# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2017
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_chenpeng_a1(34-48)
_database_code_depnum_ccdc_archive 'CCDC 1526145'
_audit_update_record
;
2017-11-21 deposited with the CCDC.
2017-11-27 downloaded from the CCDC.
;
_audit_creation_date 2017-11-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C H Cl3, C38 H52 O9'
_chemical_formula_sum 'C39 H53 Cl3 O9'
_chemical_formula_weight 772.16
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
Cl Cl 0.3639 0.7018 '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 triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 12.7541(5)
_cell_length_b 13.5008(6)
_cell_length_c 13.6961(6)
_cell_angle_alpha 94.892(4)
_cell_angle_beta 105.455(4)
_cell_angle_gamma 113.791(4)
_cell_volume 2029.59(16)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 7120
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 62.8500
_cell_measurement_theta_min 3.4430
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.463
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.64058
_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.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear light colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier light
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.264
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 820
_exptl_crystal_size_max 0.28
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.2
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0270
_diffrn_reflns_av_unetI/netI 0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 17119
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full 62.749
_diffrn_reflns_theta_max 62.749
_diffrn_reflns_theta_min 3.431
_diffrn_ambient_temperature 293.0
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 16.0288
_diffrn_detector_type Sapphire3
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -40.00 106.00 1.0000 1.3950
omega____ theta____ kappa____ phi______ frames
- 33.1184 0.0000 30.0000 146
#__ type_ start__ end____ width___ exp.time_
2 omega 108.00 162.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 0.0000 120.0000 54
#__ type_ start__ end____ width___ exp.time_
3 omega 87.00 113.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -90.0000 4.8737 26
#__ type_ start__ end____ width___ exp.time_
4 omega 75.00 108.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -93.0000 -19.2243 33
#__ type_ start__ end____ width___ exp.time_
5 omega 64.00 129.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -93.0000 -78.0495 65
#__ type_ start__ end____ width___ exp.time_
6 omega 66.00 106.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -61.0000 30.0000 40
#__ type_ start__ end____ width___ exp.time_
7 omega 52.00 77.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -45.0000 60.0000 25
#__ type_ start__ end____ width___ exp.time_
8 omega 45.00 71.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 0.0000 120.0000 26
#__ type_ start__ end____ width___ exp.time_
9 omega 40.00 71.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -45.0000 150.0000 31
#__ type_ start__ end____ width___ exp.time_
10 omega 36.00 129.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -93.0000 84.1488 93
#__ type_ start__ end____ width___ exp.time_
11 omega 88.00 114.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -93.0000 172.7701 26
#__ type_ start__ end____ width___ exp.time_
12 omega 42.00 69.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -93.0000 172.7701 27
#__ type_ start__ end____ width___ exp.time_
13 omega 39.00 65.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -94.0000 90.0000 26
#__ type_ start__ end____ width___ exp.time_
14 omega 30.00 55.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -94.0000 30.0000 25
#__ type_ start__ end____ width___ exp.time_
15 omega 32.00 57.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -90.0000 4.8737 25
#__ type_ start__ end____ width___ exp.time_
16 omega 30.00 56.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -111.0000 60.0000 26
#__ type_ start__ end____ width___ exp.time_
17 omega 18.00 71.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -111.0000 -30.0000 53
#__ type_ start__ end____ width___ exp.time_
18 omega 53.00 88.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -111.0000 -60.0000 35
#__ type_ start__ end____ width___ exp.time_
19 omega 47.00 112.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -61.0000 -60.0000 65
#__ type_ start__ end____ width___ exp.time_
20 omega 54.00 86.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -77.0000 -180.0000 32
#__ type_ start__ end____ width___ exp.time_
21 omega 48.00 86.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -77.0000 -120.0000 38
#__ type_ start__ end____ width___ exp.time_
22 omega 27.00 69.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -30.0000 0.0000 42
#__ type_ start__ end____ width___ exp.time_
23 omega 25.00 69.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -30.0000 -90.0000 44
#__ type_ start__ end____ width___ exp.time_
24 omega 19.00 70.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -94.0000 -120.0000 51
#__ type_ start__ end____ width___ exp.time_
25 omega 4.00 74.00 1.0000 1.3950
omega____ theta____ kappa____ phi______ frames
- 33.1184 -99.0000 30.0000 70
#__ type_ start__ end____ width___ exp.time_
26 omega 19.00 67.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -30.0000 150.0000 48
#__ type_ start__ end____ width___ exp.time_
27 omega 38.00 99.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 15.0000 90.0000 61
#__ type_ start__ end____ width___ exp.time_
28 omega 85.00 146.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 111.0000 30.0000 61
#__ type_ start__ end____ width___ exp.time_
29 omega 120.00 159.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 61.0000 -60.0000 39
#__ type_ start__ end____ width___ exp.time_
30 omega 137.00 162.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 111.0000 -90.0000 25
#__ type_ start__ end____ width___ exp.time_
31 omega 124.00 150.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 111.0000 -150.0000 26
#__ type_ start__ end____ width___ exp.time_
32 omega 121.00 150.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 111.0000 -60.0000 29
#__ type_ start__ end____ width___ exp.time_
33 omega 86.00 113.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 111.0000 -60.0000 27
#__ type_ start__ end____ width___ exp.time_
34 omega 71.00 96.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 61.0000 -60.0000 25
#__ type_ start__ end____ width___ exp.time_
35 omega 22.00 52.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -30.0000 60.0000 30
#__ type_ start__ end____ width___ exp.time_
36 omega 20.00 45.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 -30.0000 90.0000 25
#__ type_ start__ end____ width___ exp.time_
37 omega 18.00 44.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 0.0000 120.0000 26
#__ type_ start__ end____ width___ exp.time_
38 omega 59.00 103.00 1.0000 5.5900
omega____ theta____ kappa____ phi______ frames
- 90.5000 178.0000 -30.0000 44
#__ type_ start__ end____ width___ exp.time_
39 omega -30.00 19.00 1.0000 1.3950
omega____ theta____ kappa____ phi______ frames
- 33.1184 -38.0000 -180.0000 49
#__ type_ start__ end____ width___ exp.time_
40 omega -97.00 -71.00 1.0000 1.3950
omega____ theta____ kappa____ phi______ frames
- -33.1184 -178.0000 0.0000 26
#__ type_ start__ end____ width___ exp.time_
41 omega -100.00 -69.00 1.0000 1.3950
omega____ theta____ kappa____ phi______ frames
- -33.1184 -178.0000 -180.0000 31
#__ type_ start__ end____ width___ exp.time_
42 omega -108.00 -65.00 1.0000 1.3950
omega____ theta____ kappa____ phi______ frames
- -33.1184 178.0000 90.0000 43
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 0.1235063000
_diffrn_orient_matrix_UB_12 -0.0031463000
_diffrn_orient_matrix_UB_13 0.0374708000
_diffrn_orient_matrix_UB_21 0.0301403000
_diffrn_orient_matrix_UB_22 0.0446164000
_diffrn_orient_matrix_UB_23 -0.0938995000
_diffrn_orient_matrix_UB_31 0.0582556000
_diffrn_orient_matrix_UB_32 0.1197148000
_diffrn_orient_matrix_UB_33 0.0638871000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'sealed X-ray tube'
_diffrn_source_type 'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5545
_reflns_number_total 6474
_reflns_odcompleteness_completeness 96.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 63.60
_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, 2015)'
_computing_structure_solution 'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max 0.844
_refine_diff_density_min -0.886
_refine_diff_density_rms 0.079
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.040
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 510
_refine_ls_number_reflns 6474
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0995
_refine_ls_R_factor_gt 0.0914
_refine_ls_restrained_S_all 1.040
_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^)+(0.1804P)^2^+1.8532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2714
_refine_ls_wR_factor_ref 0.2842
_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 O(H) groups
2. Others
Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=
Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(1)
Sof(H17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=
Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
C46(H46), C8'(H8'), C9(H9), C10(H10), C17(H17A), C18(H18), C18A(H18A)
3.b Secondary CH2 refined with riding coordinates:
C11(H11A,H11B)
3.c Idealised Me refined as rotating group:
C9'(H9'A,H9'B,H9'C), C10'(H10A,H10B,H10C), C14'(H14A,H14B,H14C), C13'(H13A,
H13B,H13C), C12'(H12A,H12B,H12C), C11'(H11C,H11D,H11E), C19(H19A,H19B,H19C),
C19A(H19D,H19E,H19F), C20(H20A,H20B,H20C), C20A(H20D,H20E,H20F), C22(H22A,H22B,
H22C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,
H25B,H25C), C26(H26A,H26B,H26C)
3.d Idealised tetrahedral OH refined as rotating group:
O3(H3), O4(H4), O6(H6)
;
_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
Cl26 Cl 0.2057(3) 0.9004(3) 0.5143(2) 0.2170(18) Uani 1 1 d . . . . .
Cl28 Cl -0.0299(4) 0.8632(3) 0.5295(3) 0.2048(15) Uani 1 1 d . . . . .
Cl32 Cl 0.0026(3) 0.6909(3) 0.4371(3) 0.2112(15) Uani 1 1 d . . . . .
C46 C 0.0493(7) 0.8308(7) 0.4581(5) 0.120(2) Uani 1 1 d . . . . .
H46 H 0.027392 0.849775 0.390532 0.144 Uiso 1 1 calc R . . . .
O1 O 0.4296(2) 0.10965(18) -0.02115(18) 0.0501(6) Uani 1 1 d . . . . .
O2 O 0.2867(2) 0.13994(17) 0.02868(17) 0.0472(6) Uani 1 1 d . . . . .
O3 O 0.1705(2) 0.2572(2) 0.30270(19) 0.0572(6) Uani 1 1 d . . . . .
H3 H 0.157892 0.194173 0.310026 0.086 Uiso 1 1 calc GR . . . .
O4 O 0.3393(2) 0.50736(18) 0.10238(18) 0.0501(6) Uani 1 1 d . . . . .
H4 H 0.356699 0.554540 0.153508 0.075 Uiso 1 1 calc GR . . . .
O5 O 0.0998(3) 0.1497(2) -0.2418(2) 0.0782(9) Uani 1 1 d . . . . .
O6 O 0.2410(3) 0.4199(2) 0.4628(2) 0.0650(7) Uani 1 1 d . . . . .
H6 H 0.217100 0.373641 0.409092 0.098 Uiso 1 1 calc GR . . . .
O7 O 0.4756(5) 0.7958(3) 0.6120(3) 0.1112(15) Uani 1 1 d . . . . .
O8 O 0.4042(3) 0.6654(2) 0.26372(19) 0.0655(7) Uani 1 1 d . . . . .
O9 O 0.1714(3) 0.0790(2) 0.2834(2) 0.0679(8) Uani 1 1 d . . . . .
C1 C 0.3561(3) 0.1623(2) -0.0441(2) 0.0415(7) Uani 1 1 d . . . . .
C1' C 0.3001(3) 0.5439(3) 0.3533(2) 0.0438(7) Uani 1 1 d . . . . .
C6' C 0.3031(3) 0.5201(3) 0.4485(3) 0.0470(8) Uani 1 1 d . . . . .
C3 C 0.2785(3) 0.2211(2) 0.0875(2) 0.0390(7) Uani 1 1 d . . . . .
C5' C 0.3717(3) 0.6022(3) 0.5516(3) 0.0521(8) Uani 1 1 d . . . . .
C4 C 0.2349(3) 0.1941(2) 0.1711(2) 0.0414(7) Uani 1 1 d . . . . .
C4' C 0.4412(4) 0.7198(3) 0.5401(3) 0.0621(10) Uani 1 1 d . . . . .
C5 C 0.2164(3) 0.2785(3) 0.2249(2) 0.0429(7) Uani 1 1 d . . . . .
C3' C 0.4722(3) 0.7417(3) 0.4430(3) 0.0531(8) Uani 1 1 d . . . . .
C6 C 0.2444(3) 0.3827(3) 0.2017(2) 0.0404(7) Uani 1 1 d . . . . .
C2' C 0.3896(3) 0.6481(3) 0.3474(3) 0.0483(8) Uani 1 1 d . . . . .
C7 C 0.2991(3) 0.4060(2) 0.1253(2) 0.0400(7) Uani 1 1 d . . . . .
C7' C 0.2094(3) 0.0911(3) 0.2076(3) 0.0480(8) Uani 1 1 d . . . . .
C8 C 0.3115(3) 0.3244(2) 0.0647(2) 0.0383(7) Uani 1 1 d . . . . .
C8' C 0.2243(4) -0.0055(3) 0.1604(3) 0.0609(10) Uani 1 1 d . . . . .
H8' H 0.284055 0.021701 0.124597 0.073 Uiso 1 1 calc R . . . .
C9 C 0.3639(3) 0.3482(2) -0.0222(2) 0.0405(7) Uani 1 1 d . . . . .
H9 H 0.418026 0.427771 -0.007290 0.049 Uiso 1 1 calc R . . . .
C9' C 0.1025(6) -0.0851(4) 0.0814(5) 0.0989(18) Uani 1 1 d . . . . .
H9'A H 0.043007 -0.111031 0.115564 0.148 Uiso 1 1 calc GR . . . .
H9'B H 0.109218 -0.146981 0.048592 0.148 Uiso 1 1 calc GR . . . .
H9'C H 0.078236 -0.047532 0.029833 0.148 Uiso 1 1 calc GR . . . .
C10 C 0.4381(3) 0.2845(2) -0.0252(2) 0.0420(7) Uani 1 1 d . . . . .
H10 H 0.468465 0.297478 -0.083819 0.050 Uiso 1 1 calc R . . . .
C10' C 0.2692(7) -0.0597(5) 0.2444(5) 0.105(2) Uani 1 1 d . . . . .
H10A H 0.345770 -0.006189 0.293064 0.158 Uiso 1 1 calc GR . . . .
H10B H 0.278924 -0.120495 0.213239 0.158 Uiso 1 1 calc GR . . . .
H10C H 0.211176 -0.086701 0.279960 0.158 Uiso 1 1 calc GR . . . .
C11 C 0.5427(3) 0.2996(3) 0.0690(3) 0.0512(8) Uani 1 1 d . . . . .
H11A H 0.524622 0.308876 0.132696 0.061 Uiso 1 1 calc R . . . .
H11B H 0.617037 0.362905 0.073349 0.061 Uiso 1 1 calc R . . . .
C14' C 0.2788(4) 0.6000(4) 0.6047(3) 0.0736(12) Uani 1 1 d . . . . .
H14A H 0.220064 0.618553 0.560861 0.110 Uiso 1 1 calc GR . . . .
H14B H 0.319939 0.652967 0.669853 0.110 Uiso 1 1 calc GR . . . .
H14C H 0.238466 0.527168 0.616544 0.110 Uiso 1 1 calc GR . . . .
C12 C 0.5524(3) 0.1893(3) 0.0478(3) 0.0558(9) Uani 1 1 d . . . . .
C13' C 0.4634(4) 0.5698(4) 0.6218(3) 0.0715(11) Uani 1 1 d . . . . .
H13A H 0.421399 0.496408 0.631809 0.107 Uiso 1 1 calc GR . . . .
H13B H 0.503775 0.621366 0.687772 0.107 Uiso 1 1 calc GR . . . .
H13C H 0.522193 0.571450 0.589629 0.107 Uiso 1 1 calc GR . . . .
C12' C 0.4690(6) 0.8496(4) 0.4194(4) 0.0811(14) Uani 1 1 d . . . . .
H12A H 0.487280 0.861505 0.356598 0.122 Uiso 1 1 calc GR . . . .
H12B H 0.528043 0.910580 0.475743 0.122 Uiso 1 1 calc GR . . . .
H12C H 0.389622 0.844246 0.411224 0.122 Uiso 1 1 calc GR . . . .
C14 C 0.2622(3) 0.1131(3) -0.1528(2) 0.0471(8) Uani 1 1 d . . . . .
C11' C 0.6038(4) 0.7549(4) 0.4641(3) 0.0721(11) Uani 1 1 d . . . . .
H11C H 0.608691 0.690633 0.485707 0.108 Uiso 1 1 calc GR . . . .
H11D H 0.659404 0.819731 0.517803 0.108 Uiso 1 1 calc GR . . . .
H11E H 0.624458 0.762422 0.401764 0.108 Uiso 1 1 calc GR . . . .
C15 C 0.2002(3) 0.1889(3) -0.1786(3) 0.0497(8) Uani 1 1 d . . . . .
C16 C 0.2654(3) 0.3157(3) -0.1315(2) 0.0470(8) Uani 1 1 d . . . . .
C17 C 0.2068(3) 0.4620(3) 0.2525(3) 0.0482(8) Uani 1 1 d . . . . .
H17A H 0.145653 0.411438 0.278424 0.058 Uiso 0.589(12) 1 calc R . P A 2
H17 H 0.222(10) 0.518(8) 0.208(8) 0.058 Uiso 0.411(12) 1 d R . P A 1
C18 C 0.0769(8) 0.4183(9) 0.2473(8) 0.065(3) Uani 0.411(12) 1 d . . P A 1
H18 H 0.065914 0.370502 0.297472 0.078 Uiso 0.411(12) 1 calc R . P A 1
C18A C 0.1325(7) 0.5050(7) 0.1788(6) 0.068(2) Uani 0.589(12) 1 d . . P A 2
H18A H 0.182804 0.552634 0.142649 0.082 Uiso 0.589(12) 1 calc R . P A 2
C19 C -0.0073(13) 0.3473(19) 0.1424(15) 0.105(6) Uani 0.411(12) 1 d . . P A 1
H19A H -0.012185 0.393764 0.093773 0.157 Uiso 0.411(12) 1 calc GR . P A 1
H19B H -0.086497 0.304698 0.146449 0.157 Uiso 0.411(12) 1 calc GR . P A 1
H19C H 0.023043 0.298135 0.119872 0.157 Uiso 0.411(12) 1 calc GR . P A 1
C19A C 0.0212(11) 0.4065(11) 0.0980(9) 0.096(4) Uani 0.589(12) 1 d . . P A 2
H19D H 0.047505 0.358652 0.066417 0.144 Uiso 0.589(12) 1 calc GR . P A 2
H19E H -0.018995 0.434141 0.045560 0.144 Uiso 0.589(12) 1 calc GR . P A 2
H19F H -0.034075 0.365559 0.131919 0.144 Uiso 0.589(12) 1 calc GR . P A 2
C20 C 0.0429(14) 0.5096(15) 0.2783(17) 0.097(5) Uani 0.411(12) 1 d . . P A 1
H20A H 0.108102 0.564155 0.336404 0.145 Uiso 0.411(12) 1 calc GR . P A 1
H20B H -0.029251 0.478044 0.296982 0.145 Uiso 0.411(12) 1 calc GR . P A 1
H20C H 0.028381 0.543917 0.220852 0.145 Uiso 0.411(12) 1 calc GR . P A 1
C20A C 0.0873(13) 0.5730(13) 0.2394(9) 0.105(4) Uani 0.589(12) 1 d . . P A 2
H20D H 0.038236 0.526641 0.275102 0.158 Uiso 0.589(12) 1 calc GR . P A 2
H20E H 0.039940 0.599359 0.191665 0.158 Uiso 0.589(12) 1 calc GR . P A 2
H20F H 0.155825 0.635046 0.288918 0.158 Uiso 0.589(12) 1 calc GR . P A 2
C22 C 0.5797(5) 0.1452(4) 0.1440(4) 0.0770(13) Uani 1 1 d . . . . .
H22A H 0.519859 0.137437 0.176877 0.116 Uiso 1 1 calc GR . . . .
H22B H 0.658674 0.195809 0.191124 0.116 Uiso 1 1 calc GR . . . .
H22C H 0.577813 0.074164 0.125398 0.116 Uiso 1 1 calc GR . . . .
C21 C 0.6373(4) 0.1956(4) -0.0133(4) 0.0820(14) Uani 1 1 d . . . . .
H21A H 0.628658 0.122530 -0.035749 0.123 Uiso 1 1 calc GR . . . .
H21B H 0.719554 0.242479 0.030005 0.123 Uiso 1 1 calc GR . . . .
H21C H 0.617403 0.225649 -0.072699 0.123 Uiso 1 1 calc GR . . . .
C23 C 0.1664(4) -0.0050(3) -0.1628(3) 0.0615(10) Uani 1 1 d . . . . .
H23A H 0.205738 -0.047797 -0.132554 0.092 Uiso 1 1 calc GR . . . .
H23B H 0.121541 -0.039087 -0.234835 0.092 Uiso 1 1 calc GR . . . .
H23C H 0.111845 -0.001997 -0.127271 0.092 Uiso 1 1 calc GR . . . .
C24 C 0.3253(4) 0.1084(3) -0.2336(3) 0.0626(10) Uani 1 1 d . . . . .
H24A H 0.393636 0.178899 -0.222096 0.094 Uiso 1 1 calc GR . . . .
H24B H 0.269012 0.091523 -0.302130 0.094 Uiso 1 1 calc GR . . . .
H24C H 0.352664 0.051899 -0.226768 0.094 Uiso 1 1 calc GR . . . .
C25 C 0.1699(4) 0.3544(3) -0.1269(3) 0.0590(9) Uani 1 1 d . . . . .
H25A H 0.121472 0.311519 -0.088939 0.089 Uiso 1 1 calc GR . . . .
H25B H 0.118852 0.344863 -0.196126 0.089 Uiso 1 1 calc GR . . . .
H25C H 0.209094 0.431394 -0.092787 0.089 Uiso 1 1 calc GR . . . .
C26 C 0.3272(4) 0.3723(3) -0.2078(3) 0.0610(10) Uani 1 1 d . . . . .
H26A H 0.364572 0.451329 -0.183556 0.092 Uiso 1 1 calc GR . . . .
H26B H 0.267440 0.351807 -0.275266 0.092 Uiso 1 1 calc GR . . . .
H26C H 0.387868 0.348814 -0.212056 0.092 Uiso 1 1 calc GR . . . .
