6 3843.64 333.922 2
0 9 -6 3223.26 346.568 10
0 9 6 3273.04 324.464 2
0 9 -7 2066.33 294.378 10
0 9 7 2026.96 286.68 2
0 9 7 2240.65 146.686 15
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