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
Cl26 0.1294(18) 0.257(4) 0.146(2) -0.030(2) 0.0467(16) -0.014(2)
Cl28 0.254(4) 0.228(3) 0.204(3) 0.055(3) 0.143(3) 0.133(3)
Cl32 0.186(3) 0.157(2) 0.221(3) -0.024(2) 0.005(2) 0.061(2)
C46 0.136(6) 0.146(6) 0.073(3) -0.002(4) 0.019(4) 0.072(5)
O1 0.0531(13) 0.0416(12) 0.0503(13) -0.0027(10) 0.0096(10) 0.0232(10)
O2 0.0648(14) 0.0351(11) 0.0439(12) 0.0071(9) 0.0266(10) 0.0191(10)
O3 0.0731(16) 0.0496(13) 0.0531(14) 0.0096(11) 0.0352(12) 0.0227(12)
O4 0.0713(15) 0.0380(11) 0.0456(12) 0.0098(9) 0.0220(11) 0.0268(11)
O5 0.0647(17) 0.0661(17) 0.0716(18) 0.0029(14) -0.0116(15) 0.0219(14)
O6 0.0879(19) 0.0509(14) 0.0472(14) 0.0061(11) 0.0270(13) 0.0201(13)
O7 0.165(4) 0.0636(19) 0.071(2) -0.0146(16) 0.057(2) 0.013(2)
O8 0.093(2) 0.0495(14) 0.0445(14) 0.0060(11) 0.0235(13) 0.0226(13)
O9 0.098(2) 0.0512(14) 0.0604(16) 0.0198(12) 0.0428(15) 0.0270(14)
C1 0.0460(16) 0.0373(15) 0.0386(16) 0.0030(12) 0.0147(13) 0.0165(13)
C1' 0.0491(17) 0.0465(17) 0.0398(16) 0.0032(13) 0.0112(13) 0.0283(14)
C6' 0.0531(18) 0.0501(18) 0.0413(17) 0.0056(14) 0.0161(14) 0.0267(15)
C3 0.0404(15) 0.0347(15) 0.0348(15) 0.0014(12) 0.0086(12) 0.0135(12)
C5' 0.065(2) 0.057(2) 0.0367(17) 0.0045(14) 0.0169(15) 0.0303(17)
C4 0.0428(16) 0.0390(16) 0.0374(15) 0.0054(12) 0.0113(13) 0.0151(13)
C4' 0.079(3) 0.053(2) 0.047(2) -0.0032(17) 0.0197(18) 0.0265(19)
C5 0.0422(16) 0.0465(17) 0.0352(15) 0.0041(13) 0.0124(12) 0.0161(13)
C3' 0.067(2) 0.0447(18) 0.0449(18) 0.0045(14) 0.0131(16) 0.0261(16)
C6 0.0384(15) 0.0419(16) 0.0351(15) 0.0028(12) 0.0066(12) 0.0168(12)
C2' 0.061(2) 0.0465(18) 0.0434(18) 0.0082(14) 0.0160(15) 0.0306(16)
C7 0.0422(15) 0.0389(15) 0.0353(15) 0.0052(12) 0.0063(12) 0.0193(13)
C7' 0.0521(18) 0.0433(17) 0.0418(17) 0.0090(13) 0.0169(14) 0.0138(14)
C8 0.0411(15) 0.0383(15) 0.0331(14) 0.0055(12) 0.0101(12) 0.0170(12)
C8' 0.088(3) 0.0441(18) 0.064(2) 0.0216(17) 0.039(2) 0.0310(18)
C9 0.0441(16) 0.0342(14) 0.0397(16) 0.0064(12) 0.0143(13) 0.0141(12)
C9' 0.107(4) 0.063(3) 0.101(4) -0.013(3) 0.041(3) 0.016(3)
C10 0.0435(16) 0.0375(15) 0.0419(16) 0.0046(12) 0.0168(13) 0.0141(13)
C10' 0.178(6) 0.091(4) 0.090(4) 0.044(3) 0.057(4) 0.088(4)
C11 0.0459(17) 0.0428(17) 0.0533(19) -0.0039(14) 0.0058(14) 0.0179(14)
C14' 0.084(3) 0.080(3) 0.058(2) -0.001(2) 0.034(2) 0.035(2)
C12 0.0496(18) 0.0521(19) 0.057(2) -0.0059(16) 0.0059(16) 0.0255(16)
C13' 0.085(3) 0.081(3) 0.046(2) 0.0110(19) 0.0082(19) 0.044(2)
C12' 0.125(4) 0.053(2) 0.066(3) 0.0054(19) 0.022(3) 0.047(3)
C14 0.0533(18) 0.0401(16) 0.0387(16) 0.0018(13) 0.0121(14) 0.0150(14)
C11' 0.065(2) 0.082(3) 0.062(2) 0.013(2) 0.0150(19) 0.030(2)
C15 0.0511(19) 0.0496(18) 0.0388(16) 0.0079(14) 0.0097(15) 0.0166(15)
C16 0.0553(18) 0.0441(17) 0.0389(16) 0.0099(13) 0.0118(14) 0.0217(14)
C17 0.0485(18) 0.0561(19) 0.0412(17) 0.0013(15) 0.0101(14) 0.0290(16)
C18 0.041(5) 0.076(7) 0.068(6) -0.012(5) 0.005(4) 0.031(4)
C18A 0.070(5) 0.090(5) 0.056(4) 0.008(3) 0.010(3) 0.055(4)
C19 0.054(7) 0.133(15) 0.089(11) -0.018(10) -0.007(7) 0.031(8)
C19A 0.072(6) 0.125(9) 0.074(6) -0.009(6) -0.015(5) 0.057(6)
C20 0.066(8) 0.108(11) 0.127(13) -0.007(10) 0.023(8) 0.060(8)
C20A 0.097(8) 0.140(11) 0.099(8) -0.002(7) 0.006(6) 0.094(9)
C22 0.088(3) 0.064(2) 0.067(3) -0.005(2) -0.006(2) 0.045(2)
C21 0.060(2) 0.079(3) 0.103(4) -0.009(3) 0.026(2) 0.034(2)
C23 0.063(2) 0.0429(18) 0.054(2) -0.0007(15) 0.0073(17) 0.0095(16)
C24 0.079(3) 0.061(2) 0.0449(19) 0.0028(16) 0.0235(18) 0.0285(19)
C25 0.064(2) 0.066(2) 0.0496(19) 0.0101(17) 0.0099(16) 0.0369(19)
C26 0.081(3) 0.057(2) 0.0445(19) 0.0182(16) 0.0229(18) 0.0281(19)
_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
Cl26 C46 1.733(9) . ?
Cl28 C46 1.725(8) . ?
Cl32 C46 1.707(9) . ?
C46 H46 0.9800 . ?
O1 C1 1.379(4) . ?
O1 C12 1.477(4) . ?
O2 C1 1.476(4) . ?
O2 C3 1.359(4) . ?
O3 H3 0.8200 . ?
O3 C5 1.345(4) . ?
O4 H4 0.8200 . ?
O4 C7 1.352(4) . ?
O5 C15 1.206(4) . ?
O6 H6 0.8200 . ?
O6 C6' 1.326(4) . ?
O7 C4' 1.203(5) . ?
O8 C2' 1.235(4) . ?
O9 C7' 1.254(4) . ?
C1 C10 1.507(4) . ?
C1 C14 1.526(4) . ?
C1' C6' 1.364(5) . ?
C1' C2' 1.437(5) . ?
C1' C17 1.532(4) . ?
C6' C5' 1.510(5) . ?
C3 C4 1.415(4) . ?
C3 C8 1.375(4) . ?
C5' C4' 1.522(6) . ?
C5' C14' 1.539(5) . ?
C5' C13' 1.539(5) . ?
C4 C5 1.436(5) . ?
C4 C7' 1.459(5) . ?
C4' C3' 1.505(5) . ?
C5 C6 1.393(5) . ?
C3' C2' 1.527(5) . ?
C3' C12' 1.533(5) . ?
C3' C11' 1.557(6) . ?
C6 C7 1.396(4) . ?
C6 C17 1.524(4) . ?
C7 C8 1.408(4) . ?
C7' C8' 1.509(5) . ?
C8 C9 1.511(4) . ?
C8' H8' 0.9800 . ?
C8' C9' 1.516(7) . ?
C8' C10' 1.523(7) . ?
C9 H9 0.9800 . ?
C9 C10 1.520(4) . ?
C9 C16 1.566(4) . ?
C9' H9'A 0.9600 . ?
C9' H9'B 0.9600 . ?
C9' H9'C 0.9600 . ?
C10 H10 0.9800 . ?
C10 C11 1.518(5) . ?
C10' H10A 0.9600 . ?
C10' H10B 0.9600 . ?
C10' H10C 0.9600 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.553(5) . ?
C14' H14A 0.9600 . ?
C14' H14B 0.9600 . ?
C14' H14C 0.9600 . ?
C12 C22 1.506(6) . ?
C12 C21 1.517(6) . ?
C13' H13A 0.9600 . ?
C13' H13B 0.9600 . ?
C13' H13C 0.9600 . ?
C12' H12A 0.9600 . ?
C12' H12B 0.9600 . ?
C12' H12C 0.9600 . ?
C14 C15 1.537(5) . ?
C14 C23 1.536(5) . ?
C14 C24 1.543(5) . ?
C11' H11C 0.9600 . ?
C11' H11D 0.9600 . ?
C11' H11E 0.9600 . ?
C15 C16 1.554(5) . ?
C16 C25 1.520(5) . ?
C16 C26 1.545(5) . ?
C17 H17A 0.9800 . ?
C17 H17 1.00(11) . ?
C17 C18 1.497(10) . ?
C17 C18A 1.512(7) . ?
C18 H18 0.9800 . ?
C18 C19 1.499(18) . ?
C18 C20 1.526(16) . ?
C18A H18A 0.9800 . ?
C18A C19A 1.548(13) . ?
C18A C20A 1.555(12) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C19A H19D 0.9600 . ?
C19A H19E 0.9600 . ?
C19A H19F 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C20A H20D 0.9600 . ?
C20A H20E 0.9600 . ?
C20A H20F 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
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
Cl26 C46 H46 107.9 . . ?
Cl28 C46 Cl26 114.5(4) . . ?
Cl28 C46 H46 107.9 . . ?
Cl32 C46 Cl26 110.1(5) . . ?
Cl32 C46 Cl28 108.3(5) . . ?
Cl32 C46 H46 107.9 . . ?
C1 O1 C12 110.3(2) . . ?
C3 O2 C1 122.9(2) . . ?
C5 O3 H3 109.5 . . ?
C7 O4 H4 109.5 . . ?
C6' O6 H6 109.5 . . ?
O1 C1 O2 105.6(2) . . ?
O1 C1 C10 107.2(3) . . ?
O1 C1 C14 112.7(2) . . ?
O2 C1 C10 111.0(2) . . ?
O2 C1 C14 106.0(2) . . ?
C10 C1 C14 114.0(3) . . ?
C6' C1' C2' 118.8(3) . . ?
C6' C1' C17 122.3(3) . . ?
C2' C1' C17 118.9(3) . . ?
O6 C6' C1' 123.8(3) . . ?
O6 C6' C5' 110.1(3) . . ?
C1' C6' C5' 126.0(3) . . ?
O2 C3 C4 117.3(3) . . ?
O2 C3 C8 120.2(3) . . ?
C8 C3 C4 122.5(3) . . ?
C6' C5' C4' 112.7(3) . . ?
C6' C5' C14' 107.8(3) . . ?
C6' C5' C13' 110.8(3) . . ?
C4' C5' C14' 109.0(3) . . ?
C4' C5' C13' 107.8(3) . . ?
C14' C5' C13' 108.8(3) . . ?
C3 C4 C5 115.5(3) . . ?
C3 C4 C7' 126.4(3) . . ?
C5 C4 C7' 118.1(3) . . ?
O7 C4' C5' 118.8(4) . . ?
O7 C4' C3' 120.0(4) . . ?
C3' C4' C5' 121.2(3) . . ?
O3 C5 C4 118.9(3) . . ?
O3 C5 C6 117.5(3) . . ?
C6 C5 C4 123.6(3) . . ?
C4' C3' C2' 114.0(3) . . ?
C4' C3' C12' 110.5(3) . . ?
C4' C3' C11' 106.9(3) . . ?
C2' C3' C12' 108.8(3) . . ?
C2' C3' C11' 107.7(3) . . ?
C12' C3' C11' 108.8(4) . . ?
C5 C6 C7 116.8(3) . . ?
C5 C6 C17 120.3(3) . . ?
C7 C6 C17 122.8(3) . . ?
O8 C2' C1' 121.0(3) . . ?
O8 C2' C3' 116.8(3) . . ?
C1' C2' C3' 122.2(3) . . ?
O4 C7 C6 122.0(3) . . ?
O4 C7 C8 115.9(3) . . ?
C6 C7 C8 122.1(3) . . ?
O9 C7' C4 119.3(3) . . ?
O9 C7' C8' 115.8(3) . . ?
C4 C7' C8' 125.0(3) . . ?
C3 C8 C7 119.0(3) . . ?
C3 C8 C9 119.1(3) . . ?
C7 C8 C9 121.9(3) . . ?
C7' C8' H8' 108.9 . . ?
C7' C8' C9' 107.2(4) . . ?
C7' C8' C10' 110.5(4) . . ?
C9' C8' H8' 108.9 . . ?
C9' C8' C10' 112.4(4) . . ?
C10' C8' H8' 108.9 . . ?
C8 C9 H9 108.6 . . ?
C8 C9 C10 108.7(2) . . ?
C8 C9 C16 113.6(2) . . ?
C10 C9 H9 108.6 . . ?
C10 C9 C16 108.7(2) . . ?
C16 C9 H9 108.6 . . ?
C8' C9' H9'A 109.5 . . ?
C8' C9' H9'B 109.5 . . ?
C8' C9' H9'C 109.5 . . ?
H9'A C9' H9'B 109.5 . . ?
H9'A C9' H9'C 109.5 . . ?
H9'B C9' H9'C 109.5 . . ?
C1 C10 C9 108.8(3) . . ?
C1 C10 H10 108.2 . . ?
C1 C10 C11 101.5(3) . . ?
C9 C10 H10 108.2 . . ?
C11 C10 C9 121.4(3) . . ?
C11 C10 H10 108.2 . . ?
C8' C10' H10A 109.5 . . ?
C8' C10' H10B 109.5 . . ?
C8' C10' H10C 109.5 . . ?
H10A C10' H10B 109.5 . . ?
H10A C10' H10C 109.5 . . ?
H10B C10' H10C 109.5 . . ?
C10 C11 H11A 111.3 . . ?
C10 C11 H11B 111.3 . . ?
C10 C11 C12 102.4(3) . . ?
H11A C11 H11B 109.2 . . ?
C12 C11 H11A 111.3 . . ?
C12 C11 H11B 111.3 . . ?
C5' C14' H14A 109.5 . . ?
C5' C14' H14B 109.5 . . ?
C5' C14' H14C 109.5 . . ?
H14A C14' H14B 109.5 . . ?
H14A C14' H14C 109.5 . . ?
H14B C14' H14C 109.5 . . ?
O1 C12 C11 104.1(3) . . ?
O1 C12 C22 107.4(3) . . ?
O1 C12 C21 106.1(3) . . ?
C22 C12 C11 113.2(3) . . ?
C22 C12 C21 112.7(4) . . ?
C21 C12 C11 112.6(4) . . ?
C5' C13' H13A 109.5 . . ?
C5' C13' H13B 109.5 . . ?
C5' C13' H13C 109.5 . . ?
H13A C13' H13B 109.5 . . ?
H13A C13' H13C 109.5 . . ?
H13B C13' H13C 109.5 . . ?
C3' C12' H12A 109.5 . . ?
C3' C12' H12B 109.5 . . ?
C3' C12' H12C 109.5 . . ?
H12A C12' H12B 109.5 . . ?
H12A C12' H12C 109.5 . . ?
H12B C12' H12C 109.5 . . ?
C1 C14 C15 108.9(3) . . ?
C1 C14 C23 112.3(3) . . ?
C1 C14 C24 110.0(3) . . ?
C15 C14 C24 107.8(3) . . ?
C23 C14 C15 109.8(3) . . ?
C23 C14 C24 107.9(3) . . ?
C3' C11' H11C 109.5 . . ?
C3' C11' H11D 109.5 . . ?
C3' C11' H11E 109.5 . . ?
H11C C11' H11D 109.5 . . ?
H11C C11' H11E 109.5 . . ?
H11D C11' H11E 109.5 . . ?
O5 C15 C14 118.8(3) . . ?
O5 C15 C16 118.7(3) . . ?
C14 C15 C16 122.4(3) . . ?
C15 C16 C9 113.2(3) . . ?
C25 C16 C9 111.2(3) . . ?
C25 C16 C15 108.5(3) . . ?
C25 C16 C26 108.0(3) . . ?
C26 C16 C9 109.0(3) . . ?
C26 C16 C15 106.8(3) . . ?
C1' C17 H17A 101.3 . . ?
C1' C17 H17 95(6) . . ?
C6 C17 C1' 116.4(3) . . ?
C6 C17 H17A 101.3 . . ?
C6 C17 H17 99(6) . . ?
C18 C17 C1' 115.6(4) . . ?
C18 C17 C6 117.5(4) . . ?
C18 C17 H17 108(6) . . ?
C18A C17 C1' 116.7(4) . . ?
C18A C17 C6 115.7(4) . . ?
C18A C17 H17A 101.3 . . ?
C17 C18 H18 107.1 . . ?
C17 C18 C19 111.3(9) . . ?
C17 C18 C20 112.9(9) . . ?
C19 C18 H18 107.1 . . ?
C19 C18 C20 110.9(13) . . ?
C20 C18 H18 107.1 . . ?
C17 C18A H18A 109.2 . . ?
C17 C18A C19A 109.8(7) . . ?
C17 C18A C20A 110.4(6) . . ?
C19A C18A H18A 109.2 . . ?
C19A C18A C20A 108.9(9) . . ?
C20A C18A H18A 109.2 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18A C19A H19D 109.5 . . ?
C18A C19A H19E 109.5 . . ?
C18A C19A H19F 109.5 . . ?
H19D C19A H19E 109.5 . . ?
H19D C19A H19F 109.5 . . ?
H19E C19A H19F 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18A C20A H20D 109.5 . . ?
C18A C20A H20E 109.5 . . ?
C18A C20A H20F 109.5 . . ?
H20D C20A H20E 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
C12 C22 H22A 109.5 . . ?
C12 C22 H22B 109.5 . . ?
C12 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C12 C21 H21A 109.5 . . ?
C12 C21 H21B 109.5 . . ?
C12 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C14 C23 H23A 109.5 . . ?
C14 C23 H23B 109.5 . . ?
C14 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C14 C24 H24A 109.5 . . ?
C14 C24 H24B 109.5 . . ?
C14 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C16 C25 H25A 109.5 . . ?
C16 C25 H25B 109.5 . . ?
C16 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C16 C26 H26A 109.5 . . ?
C16 C26 H26B 109.5 . . ?
C16 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C10 C9 -165.4(2) . . . . ?
O1 C1 C10 C11 -36.3(3) . . . . ?
O1 C1 C14 C15 -170.2(3) . . . . ?
O1 C1 C14 C23 67.9(4) . . . . ?
O1 C1 C14 C24 -52.2(4) . . . . ?
O2 C1 C10 C9 -50.5(3) . . . . ?
O2 C1 C10 C11 78.6(3) . . . . ?
O2 C1 C14 C15 74.8(3) . . . . ?
O2 C1 C14 C23 -47.1(4) . . . . ?
O2 C1 C14 C24 -167.3(3) . . . . ?
O2 C3 C4 C5 -174.1(3) . . . . ?
O2 C3 C4 C7' 6.8(5) . . . . ?
O2 C3 C8 C7 178.4(3) . . . . ?
O2 C3 C8 C9 -3.7(4) . . . . ?
O3 C5 C6 C7 176.0(3) . . . . ?
O3 C5 C6 C17 -8.7(4) . . . . ?
O4 C7 C8 C3 176.5(3) . . . . ?
O4 C7 C8 C9 -1.4(4) . . . . ?
O5 C15 C16 C9 155.4(3) . . . . ?
O5 C15 C16 C25 31.5(5) . . . . ?
O5 C15 C16 C26 -84.7(4) . . . . ?
O6 C6' C5' C4' -177.8(3) . . . . ?
O6 C6' C5' C14' -57.5(4) . . . . ?
O6 C6' C5' C13' 61.3(4) . . . . ?
O7 C4' C3' C2' -159.9(5) . . . . ?
O7 C4' C3' C12' -37.0(6) . . . . ?
O7 C4' C3' C11' 81.3(5) . . . . ?
O9 C7' C8' C9' 86.3(4) . . . . ?
O9 C7' C8' C10' -36.6(5) . . . . ?
C1 O1 C12 C11 2.7(4) . . . . ?
C1 O1 C12 C22 123.0(3) . . . . ?
C1 O1 C12 C21 -116.2(3) . . . . ?
C1 O2 C3 C4 -165.2(3) . . . . ?
C1 O2 C3 C8 15.0(4) . . . . ?
C1 C10 C11 C12 36.1(3) . . . . ?
C1 C14 C15 O5 -155.4(3) . . . . ?
C1 C14 C15 C16 28.5(4) . . . . ?
C1' C6' C5' C4' -0.2(5) . . . . ?
C1' C6' C5' C14' 120.1(4) . . . . ?
C1' C6' C5' C13' -121.1(4) . . . . ?
C1' C17 C18 C19 174.8(12) . . . . ?
C1' C17 C18 C20 49.3(13) . . . . ?
C1' C17 C18A C19A -164.4(7) . . . . ?
C1' C17 C18A C20A -44.3(10) . . . . ?
C6' C1' C2' O8 167.1(3) . . . . ?
C6' C1' C2' C3' -11.9(5) . . . . ?
C6' C1' C17 C6 -91.1(4) . . . . ?
C6' C1' C17 C18 52.9(6) . . . . ?
C6' C1' C17 C18A 126.6(5) . . . . ?
C6' C5' C4' O7 162.9(5) . . . . ?
C6' C5' C4' C3' -20.0(5) . . . . ?
C3 O2 C1 O1 129.6(3) . . . . ?
C3 O2 C1 C10 13.7(4) . . . . ?
C3 O2 C1 C14 -110.6(3) . . . . ?
C3 C4 C5 O3 177.4(3) . . . . ?
C3 C4 C5 C6 -3.2(4) . . . . ?
C3 C4 C7' O9 179.7(3) . . . . ?
C3 C4 C7' C8' -0.7(6) . . . . ?
C3 C8 C9 C10 -33.9(4) . . . . ?
C3 C8 C9 C16 87.3(3) . . . . ?
C5' C4' C3' C2' 23.1(5) . . . . ?
C5' C4' C3' C12' 145.9(4) . . . . ?
C5' C4' C3' C11' -95.8(4) . . . . ?
C4 C3 C8 C7 -1.4(4) . . . . ?
C4 C3 C8 C9 176.5(3) . . . . ?
C4 C5 C6 C7 -3.4(4) . . . . ?
C4 C5 C6 C17 171.9(3) . . . . ?
C4 C7' C8' C9' -93.3(4) . . . . ?
C4 C7' C8' C10' 143.8(4) . . . . ?
C4' C3' C2' O8 174.0(3) . . . . ?
C4' C3' C2' C1' -6.9(5) . . . . ?
C5 C4 C7' O9 0.6(5) . . . . ?
C5 C4 C7' C8' -179.8(3) . . . . ?
C5 C6 C7 O4 -174.5(3) . . . . ?
C5 C6 C7 C8 8.1(4) . . . . ?
C5 C6 C17 C1' 92.1(4) . . . . ?
C5 C6 C17 C18 -51.2(6) . . . . ?
C5 C6 C17 C18A -125.2(5) . . . . ?
C6 C7 C8 C3 -5.8(4) . . . . ?
C6 C7 C8 C9 176.3(3) . . . . ?
C6 C17 C18 C19 -41.6(14) . . . . ?
C6 C17 C18 C20 -167.1(11) . . . . ?
C6 C17 C18A C19A 53.1(9) . . . . ?
C6 C17 C18A C20A 173.2(8) . . . . ?
C2' C1' C6' O6 -166.8(3) . . . . ?
C2' C1' C6' C5' 15.9(5) . . . . ?
C2' C1' C17 C6 87.1(4) . . . . ?
C2' C1' C17 C18 -128.9(6) . . . . ?
C2' C1' C17 C18A -55.1(5) . . . . ?
C7 C6 C17 C1' -92.8(4) . . . . ?
C7 C6 C17 C18 123.9(6) . . . . ?
C7 C6 C17 C18A 49.8(6) . . . . ?
C7 C8 C9 C10 144.0(3) . . . . ?
C7 C8 C9 C16 -94.9(3) . . . . ?
C7' C4 C5 O3 -3.4(4) . . . . ?
C7' C4 C5 C6 176.0(3) . . . . ?
C8 C3 C4 C5 5.7(4) . . . . ?
C8 C3 C4 C7' -173.4(3) . . . . ?
C8 C9 C10 C1 60.0(3) . . . . ?
C8 C9 C10 C11 -57.0(4) . . . . ?
C8 C9 C16 C15 -77.1(3) . . . . ?
C8 C9 C16 C25 45.3(4) . . . . ?
C8 C9 C16 C26 164.3(3) . . . . ?
C9 C10 C11 C12 156.6(3) . . . . ?
C10 C1 C14 C15 -47.7(4) . . . . ?
C10 C1 C14 C23 -169.5(3) . . . . ?
C10 C1 C14 C24 70.3(4) . . . . ?
C10 C9 C16 C15 44.0(4) . . . . ?
C10 C9 C16 C25 166.4(3) . . . . ?
C10 C9 C16 C26 -74.6(3) . . . . ?
C10 C11 C12 O1 -24.8(4) . . . . ?
C10 C11 C12 C22 -141.0(3) . . . . ?
C10 C11 C12 C21 89.7(4) . . . . ?
C14' C5' C4' O7 43.3(6) . . . . ?
C14' C5' C4' C3' -139.6(4) . . . . ?
C12 O1 C1 O2 -97.4(3) . . . . ?
C12 O1 C1 C10 21.1(3) . . . . ?
C12 O1 C1 C14 147.4(3) . . . . ?
C13' C5' C4' O7 -74.6(5) . . . . ?
C13' C5' C4' C3' 102.5(4) . . . . ?
C12' C3' C2' O8 50.3(5) . . . . ?
C12' C3' C2' C1' -130.7(4) . . . . ?
C14 C1 C10 C9 69.1(3) . . . . ?
C14 C1 C10 C11 -161.8(3) . . . . ?
C14 C15 C16 C9 -28.5(4) . . . . ?
C14 C15 C16 C25 -152.4(3) . . . . ?
C14 C15 C16 C26 91.4(4) . . . . ?
C11' C3' C2' O8 -67.5(4) . . . . ?
C11' C3' C2' C1' 111.5(4) . . . . ?
C16 C9 C10 C1 -64.1(3) . . . . ?
C16 C9 C10 C11 179.0(3) . . . . ?
C17 C1' C6' O6 11.4(5) . . . . ?
C17 C1' C6' C5' -165.8(3) . . . . ?
C17 C1' C2' O8 -11.2(5) . . . . ?
C17 C1' C2' C3' 169.8(3) . . . . ?
C17 C6 C7 O4 10.3(4) . . . . ?
C17 C6 C7 C8 -167.2(3) . . . . ?
C23 C14 C15 O5 -32.0(4) . . . . ?
C23 C14 C15 C16 151.9(3) . . . . ?
C24 C14 C15 O5 85.3(4) . . . . ?
C24 C14 C15 C16 -90.8(4) . . . . ?
_iucr_refine_instructions_details
;
TITL CHENPENG_A1(34-48) in P-1 #2
chenpeng_a1(34-48).res
created by SHELXL-2017/1 at 15:20:05 on 19-Nov-2017
CELL 1.54184 12.754097 13.500751 13.69607 94.8923 105.4548 113.7913
ZERR 2 0.000539 0.000552 0.000607 0.0035 0.0038 0.004
LATT 1
SFAC C H Cl O
UNIT 78 106 6 18
L.S. 10
PLAN 20
TEMP 19.85
BOND $H
MORE -1
CONF
fmap 2
acta
REM
REM
REM
WGHT 0.180400 1.853200
FVAR 7.07663 0.41116
CL26 3 0.205741 0.900362 0.514325 11.00000 0.12941 0.25695 =
0.14625 -0.02999 0.04672 -0.01388
CL28 3 -0.029880 0.863232 0.529469 11.00000 0.25444 0.22832 =
0.20387 0.05464 0.14251 0.13288
CL32 3 0.002590 0.690877 0.437150 11.00000 0.18553 0.15720 =
0.22138 -0.02364 0.00480 0.06138
C46 1 0.049260 0.830785 0.458095 11.00000 0.13613 0.14552 =
0.07259 -0.00246 0.01934 0.07194
AFIX 13
H46 2 0.027392 0.849775 0.390532 11.00000 -1.20000
AFIX 0
O1 4 0.429592 0.109650 -0.021148 11.00000 0.05306 0.04163 =
0.05030 -0.00268 0.00957 0.02323
O2 4 0.286668 0.139938 0.028678 11.00000 0.06482 0.03513 =
0.04394 0.00714 0.02663 0.01906
O3 4 0.170533 0.257192 0.302704 11.00000 0.07312 0.04964 =
0.05308 0.00964 0.03524 0.02269
AFIX 147
H3 2 0.157892 0.194173 0.310026 11.00000 -1.50000
AFIX 0
O4 4 0.339298 0.507361 0.102377 11.00000 0.07129 0.03802 =
0.04560 0.00980 0.02197 0.02683
AFIX 147
H4 2 0.356699 0.554540 0.153508 11.00000 -1.50000
AFIX 0
O5 4 0.099805 0.149697 -0.241795 11.00000 0.06472 0.06610 =
0.07161 0.00292 -0.01156 0.02191
O6 4 0.240985 0.419887 0.462795 11.00000 0.08789 0.05090 =
0.04718 0.00614 0.02702 0.02007
AFIX 147
H6 2 0.217100 0.373641 0.409092 11.00000 -1.50000
AFIX 0
O7 4 0.475622 0.795794 0.612012 11.00000 0.16543 0.06365 =
0.07079 -0.01464 0.05689 0.01304
O8 4 0.404240 0.665405 0.263716 11.00000 0.09292 0.04951 =
0.04447 0.00598 0.02349 0.02262
O9 4 0.171389 0.079040 0.283435 11.00000 0.09801 0.05119 =
0.06044 0.01978 0.04281 0.02696
C1 1 0.356136 0.162308 -0.044149 11.00000 0.04605 0.03727 =
0.03862 0.00303 0.01471 0.01654
C1' 1 0.300078 0.543860 0.353303 11.00000 0.04905 0.04652 =
0.03976 0.00322 0.01118 0.02829
C6' 1 0.303120 0.520054 0.448534 11.00000 0.05313 0.05007 =
0.04135 0.00562 0.01613 0.02670
C3 1 0.278478 0.221067 0.087490 11.00000 0.04039 0.03470 =
0.03478 0.00144 0.00862 0.01347
C5' 1 0.371657 0.602179 0.551578 11.00000 0.06520 0.05669 =
0.03674 0.00452 0.01688 0.03030
C4 1 0.234870 0.194129 0.171122 11.00000 0.04278 0.03904 =
0.03743 0.00535 0.01131 0.01513
C4' 1 0.441202 0.719849 0.540110 11.00000 0.07940 0.05321 =
0.04706 -0.00317 0.01968 0.02650
C5 1 0.216365 0.278490 0.224879 11.00000 0.04220 0.04653 =
0.03515 0.00410 0.01242 0.01614
C3' 1 0.472244 0.741717 0.443045 11.00000 0.06673 0.04467 =
0.04486 0.00455 0.01308 0.02612
C6 1 0.244362 0.382696 0.201664 11.00000 0.03836 0.04194 =
0.03507 0.00284 0.00660 0.01684
C2' 1 0.389619 0.648119 0.347364 11.00000 0.06095 0.04649 =
0.04339 0.00821 0.01596 0.03060
C7 1 0.299068 0.406012 0.125292 11.00000 0.04225 0.03887 =
0.03527 0.00518 0.00633 0.01928
C7' 1 0.209357 0.091118 0.207621 11.00000 0.05208 0.04327 =
0.04178 0.00899 0.01689 0.01380
C8 1 0.311482 0.324369 0.064701 11.00000 0.04108 0.03829 =
0.03310 0.00554 0.01007 0.01697
C8' 1 0.224320 -0.005488 0.160430 11.00000 0.08763 0.04405 =
0.06405 0.02163 0.03910 0.03100
AFIX 13
H8' 2 0.284055 0.021701 0.124597 11.00000 -1.20000
AFIX 0
C9 1 0.363917 0.348249 -0.022153 11.00000 0.04414 0.03423 =
0.03973 0.00643 0.01431 0.01408
AFIX 13
H9 2 0.418026 0.427771 -0.007290 11.00000 -1.20000
AFIX 0
C9' 1 0.102528 -0.085054 0.081354 11.00000 0.10718 0.06316 =
0.10121 -0.01284 0.04082 0.01559
AFIX 137
H9'A 2 0.043007 -0.111031 0.115564 11.00000 -1.50000
H9'B 2 0.109218 -0.146981 0.048592 11.00000 -1.50000
H9'C 2 0.078236 -0.047532 0.029833 11.00000 -1.50000
AFIX 0
C10 1 0.438117 0.284467 -0.025186 11.00000 0.04347 0.03747 =
0.04194 0.00460 0.01679 0.01414
AFIX 13
H10 2 0.468465 0.297478 -0.083819 11.00000 -1.20000
AFIX 0
C10' 1 0.269193 -0.059729 0.244433 11.00000 0.17803 0.09135 =
0.08982 0.04419 0.05704 0.08803
AFIX 137
H10A 2 0.345770 -0.006189 0.293064 11.00000 -1.50000
H10B 2 0.278924 -0.120495 0.213239 11.00000 -1.50000
H10C 2 0.211176 -0.086701 0.279960 11.00000 -1.50000
AFIX 0
C11 1 0.542718 0.299563 0.069049 11.00000 0.04591 0.04278 =
0.05329 -0.00386 0.00585 0.01791
AFIX 23
H11A 2 0.524622 0.308876 0.132696 11.00000 -1.20000
H11B 2 0.617037 0.362905 0.073349 11.00000 -1.20000
AFIX 0
C14' 1 0.278800 0.600013 0.604705 11.00000 0.08413 0.08029 =
0.05801 -0.00133 0.03368 0.03480
AFIX 137
H14A 2 0.220064 0.618553 0.560861 11.00000 -1.50000
H14B 2 0.319939 0.652967 0.669853 11.00000 -1.50000
H14C 2 0.238466 0.527168 0.616544 11.00000 -1.50000
AFIX 0
C12 1 0.552382 0.189264 0.047824 11.00000 0.04960 0.05210 =
0.05738 -0.00585 0.00589 0.02555
C13' 1 0.463387 0.569805 0.621804 11.00000 0.08548 0.08095 =
0.04574 0.01102 0.00818 0.04367
AFIX 137
H13A 2 0.421399 0.496408 0.631809 11.00000 -1.50000
H13B 2 0.503775 0.621366 0.687772 11.00000 -1.50000
H13C 2 0.522193 0.571450 0.589629 11.00000 -1.50000
AFIX 0
C12' 1 0.468994 0.849588 0.419448 11.00000 0.12460 0.05255 =
0.06640 0.00538 0.02206 0.04682
AFIX 137
H12A 2 0.487280 0.861505 0.356598 11.00000 -1.50000
H12B 2 0.528043 0.910580 0.475743 11.00000 -1.50000
H12C 2 0.389622 0.844246 0.411224 11.00000 -1.50000
AFIX 0
C14 1 0.262249 0.113123 -0.152793 11.00000 0.05326 0.04005 =
0.03867 0.00180 0.01212 0.01499
C11' 1 0.603805 0.754888 0.464097 11.00000 0.06500 0.08194 =
0.06158 0.01282 0.01497 0.02953
AFIX 137
H11C 2 0.608691 0.690633 0.485707 11.00000 -1.50000
H11D 2 0.659404 0.819731 0.517803 11.00000 -1.50000
H11E 2 0.624458 0.762422 0.401764 11.00000 -1.50000
AFIX 0
C15 1 0.200234 0.188923 -0.178638 11.00000 0.05106 0.04956 =
0.03877 0.00793 0.00971 0.01659
C16 1 0.265368 0.315666 -0.131478 11.00000 0.05533 0.04415 =
0.03890 0.00993 0.01182 0.02168
C17 1 0.206806 0.462000 0.252461 11.00000 0.04846 0.05610 =
0.04124 0.00133 0.01010 0.02904
PART 2
AFIX 13
H17A 2 0.145653 0.411438 0.278424 -21.00000 -1.20000
AFIX 0
PART 0
PART 1
H17 2 0.222098 0.517969 0.207932 21.00000 -1.20000
C18 1 0.076897 0.418250 0.247346 21.00000 0.04124 0.07626 =
0.06798 -0.01169 0.00452 0.03054
AFIX 13
H18 2 0.065914 0.370502 0.297472 21.00000 -1.20000
AFIX 0
PART 0
PART 2
C18A 1 0.132527 0.504973 0.178768 -21.00000 0.07034 0.09018 =
0.05641 0.00814 0.01044 0.05549
AFIX 13
H18A 2 0.182804 0.552634 0.142649 -21.00000 -1.20000
AFIX 0
PART 0
PART 1
C19 1 -0.007252 0.347335 0.142425 21.00000 0.05383 0.13300 =
0.08857 -0.01781 -0.00708 0.03135
AFIX 137
H19A 2 -0.012185 0.393764 0.093773 21.00000 -1.50000
H19B 2 -0.086497 0.304698 0.146449 21.00000 -1.50000
H19C 2 0.023043 0.298135 0.119872 21.00000 -1.50000
AFIX 0
PART 0
PART 2
C19A 1 0.021161 0.406474 0.097993 -21.00000 0.07186 0.12461 =
0.07438 -0.00915 -0.01461 0.05689
AFIX 137
H19D 2 0.047505 0.358652 0.066417 -21.00000 -1.50000
H19E 2 -0.018995 0.434141 0.045560 -21.00000 -1.50000
H19F 2 -0.034075 0.365559 0.131919 -21.00000 -1.50000
AFIX 0
PART 0
PART 1
C20 1 0.042880 0.509554 0.278261 21.00000 0.06587 0.10828 =
0.12662 -0.00681 0.02339 0.05971
AFIX 137
H20A 2 0.108102 0.564155 0.336404 21.00000 -1.50000
H20B 2 -0.029251 0.478044 0.296982 21.00000 -1.50000
H20C 2 0.028381 0.543917 0.220852 21.00000 -1.50000
AFIX 0
PART 0
PART 2
C20A 1 0.087304 0.573017 0.239417 -21.00000 0.09658 0.14033 =
0.09915 -0.00204 0.00578 0.09367
AFIX 137
H20D 2 0.038236 0.526641 0.275102 -21.00000 -1.50000
H20E 2 0.039940 0.599359 0.191665 -21.00000 -1.50000
H20F 2 0.155825 0.635046 0.288918 -21.00000 -1.50000
AFIX 0
PART 0
C22 1 0.579654 0.145172 0.144025 11.00000 0.08763 0.06446 =
0.06650 -0.00479 -0.00561 0.04506
AFIX 137
H22A 2 0.519859 0.137437 0.176877 11.00000 -1.50000
H22B 2 0.658674 0.195809 0.191124 11.00000 -1.50000
H22C 2 0.577813 0.074164 0.125398 11.00000 -1.50000
AFIX 0
C21 1 0.637292 0.195558 -0.013260 11.00000 0.05960 0.07948 =
0.10343 -0.00945 0.02643 0.03360
AFIX 137
H21A 2 0.628658 0.122530 -0.035749 11.00000 -1.50000
H21B 2 0.719554 0.242479 0.030005 11.00000 -1.50000
H21C 2 0.617403 0.225649 -0.072699 11.00000 -1.50000
AFIX 0
C23 1 0.166358 -0.005008 -0.162801 11.00000 0.06252 0.04291 =
0.05428 -0.00067 0.00730 0.00952
AFIX 137
H23A 2 0.205738 -0.047797 -0.132554 11.00000 -1.50000
H23B 2 0.121541 -0.039087 -0.234835 11.00000 -1.50000
H23C 2 0.111845 -0.001997 -0.127271 11.00000 -1.50000
AFIX 0
C24 1 0.325348 0.108417 -0.233574 11.00000 0.07939 0.06101 =
0.04492 0.00279 0.02351 0.02852
AFIX 137
H24A 2 0.393636 0.178899 -0.222096 11.00000 -1.50000
H24B 2 0.269012 0.091523 -0.302130 11.00000 -1.50000
H24C 2 0.352664 0.051899 -0.226768 11.00000 -1.50000
AFIX 0
C25 1 0.169908 0.354429 -0.126912 11.00000 0.06358 0.06613 =
0.04960 0.01010 0.00985 0.03689
AFIX 137
H25A 2 0.121472 0.311519 -0.088939 11.00000 -1.50000
H25B 2 0.118852 0.344863 -0.196126 11.00000 -1.50000
H25C 2 0.209094 0.431394 -0.092787 11.00000 -1.50000
AFIX 0
C26 1 0.327163 0.372263 -0.207817 11.00000 0.08148 0.05721 =
0.04450 0.01817 0.02291 0.02815
AFIX 137
H26A 2 0.364572 0.451329 -0.183556 11.00000 -1.50000
H26B 2 0.267440 0.351807 -0.275266 11.00000 -1.50000
H26C 2 0.387868 0.348814 -0.212056 11.00000 -1.50000
AFIX 0
HKLF 4
REM CHENPENG_A1(34-48) in P-1 #2
REM R1 = 0.0914 for 5545 Fo > 4sig(Fo) and 0.0995 for all 6474 data
REM 510 parameters refined using 0 restraints
END
WGHT 0.1804 1.8532
REM Highest difference peak 0.844, deepest hole -0.886, 1-sigma level 0.079
Q1 1 0.0549 0.9579 0.5119 11.00000 0.05 0.84
Q2 1 -0.0474 0.7486 0.4746 11.00000 0.05 0.67
Q3 1 0.0533 0.7213 0.5314 11.00000 0.05 0.66
Q4 1 0.0780 0.7409 0.6245 11.00000 0.05 0.62
Q5 1 0.0857 0.7384 0.4009 11.00000 0.05 0.54
Q6 1 0.0244 0.8124 0.5849 11.00000 0.05 0.49
Q7 1 0.1958 0.8359 0.4714 11.00000 0.05 0.40
Q8 1 0.1364 0.9284 0.4466 11.00000 0.05 0.40
Q9 1 0.2050 0.8390 0.5975 11.00000 0.05 0.25
Q10 1 0.1620 0.8547 0.5664 11.00000 0.05 0.25
Q11 1 0.4011 0.2361 -0.0307 11.00000 0.05 0.24
Q12 1 0.2606 0.8603 0.5992 11.00000 0.05 0.23
Q13 1 0.1558 0.1645 -0.2560 11.00000 0.05 0.23
Q14 1 0.1820 -0.1168 0.1971 11.00000 0.05 0.21
Q15 1 0.1819 0.4360 0.4385 11.00000 0.05 0.20
Q16 1 0.1822 -0.1994 0.1609 11.00000 0.05 0.18
Q17 1 0.5313 0.7627 0.6214 11.00000 0.05 0.17
Q18 1 0.1194 0.1648 -0.1895 11.00000 0.05 0.17
Q19 1 0.3109 0.1410 -0.0963 11.00000 0.05 0.17
Q20 1 0.1350 0.0659 0.2395 11.00000 0.05 0.17
REM The information below was added by Olex2.
REM
REM R1 = 0.0914 for 5545 Fo > 4sig(Fo) and 0.0995 for all 17119 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.84, deepest hole -0.89
REM Mean Shift 0, Max Shift 0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0995
REM R1_gt = 0.0914
REM wR_ref = 0.2842
REM GOOF = 1.040
REM Shift_max = 0.001
REM Shift_mean = 0
REM Reflections_all = 17119
REM Reflections_gt = 5545
REM Parameters = n/a
REM Hole = -0.89
REM Peak = 0.84
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_cm102
_database_code_depnum_ccdc_archive 'CCDC 1582656'
_audit_update_record
;
2017-10-28 deposited with the CCDC.
2017-11-27 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014/6
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C39 H54 O9'
_chemical_formula_weight 666.82
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 10.6706(10)
_cell_length_b 13.8828(12)
_cell_length_c 14.1078(13)
_cell_angle_alpha 70.567(3)
_cell_angle_beta 84.605(3)
_cell_angle_gamma 69.424(3)
_cell_volume 1844.5(3)
_cell_formula_units_Z 2
_cell_measurement_temperature 296(2)
_cell_measurement_reflns_used 220
_cell_measurement_theta_min 15
_cell_measurement_theta_max 15
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.201
_exptl_crystal_F_000 720
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.400
_exptl_crystal_size_mid 0.300
_exptl_crystal_size_min 0.200
_exptl_absorpt_coefficient_mu 0.084
_shelx_estimated_absorpt_T_min 0.967
_shelx_estimated_absorpt_T_max 0.983
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6123
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_process_details ?
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 296(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_source ?
_diffrn_measurement_device_type 'BRUKER D8VENTURE DIFFRACTOMETER'
_diffrn_measurement_method 'PHI & OMEGA SCAN'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 57279
_diffrn_reflns_av_unetI/netI 0.0411
_diffrn_reflns_av_R_equivalents 0.0634
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_theta_min 2.340
_diffrn_reflns_theta_max 25.250
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total 6672
_reflns_number_gt 4469
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'BRUKER D8VENTURE DIFFRACTOMETER'
_computing_cell_refinement 'BRUKER D8VENTURE DIFFRACTOMETER'
_computing_data_reduction 'BRUKER D8VENTURE DIFFRACTOMETER'
_computing_structure_solution ?
_computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics 'BRUKER SHELXTL'
_computing_publication_material 'BRUKER SHELXTL'
_refine_special_details ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+0.6420P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens mixed
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 6672
_refine_ls_number_parameters 449
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0904
_refine_ls_R_factor_gt 0.0509
_refine_ls_wR_factor_ref 0.1273
_refine_ls_wR_factor_gt 0.1095
_refine_ls_goodness_of_fit_ref 1.015
_refine_ls_restrained_S_all 1.015
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.50490(18) 0.18055(13) 0.67204(17) 0.0731(6) Uani 1 1 d . . . . .
O2 O 0.82898(16) 0.34877(12) 0.62168(13) 0.0537(4) Uani 1 1 d . . . . .
O3 O 0.40786(13) 0.50552(10) 0.73604(11) 0.0378(4) Uani 1 1 d . . . . .
O4 O 0.14934(15) 0.65627(14) 0.68662(12) 0.0533(4) Uani 1 1 d . . . . .
O5 O 0.71350(13) 0.69399(11) 0.72750(12) 0.0420(4) Uani 1 1 d . . . . .
H5A H 0.7673 0.6438 0.7108 0.063 Uiso 1 1 calc R U . . .
O6 O 0.25069(12) 0.85351(10) 0.76819(11) 0.0373(4) Uani 1 1 d . . . . .
O7 O 0.38226(17) 0.85428(15) 1.01749(13) 0.0631(5) Uani 1 1 d . . . . .
O8 O 0.15918(13) 1.03694(11) 0.69812(11) 0.0418(4) Uani 1 1 d . . . . .
O9 O -0.05194(16) 0.57586(16) 0.67975(14) 0.0602(5) Uani 1 1 d . . . . .
C1 C 0.5404(2) 0.25569(16) 0.66663(17) 0.0420(5) Uani 1 1 d . . . . .
C2 C 0.6850(2) 0.24704(16) 0.64333(17) 0.0414(5) Uani 1 1 d . . . . .
C3 C 0.7223(2) 0.33966(16) 0.65345(16) 0.0358(5) Uani 1 1 d . . . . .
C4 C 0.63166(19) 0.41527(15) 0.70171(15) 0.0300(5) Uani 1 1 d . . . . .
C5 C 0.50262(19) 0.42564(15) 0.70672(15) 0.0310(5) Uani 1 1 d . . . . .
C6 C 0.4368(2) 0.35917(15) 0.67813(16) 0.0342(5) Uani 1 1 d . . . . .
C7 C 0.7097(3) 0.2435(2) 0.5355(2) 0.0752(9) Uani 1 1 d . . . . .
H7A H 0.8007 0.2380 0.5188 0.113 Uiso 1 1 calc R U . . .
H7B H 0.6936 0.1815 0.5303 0.113 Uiso 1 1 calc R U . . .
H7C H 0.6503 0.3086 0.4898 0.113 Uiso 1 1 calc R U . . .
C8 C 0.7755(3) 0.14193(19) 0.7183(2) 0.0702(8) Uani 1 1 d . . . . .
H8A H 0.8676 0.1350 0.7047 0.105 Uiso 1 1 calc R U . . .
H8B H 0.7565 0.1442 0.7855 0.105 Uiso 1 1 calc R U . . .
H8C H 0.7592 0.0808 0.7114 0.105 Uiso 1 1 calc R U . . .
C9 C 0.3644(2) 0.42523(18) 0.57545(18) 0.0510(6) Uani 1 1 d . . . . .
H9A H 0.3221 0.3834 0.5566 0.076 Uiso 1 1 calc R U . . .
H9B H 0.2979 0.4913 0.5798 0.076 Uiso 1 1 calc R U . . .
H9C H 0.4281 0.4422 0.5258 0.076 Uiso 1 1 calc R U . . .
C10 C 0.3357(3) 0.3303(2) 0.7569(2) 0.0561(7) Uani 1 1 d . . . . .
H10A H 0.2947 0.2879 0.7375 0.084 Uiso 1 1 calc R U . . .
H10B H 0.3810 0.2890 0.8210 0.084 Uiso 1 1 calc R U . . .
H10C H 0.2681 0.3957 0.7616 0.084 Uiso 1 1 calc R U . . .
C11 C 0.68253(19) 0.48745(15) 0.73601(15) 0.0309(5) Uani 1 1 d . . . . .
H11A H 0.7510 0.5058 0.6893 0.037 Uiso 1 1 calc R U . . .
C12 C 0.7469(2) 0.43161(17) 0.84367(17) 0.0410(5) Uani 1 1 d . . . . .
H12A H 0.7746 0.4848 0.8596 0.049 Uiso 1 1 calc R U . . .
C13 C 0.6463(3) 0.4030(2) 0.92186(19) 0.0610(7) Uani 1 1 d . . . . .
H13A H 0.5685 0.4665 0.9157 0.092 Uiso 1 1 calc R U . . .
H13B H 0.6208 0.3475 0.9114 0.092 Uiso 1 1 calc R U . . .
H13C H 0.6861 0.3771 0.9879 0.092 Uiso 1 1 calc R U . . .
C14 C 0.8722(3) 0.3333(2) 0.8505(2) 0.0646(7) Uani 1 1 d . . . . .
H14A H 0.9337 0.3538 0.8004 0.097 Uiso 1 1 calc R U . . .
H14B H 0.9137 0.3068 0.9161 0.097 Uiso 1 1 calc R U . . .
H14C H 0.8484 0.2772 0.8395 0.097 Uiso 1 1 calc R U . . .
C15 C 0.56931(18) 0.59167(15) 0.73146(15) 0.0289(4) Uani 1 1 d . . . . .
C16 C 0.43851(19) 0.59464(15) 0.73669(15) 0.0296(5) Uani 1 1 d . . . . .
C17 C 0.32876(18) 0.68105(15) 0.74833(15) 0.0291(4) Uani 1 1 d . . . . .
C18 C 0.18955(19) 0.67927(15) 0.75075(16) 0.0322(5) Uani 1 1 d . . . . .
C19 C 0.1022(2) 0.6996(2) 0.83667(18) 0.0484(6) Uani 1 1 d . . . . .
H19A H 0.1482 0.7227 0.8775 0.058 Uiso 1 1 calc R U . . .
C20 C -0.0310(3) 0.7898(3) 0.7984(3) 0.1054(13) Uani 1 1 d . . . . .
H20A H -0.0853 0.8015 0.8544 0.158 Uiso 1 1 calc R U . . .
H20B H -0.0150 0.8555 0.7595 0.158 Uiso 1 1 calc R U . . .
H20C H -0.0766 0.7691 0.7571 0.158 Uiso 1 1 calc R U . . .
C21 C 0.0845(4) 0.5936(3) 0.9010(2) 0.1125(15) Uani 1 1 d . . . . .
H21A H 0.0287 0.6051 0.9565 0.169 Uiso 1 1 calc R U . . .
H21B H 0.0431 0.5683 0.8611 0.169 Uiso 1 1 calc R U . . .
H21C H 0.1703 0.5404 0.9260 0.169 Uiso 1 1 calc R U . . .
C22 C 0.35741(18) 0.76871(15) 0.75689(15) 0.0293(4) Uani 1 1 d . . . . .
C23 C 0.48687(18) 0.77134(15) 0.75116(15) 0.0295(4) Uani 1 1 d . . . . .
C24 C 0.59058(18) 0.68431(15) 0.73507(15) 0.0297(5) Uani 1 1 d . . . . .
C25 C 0.50798(19) 0.86845(15) 0.76295(15) 0.0299(5) Uani 1 1 d . . . . .
H25A H 0.5904 0.8755 0.7292 0.036 Uiso 1 1 calc R U . . .
C26 C 0.39092(19) 0.96921(15) 0.71131(15) 0.0323(5) Uani 1 1 d . . . . .
H26A H 0.4037 1.0320 0.7208 0.039 Uiso 1 1 calc R U . . .
C27 C 0.26350(19) 0.95822(15) 0.76149(16) 0.0328(5) Uani 1 1 d . . . . .
C28 C 0.2521(2) 0.96432(16) 0.86802(16) 0.0376(5) Uani 1 1 d . . . . .
C29 C 0.1339(2) 0.9334(2) 0.9225(2) 0.0557(7) Uani 1 1 d . . . . .
H29A H 0.1301 0.9382 0.9891 0.083 Uiso 1 1 calc R U . . .
H29B H 0.0521 0.9822 0.8861 0.083 Uiso 1 1 calc R U . . .
H29C H 0.1454 0.8604 0.9266 0.083 Uiso 1 1 calc R U . . .
C30 C 0.2319(3) 1.08041(18) 0.8661(2) 0.0560(7) Uani 1 1 d . . . . .
H30A H 0.2249 1.0829 0.9337 0.084 Uiso 1 1 calc R U . . .
H30B H 0.3069 1.1006 0.8350 0.084 Uiso 1 1 calc R U . . .
H30C H 0.1514 1.1301 0.8285 0.084 Uiso 1 1 calc R U . . .
C31 C 0.3839(2) 0.88795(17) 0.92674(18) 0.0393(5) Uani 1 1 d . . . . .
C32 C 0.5202(2) 0.85996(16) 0.87483(16) 0.0361(5) Uani 1 1 d . . . . .
C33 C 0.6099(2) 0.74638(19) 0.93600(18) 0.0532(6) Uani 1 1 d . . . . .
H33A H 0.6948 0.7281 0.9044 0.080 Uiso 1 1 calc R U . . .
H33B H 0.6232 0.7451 1.0028 0.080 Uiso 1 1 calc R U . . .
H33C H 0.5679 0.6945 0.9392 0.080 Uiso 1 1 calc R U . . .
C34 C 0.5848(2) 0.9421(2) 0.8799(2) 0.0531(6) Uani 1 1 d . . . . .
H34A H 0.5302 1.0143 0.8419 0.080 Uiso 1 1 calc R U . . .
H34B H 0.5917 0.9378 0.9487 0.080 Uiso 1 1 calc R U . . .
H34C H 0.6725 0.9253 0.8522 0.080 Uiso 1 1 calc R U . . .
C35 C 0.3547(2) 0.99850(18) 0.60150(17) 0.0435(5) Uani 1 1 d . . . . .
H35A H 0.3690 0.9339 0.5834 0.052 Uiso 1 1 calc R U . . .
H35B H 0.4068 1.0399 0.5581 0.052 Uiso 1 1 calc R U . . .
C36 C 0.2056(2) 1.06734(18) 0.59455(18) 0.0466(6) Uani 1 1 d . . . . .
C37 C 0.1242(3) 1.0410(3) 0.5310(2) 0.0821(10) Uani 1 1 d . . . . .
H37A H 0.1522 1.0600 0.4626 0.123 Uiso 1 1 calc R U . . .
H37B H 0.1376 0.9647 0.5561 0.123 Uiso 1 1 calc R U . . .
H37C H 0.0311 1.0816 0.5340 0.123 Uiso 1 1 calc R U . . .
C38 C 0.1821(3) 1.1881(2) 0.5634(2) 0.0722(8) Uani 1 1 d . . . . .
H38A H 0.2110 1.2123 0.4958 0.108 Uiso 1 1 calc R U . . .
H38B H 0.0885 1.2269 0.5669 0.108 Uiso 1 1 calc R U . . .
H38C H 0.2321 1.2014 0.6079 0.108 Uiso 1 1 calc R U . . .
C39 C -0.0125(3) 0.5350(3) 0.5995(3) 0.0613(7) Uani 1 1 d . . . . .
H39C H 0.043(4) 0.459(3) 0.624(3) 0.135(15) Uiso 1 1 d . . . . .
H9 H 0.000(3) 0.612(3) 0.682(2) 0.097(11) Uiso 1 1 d . . . . .
H39B H 0.046(4) 0.572(3) 0.550(3) 0.118(12) Uiso 1 1 d . . . . .
H39A H -0.093(4) 0.540(3) 0.564(3) 0.113(12) Uiso 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0635(12) 0.0407(10) 0.1332(18) -0.0432(11) 0.0025(11) -0.0249(9)
O2 0.0447(10) 0.0503(10) 0.0784(12) -0.0374(9) 0.0237(9) -0.0205(8)
O3 0.0290(7) 0.0314(8) 0.0642(10) -0.0264(7) 0.0083(7) -0.0149(6)
O4 0.0382(9) 0.0858(12) 0.0627(11) -0.0444(10) 0.0100(8) -0.0357(9)
O5 0.0238(7) 0.0407(8) 0.0744(11) -0.0318(8) 0.0099(7) -0.0158(6)
O6 0.0271(7) 0.0296(7) 0.0636(10) -0.0256(7) 0.0119(7) -0.0122(6)
O7 0.0640(12) 0.0753(12) 0.0426(11) -0.0181(9) 0.0098(9) -0.0179(10)
O8 0.0317(8) 0.0348(8) 0.0556(10) -0.0156(7) -0.0012(7) -0.0059(7)
O9 0.0367(9) 0.0875(13) 0.0884(14) -0.0613(12) 0.0210(9) -0.0327(9)
C1 0.0512(14) 0.0292(12) 0.0508(14) -0.0155(10) -0.0044(11) -0.0160(10)
C2 0.0463(13) 0.0297(11) 0.0510(14) -0.0187(10) 0.0062(11) -0.0123(10)
C3 0.0368(12) 0.0304(11) 0.0395(13) -0.0125(10) 0.0034(10) -0.0098(9)
C4 0.0305(11) 0.0238(10) 0.0353(12) -0.0096(9) 0.0011(9) -0.0089(8)
C5 0.0344(11) 0.0241(10) 0.0369(12) -0.0122(9) 0.0033(9) -0.0114(9)
C6 0.0380(12) 0.0279(11) 0.0426(13) -0.0132(10) 0.0004(10) -0.0164(9)
C7 0.097(2) 0.083(2) 0.077(2) -0.0575(18) 0.0279(17) -0.0438(18)
C8 0.0544(16) 0.0342(14) 0.108(2) -0.0114(14) -0.0060(16) -0.0079(12)
C9 0.0533(15) 0.0440(13) 0.0585(16) -0.0140(12) -0.0131(12) -0.0186(11)
C10 0.0672(16) 0.0554(15) 0.0684(18) -0.0299(13) 0.0219(14) -0.0432(13)
C11 0.0260(10) 0.0299(10) 0.0399(12) -0.0143(9) 0.0045(9) -0.0114(9)
C12 0.0398(12) 0.0367(12) 0.0475(14) -0.0159(11) -0.0064(10) -0.0102(10)
C13 0.0647(17) 0.0685(17) 0.0426(15) -0.0081(13) -0.0022(13) -0.0223(14)
C14 0.0537(16) 0.0569(16) 0.0647(18) -0.0131(14) -0.0160(13) 0.0012(13)
C15 0.0267(10) 0.0277(10) 0.0364(12) -0.0141(9) 0.0019(8) -0.0108(8)
C16 0.0300(11) 0.0287(10) 0.0393(12) -0.0172(9) 0.0038(9) -0.0158(9)
C17 0.0240(10) 0.0295(10) 0.0398(12) -0.0164(9) 0.0027(8) -0.0120(8)
C18 0.0270(10) 0.0288(11) 0.0466(13) -0.0158(10) 0.0023(9) -0.0134(9)
C19 0.0411(13) 0.0729(16) 0.0554(15) -0.0380(13) 0.0186(11) -0.0362(12)
C20 0.0342(16) 0.150(3) 0.164(4) -0.113(3) 0.0138(18) -0.0137(18)
C21 0.190(4) 0.152(3) 0.064(2) -0.042(2) 0.045(2) -0.144(3)
C22 0.0261(10) 0.0282(10) 0.0380(12) -0.0164(9) 0.0049(9) -0.0100(9)
C23 0.0276(10) 0.0292(10) 0.0384(12) -0.0153(9) 0.0028(9) -0.0138(9)
C24 0.0227(10) 0.0322(11) 0.0399(12) -0.0159(9) 0.0036(8) -0.0128(9)
C25 0.0264(10) 0.0284(10) 0.0416(12) -0.0160(9) 0.0063(9) -0.0142(8)
C26 0.0343(11) 0.0283(10) 0.0401(13) -0.0144(9) 0.0029(9) -0.0148(9)
C27 0.0288(11) 0.0242(10) 0.0489(13) -0.0163(10) 0.0021(10) -0.0091(9)
C28 0.0365(12) 0.0336(11) 0.0470(14) -0.0207(10) 0.0099(10) -0.0119(9)
C29 0.0448(14) 0.0654(16) 0.0645(17) -0.0338(14) 0.0228(12) -0.0211(12)
C30 0.0620(16) 0.0420(14) 0.0694(18) -0.0333(13) 0.0038(13) -0.0103(12)
C31 0.0474(13) 0.0369(12) 0.0418(15) -0.0193(11) 0.0074(10) -0.0193(10)
C32 0.0343(11) 0.0355(11) 0.0435(13) -0.0178(10) 0.0001(9) -0.0129(9)
C33 0.0487(14) 0.0534(15) 0.0497(15) -0.0171(12) -0.0056(12) -0.0059(12)
C34 0.0495(14) 0.0651(16) 0.0665(17) -0.0381(14) 0.0013(12) -0.0292(12)
C35 0.0445(13) 0.0428(13) 0.0430(14) -0.0132(11) 0.0048(10) -0.0160(11)
C36 0.0453(13) 0.0469(14) 0.0443(14) -0.0150(11) -0.0048(11) -0.0097(11)
C37 0.0574(17) 0.115(3) 0.085(2) -0.057(2) -0.0163(16) -0.0138(17)
C38 0.0748(19) 0.0451(15) 0.071(2) -0.0006(14) -0.0003(15) -0.0070(14)
C39 0.0518(17) 0.075(2) 0.075(2) -0.0450(17) 0.0160(15) -0.0271(16)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.207(2) . ?
O2 C3 1.217(2) . ?
O3 C5 1.364(2) . ?
O3 C16 1.389(2) . ?
O4 C18 1.211(2) . ?
O5 C24 1.356(2) . ?
O6 C22 1.363(2) . ?
O6 C27 1.479(2) . ?
O7 C31 1.209(3) . ?
O8 C27 1.384(2) . ?
O8 C36 1.469(3) . ?
O9 C39 1.397(3) . ?
C1 C2 1.517(3) . ?
C1 C6 1.522(3) . ?
C2 C3 1.525(3) . ?
C2 C7 1.534(3) . ?
C2 C8 1.535(3) . ?
C3 C4 1.462(3) . ?
C4 C5 1.331(3) . ?
C4 C11 1.512(3) . ?
C5 C6 1.505(3) . ?
C6 C10 1.530(3) . ?
C6 C9 1.538(3) . ?
C11 C15 1.510(3) . ?
C11 C12 1.555(3) . ?
C12 C13 1.520(3) . ?
C12 C14 1.521(3) . ?
C15 C16 1.377(3) . ?
C15 C24 1.400(3) . ?
C16 C17 1.395(3) . ?
C17 C22 1.398(3) . ?
C17 C18 1.491(3) . ?
C18 C19 1.499(3) . ?
C19 C21 1.517(4) . ?
C19 C20 1.524(4) . ?
C22 C23 1.389(3) . ?
C23 C24 1.390(3) . ?
C23 C25 1.505(3) . ?
C25 C26 1.521(3) . ?
C25 C32 1.558(3) . ?
C26 C27 1.505(3) . ?
C26 C35 1.516(3) . ?
C27 C28 1.524(3) . ?
C28 C29 1.531(3) . ?
C28 C30 1.540(3) . ?
C28 C31 1.541(3) . ?
C31 C32 1.547(3) . ?
C32 C33 1.528(3) . ?
C32 C34 1.548(3) . ?
C35 C36 1.534(3) . ?
C36 C37 1.509(3) . ?
C36 C38 1.517(3) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C5 O3 C16 118.97(14) . . ?
C22 O6 C27 122.00(14) . . ?
C27 O8 C36 110.01(15) . . ?
O1 C1 C2 119.44(19) . . ?
O1 C1 C6 118.8(2) . . ?
C2 C1 C6 121.65(17) . . ?
C1 C2 C3 114.38(17) . . ?
C1 C2 C7 107.8(2) . . ?
C3 C2 C7 109.24(19) . . ?
C1 C2 C8 108.21(19) . . ?
C3 C2 C8 106.70(19) . . ?
C7 C2 C8 110.5(2) . . ?
O2 C3 C4 120.78(18) . . ?
O2 C3 C2 118.91(18) . . ?
C4 C3 C2 120.31(18) . . ?
C5 C4 C3 118.77(18) . . ?
C5 C4 C11 121.07(17) . . ?
C3 C4 C11 119.91(17) . . ?
C4 C5 O3 122.63(17) . . ?
C4 C5 C6 127.66(17) . . ?
O3 C5 C6 109.65(16) . . ?
C5 C6 C1 111.01(17) . . ?
C5 C6 C10 110.55(17) . . ?
C1 C6 C10 109.71(17) . . ?
C5 C6 C9 108.93(16) . . ?
C1 C6 C9 107.05(17) . . ?
C10 C6 C9 109.51(19) . . ?
C15 C11 C4 109.61(15) . . ?
C15 C11 C12 109.90(16) . . ?
C4 C11 C12 112.90(16) . . ?
C13 C12 C14 111.4(2) . . ?
C13 C12 C11 111.75(18) . . ?
C14 C12 C11 112.70(18) . . ?
C16 C15 C24 116.51(16) . . ?
C16 C15 C11 120.26(16) . . ?
C24 C15 C11 122.71(16) . . ?
C15 C16 O3 120.65(16) . . ?
C15 C16 C17 124.66(17) . . ?
O3 C16 C17 114.60(16) . . ?
C16 C17 C22 116.03(16) . . ?
C16 C17 C18 121.45(16) . . ?
C22 C17 C18 122.52(16) . . ?
O4 C18 C17 120.39(18) . . ?
O4 C18 C19 120.04(18) . . ?
C17 C18 C19 119.47(18) . . ?
C18 C19 C21 108.3(2) . . ?
C18 C19 C20 110.8(2) . . ?
C21 C19 C20 112.4(3) . . ?
O6 C22 C23 121.41(16) . . ?
O6 C22 C17 116.39(16) . . ?
C23 C22 C17 122.17(16) . . ?
C22 C23 C24 118.55(16) . . ?
C22 C23 C25 118.27(16) . . ?
C24 C23 C25 123.18(16) . . ?
O5 C24 C23 115.21(16) . . ?
O5 C24 C15 122.85(16) . . ?
C23 C24 C15 121.89(17) . . ?
C23 C25 C26 108.28(15) . . ?
C23 C25 C32 113.17(16) . . ?
C26 C25 C32 109.56(15) . . ?
C27 C26 C35 101.64(16) . . ?
C27 C26 C25 108.97(16) . . ?
C35 C26 C25 121.38(17) . . ?
O8 C27 O6 105.20(15) . . ?
O8 C27 C26 106.58(16) . . ?
O6 C27 C26 111.29(14) . . ?
O8 C27 C28 112.91(16) . . ?
O6 C27 C28 106.78(16) . . ?
C26 C27 C28 113.80(16) . . ?
C27 C28 C29 111.99(18) . . ?
C27 C28 C30 110.50(18) . . ?
C29 C28 C30 107.76(18) . . ?
C27 C28 C31 108.71(16) . . ?
C29 C28 C31 110.07(19) . . ?
C30 C28 C31 107.73(18) . . ?
O7 C31 C28 118.69(19) . . ?
O7 C31 C32 118.5(2) . . ?
C28 C31 C32 122.59(19) . . ?
C33 C32 C31 108.76(18) . . ?
C33 C32 C34 107.81(19) . . ?
C31 C32 C34 106.25(16) . . ?
C33 C32 C25 110.95(16) . . ?
C31 C32 C25 113.66(17) . . ?
C34 C32 C25 109.15(17) . . ?
C26 C35 C36 103.12(17) . . ?
O8 C36 C37 107.4(2) . . ?
O8 C36 C38 106.08(19) . . ?
C37 C36 C38 112.3(2) . . ?
O8 C36 C35 104.79(17) . . ?
C37 C36 C35 112.9(2) . . ?
C38 C36 C35 112.6(2) . . ?
_refine_diff_density_max 0.169
_refine_diff_density_min -0.195
_refine_diff_density_rms 0.042
_shelxl_version_number 2014/6
_shelx_res_file
;
TITL P in P-1
CELL 0.71073 10.67060 13.88280 14.10780 70.5671 84.6047 69.4237
ZERR 2.00 0.00100 0.00120 0.00130 0.0028 0.0031 0.0027
LATT 1
SFAC C H O
UNIT 78 108 18
REM C39 H54 O9
REM D8VENTURE BLOCK COLOURLESS
OMIT -3 50.5
SIZE 0.40 0.30 0.20
ACTA
L.S. 4
BOND
FMAP 2
PLAN 20
TEMP 23
WGHT 0.056900 0.642000
FVAR 0.26571
O1 3 0.504900 0.180553 0.672038 11.00000 0.06349 0.04068 =
0.13323 -0.04316 0.00254 -0.02487
O2 3 0.828979 0.348767 0.621676 11.00000 0.04467 0.05035 =
0.07844 -0.03745 0.02367 -0.02045
O3 3 0.407860 0.505521 0.736044 11.00000 0.02896 0.03144 =
0.06423 -0.02645 0.00833 -0.01494
O4 3 0.149338 0.656267 0.686619 11.00000 0.03820 0.08582 =
0.06272 -0.04440 0.01003 -0.03569
O5 3 0.713498 0.693991 0.727496 11.00000 0.02379 0.04072 =
0.07439 -0.03176 0.00992 -0.01579
AFIX 83
H5A 2 0.767324 0.643833 0.710836 11.00000 -1.50000
AFIX 0
O6 3 0.250687 0.853508 0.768190 11.00000 0.02705 0.02960 =
0.06356 -0.02563 0.01186 -0.01221
O7 3 0.382262 0.854276 1.017493 11.00000 0.06400 0.07533 =
0.04261 -0.01812 0.00977 -0.01792
O8 3 0.159176 1.036937 0.698118 11.00000 0.03170 0.03484 =
0.05559 -0.01560 -0.00120 -0.00588
O9 3 -0.051937 0.575857 0.679753 11.00000 0.03671 0.08750 =
0.08838 -0.06133 0.02098 -0.03270
C1 1 0.540437 0.255690 0.666629 11.00000 0.05116 0.02921 =
0.05077 -0.01552 -0.00444 -0.01597
C2 1 0.684966 0.247043 0.643330 11.00000 0.04634 0.02970 =
0.05100 -0.01866 0.00619 -0.01234
C3 1 0.722284 0.339660 0.653452 11.00000 0.03678 0.03038 =
0.03952 -0.01252 0.00341 -0.00984
C4 1 0.631661 0.415271 0.701712 11.00000 0.03048 0.02380 =
0.03534 -0.00958 0.00106 -0.00888
C5 1 0.502624 0.425644 0.706716 11.00000 0.03442 0.02415 =
0.03695 -0.01224 0.00327 -0.01145
C6 1 0.436786 0.359167 0.678128 11.00000 0.03799 0.02793 =
0.04257 -0.01318 0.00044 -0.01645
C7 1 0.709697 0.243453 0.535477 11.00000 0.09681 0.08258 =
0.07722 -0.05746 0.02789 -0.04382
AFIX 33
H7A 2 0.800736 0.237966 0.518839 11.00000 -1.50000
H7B 2 0.693582 0.181542 0.530306 11.00000 -1.50000
H7C 2 0.650251 0.308603 0.489788 11.00000 -1.50000
AFIX 0
C8 1 0.775548 0.141926 0.718250 11.00000 0.05438 0.03421 =
0.10838 -0.01140 -0.00597 -0.00793
AFIX 33
H8A 2 0.867633 0.134965 0.704708 11.00000 -1.50000
H8B 2 0.756507 0.144250 0.785487 11.00000 -1.50000
H8C 2 0.759164 0.080808 0.711421 11.00000 -1.50000
AFIX 0
C9 1 0.364437 0.425231 0.575450 11.00000 0.05327 0.04398 =
0.05845 -0.01400 -0.01310 -0.01856
AFIX 33
H9A 2 0.322126 0.383371 0.556637 11.00000 -1.50000
H9B 2 0.297867 0.491337 0.579797 11.00000 -1.50000
H9C 2 0.428146 0.442235 0.525809 11.00000 -1.50000
AFIX 0
C10 1 0.335737 0.330267 0.756908 11.00000 0.06722 0.05535 =
0.06836 -0.02991 0.02192 -0.04321
AFIX 33
H10A 2 0.294727 0.287933 0.737546 11.00000 -1.50000
H10B 2 0.380970 0.288988 0.820990 11.00000 -1.50000
H10C 2 0.268111 0.395748 0.761617 11.00000 -1.50000
AFIX 0
C11 1 0.682532 0.487453 0.736009 11.00000 0.02598 0.02995 =
0.03994 -0.01428 0.00447 -0.01141
AFIX 13
H11A 2 0.750953 0.505832 0.689338 11.00000 -1.20000
AFIX 0
C12 1 0.746888 0.431609 0.843669 11.00000 0.03977 0.03668 =
0.04753 -0.01591 -0.00636 -0.01017
AFIX 13
H12A 2 0.774602 0.484811 0.859630 11.00000 -1.20000
AFIX 0
C13 1 0.646330 0.403048 0.921865 11.00000 0.06468 0.06848 =
0.04262 -0.00812 -0.00217 -0.02233
AFIX 33
H13A 2 0.568516 0.466512 0.915689 11.00000 -1.50000
H13B 2 0.620843 0.347490 0.911386 11.00000 -1.50000
H13C 2 0.686130 0.377105 0.987900 11.00000 -1.50000
AFIX 0
C14 1 0.872247 0.333308 0.850547 11.00000 0.05374 0.05695 =
0.06469 -0.01307 -0.01598 0.00121
AFIX 33
H14A 2 0.933696 0.353809 0.800388 11.00000 -1.50000
H14B 2 0.913720 0.306849 0.916054 11.00000 -1.50000
H14C 2 0.848433 0.277234 0.839540 11.00000 -1.50000
AFIX 0
C15 1 0.569306 0.591674 0.731460 11.00000 0.02673 0.02770 =
0.03638 -0.01408 0.00195 -0.01077
C16 1 0.438513 0.594638 0.736691 11.00000 0.02999 0.02872 =
0.03930 -0.01719 0.00385 -0.01577
C17 1 0.328761 0.681052 0.748328 11.00000 0.02405 0.02948 =
0.03982 -0.01637 0.00269 -0.01197
C18 1 0.189550 0.679271 0.750753 11.00000 0.02699 0.02876 =
0.04663 -0.01576 0.00226 -0.01335
C19 1 0.102233 0.699645 0.836668 11.00000 0.04114 0.07288 =
0.05543 -0.03801 0.01860 -0.03624
AFIX 13
H19A 2 0.148197 0.722657 0.877512 11.00000 -1.20000
AFIX 0
C20 1 -0.031005 0.789801 0.798361 11.00000 0.03417 0.15037 =
0.16415 -0.11340 0.01385 -0.01372
AFIX 33
H20A 2 -0.085309 0.801548 0.854444 11.00000 -1.50000
H20B 2 -0.015046 0.855543 0.759453 11.00000 -1.50000
H20C 2 -0.076573 0.769093 0.757059 11.00000 -1.50000
AFIX 0
C21 1 0.084464 0.593613 0.900961 11.00000 0.19039 0.15235 =
0.06360 -0.04168 0.04466 -0.14373
AFIX 33
H21A 2 0.028703 0.605105 0.956473 11.00000 -1.50000
H21B 2 0.043104 0.568257 0.861146 11.00000 -1.50000
H21C 2 0.170340 0.540372 0.925953 11.00000 -1.50000
AFIX 0
C22 1 0.357407 0.768705 0.756886 11.00000 0.02612 0.02822 =
0.03805 -0.01644 0.00491 -0.01002
C23 1 0.486869 0.771338 0.751159 11.00000 0.02758 0.02921 =
0.03839 -0.01533 0.00276 -0.01382
C24 1 0.590575 0.684313 0.735072 11.00000 0.02270 0.03221 =
0.03989 -0.01592 0.00357 -0.01279
C25 1 0.507979 0.868447 0.762947 11.00000 0.02642 0.02838 =
0.04163 -0.01596 0.00633 -0.01420
AFIX 13
H25A 2 0.590385 0.875475 0.729167 11.00000 -1.20000
AFIX 0
C26 1 0.390925 0.969208 0.711306 11.00000 0.03427 0.02831 =
0.04011 -0.01438 0.00292 -0.01476
AFIX 13
H26A 2 0.403710 1.031977 0.720787 11.00000 -1.20000
AFIX 0
C27 1 0.263500 0.958221 0.761490 11.00000 0.02880 0.02416 =
0.04888 -0.01633 0.00208 -0.00913
C28 1 0.252083 0.964325 0.868016 11.00000 0.03648 0.03361 =
0.04702 -0.02066 0.00988 -0.01191
C29 1 0.133919 0.933379 0.922542 11.00000 0.04478 0.06539 =
0.06449 -0.03378 0.02280 -0.02113
AFIX 33
H29A 2 0.130119 0.938207 0.989135 11.00000 -1.50000
H29B 2 0.052148 0.982171 0.886106 11.00000 -1.50000
H29C 2 0.145405 0.860356 0.926569 11.00000 -1.50000
AFIX 0
C30 1 0.231928 1.080411 0.866126 11.00000 0.06202 0.04200 =
0.06939 -0.03334 0.00376 -0.01030
AFIX 33
H30A 2 0.224930 1.082897 0.933675 11.00000 -1.50000
H30B 2 0.306924 1.100623 0.835020 11.00000 -1.50000
H30C 2 0.151367 1.130055 0.828506 11.00000 -1.50000
AFIX 0
C31 1 0.383919 0.887952 0.926743 11.00000 0.04737 0.03690 =
0.04181 -0.01925 0.00744 -0.01926
C32 1 0.520197 0.859958 0.874831 11.00000 0.03433 0.03554 =
0.04349 -0.01776 0.00013 -0.01286
C33 1 0.609870 0.746378 0.935995 11.00000 0.04875 0.05339 =
0.04971 -0.01712 -0.00555 -0.00595
AFIX 33
H33A 2 0.694803 0.728147 0.904428 11.00000 -1.50000
H33B 2 0.623190 0.745123 1.002812 11.00000 -1.50000
H33C 2 0.567945 0.694522 0.939165 11.00000 -1.50000
AFIX 0
C34 1 0.584776 0.942134 0.879891 11.00000 0.04950 0.06507 =
0.06651 -0.03812 0.00132 -0.02919
AFIX 33
H34A 2 0.530219 1.014335 0.841942 11.00000 -1.50000
H34B 2 0.591654 0.937760 0.948668 11.00000 -1.50000
H34C 2 0.672493 0.925257 0.852200 11.00000 -1.50000
AFIX 0
C35 1 0.354723 0.998498 0.601502 11.00000 0.04445 0.04282 =
0.04296 -0.01325 0.00476 -0.01602
AFIX 23
H35A 2 0.368999 0.933931 0.583402 11.00000 -1.20000
H35B 2 0.406816 1.039940 0.558138 11.00000 -1.20000
AFIX 0
C36 1 0.205594 1.067337 0.594546 11.00000 0.04526 0.04687 =
0.04427 -0.01496 -0.00484 -0.00975
C37 1 0.124222 1.041035 0.531018 11.00000 0.05737 0.11497 =
0.08462 -0.05728 -0.01632 -0.01384
AFIX 33
H37A 2 0.152201 1.060016 0.462621 11.00000 -1.50000
H37B 2 0.137642 0.964720 0.556059 11.00000 -1.50000
H37C 2 0.031061 1.081637 0.533961 11.00000 -1.50000
AFIX 0
C38 1 0.182121 1.188058 0.563414 11.00000 0.07480 0.04506 =
0.07131 -0.00055 -0.00029 -0.00698
AFIX 33
H38A 2 0.210962 1.212253 0.495804 11.00000 -1.50000
H38B 2 0.088460 1.226916 0.566869 11.00000 -1.50000
H38C 2 0.232083 1.201417 0.607863 11.00000 -1.50000
AFIX 0
C39 1 -0.012510 0.534985 0.599492 11.00000 0.05179 0.07540 =
0.07481 -0.04495 0.01600 -0.02708
H39C 2 0.042919 0.459350 0.623762 11.00000 0.13482
H9 2 -0.000043 0.611532 0.682431 11.00000 0.09682
H39B 2 0.046180 0.571666 0.549548 11.00000 0.11801
H39A 2 -0.093396 0.540157 0.564387 11.00000 0.11288
HKLF 4
REM P in P-1
REM R1 = 0.0509 for 4469 Fo > 4sig(Fo) and 0.0904 for all 6672 data
REM 449 parameters refined using 0 restraints
END
WGHT 0.0569 0.6408
REM Highest difference peak 0.169, deepest hole -0.195, 1-sigma level 0.042
Q1 1 0.5725 0.4408 0.6694 11.00000 0.05 0.17
Q2 1 -0.0169 0.4529 0.6217 11.00000 0.05 0.16
Q3 1 0.1960 0.8293 0.9560 11.00000 0.05 0.16
Q4 1 0.5813 0.3909 0.7390 11.00000 0.05 0.16
Q5 1 0.5182 0.7548 0.7145 11.00000 0.05 0.15
Q6 1 0.2000 0.5412 0.9097 11.00000 0.05 0.15
Q7 1 0.6200 0.5363 0.7398 11.00000 0.05 0.14
Q8 1 0.5616 0.1187 0.5303 11.00000 0.05 0.14
Q9 1 0.4241 0.7799 0.7319 11.00000 0.05 0.14
Q10 1 0.5188 0.5785 0.7632 11.00000 0.05 0.14
Q11 1 0.6504 0.4525 0.7079 11.00000 0.05 0.14
Q12 1 -0.0486 0.6379 0.8395 11.00000 0.05 0.14
Q13 1 0.0010 0.7077 0.8514 11.00000 0.05 0.13
Q14 1 1.0184 0.2803 0.6924 11.00000 0.05 0.13
Q15 1 0.6059 0.6016 0.7830 11.00000 0.05 0.13
Q16 1 0.2568 0.6928 0.7352 11.00000 0.05 0.13
Q17 1 0.2633 1.2483 0.6631 11.00000 0.05 0.13
Q18 1 0.7157 0.4535 0.7849 11.00000 0.05 0.13
Q19 1 0.6620 0.8407 0.7517 11.00000 0.05 0.13
Q20 1 0.3684 0.6619 0.7119 11.00000 0.05 0.13
;
_shelx_res_checksum 98799
#######################################################################
#
# 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_3+2_1f_tw_sq
_database_code_depnum_ccdc_archive 'CCDC 1582658'
_audit_update_record
;
2017-10-28 deposited with the CCDC.
2017-11-27 downloaded from the CCDC.
;
_audit_creation_date 2016-11-15
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C34 H44 O6'
_chemical_formula_sum 'C34 H44 O6'
_chemical_formula_weight 548.69
_chemical_absolute_configuration ad
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
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 4
_space_group_name_H-M_alt 'P 1 21 1'
_space_group_name_Hall 'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
_cell_length_a 11.5410(2)
_cell_length_b 16.4653(3)
_cell_length_c 32.9338(5)
_cell_angle_alpha 90
_cell_angle_beta 95.7200(10)
_cell_angle_gamma 90
_cell_volume 6227.12(18)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 22536
_cell_measurement_temperature 100.01(10)
_cell_measurement_theta_max 73.4930
_cell_measurement_theta_min 3.8360
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.631
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details ?
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.171
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 2368
_exptl_crystal_size_max ?
_exptl_crystal_size_mid ?
_exptl_crystal_size_min ?
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents ?
_diffrn_reflns_av_unetI/netI 0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 39
_diffrn_reflns_limit_l_min -3
_diffrn_reflns_number 20250
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 68.236
_diffrn_reflns_theta_min 3.806
_diffrn_ambient_temperature 100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type 'CCD Area Detector'
_diffrn_measurement_method ?
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source ?
_reflns_Friedel_coverage 0.762
_reflns_Friedel_fraction_full 0.817
_reflns_Friedel_fraction_max 0.813
_reflns_number_gt 19521
_reflns_number_total 20250
_reflns_special_details
;
Structure factors included contributions from the .fab file.
_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 ?
_computing_data_collection ?
_computing_data_reduction ?
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution ?
_refine_diff_density_max 0.921
_refine_diff_density_min -0.618
_refine_diff_density_rms 0.076
_refine_ls_abs_structure_details
;
Flack x determined using 7501 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.05(8)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.061
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 1511
_refine_ls_number_reflns 20250
_refine_ls_number_restraints 81
_refine_ls_R_factor_all 0.0732
_refine_ls_R_factor_gt 0.0714
_refine_ls_restrained_S_all 1.064
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0827P)^2^+11.2360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1899
_refine_ls_wR_factor_ref 0.1914
_refine_special_details
;
Refined as a 2-component twin.
;
_olex2_refinement_description
;
1. Twinned data refinement
Scales: 0.887(4) 0.113(4)
2. 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 O(H) groups
3. Restrained distances
C51-C45
1.5 with sigma of 0.001
C45-C50A
1.5 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C50A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C30) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C50) \\sim Ueq, Uanis(C51A) \\sim Ueq, Uanis(C51) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
C45, C50, C51, C51A, C50A
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
C25, C28, C29, C30
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
Sof(C51A)=Sof(H51D)=Sof(H51E)=Sof(H51F)=Sof(C50A)=Sof(H50D)=Sof(H50E)=
Sof(H50F)=1-FVAR(1)
Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=
FVAR(1)
7.a Ternary CH refined with riding coordinates:
C4(H4), C18(H18), C22(H22), C25(H25), C28(H28), C32(H32), C38(H38), C52(H52),
C56(H56), C59(H59), C62(H62), C66(H66), C72(H72), C86(H86), C90(H90), C93(H93),
C96(H96), C100(H100), C106(H106), C120(H120), C124(H124), C127(H127),
C130(H130), C134(H134)
7.b Secondary CH2 refined with riding coordinates:
C24(H24A,H24B), C58(H58A,H58B), C92(H92A,H92B), C126(H12A,H12B)
7.c Aromatic/amide H refined with riding coordinates:
C26(H26), C27(H27), C60(H60), C61(H61), C94(H94), C95(H95), C128(H128),
C129(H129)
7.d Idealised Me refined as rotating group:
C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C29(H29A,H29B,H29C), C30(H30A,H30B,
H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C39(H39A,
H39B,H39C), C40(H40A,H40B,H40C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C),
C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C63(H63A,H63B,H63C), C64(H64A,H64B,
H64C), C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C73(H73A,
H73B,H73C), C74(H74A,H74B,H74C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C),
C84(H84A,H84B,H84C), C85(H85A,H85B,H85C), C97(H97A,H97B,H97C), C98(H98A,H98B,
H98C), C99(H99A,H99B,H99C), C101(H10A,H10B,H10C), C102(H10D,H10E,H10F),
C107(H10G,H10H,H10I), C108(H10J,H10K,H10L), C116(H11A,H11B,H11C), C117(H11D,
H11E,H11F), C118(H11G,H11H,H11I), C119(H11J,H11K,H11L), C131(H13A,H13B,H13C),
C132(H13D,H13E,H13F), C133(H13G,H13H,H13I), C135(H13J,H13K,H13L), C136(H13M,
H13N,H13O), C51A(H51D,H51E,H51F), C50A(H50D,H50E,H50F)
7.e Idealised tetrahedral OH refined as rotating group:
O1(H1), O7(H7), O13(H13), O19(H19)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.7139(4) 0.1202(3) 0.31585(12) 0.0248(9) Uani 1 1 d . . . . .
H1 H 0.7309 0.0706 0.3162 0.037 Uiso 1 1 calc GR . . . .
O2 O 0.7078(4) -0.0230(3) 0.33720(13) 0.0303(10) Uani 1 1 d . . . . .
O3 O 0.5924(3) 0.0514(2) 0.44774(11) 0.0178(8) Uani 1 1 d . . . . .
O4 O 0.5788(4) 0.2602(3) 0.54370(13) 0.0295(10) Uani 1 1 d . . . . .
O5 O 0.6395(5) -0.0066(3) 0.58895(14) 0.0399(12) Uani 1 1 d . . . . .
O6 O 0.5848(3) 0.3241(2) 0.39716(12) 0.0203(8) Uani 1 1 d . . . . .
C1 C 0.6688(5) 0.1401(3) 0.35077(16) 0.0188(11) Uani 1 1 d . . . . .
C2 C 0.6470(4) 0.0792(3) 0.38011(17) 0.0175(11) Uani 1 1 d . . . . .
C3 C 0.6638(5) -0.0063(4) 0.36970(17) 0.0201(11) Uani 1 1 d . . . . .
C4 C 0.6225(5) -0.0766(3) 0.39398(18) 0.0227(12) Uani 1 1 d . . . . .
H4 H 0.6449 -0.0657 0.4236 0.027 Uiso 1 1 calc R . . . .
C5 C 0.6819(6) -0.1569(4) 0.3824(2) 0.0298(14) Uani 1 1 d . . . . .
H5A H 0.6530 -0.1723 0.3545 0.045 Uiso 1 1 calc GR . . . .
H5B H 0.6637 -0.2000 0.4013 0.045 Uiso 1 1 calc GR . . . .
H5C H 0.7664 -0.1490 0.3842 0.045 Uiso 1 1 calc GR . . . .
C6 C 0.4907(6) -0.0823(4) 0.3871(2) 0.0321(14) Uani 1 1 d . . . . .
H6A H 0.4565 -0.0296 0.3928 0.048 Uiso 1 1 calc GR . . . .
H6B H 0.4631 -0.1235 0.4054 0.048 Uiso 1 1 calc GR . . . .
H6C H 0.4674 -0.0976 0.3587 0.048 Uiso 1 1 calc GR . . . .
C7 C 0.6059(4) 0.1083(3) 0.41706(16) 0.0146(10) Uani 1 1 d . . . . .
C8 C 0.5873(4) 0.0786(3) 0.48700(16) 0.0155(10) Uani 1 1 d . . . . .
C9 C 0.5602(4) 0.1567(3) 0.49499(16) 0.0159(11) Uani 1 1 d . . . . .
C10 C 0.5736(5) 0.1879(3) 0.53708(16) 0.0184(11) Uani 1 1 d . . . . .
C11 C 0.5781(5) 0.1276(3) 0.57208(18) 0.0234(12) Uani 1 1 d . . . . .
C12 C 0.6131(5) 0.0422(3) 0.56208(17) 0.0196(11) Uani 1 1 d . . . . .
C13 C 0.6094(5) 0.0117(3) 0.51733(17) 0.0181(11) Uani 1 1 d . . . . .
C14 C 0.7282(5) -0.0313(3) 0.51353(17) 0.0192(11) Uani 1 1 d . . . . .
H14A H 0.7300 -0.0520 0.4857 0.029 Uiso 1 1 calc GR . . . .
H14B H 0.7375 -0.0767 0.5329 0.029 Uiso 1 1 calc GR . . . .
H14C H 0.7919 0.0076 0.5196 0.029 Uiso 1 1 calc GR . . . .
C15 C 0.5110(5) -0.0505(3) 0.51086(19) 0.0233(12) Uani 1 1 d . . . . .
H15A H 0.4358 -0.0225 0.5093 0.035 Uiso 1 1 calc GR . . . .
H15B H 0.5165 -0.0888 0.5338 0.035 Uiso 1 1 calc GR . . . .
H15C H 0.5176 -0.0802 0.4854 0.035 Uiso 1 1 calc GR . . . .
C16 C 0.4519(6) 0.1203(4) 0.5837(2) 0.0387(17) Uani 1 1 d . . . . .
H16A H 0.4232 0.1743 0.5904 0.058 Uiso 1 1 calc GR . . . .
H16B H 0.4506 0.0846 0.6075 0.058 Uiso 1 1 calc GR . . . .
H16C H 0.4020 0.0976 0.5607 0.058 Uiso 1 1 calc GR . . . .
C17 C 0.6572(8) 0.1585(4) 0.6092(2) 0.0454(19) Uani 1 1 d . . . . .
H17A H 0.7381 0.1599 0.6026 0.068 Uiso 1 1 calc GR . . . .
H17B H 0.6511 0.1220 0.6324 0.068 Uiso 1 1 calc GR . . . .
H17C H 0.6328 0.2133 0.6163 0.068 Uiso 1 1 calc GR . . . .
C18 C 0.5226(4) 0.2134(3) 0.46087(16) 0.0164(11) Uani 1 1 d . . . . .
H18 H 0.5516 0.2688 0.4690 0.020 Uiso 1 1 calc R . . . .
C19 C 0.5792(4) 0.1887(3) 0.42398(17) 0.0163(11) Uani 1 1 d . . . . .
C20 C 0.6022(4) 0.2439(3) 0.39330(16) 0.0153(10) Uani 1 1 d . . . . .
C21 C 0.6099(5) 0.3637(3) 0.35748(16) 0.0208(12) Uani 1 1 d . . . . .
C22 C 0.6659(5) 0.2964(3) 0.33307(17) 0.0201(11) Uani 1 1 d . . . . .
H22 H 0.7517 0.3065 0.3348 0.024 Uiso 1 1 calc R . . . .
C23 C 0.6457(4) 0.2214(3) 0.35738(16) 0.0164(10) Uani 1 1 d . . . . .
C24 C 0.6184(6) 0.2951(4) 0.28798(18) 0.0303(14) Uani 1 1 d . . . . .
H24A H 0.6499 0.2471 0.2747 0.036 Uiso 1 1 calc R . . . .
H24B H 0.6454 0.3442 0.2744 0.036 Uiso 1 1 calc R . . . .
C25 C 0.4840(7) 0.2920(4) 0.2822(2) 0.0438(19) Uani 1 1 d . U . . .
H25 H 0.4608 0.2408 0.2956 0.053 Uiso 1 1 calc R . . . .
C26 C 0.4381(6) 0.3604(5) 0.3057(2) 0.0353(16) Uani 1 1 d . . . . .
H26 H 0.3638 0.3820 0.2963 0.042 Uiso 1 1 calc R . . . .
C27 C 0.4942(5) 0.3925(4) 0.33852(19) 0.0300(14) Uani 1 1 d . . . . .
H27 H 0.4589 0.4369 0.3510 0.036 Uiso 1 1 calc R . . . .
C28 C 0.4261(8) 0.2896(6) 0.2383(3) 0.057(2) Uani 1 1 d . U . . .
H28 H 0.3399 0.2915 0.2396 0.068 Uiso 1 1 calc R . . . .
C29 C 0.4597(8) 0.3643(6) 0.2145(3) 0.056(2) Uani 1 1 d . U . . .
H29A H 0.4327 0.4135 0.2275 0.084 Uiso 1 1 calc GR . . . .
H29B H 0.4234 0.3610 0.1863 0.084 Uiso 1 1 calc GR . . . .
H29C H 0.5446 0.3664 0.2145 0.084 Uiso 1 1 calc GR . . . .
C30 C 0.4546(11) 0.2089(7) 0.2188(4) 0.081(3) Uani 1 1 d . U . . .
H30A H 0.5355 0.2096 0.2122 0.121 Uiso 1 1 calc GR . . . .
H30B H 0.4024 0.2006 0.1938 0.121 Uiso 1 1 calc GR . . . .
H30C H 0.4442 0.1645 0.2380 0.121 Uiso 1 1 calc GR . . . .
C31 C 0.6914(5) 0.4335(4) 0.36969(19) 0.0247(12) Uani 1 1 d . . . . .
H31A H 0.6502 0.4744 0.3844 0.037 Uiso 1 1 calc GR . . . .
H31B H 0.7182 0.4581 0.3452 0.037 Uiso 1 1 calc GR . . . .
H31C H 0.7586 0.4133 0.3873 0.037 Uiso 1 1 calc GR . . . .
C32 C 0.3883(5) 0.2186(4) 0.45110(18) 0.0227(12) Uani 1 1 d . . . . .
H32 H 0.3721 0.2614 0.4297 0.027 Uiso 1 1 calc R . . . .
C33 C 0.3344(5) 0.1394(4) 0.4338(2) 0.0268(13) Uani 1 1 d . . . . .
H33A H 0.3666 0.1263 0.4082 0.040 Uiso 1 1 calc GR . . . .
H33B H 0.2498 0.1458 0.4287 0.040 Uiso 1 1 calc GR . . . .
H33C H 0.3523 0.0954 0.4535 0.040 Uiso 1 1 calc GR . . . .
C34 C 0.3258(6) 0.2444(4) 0.4885(2) 0.0305(14) Uani 1 1 d . . . . .
H34A H 0.3283 0.1995 0.5082 0.046 Uiso 1 1 calc GR . . . .
H34B H 0.2446 0.2580 0.4797 0.046 Uiso 1 1 calc GR . . . .
H34C H 0.3650 0.2919 0.5015 0.046 Uiso 1 1 calc GR . . . .
O7 O 0.3290(4) 0.8817(3) 0.18722(13) 0.0275(9) Uani 1 1 d . . . . .
H7 H 0.3411 0.9320 0.1874 0.041 Uiso 1 1 calc GR . . . .
O8 O 0.3108(4) 1.0249(3) 0.16356(14) 0.0363(11) Uani 1 1 d . . . . .
O9 O 0.1275(3) 0.9451(2) 0.05548(12) 0.0183(8) Uani 1 1 d . . . . .
O10 O 0.0387(4) 0.7354(3) -0.03829(13) 0.0331(10) Uani 1 1 d . . . . .
O11 O 0.0696(6) 0.9991(3) -0.08593(15) 0.0516(15) Uani 1 1 d . . . . .
O12 O 0.1466(3) 0.6755(2) 0.10990(12) 0.0211(8) Uani 1 1 d . . . . .
C35 C 0.2626(5) 0.8612(4) 0.15271(17) 0.0211(12) Uani 1 1 d . . . . .
C36 C 0.2227(5) 0.9193(4) 0.12251(17) 0.0203(11) Uani 1 1 d . . . . .
C37 C 0.2469(5) 1.0057(4) 0.13215(18) 0.0234(12) Uani 1 1 d . . . . .
C38 C 0.1909(5) 1.0758(4) 0.1068(2) 0.0283(13) Uani 1 1 d . . . . .
H38 H 0.1971 1.0646 0.0773 0.034 Uiso 1 1 calc R . . . .
C39 C 0.0609(6) 1.0803(4) 0.1141(2) 0.0323(14) Uani 1 1 d . . . . .
H39A H 0.0225 1.0290 0.1057 0.048 Uiso 1 1 calc GR . . . .
H39B H 0.0237 1.1250 0.0981 0.048 Uiso 1 1 calc GR . . . .
H39C H 0.0541 1.0897 0.1431 0.048 Uiso 1 1 calc GR . . . .
C40 C 0.2501(7) 1.1566(4) 0.1181(2) 0.0379(16) Uani 1 1 d . . . . .
H40A H 0.2293 1.1742 0.1449 0.057 Uiso 1 1 calc GR . . . .
H40B H 0.2243 1.1976 0.0976 0.057 Uiso 1 1 calc GR . . . .
H40C H 0.3348 1.1501 0.1192 0.057 Uiso 1 1 calc GR . . . .
C41 C 0.1586(4) 0.8902(3) 0.08660(17) 0.0141(10) Uani 1 1 d . . . . .
C42 C 0.0947(4) 0.9160(3) 0.01674(17) 0.0164(11) Uani 1 1 d . . . . .
C43 C 0.0582(4) 0.8398(3) 0.01033(18) 0.0190(11) Uani 1 1 d . . . . .
C44 C 0.0408(5) 0.8077(4) -0.03181(19) 0.0265(13) Uani 1 1 d . . . . .
C45 C 0.0203(6) 0.8668(4) -0.0675(2) 0.0422(17) Uani 1 1 d D U . . .
C46 C 0.0644(5) 0.9533(4) -0.05805(19) 0.0261(13) Uani 1 1 d . . . . .
C47 C 0.1000(5) 0.9831(3) -0.01443(18) 0.0199(11) Uani 1 1 d . . . . .
C48 C 0.2235(5) 1.0203(4) -0.0139(2) 0.0247(12) Uani 1 1 d . . . . .
H48A H 0.2470 1.0432 0.0131 0.037 Uiso 1 1 calc GR . . . .
H48B H 0.2228 1.0634 -0.0345 0.037 Uiso 1 1 calc GR . . . .
H48C H 0.2788 0.9780 -0.0200 0.037 Uiso 1 1 calc GR . . . .
C49 C 0.0118(5) 1.0492(4) -0.0057(2) 0.0287(14) Uani 1 1 d . . . . .
H49A H -0.0634 1.0239 -0.0020 0.043 Uiso 1 1 calc GR . . . .
H49B H 0.0022 1.0873 -0.0286 0.043 Uiso 1 1 calc GR . . . .
H49C H 0.0402 1.0786 0.0192 0.043 Uiso 1 1 calc GR . . . .
C50 C 0.0324(17) 0.8341(11) -0.1053(5) 0.052(4) Uani 0.54(2) 1 d . U P A 1
H50A H 0.1152 0.8259 -0.1083 0.079 Uiso 0.54(2) 1 calc GR . P A 1
H50B H -0.0011 0.8713 -0.1265 0.079 Uiso 0.54(2) 1 calc GR . P A 1
H50C H -0.0083 0.7818 -0.1079 0.079 Uiso 0.54(2) 1 calc GR . P A 1
C51 C -0.1085(7) 0.8812(11) -0.0689(6) 0.056(4) Uani 0.54(2) 1 d D U P A 1
H51A H -0.1494 0.8290 -0.0702 0.084 Uiso 0.54(2) 1 calc GR . P A 1
H51B H -0.1346 0.9134 -0.0932 0.084 Uiso 0.54(2) 1 calc GR . P A 1
H51C H -0.1256 0.9107 -0.0444 0.084 Uiso 0.54(2) 1 calc GR . P A 1
C52 C 0.0448(5) 0.7830(3) 0.04527(17) 0.0179(11) Uani 1 1 d . . . . .
H52 H 0.0679 0.7272 0.0371 0.021 Uiso 1 1 calc R . . . .
C53 C 0.1256(4) 0.8093(3) 0.08097(17) 0.0179(11) Uani 1 1 d . . . . .
C54 C 0.1673(5) 0.7559(3) 0.11193(17) 0.0175(11) Uani 1 1 d . . . . .
C55 C 0.1828(5) 0.6405(4) 0.15099(17) 0.0219(12) Uani 1 1 d . . . . .
C56 C 0.2686(5) 0.7046(4) 0.17195(18) 0.0217(12) Uani 1 1 d . . . . .
H56 H 0.3495 0.6891 0.1667 0.026 Uiso 1 1 calc R . . . .
C57 C 0.2344(4) 0.7800(4) 0.14695(17) 0.0193(11) Uani 1 1 d . . . . .
C58 C 0.2636(5) 0.7089(4) 0.21786(18) 0.0245(12) Uani 1 1 d . . . . .
H58A H 0.3187 0.7509 0.2294 0.029 Uiso 1 1 calc R . . . .
H58B H 0.2886 0.6561 0.2301 0.029 Uiso 1 1 calc R . . . .
C59 C 0.1407(6) 0.7290(4) 0.22942(18) 0.0302(14) Uani 1 1 d . . . . .
H59 H 0.1231 0.7865 0.2210 0.036 Uiso 1 1 calc R . . . .
C60 C 0.0537(5) 0.6754(5) 0.2052(2) 0.0337(15) Uani 1 1 d . . . . .
H60 H -0.0207 0.6696 0.2149 0.040 Uiso 1 1 calc R . . . .
C61 C 0.0725(5) 0.6361(4) 0.17185(19) 0.0293(14) Uani 1 1 d . . . . .
H61 H 0.0117 0.6022 0.1599 0.035 Uiso 1 1 calc R . . . .
C62 C 0.1297(6) 0.7228(4) 0.27566(19) 0.0317(14) Uani 1 1 d . . . . .
H62 H 0.0507 0.7438 0.2802 0.038 Uiso 1 1 calc R . . . .
C63 C 0.2174(7) 0.7769(4) 0.3000(2) 0.0376(16) Uani 1 1 d . . . . .
H63A H 0.2962 0.7561 0.2980 0.056 Uiso 1 1 calc GR . . . .
H63B H 0.2014 0.7774 0.3286 0.056 Uiso 1 1 calc GR . . . .
H63C H 0.2114 0.8322 0.2890 0.056 Uiso 1 1 calc GR . . . .
C64 C 0.1367(7) 0.6365(5) 0.2919(2) 0.0387(16) Uani 1 1 d . . . . .
H64A H 0.0717 0.6047 0.2787 0.058 Uiso 1 1 calc GR . . . .
H64B H 0.1325 0.6372 0.3214 0.058 Uiso 1 1 calc GR . . . .
H64C H 0.2105 0.6119 0.2859 0.058 Uiso 1 1 calc GR . . . .
C65 C 0.2380(6) 0.5596(4) 0.1446(2) 0.0339(15) Uani 1 1 d . . . . .
H65A H 0.1781 0.5211 0.1336 0.051 Uiso 1 1 calc GR . . . .
H65B H 0.2751 0.5394 0.1707 0.051 Uiso 1 1 calc GR . . . .
H65C H 0.2967 0.5656 0.1253 0.051 Uiso 1 1 calc GR . . . .
C66 C -0.0828(5) 0.7794(4) 0.0570(2) 0.0257(13) Uani 1 1 d . . . . .
H66 H -0.0845 0.7376 0.0789 0.031 Uiso 1 1 calc R . . . .
C67 C -0.1239(5) 0.8586(4) 0.0743(2) 0.0311(14) Uani 1 1 d . . . . .
H67A H -0.0732 0.8729 0.0989 0.047 Uiso 1 1 calc GR . . . .
H67B H -0.2041 0.8522 0.0812 0.047 Uiso 1 1 calc GR . . . .
H67C H -0.1210 0.9018 0.0539 0.047 Uiso 1 1 calc GR . . . .
C68 C -0.1700(5) 0.7520(4) 0.0213(2) 0.0375(17) Uani 1 1 d . . . . .
H68A H -0.1846 0.7969 0.0020 0.056 Uiso 1 1 calc GR . . . .
H68B H -0.2432 0.7360 0.0318 0.056 Uiso 1 1 calc GR . . . .
H68C H -0.1378 0.7057 0.0075 0.056 Uiso 1 1 calc GR . . . .
O13 O 0.8891(4) 0.0669(3) 0.45708(13) 0.0289(10) Uani 1 1 d . . . . .
H13 H 0.9466 0.0359 0.4622 0.043 Uiso 1 1 calc GR . . . .
O14 O 0.9432(5) -0.0292(3) 0.40432(14) 0.0368(11) Uani 1 1 d . . . . .
O15 O 1.0133(3) 0.1641(3) 0.33040(12) 0.0231(9) Uani 1 1 d . . . . .
O16 O 0.8921(4) 0.4231(3) 0.28720(14) 0.0357(11) Uani 1 1 d . . . . .
O17 O 1.0570(6) 0.2461(4) 0.19697(16) 0.0642(18) Uani 1 1 d . . . . .
O18 O 0.9088(3) 0.3435(2) 0.43576(11) 0.0205(8) Uani 1 1 d . . . . .
C69 C 0.9181(5) 0.1276(3) 0.43257(17) 0.0206(12) Uani 1 1 d . . . . .
C70 C 0.9621(5) 0.1107(3) 0.39420(17) 0.0205(12) Uani 1 1 d . . . . .
C71 C 0.9821(5) 0.0259(4) 0.3843(2) 0.0268(13) Uani 1 1 d . . . . .
C72 C 1.0628(8) -0.0013(5) 0.3537(3) 0.056(2) Uani 1 1 d . . . . .
H72 H 1.0944 0.0458 0.3391 0.068 Uiso 1 1 calc R . . . .
C73 C 1.0046(7) -0.0612(8) 0.3246(3) 0.073(3) Uani 1 1 d . . . . .
H73A H 0.9906 -0.1116 0.3392 0.109 Uiso 1 1 calc GR . . . .
H73B H 1.0547 -0.0726 0.3029 0.109 Uiso 1 1 calc GR . . . .
H73C H 0.9302 -0.0390 0.3126 0.109 Uiso 1 1 calc GR . . . .
C74 C 1.1649(8) -0.0508(6) 0.3800(3) 0.064(3) Uani 1 1 d . . . . .
H74A H 1.1983 -0.0170 0.4027 0.096 Uiso 1 1 calc GR . . . .
H74B H 1.2258 -0.0650 0.3625 0.096 Uiso 1 1 calc GR . . . .
H74C H 1.1327 -0.1006 0.3907 0.096 Uiso 1 1 calc GR . . . .
C75 C 0.9811(4) 0.1808(3) 0.36973(17) 0.0170(11) Uani 1 1 d . . . . .
C76 C 1.0004(5) 0.2247(4) 0.30171(17) 0.0236(12) Uani 1 1 d . . . . .
C77 C 0.9812(5) 0.3026(4) 0.31115(17) 0.0211(12) Uani 1 1 d . . . . .
C78 C 0.9409(5) 0.3590(4) 0.27910(18) 0.0269(13) Uani 1 1 d . . . . .
C79 C 0.9560(7) 0.3408(5) 0.23417(19) 0.0362(16) Uani 1 1 d . . . . .
C80 C 1.0132(7) 0.2598(5) 0.2280(2) 0.0390(17) Uani 1 1 d . . . . .
C81 C 1.0095(6) 0.1908(4) 0.25924(19) 0.0286(14) Uani 1 1 d . . . . .
C82 C 1.1234(6) 0.1406(5) 0.2598(2) 0.0420(18) Uani 1 1 d . . . . .
H82A H 1.1894 0.1738 0.2710 0.063 Uiso 1 1 calc GR . . . .
H82B H 1.1352 0.1242 0.2319 0.063 Uiso 1 1 calc GR . . . .
H82C H 1.1175 0.0922 0.2767 0.063 Uiso 1 1 calc GR . . . .
C83 C 0.9041(7) 0.1353(5) 0.24583(19) 0.0379(16) Uani 1 1 d . . . . .
H83A H 0.9054 0.0879 0.2639 0.057 Uiso 1 1 calc GR . . . .
H83B H 0.9087 0.1173 0.2177 0.057 Uiso 1 1 calc GR . . . .
H83C H 0.8317 0.1657 0.2475 0.057 Uiso 1 1 calc GR . . . .
C84 C 0.8343(8) 0.3402(6) 0.2100(2) 0.054(2) Uani 1 1 d . . . . .
H84A H 0.7846 0.3005 0.2222 0.080 Uiso 1 1 calc GR . . . .
H84B H 0.8416 0.3253 0.1816 0.080 Uiso 1 1 calc GR . . . .
H84C H 0.7993 0.3943 0.2110 0.080 Uiso 1 1 calc GR . . . .
C85 C 1.0320(9) 0.4080(6) 0.2187(3) 0.060(2) Uani 1 1 d . . . . .
H85A H 0.9919 0.4603 0.2199 0.090 Uiso 1 1 calc GR . . . .
H85B H 1.0465 0.3965 0.1905 0.090 Uiso 1 1 calc GR . . . .
H85C H 1.1063 0.4103 0.2359 0.090 Uiso 1 1 calc GR . . . .
C86 C 0.9895(5) 0.3310(3) 0.35504(17) 0.0180(11) Uani 1 1 d . . . . .
H86 H 0.9273 0.3724 0.3577 0.022 Uiso 1 1 calc R . . . .
C87 C 0.9662(4) 0.2587(3) 0.38127(16) 0.0174(11) Uani 1 1 d . . . . .
C88 C 0.9279(4) 0.2695(3) 0.42051(17) 0.0175(11) Uani 1 1 d . . . . .
C89 C 0.8874(5) 0.3317(4) 0.47956(17) 0.0199(11) Uani 1 1 d . . . . .
C90 C 0.8539(4) 0.2401(3) 0.48265(16) 0.0181(11) Uani 1 1 d . . . . .
H90 H 0.7672 0.2348 0.4787 0.022 Uiso 1 1 calc R . . . .
C91 C 0.9051(5) 0.2060(4) 0.44564(16) 0.0197(12) Uani 1 1 d . . . . .
C92 C 0.8989(5) 0.2035(4) 0.52378(16) 0.0205(12) Uani 1 1 d . . . . .
H92A H 0.8589 0.2301 0.5454 0.025 Uiso 1 1 calc R . . . .
H92B H 0.8784 0.1451 0.5237 0.025 Uiso 1 1 calc R . . . .
C93 C 1.0287(5) 0.2120(4) 0.53396(17) 0.0229(12) Uani 1 1 d . . . . .
H93 H 1.0661 0.1782 0.5137 0.027 Uiso 1 1 calc R . . . .
C94 C 1.0640(5) 0.2984(4) 0.52709(17) 0.0209(12) Uani 1 1 d . . . . .
H94 H 1.1365 0.3164 0.5402 0.025 Uiso 1 1 calc R . . . .
C95 C 1.0008(5) 0.3512(4) 0.50389(17) 0.0218(12) Uani 1 1 d . . . . .
H95 H 1.0294 0.4051 0.5026 0.026 Uiso 1 1 calc R . . . .
C96 C 1.0764(5) 0.1813(4) 0.57627(19) 0.0285(13) Uani 1 1 d . . . . .
H96 H 1.1622 0.1915 0.5791 0.034 Uiso 1 1 calc R . . . .
C97 C 1.0258(6) 0.2281(5) 0.61091(19) 0.0362(16) Uani 1 1 d . . . . .
H97A H 1.0355 0.2866 0.6068 0.054 Uiso 1 1 calc GR . . . .
H97B H 1.0669 0.2121 0.6372 0.054 Uiso 1 1 calc GR . . . .
H97C H 0.9428 0.2154 0.6108 0.054 Uiso 1 1 calc GR . . . .
C98 C 1.0594(8) 0.0900(5) 0.5811(3) 0.054(2) Uani 1 1 d . . . . .
H98A H 0.9767 0.0767 0.5753 0.080 Uiso 1 1 calc GR . . . .
H98B H 1.0865 0.0739 0.6091 0.080 Uiso 1 1 calc GR . . . .
H98C H 1.1043 0.0609 0.5619 0.080 Uiso 1 1 calc GR . . . .
C99 C 0.7917(6) 0.3895(4) 0.48766(19) 0.0307(14) Uani 1 1 d . . . . .
H99A H 0.8197 0.4454 0.4859 0.046 Uiso 1 1 calc GR . . . .
H99B H 0.7683 0.3796 0.5150 0.046 Uiso 1 1 calc GR . . . .
H99C H 0.7248 0.3811 0.4674 0.046 Uiso 1 1 calc GR . . . .
C100 C 1.1094(5) 0.3705(4) 0.36873(19) 0.0268(13) Uani 1 1 d . . . . .
H100 H 1.1093 0.3857 0.3981 0.032 Uiso 1 1 calc R . . . .
C101 C 1.1288(6) 0.4478(4) 0.3453(2) 0.0355(15) Uani 1 1 d . . . . .
H10A H 1.1408 0.4341 0.3170 0.053 Uiso 1 1 calc GR . . . .
H10B H 1.1977 0.4760 0.3581 0.053 Uiso 1 1 calc GR . . . .
H10C H 1.0605 0.4831 0.3455 0.053 Uiso 1 1 calc GR . . . .
C102 C 1.2099(6) 0.3108(5) 0.3657(3) 0.0423(19) Uani 1 1 d . . . . .
H10D H 1.2004 0.2641 0.3835 0.063 Uiso 1 1 calc GR . . . .
H10E H 1.2840 0.3379 0.3741 0.063 Uiso 1 1 calc GR . . . .
H10F H 1.2096 0.2921 0.3374 0.063 Uiso 1 1 calc GR . . . .
O19 O 0.4142(4) 0.9191(3) 0.04398(13) 0.0321(10) Uani 1 1 d . . . . .
H19 H 0.4381 0.9641 0.0536 0.048 Uiso 1 1 calc GR . . . .
O20 O 0.5081(5) 1.0162(3) 0.09426(15) 0.0408(12) Uani 1 1 d . . . . .
O21 O 0.6237(3) 0.8235(2) 0.16882(12) 0.0220(9) Uani 1 1 d . . . . .
O22 O 0.5173(4) 0.5746(3) 0.22042(14) 0.0353(11) Uani 1 1 d . . . . .
O23 O 0.7849(5) 0.7454(3) 0.29757(16) 0.0540(16) Uani 1 1 d . . . . .
O24 O 0.4337(3) 0.6440(2) 0.06859(11) 0.0213(8) Uani 1 1 d . . . . .
C103 C 0.4561(5) 0.8591(4) 0.06896(17) 0.0215(12) Uani 1 1 d . . . . .
C104 C 0.5274(5) 0.8758(4) 0.10661(18) 0.0212(12) Uani 1 1 d . . . . .
C105 C 0.5596(6) 0.9612(4) 0.1148(2) 0.0307(14) Uani 1 1 d . . . . .
C106 C 0.6608(7) 0.9881(4) 0.1431(3) 0.0439(19) Uani 1 1 d . . . . .
H106 H 0.7054 0.9399 0.1547 0.053 Uiso 1 1 calc R . . . .
C107 C 0.6159(7) 1.0370(7) 0.1771(3) 0.065(3) Uani 1 1 d . . . . .
H10G H 0.5639 1.0798 0.1654 0.097 Uiso 1 1 calc GR . . . .
H10H H 0.6816 1.0616 0.1938 0.097 Uiso 1 1 calc GR . . . .
H10I H 0.5730 1.0012 0.1941 0.097 Uiso 1 1 calc GR . . . .
C108 C 0.7404(8) 1.0429(6) 0.1198(3) 0.060(2) Uani 1 1 d . . . . .
H10J H 0.7615 1.0143 0.0955 0.090 Uiso 1 1 calc GR . . . .
H10K H 0.8112 1.0561 0.1375 0.090 Uiso 1 1 calc GR . . . .
H10L H 0.6990 1.0932 0.1115 0.090 Uiso 1 1 calc GR . . . .
C109 C 0.5602(4) 0.8077(3) 0.13143(16) 0.0162(11) Uani 1 1 d . . . . .
C110 C 0.6322(5) 0.7641(4) 0.19824(17) 0.0221(12) Uani 1 1 d . . . . .
C111 C 0.6004(5) 0.6864(3) 0.19054(17) 0.0196(11) Uani 1 1 d . . . . .
C112 C 0.5823(5) 0.6323(4) 0.22524(17) 0.0244(12) Uani 1 1 d . . . . .
C113 C 0.6505(6) 0.6495(4) 0.26649(19) 0.0328(15) Uani 1 1 d . . . . .
C114 C 0.7102(6) 0.7312(4) 0.26963(18) 0.0312(15) Uani 1 1 d . . . . .
C115 C 0.6732(5) 0.7992(4) 0.23956(19) 0.0276(14) Uani 1 1 d . . . . .
C116 C 0.5727(6) 0.8469(4) 0.25681(19) 0.0330(15) Uani 1 1 d . . . . .
H11A H 0.5476 0.8914 0.2382 0.049 Uiso 1 1 calc GR . . . .
H11B H 0.6002 0.8692 0.2836 0.049 Uiso 1 1 calc GR . . . .
H11C H 0.5071 0.8102 0.2595 0.049 Uiso 1 1 calc GR . . . .
C117 C 0.7780(7) 0.8561(5) 0.2364(2) 0.0457(19) Uani 1 1 d . . . . .
H11D H 0.8398 0.8266 0.2243 0.069 Uiso 1 1 calc GR . . . .
H11E H 0.8073 0.8752 0.2636 0.069 Uiso 1 1 calc GR . . . .
H11F H 0.7535 0.9028 0.2191 0.069 Uiso 1 1 calc GR . . . .
C118 C 0.5685(8) 0.6415(6) 0.3003(2) 0.050(2) Uani 1 1 d . . . . .
H11G H 0.5077 0.6832 0.2966 0.075 Uiso 1 1 calc GR . . . .
H11H H 0.6130 0.6487 0.3270 0.075 Uiso 1 1 calc GR . . . .
H11I H 0.5324 0.5876 0.2990 0.075 Uiso 1 1 calc GR . . . .
C119 C 0.7466(8) 0.5824(5) 0.2725(2) 0.047(2) Uani 1 1 d . . . . .
H11J H 0.7099 0.5287 0.2706 0.070 Uiso 1 1 calc GR . . . .
H11K H 0.7903 0.5888 0.2994 0.070 Uiso 1 1 calc GR . . . .
H11L H 0.7997 0.5877 0.2512 0.070 Uiso 1 1 calc GR . . . .
C120 C 0.5693(4) 0.6566(3) 0.14772(16) 0.0174(11) Uani 1 1 d . . . . .
H120 H 0.5009 0.6194 0.1480 0.021 Uiso 1 1 calc R . . . .
C121 C 0.5316(4) 0.7288(3) 0.12140(16) 0.0166(11) Uani 1 1 d . . . . .
C122 C 0.4673(4) 0.7182(4) 0.08291(16) 0.0167(11) Uani 1 1 d . . . . .
C123 C 0.3888(5) 0.6550(4) 0.02468(17) 0.0238(13) Uani 1 1 d . . . . .
C124 C 0.3569(5) 0.7462(4) 0.02153(17) 0.0231(12) Uani 1 1 d . . . . .
H124 H 0.2731 0.7525 0.0262 0.028 Uiso 1 1 calc R . . . .
C125 C 0.4308(5) 0.7808(4) 0.05779(17) 0.0211(12) Uani 1 1 d . . . . .
C126 C 0.3751(5) 0.7813(4) -0.02079(18) 0.0288(14) Uani 1 1 d . . . . .
H12A H 0.3245 0.7522 -0.0420 0.035 Uiso 1 1 calc R . . . .
H12B H 0.3525 0.8393 -0.0218 0.035 Uiso 1 1 calc R . . . .
C127 C 0.5014(5) 0.7733(4) -0.02964(18) 0.0270(13) Uani 1 1 d . . . . .
H127 H 0.5489 0.8076 -0.0092 0.032 Uiso 1 1 calc R . . . .
C128 C 0.5409(5) 0.6870(4) -0.02258(19) 0.0261(13) Uani 1 1 d . . . . .
H128 H 0.6054 0.6685 -0.0358 0.031 Uiso 1 1 calc R . . . .
C129 C 0.4907(5) 0.6349(4) 0.00110(18) 0.0242(12) Uani 1 1 d . . . . .
H129 H 0.5211 0.5813 0.0033 0.029 Uiso 1 1 calc R . . . .
C130 C 0.5261(7) 0.8037(4) -0.0725(2) 0.0362(15) Uani 1 1 d . . . . .
H130 H 0.6097 0.7918 -0.0757 0.043 Uiso 1 1 calc R . . . .
C131 C 0.4531(7) 0.7596(5) -0.10672(19) 0.0432(18) Uani 1 1 d . . . . .
H13A H 0.4557 0.7011 -0.1014 0.065 Uiso 1 1 calc GR . . . .
H13B H 0.4843 0.7708 -0.1328 0.065 Uiso 1 1 calc GR . . . .
H13C H 0.3724 0.7786 -0.1080 0.065 Uiso 1 1 calc GR . . . .
C132 C 0.5093(9) 0.8953(5) -0.0770(3) 0.056(2) Uani 1 1 d . . . . .
H13D H 0.4291 0.9095 -0.0724 0.084 Uiso 1 1 calc GR . . . .
H13E H 0.5244 0.9120 -0.1045 0.084 Uiso 1 1 calc GR . . . .
H13F H 0.5635 0.9233 -0.0569 0.084 Uiso 1 1 calc GR . . . .
C133 C 0.2877(6) 0.5975(5) 0.01615(19) 0.0348(16) Uani 1 1 d . . . . .
H13G H 0.3151 0.5414 0.0201 0.052 Uiso 1 1 calc GR . . . .
H13H H 0.2535 0.6046 -0.0121 0.052 Uiso 1 1 calc GR . . . .
H13I H 0.2288 0.6091 0.0348 0.052 Uiso 1 1 calc GR . . . .
C134 C 0.6690(5) 0.6083(4) 0.12989(17) 0.0210(12) Uani 1 1 d . . . . .
H134 H 0.6393 0.5915 0.1016 0.025 Uiso 1 1 calc R . . . .
C135 C 0.7006(6) 0.5315(4) 0.1538(2) 0.0333(15) Uani 1 1 d . . . . .
H13J H 0.7256 0.5454 0.1822 0.050 Uiso 1 1 calc GR . . . .
H13K H 0.7641 0.5036 0.1418 0.050 Uiso 1 1 calc GR . . . .
H13L H 0.6325 0.4957 0.1527 0.050 Uiso 1 1 calc GR . . . .
C136 C 0.7743(5) 0.6608(4) 0.1266(2) 0.0314(14) Uani 1 1 d . . . . .
H13M H 0.7512 0.7102 0.1112 0.047 Uiso 1 1 calc GR . . . .
H13N H 0.8316 0.6309 0.1124 0.047 Uiso 1 1 calc GR . . . .
H13O H 0.8088 0.6756 0.1540 0.047 Uiso 1 1 calc GR . . . .
C51A C -0.0853(15) 0.8580(11) -0.0919(6) 0.043(4) Uani 0.46(2) 1 d . U P A 2
H51D H -0.0942 0.8015 -0.1011 0.065 Uiso 0.46(2) 1 calc GR . P A 2
H51E H -0.0859 0.8938 -0.1157 0.065 Uiso 0.46(2) 1 calc GR . P A 2
H51F H -0.1497 0.8725 -0.0761 0.065 Uiso 0.46(2) 1 calc GR . P A 2
C50A C 0.1017(17) 0.8406(14) -0.0979(6) 0.061(5) Uani 0.46(2) 1 d D U P A 2
H50D H 0.1821 0.8425 -0.0851 0.092 Uiso 0.46(2) 1 calc GR . P A 2
H50E H 0.0935 0.8772 -0.1214 0.092 Uiso 0.46(2) 1 calc GR . P A 2
H50F H 0.0826 0.7850 -0.1069 0.092 Uiso 0.46(2) 1 calc GR . P A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.031(2) 0.021(2) 0.023(2) -0.0019(18) 0.0058(17) 0.0034(17)
O2 0.045(3) 0.021(2) 0.026(2) -0.0024(19) 0.0047(19) 0.0082(19)
O3 0.0225(18) 0.0128(18) 0.0174(19) 0.0027(15) -0.0011(15) 0.0003(15)
O4 0.046(3) 0.019(2) 0.023(2) -0.0010(18) 0.0065(19) -0.0002(19)
O5 0.068(3) 0.030(3) 0.022(2) 0.010(2) 0.011(2) 0.019(2)
O6 0.030(2) 0.0127(19) 0.0187(19) 0.0049(16) 0.0045(16) -0.0007(16)
C1 0.019(2) 0.020(3) 0.017(3) 0.002(2) -0.001(2) 0.000(2)
C2 0.016(2) 0.014(3) 0.021(3) -0.003(2) -0.004(2) 0.000(2)
C3 0.021(3) 0.018(3) 0.021(3) -0.001(2) -0.002(2) 0.003(2)
C4 0.033(3) 0.013(3) 0.022(3) -0.002(2) -0.002(2) 0.005(2)
C5 0.045(4) 0.014(3) 0.029(3) 0.000(3) 0.000(3) 0.009(3)
C6 0.034(3) 0.027(3) 0.036(4) 0.000(3) 0.003(3) -0.004(3)
C7 0.016(2) 0.011(2) 0.016(2) 0.003(2) -0.0055(19) -0.0007(19)
C8 0.014(2) 0.013(2) 0.019(3) -0.001(2) -0.0015(19) -0.005(2)
C9 0.019(2) 0.012(3) 0.016(3) 0.001(2) 0.000(2) -0.002(2)
C10 0.022(3) 0.018(3) 0.015(3) -0.002(2) 0.002(2) -0.001(2)
C11 0.035(3) 0.013(3) 0.022(3) 0.002(2) 0.006(2) 0.001(2)
C12 0.023(3) 0.015(3) 0.021(3) 0.002(2) 0.004(2) 0.000(2)
C13 0.018(3) 0.016(3) 0.021(3) 0.004(2) 0.004(2) 0.001(2)
C14 0.019(3) 0.017(3) 0.021(3) 0.005(2) 0.000(2) 0.001(2)
C15 0.021(3) 0.016(3) 0.033(3) 0.003(3) 0.000(2) -0.002(2)
C16 0.049(4) 0.024(3) 0.047(4) 0.018(3) 0.026(3) 0.009(3)
C17 0.079(6) 0.027(4) 0.028(3) 0.005(3) -0.008(4) -0.014(4)
C18 0.018(2) 0.012(2) 0.019(3) 0.000(2) 0.000(2) -0.002(2)
C19 0.017(2) 0.012(2) 0.019(3) 0.000(2) -0.003(2) 0.002(2)
C20 0.018(2) 0.010(2) 0.017(2) 0.002(2) -0.002(2) -0.0019(19)
C21 0.030(3) 0.019(3) 0.014(3) 0.009(2) 0.002(2) 0.001(2)
C22 0.023(3) 0.015(3) 0.021(3) 0.001(2) 0.002(2) -0.001(2)
C23 0.013(2) 0.015(3) 0.020(3) 0.001(2) -0.0026(19) 0.002(2)
C24 0.054(4) 0.019(3) 0.017(3) 0.004(2) 0.001(3) 0.003(3)
C25 0.057(4) 0.027(3) 0.043(4) 0.008(3) -0.021(3) -0.012(3)
C26 0.023(3) 0.045(4) 0.037(4) 0.008(3) -0.002(3) -0.006(3)
C27 0.027(3) 0.039(4) 0.024(3) 0.011(3) 0.007(2) 0.009(3)
C28 0.058(2) 0.056(2) 0.056(2) -0.0001(13) 0.0026(13) 0.0003(13)
C29 0.060(3) 0.057(3) 0.050(3) 0.003(2) 0.003(2) 0.009(2)
C30 0.084(4) 0.079(4) 0.079(4) -0.005(2) 0.004(3) -0.002(2)
C31 0.030(3) 0.016(3) 0.028(3) -0.004(2) 0.004(2) 0.000(2)
C32 0.021(3) 0.018(3) 0.028(3) 0.005(3) 0.000(2) 0.005(2)
C33 0.016(3) 0.024(3) 0.039(3) 0.001(3) -0.004(2) -0.002(2)
C34 0.032(3) 0.023(3) 0.039(4) 0.007(3) 0.016(3) 0.003(3)
O7 0.029(2) 0.027(2) 0.024(2) -0.0033(18) -0.0098(17) -0.0055(18)
O8 0.044(3) 0.027(2) 0.036(3) -0.003(2) -0.007(2) -0.009(2)
O9 0.0227(19) 0.0112(18) 0.0203(19) -0.0004(16) -0.0005(15) 0.0005(15)
O10 0.053(3) 0.019(2) 0.026(2) -0.0002(19) -0.005(2) -0.005(2)
O11 0.088(4) 0.036(3) 0.029(3) 0.011(2) -0.003(3) -0.023(3)
O12 0.027(2) 0.0129(19) 0.023(2) 0.0051(16) -0.0007(16) 0.0006(16)
C35 0.020(3) 0.026(3) 0.016(3) -0.005(2) -0.001(2) 0.000(2)
C36 0.020(3) 0.019(3) 0.021(3) -0.001(2) -0.001(2) 0.001(2)
C37 0.023(3) 0.023(3) 0.024(3) -0.003(3) 0.002(2) -0.004(2)
C38 0.033(3) 0.022(3) 0.030(3) -0.003(3) 0.003(3) -0.005(3)
C39 0.030(3) 0.034(4) 0.033(3) -0.003(3) 0.002(3) 0.005(3)
C40 0.054(4) 0.024(3) 0.035(4) -0.003(3) -0.002(3) -0.007(3)
C41 0.012(2) 0.008(2) 0.022(3) 0.000(2) -0.001(2) -0.0002(18)
C42 0.014(2) 0.013(2) 0.021(3) -0.001(2) -0.006(2) 0.003(2)
C43 0.016(2) 0.015(3) 0.025(3) 0.000(2) -0.004(2) 0.001(2)
C44 0.033(3) 0.018(3) 0.027(3) 0.001(3) -0.005(2) -0.007(2)
C45 0.064(4) 0.030(4) 0.027(3) 0.006(3) -0.021(3) -0.011(3)
C46 0.032(3) 0.020(3) 0.024(3) 0.008(3) -0.005(2) -0.001(2)
C47 0.020(3) 0.013(3) 0.025(3) 0.005(2) -0.002(2) 0.000(2)
C48 0.020(3) 0.019(3) 0.034(3) 0.007(3) -0.001(2) 0.001(2)
C49 0.026(3) 0.019(3) 0.039(4) 0.005(3) -0.005(3) 0.006(2)
C50 0.056(5) 0.052(5) 0.049(5) -0.001(3) 0.001(3) -0.003(3)
C51 0.058(5) 0.053(5) 0.056(5) 0.004(3) -0.002(3) -0.003(3)
C52 0.019(2) 0.009(2) 0.025(3) -0.002(2) -0.004(2) -0.003(2)
C53 0.015(2) 0.015(3) 0.022(3) 0.003(2) -0.001(2) 0.000(2)
C54 0.017(2) 0.012(3) 0.023(3) 0.001(2) -0.002(2) 0.002(2)
C55 0.024(3) 0.018(3) 0.022(3) 0.010(2) -0.006(2) -0.001(2)
C56 0.014(2) 0.024(3) 0.027(3) 0.005(3) 0.000(2) 0.004(2)
C57 0.015(2) 0.021(3) 0.021(3) 0.002(2) -0.001(2) 0.003(2)
C58 0.029(3) 0.022(3) 0.023(3) 0.008(3) -0.001(2) 0.006(2)
C59 0.038(3) 0.030(3) 0.024(3) 0.010(3) 0.007(3) 0.009(3)
C60 0.022(3) 0.044(4) 0.035(4) 0.016(3) 0.002(3) 0.005(3)
C61 0.024(3) 0.032(3) 0.032(3) 0.016(3) -0.002(2) -0.001(3)
C62 0.039(3) 0.034(4) 0.023(3) 0.000(3) 0.006(3) 0.013(3)
C63 0.054(4) 0.029(4) 0.031(3) 0.003(3) 0.009(3) 0.011(3)
C64 0.051(4) 0.044(4) 0.022(3) 0.008(3) 0.007(3) -0.001(3)
C65 0.040(4) 0.021(3) 0.038(4) 0.002(3) -0.006(3) 0.004(3)
C66 0.016(3) 0.019(3) 0.041(4) 0.008(3) 0.002(2) 0.000(2)
C67 0.020(3) 0.024(3) 0.050(4) -0.010(3) 0.005(3) 0.000(2)
C68 0.017(3) 0.028(3) 0.066(5) -0.002(3) -0.006(3) -0.002(2)
O13 0.038(2) 0.024(2) 0.024(2) 0.0051(19) -0.0009(18) -0.0100(19)
O14 0.058(3) 0.022(2) 0.031(2) 0.003(2) 0.004(2) -0.006(2)
O15 0.025(2) 0.026(2) 0.0185(19) 0.0024(17) 0.0032(16) 0.0056(17)
O16 0.043(3) 0.036(3) 0.028(2) 0.012(2) 0.0008(19) 0.017(2)
O17 0.104(5) 0.065(4) 0.029(3) 0.010(3) 0.032(3) 0.022(4)
O18 0.0252(19) 0.020(2) 0.0160(19) 0.0010(16) 0.0019(15) 0.0022(16)
C69 0.021(3) 0.018(3) 0.021(3) 0.004(2) -0.008(2) -0.009(2)
C70 0.022(3) 0.019(3) 0.019(3) -0.001(2) -0.007(2) -0.001(2)
C71 0.031(3) 0.017(3) 0.032(3) 0.000(3) -0.003(3) -0.004(2)
C72 0.069(5) 0.017(3) 0.091(7) -0.004(4) 0.051(5) -0.004(4)
C73 0.039(4) 0.130(10) 0.047(5) -0.045(6) -0.006(4) 0.019(5)
C74 0.053(5) 0.052(5) 0.083(7) -0.009(5) -0.012(5) 0.005(4)
C75 0.015(2) 0.016(3) 0.019(3) 0.000(2) -0.002(2) -0.001(2)
C76 0.022(3) 0.029(3) 0.019(3) 0.003(3) -0.001(2) 0.001(2)
C77 0.017(3) 0.027(3) 0.019(3) 0.005(2) -0.001(2) 0.001(2)
C78 0.031(3) 0.028(3) 0.021(3) 0.002(3) 0.000(2) 0.007(3)
C79 0.052(4) 0.039(4) 0.017(3) 0.005(3) 0.005(3) 0.009(3)
C80 0.053(4) 0.043(4) 0.022(3) 0.003(3) 0.010(3) 0.005(3)
C81 0.036(3) 0.029(3) 0.022(3) -0.004(3) 0.008(3) 0.004(3)
C82 0.042(4) 0.053(5) 0.034(4) 0.002(4) 0.014(3) 0.017(4)
C83 0.049(4) 0.045(4) 0.018(3) -0.010(3) 0.002(3) -0.002(3)
C84 0.069(5) 0.070(6) 0.020(3) 0.002(4) -0.010(3) 0.025(5)
C85 0.091(7) 0.053(5) 0.042(5) 0.012(4) 0.032(5) 0.000(5)
C86 0.020(3) 0.015(3) 0.018(3) 0.006(2) -0.002(2) 0.003(2)
C87 0.015(2) 0.016(3) 0.020(3) 0.002(2) -0.003(2) -0.007(2)
C88 0.015(2) 0.015(3) 0.021(3) 0.001(2) -0.005(2) -0.002(2)
C89 0.021(3) 0.022(3) 0.016(3) 0.002(2) 0.000(2) 0.000(2)
C90 0.016(2) 0.021(3) 0.017(3) 0.000(2) -0.001(2) -0.005(2)
C91 0.020(3) 0.024(3) 0.014(2) 0.002(2) -0.003(2) -0.008(2)
C92 0.021(3) 0.024(3) 0.016(3) 0.002(2) -0.001(2) -0.004(2)
C93 0.022(3) 0.028(3) 0.019(3) -0.002(2) 0.000(2) 0.002(2)
C94 0.016(2) 0.028(3) 0.018(3) -0.001(2) -0.001(2) -0.003(2)
C95 0.025(3) 0.020(3) 0.020(3) -0.003(2) 0.003(2) -0.003(2)
C96 0.029(3) 0.033(3) 0.022(3) 0.003(3) -0.007(2) 0.003(3)
C97 0.034(3) 0.053(5) 0.020(3) 0.001(3) -0.002(3) -0.007(3)
C98 0.063(5) 0.039(4) 0.055(5) 0.011(4) -0.013(4) -0.002(4)
C99 0.034(3) 0.033(4) 0.026(3) 0.002(3) 0.006(3) 0.006(3)
C100 0.028(3) 0.023(3) 0.027(3) 0.007(3) -0.009(2) -0.009(2)
C101 0.043(4) 0.025(3) 0.037(4) 0.010(3) -0.002(3) -0.010(3)
C102 0.020(3) 0.046(4) 0.059(5) 0.030(4) -0.009(3) -0.004(3)
O19 0.042(3) 0.029(2) 0.025(2) 0.004(2) -0.0008(19) 0.016(2)
O20 0.057(3) 0.024(2) 0.040(3) 0.004(2) -0.005(2) 0.015(2)
O21 0.0217(19) 0.025(2) 0.0169(19) -0.0021(17) -0.0085(15) 0.0000(16)
O22 0.040(3) 0.036(3) 0.030(2) 0.009(2) 0.006(2) -0.001(2)
O23 0.069(4) 0.048(3) 0.038(3) -0.012(3) -0.033(3) 0.018(3)
O24 0.0201(18) 0.024(2) 0.0179(19) -0.0025(17) -0.0077(15) -0.0028(16)
C103 0.023(3) 0.024(3) 0.017(3) 0.002(2) -0.001(2) 0.011(2)
C104 0.021(3) 0.020(3) 0.022(3) 0.001(2) 0.001(2) 0.008(2)
C105 0.037(3) 0.014(3) 0.041(4) 0.004(3) 0.004(3) 0.008(3)
C106 0.041(4) 0.020(3) 0.067(5) 0.000(4) -0.017(4) -0.004(3)
C107 0.030(4) 0.119(9) 0.044(5) -0.002(5) -0.007(3) -0.015(5)
C108 0.044(4) 0.044(5) 0.094(7) 0.002(5) 0.012(5) 0.001(4)
C109 0.009(2) 0.022(3) 0.017(3) 0.000(2) -0.0037(19) 0.002(2)
C110 0.021(3) 0.023(3) 0.020(3) -0.001(3) -0.005(2) 0.001(2)
C111 0.022(3) 0.019(3) 0.018(3) 0.001(2) -0.002(2) 0.005(2)
C112 0.028(3) 0.026(3) 0.019(3) 0.005(3) 0.003(2) 0.006(3)
C113 0.044(4) 0.035(4) 0.019(3) 0.007(3) 0.001(3) 0.013(3)
C114 0.037(3) 0.034(4) 0.021(3) -0.011(3) -0.010(3) 0.011(3)
C115 0.033(3) 0.024(3) 0.024(3) -0.005(3) -0.010(2) 0.008(3)
C116 0.040(4) 0.036(4) 0.020(3) -0.009(3) -0.007(3) 0.007(3)
C117 0.040(4) 0.053(5) 0.040(4) -0.007(4) -0.016(3) -0.012(4)
C118 0.064(5) 0.063(5) 0.024(3) 0.005(4) 0.018(3) 0.007(4)
C119 0.063(5) 0.034(4) 0.039(4) 0.004(3) -0.016(4) 0.022(4)
C120 0.014(2) 0.018(3) 0.019(3) -0.001(2) -0.001(2) 0.002(2)
C121 0.014(2) 0.019(3) 0.015(2) -0.001(2) -0.0058(19) 0.003(2)
C122 0.009(2) 0.025(3) 0.015(2) -0.004(2) -0.0028(19) 0.002(2)
C123 0.019(3) 0.034(3) 0.017(3) -0.001(3) -0.005(2) -0.003(2)
C124 0.016(2) 0.031(3) 0.021(3) 0.002(3) -0.005(2) 0.007(2)
C125 0.019(3) 0.028(3) 0.016(3) 0.003(2) -0.002(2) 0.007(2)
C126 0.028(3) 0.036(4) 0.021(3) 0.002(3) -0.004(2) 0.008(3)
C127 0.028(3) 0.033(3) 0.019(3) -0.003(3) 0.002(2) -0.003(3)
C128 0.024(3) 0.028(3) 0.026(3) -0.009(3) 0.001(2) 0.000(2)
C129 0.022(3) 0.027(3) 0.023(3) -0.007(3) -0.003(2) 0.000(2)
C130 0.049(4) 0.033(4) 0.027(3) 0.002(3) 0.005(3) 0.002(3)
C131 0.058(5) 0.055(5) 0.017(3) 0.000(3) 0.003(3) 0.000(4)
C132 0.089(7) 0.039(5) 0.042(5) 0.006(4) 0.013(4) 0.001(4)
C133 0.030(3) 0.049(4) 0.024(3) -0.005(3) -0.006(3) -0.012(3)
C134 0.020(3) 0.023(3) 0.021(3) -0.005(2) 0.001(2) 0.003(2)
C135 0.038(3) 0.027(3) 0.036(4) 0.002(3) 0.007(3) 0.009(3)
C136 0.023(3) 0.024(3) 0.048(4) -0.002(3) 0.010(3) -0.002(2)
C51A 0.045(5) 0.042(5) 0.041(5) 0.001(3) 0.000(3) -0.002(3)
C50A 0.064(6) 0.061(6) 0.060(6) 0.002(3) 0.005(3) 0.000(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 H1 0.8400 . ?
O1 C1 1.349(7) . ?
O2 C3 1.260(7) . ?
O3 C7 1.399(6) . ?
O3 C8 1.375(7) . ?
O4 C10 1.212(7) . ?
O5 C12 1.212(7) . ?
O6 C20 1.344(6) . ?
O6 C21 1.514(6) . ?
C1 C2 1.432(8) . ?
C1 C23 1.387(8) . ?
C2 C3 1.467(8) . ?
C2 C7 1.432(8) . ?
C3 C4 1.510(8) . ?
C4 H4 1.0000 . ?
C4 C5 1.554(8) . ?
C4 C6 1.518(9) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C19 1.382(8) . ?
C8 C9 1.355(8) . ?
C8 C13 1.492(8) . ?
C9 C10 1.472(7) . ?
C9 C18 1.492(7) . ?
C10 C11 1.518(8) . ?
C11 C12 1.508(8) . ?
C11 C16 1.547(9) . ?
C11 C17 1.538(9) . ?
C12 C13 1.554(8) . ?
C13 C14 1.560(7) . ?
C13 C15 1.529(8) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18 1.0000 . ?
C18 C19 1.492(8) . ?
C18 C32 1.553(7) . ?
C19 C20 1.404(8) . ?
C20 C23 1.381(8) . ?
C21 C22 1.548(8) . ?
C21 C27 1.494(8) . ?
C21 C31 1.515(8) . ?
C22 H22 1.0000 . ?
C22 C23 1.501(8) . ?
C22 C24 1.531(8) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.545(11) . ?
C25 H25 1.0000 . ?
C25 C26 1.493(11) . ?
C25 C28 1.533(11) . ?
C26 H26 0.9500 . ?
C26 C27 1.315(10) . ?
C27 H27 0.9500 . ?
C28 H28 1.0000 . ?
C28 C29 1.529(13) . ?
C28 C30 1.525(15) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32 1.0000 . ?
C32 C33 1.530(8) . ?
C32 C34 1.548(8) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
O7 H7 0.8400 . ?
O7 C35 1.348(7) . ?
O8 C37 1.250(7) . ?
O9 C41 1.386(6) . ?
O9 C42 1.380(7) . ?
O10 C44 1.208(7) . ?
O11 C46 1.195(8) . ?
O12 C54 1.346(7) . ?
O12 C55 1.492(6) . ?
C35 C36 1.424(8) . ?
C35 C57 1.385(8) . ?
C36 C37 1.478(8) . ?
C36 C41 1.414(8) . ?
C37 C38 1.529(9) . ?
C38 H38 1.0000 . ?
C38 C39 1.544(9) . ?
C38 C40 1.526(9) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C53 1.393(7) . ?
C42 C43 1.334(8) . ?
C42 C47 1.514(8) . ?
C43 C44 1.480(8) . ?
C43 C52 1.503(8) . ?
C44 C45 1.527(9) . ?
C45 C46 1.533(9) . ?
C45 C50 1.374(18) . ?
C45 C51 1.5017(14) . ?
C45 C51A 1.399(18) . ?
C45 C50A 1.5010(14) . ?
C46 C47 1.535(8) . ?
C47 C48 1.550(8) . ?
C47 C49 1.537(8) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52 1.0000 . ?
C52 C53 1.491(7) . ?
C52 C66 1.560(8) . ?
C53 C54 1.395(8) . ?
C54 C57 1.381(8) . ?
C55 C56 1.560(8) . ?
C55 C61 1.508(9) . ?
C55 C65 1.500(9) . ?
C56 H56 1.0000 . ?
C56 C57 1.519(8) . ?
C56 C58 1.521(8) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C58 C59 1.541(9) . ?
C59 H59 1.0000 . ?
C59 C60 1.504(10) . ?
C59 C62 1.544(8) . ?
C60 H60 0.9500 . ?
C60 C61 1.312(10) . ?
C61 H61 0.9500 . ?
C62 H62 1.0000 . ?
C62 C63 1.516(10) . ?
C62 C64 1.517(10) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66 1.0000 . ?
C66 C67 1.517(9) . ?
C66 C68 1.535(9) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
O13 H13 0.8400 . ?
O13 C69 1.348(7) . ?
O14 C71 1.234(8) . ?
O15 C75 1.410(7) . ?
O15 C76 1.371(7) . ?
O16 C78 1.237(8) . ?
O17 C80 1.205(9) . ?
O18 C88 1.344(7) . ?
O18 C89 1.500(7) . ?
C69 C70 1.435(8) . ?
C69 C91 1.373(8) . ?
C70 C71 1.458(8) . ?
C70 C75 1.436(8) . ?
C71 C72 1.507(10) . ?
C72 H72 1.0000 . ?
C72 C73 1.487(13) . ?
C72 C74 1.613(13) . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 C87 1.354(8) . ?
C76 C77 1.344(9) . ?
C76 C81 1.519(8) . ?
C77 C78 1.448(8) . ?
C77 C86 1.513(8) . ?
C78 C79 1.537(8) . ?
C79 C80 1.512(10) . ?
C79 C84 1.544(11) . ?
C79 C85 1.531(11) . ?
C80 C81 1.537(10) . ?
C81 C82 1.551(9) . ?
C81 C83 1.549(10) . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C86 H86 1.0000 . ?
C86 C87 1.511(8) . ?
C86 C100 1.554(8) . ?
C87 C88 1.418(8) . ?
C88 C91 1.375(8) . ?
C89 C90 1.562(8) . ?
C89 C95 1.500(8) . ?
C89 C99 1.502(8) . ?
C90 H90 1.0000 . ?
C90 C91 1.515(8) . ?
C90 C92 1.526(7) . ?
C92 H92A 0.9900 . ?
C92 H92B 0.9900 . ?
C92 C93 1.509(7) . ?
C93 H93 1.0000 . ?
C93 C94 1.503(9) . ?
C93 C96 1.532(8) . ?
C94 H94 0.9500 . ?
C94 C95 1.327(8) . ?
C95 H95 0.9500 . ?
C96 H96 1.0000 . ?
C96 C97 1.539(10) . ?
C96 C98 1.525(10) . ?
C97 H97A 0.9800 . ?
C97 H97B 0.9800 . ?
C97 H97C 0.9800 . ?
C98 H98A 0.9800 . ?
C98 H98B 0.9800 . ?
C98 H98C 0.9800 . ?
C99 H99A 0.9800 . ?
C99 H99B 0.9800 . ?
C99 H99C 0.9800 . ?
C100 H100 1.0000 . ?
C100 C101 1.516(9) . ?
C100 C102 1.532(10) . ?
C101 H10A 0.9800 . ?
C101 H10B 0.9800 . ?
C101 H10C 0.9800 . ?
C102 H10D 0.9800 . ?
C102 H10E 0.9800 . ?
C102 H10F 0.9800 . ?
O19 H19 0.8400 . ?
O19 C103 1.345(7) . ?
O20 C105 1.246(8) . ?
O21 C109 1.393(6) . ?
O21 C110 1.373(7) . ?
O22 C112 1.211(8) . ?
O23 C114 1.219(8) . ?
O24 C122 1.352(7) . ?
O24 C123 1.497(6) . ?
C103 C104 1.444(8) . ?
C103 C125 1.364(9) . ?
C104 C105 1.472(9) . ?
C104 C109 1.417(8) . ?
C105 C106 1.488(10) . ?
C106 H106 1.0000 . ?
C106 C107 1.510(13) . ?
C106 C108 1.547(12) . ?
C107 H10G 0.9800 . ?
C107 H10H 0.9800 . ?
C107 H10I 0.9800 . ?
C108 H10J 0.9800 . ?
C108 H10K 0.9800 . ?
C108 H10L 0.9800 . ?
C109 C121 1.373(8) . ?
C110 C111 1.349(8) . ?
C110 C115 1.510(8) . ?
C111 C112 1.480(8) . ?
C111 C120 1.502(8) . ?
C112 C113 1.527(8) . ?
C113 C114 1.510(10) . ?
C113 C118 1.538(10) . ?
C113 C119 1.565(9) . ?
C114 C115 1.527(9) . ?
C115 C116 1.554(9) . ?
C115 C117 1.541(10) . ?
C116 H11A 0.9800 . ?
C116 H11B 0.9800 . ?
C116 H11C 0.9800 . ?
C117 H11D 0.9800 . ?
C117 H11E 0.9800 . ?
C117 H11F 0.9800 . ?
C118 H11G 0.9800 . ?
C118 H11H 0.9800 . ?
C118 H11I 0.9800 . ?
C119 H11J 0.9800 . ?
C119 H11K 0.9800 . ?
C119 H11L 0.9800 . ?
C120 H120 1.0000 . ?
C120 C121 1.510(8) . ?
C120 C134 1.560(7) . ?
C121 C122 1.414(7) . ?
C122 C125 1.362(8) . ?
C123 C124 1.547(9) . ?
C123 C129 1.509(8) . ?
C123 C133 1.507(8) . ?
C124 H124 1.0000 . ?
C124 C125 1.509(8) . ?
C124 C126 1.543(8) . ?
C126 H12A 0.9900 . ?
C126 H12B 0.9900 . ?
C126 C127 1.520(9) . ?
C127 H127 1.0000 . ?
C127 C128 1.504(9) . ?
C127 C130 1.552(9) . ?
C128 H128 0.9500 . ?
C128 C129 1.330(9) . ?
C129 H129 0.9500 . ?
C130 H130 1.0000 . ?
C130 C131 1.521(10) . ?
C130 C132 1.526(11) . ?
C131 H13A 0.9800 . ?
C131 H13B 0.9800 . ?
C131 H13C 0.9800 . ?
C132 H13D 0.9800 . ?
C132 H13E 0.9800 . ?
C132 H13F 0.9800 . ?
C133 H13G 0.9800 . ?
C133 H13H 0.9800 . ?
C133 H13I 0.9800 . ?
C134 H134 1.0000 . ?
C134 C135 1.515(9) . ?
C134 C136 1.505(8) . ?
C135 H13J 0.9800 . ?
C135 H13K 0.9800 . ?
C135 H13L 0.9800 . ?
C136 H13M 0.9800 . ?
C136 H13N 0.9800 . ?
C136 H13O 0.9800 . ?
C51A H51D 0.9800 . ?
C51A H51E 0.9800 . ?
C51A H51F 0.9800 . ?
C50A H50D 0.9800 . ?
C50A H50E 0.9800 . ?
C50A H50F 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
C1 O1 H1 109.5 . . ?
C8 O3 C7 118.6(4) . . ?
C20 O6 C21 107.4(4) . . ?
O1 C1 C2 120.9(5) . . ?
O1 C1 C23 117.7(5) . . ?
C23 C1 C2 121.4(5) . . ?
C1 C2 C3 118.6(5) . . ?
C1 C2 C7 115.8(5) . . ?
C7 C2 C3 125.6(5) . . ?
O2 C3 C2 118.8(5) . . ?
O2 C3 C4 117.2(5) . . ?
C2 C3 C4 123.8(5) . . ?
C3 C4 H4 108.3 . . ?
C3 C4 C5 110.6(5) . . ?
C3 C4 C6 109.5(5) . . ?
C5 C4 H4 108.3 . . ?
C6 C4 H4 108.3 . . ?
C6 C4 C5 111.7(5) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O3 C7 C2 117.4(5) . . ?
C19 C7 O3 118.7(5) . . ?
C19 C7 C2 124.0(5) . . ?
O3 C8 C13 111.6(5) . . ?
C9 C8 O3 121.7(5) . . ?
C9 C8 C13 126.7(5) . . ?
C8 C9 C10 120.6(5) . . ?
C8 C9 C18 120.2(5) . . ?
C10 C9 C18 119.1(5) . . ?
O4 C10 C9 120.8(5) . . ?
O4 C10 C11 120.6(5) . . ?
C9 C10 C11 118.6(5) . . ?
C10 C11 C16 106.1(5) . . ?
C10 C11 C17 111.1(5) . . ?
C12 C11 C10 115.7(5) . . ?
C12 C11 C16 105.2(5) . . ?
C12 C11 C17 109.4(5) . . ?
C17 C11 C16 109.1(6) . . ?
O5 C12 C11 120.8(5) . . ?
O5 C12 C13 117.3(5) . . ?
C11 C12 C13 121.8(5) . . ?
C8 C13 C12 112.5(5) . . ?
C8 C13 C14 112.0(4) . . ?
C8 C13 C15 109.1(4) . . ?
C12 C13 C14 106.4(4) . . ?
C15 C13 C12 107.4(5) . . ?
C15 C13 C14 109.4(5) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C11 C17 H17A 109.5 . . ?
C11 C17 H17B 109.5 . . ?
C11 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C9 C18 H18 107.8 . . ?
C9 C18 C19 109.0(4) . . ?
C9 C18 C32 113.6(4) . . ?
C19 C18 H18 107.8 . . ?
C19 C18 C32 110.8(4) . . ?
C32 C18 H18 107.8 . . ?
C7 C19 C18 121.2(5) . . ?
C7 C19 C20 116.1(5) . . ?
C20 C19 C18 122.6(5) . . ?
O6 C20 C19 121.8(5) . . ?
O6 C20 C23 114.5(5) . . ?
C23 C20 C19 123.7(5) . . ?
O6 C21 C22 105.4(4) . . ?
O6 C21 C31 105.3(4) . . ?
C27 C21 O6 105.0(4) . . ?
C27 C21 C22 114.4(5) . . ?
C27 C21 C31 112.0(5) . . ?
C31 C21 C22 113.6(5) . . ?
C21 C22 H22 108.3 . . ?
C23 C22 C21 102.5(4) . . ?
C23 C22 H22 108.3 . . ?
C23 C22 C24 116.5(5) . . ?
C24 C22 C21 112.7(5) . . ?
C24 C22 H22 108.3 . . ?
C1 C23 C22 131.9(5) . . ?
C20 C23 C1 119.0(5) . . ?
C20 C23 C22 109.0(5) . . ?
C22 C24 H24A 109.2 . . ?
C22 C24 H24B 109.2 . . ?
C22 C24 C25 112.2(6) . . ?
H24A C24 H24B 107.9 . . ?
C25 C24 H24A 109.2 . . ?
C25 C24 H24B 109.2 . . ?
C24 C25 H25 106.4 . . ?
C26 C25 C24 108.4(5) . . ?
C26 C25 H25 106.4 . . ?
C26 C25 C28 111.4(6) . . ?
C28 C25 C24 117.1(7) . . ?
C28 C25 H25 106.4 . . ?
C25 C26 H26 118.0 . . ?
C27 C26 C25 123.9(6) . . ?
C27 C26 H26 118.0 . . ?
C21 C27 H27 117.9 . . ?
C26 C27 C21 124.2(6) . . ?
C26 C27 H27 117.9 . . ?
C25 C28 H28 107.5 . . ?
C29 C28 C25 110.7(7) . . ?
C29 C28 H28 107.5 . . ?
C30 C28 C25 109.1(8) . . ?
C30 C28 H28 107.5 . . ?
C30 C28 C29 114.2(8) . . ?
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 . . ?
C21 C31 H31A 109.5 . . ?
C21 C31 H31B 109.5 . . ?
C21 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C18 C32 H32 107.3 . . ?
C33 C32 C18 112.9(5) . . ?
C33 C32 H32 107.3 . . ?
C33 C32 C34 109.0(5) . . ?
C34 C32 C18 112.6(5) . . ?
C34 C32 H32 107.3 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C35 O7 H7 109.5 . . ?
C42 O9 C41 119.0(4) . . ?
C54 O12 C55 107.6(4) . . ?
O7 C35 C36 122.5(5) . . ?
O7 C35 C57 117.6(5) . . ?
C57 C35 C36 119.9(5) . . ?
C35 C36 C37 117.1(5) . . ?
C41 C36 C35 117.5(5) . . ?
C41 C36 C37 125.3(5) . . ?
O8 C37 C36 120.3(5) . . ?
O8 C37 C38 116.4(5) . . ?
C36 C37 C38 123.2(5) . . ?
C37 C38 H38 109.0 . . ?
C37 C38 C39 108.4(5) . . ?
C39 C38 H38 109.0 . . ?
C40 C38 C37 111.7(5) . . ?
C40 C38 H38 109.0 . . ?
C40 C38 C39 109.8(6) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O9 C41 C36 118.2(5) . . ?
O9 C41 C53 118.5(5) . . ?
C53 C41 C36 123.3(5) . . ?
O9 C42 C47 110.4(4) . . ?
C43 C42 O9 121.7(5) . . ?
C43 C42 C47 127.8(5) . . ?
C42 C43 C44 119.7(5) . . ?
C42 C43 C52 121.3(5) . . ?
C44 C43 C52 118.8(5) . . ?
O10 C44 C43 121.0(6) . . ?
O10 C44 C45 119.5(6) . . ?
C43 C44 C45 119.4(5) . . ?
C44 C45 C46 114.3(5) . . ?
C50 C45 C44 115.2(9) . . ?
C50 C45 C46 119.1(9) . . ?
C50 C45 C51 102.9(11) . . ?
C51 C45 C44 101.6(9) . . ?
C51 C45 C46 99.6(9) . . ?
C51A C45 C44 115.8(9) . . ?
C51A C45 C46 117.7(9) . . ?
C51A C45 C50A 98.9(12) . . ?
C50A C45 C44 105.7(10) . . ?
C50A C45 C46 100.7(11) . . ?
O11 C46 C45 118.1(6) . . ?
O11 C46 C47 119.2(6) . . ?
C45 C46 C47 122.7(5) . . ?
C42 C47 C46 112.1(5) . . ?
C42 C47 C48 112.4(4) . . ?
C42 C47 C49 108.5(5) . . ?
C46 C47 C48 107.3(5) . . ?
C46 C47 C49 106.4(5) . . ?
C49 C47 C48 110.1(5) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C45 C50 H50A 109.5 . . ?
C45 C50 H50B 109.5 . . ?
C45 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C45 C51 H51A 109.5 . . ?
C45 C51 H51B 109.5 . . ?
C45 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C43 C52 H52 108.4 . . ?
C43 C52 C66 112.6(4) . . ?
C53 C52 C43 108.6(4) . . ?
C53 C52 H52 108.4 . . ?
C53 C52 C66 110.4(5) . . ?
C66 C52 H52 108.4 . . ?
C41 C53 C52 121.6(5) . . ?
C41 C53 C54 115.8(5) . . ?
C54 C53 C52 122.5(5) . . ?
O12 C54 C53 122.5(5) . . ?
O12 C54 C57 113.9(5) . . ?
C57 C54 C53 123.6(5) . . ?
O12 C55 C56 104.4(4) . . ?
O12 C55 C61 105.0(4) . . ?
O12 C55 C65 107.5(5) . . ?
C61 C55 C56 111.0(5) . . ?
C65 C55 C56 113.8(5) . . ?
C65 C55 C61 114.2(5) . . ?
C55 C56 H56 108.2 . . ?
C57 C56 C55 101.1(4) . . ?
C57 C56 H56 108.2 . . ?
C57 C56 C58 117.9(5) . . ?
C58 C56 C55 112.7(5) . . ?
C58 C56 H56 108.2 . . ?
C35 C57 C56 132.0(5) . . ?
C54 C57 C35 119.7(5) . . ?
C54 C57 C56 108.2(5) . . ?
C56 C58 H58A 109.1 . . ?
C56 C58 H58B 109.1 . . ?
C56 C58 C59 112.5(5) . . ?
H58A C58 H58B 107.8 . . ?
C59 C58 H58A 109.1 . . ?
C59 C58 H58B 109.1 . . ?
C58 C59 H59 107.6 . . ?
C58 C59 C62 113.4(5) . . ?
C60 C59 C58 108.9(5) . . ?
C60 C59 H59 107.6 . . ?
C60 C59 C62 111.6(5) . . ?
C62 C59 H59 107.6 . . ?
C59 C60 H60 117.4 . . ?
C61 C60 C59 125.2(6) . . ?
C61 C60 H60 117.4 . . ?
C55 C61 H61 117.5 . . ?
C60 C61 C55 125.1(6) . . ?
C60 C61 H61 117.5 . . ?
C59 C62 H62 106.8 . . ?
C63 C62 C59 111.4(6) . . ?
C63 C62 H62 106.8 . . ?
C63 C62 C64 110.8(5) . . ?
C64 C62 C59 113.8(5) . . ?
C64 C62 H62 106.8 . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C62 C64 H64A 109.5 . . ?
C62 C64 H64B 109.5 . . ?
C62 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C55 C65 H65A 109.5 . . ?
C55 C65 H65B 109.5 . . ?
C55 C65 H65C 109.5 . . ?
H65A C65 H65B 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C52 C66 H66 106.9 . . ?
C67 C66 C52 113.5(5) . . ?
C67 C66 H66 106.9 . . ?
C67 C66 C68 109.5(5) . . ?
C68 C66 C52 112.7(5) . . ?
C68 C66 H66 106.9 . . ?
C66 C67 H67A 109.5 . . ?
C66 C67 H67B 109.5 . . ?
C66 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C66 C68 H68A 109.5 . . ?
C66 C68 H68B 109.5 . . ?
C66 C68 H68C 109.5 . . ?
H68A C68 H68B 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C69 O13 H13 109.5 . . ?
C76 O15 C75 118.1(4) . . ?
C88 O18 C89 106.9(4) . . ?
O13 C69 C70 121.0(5) . . ?
O13 C69 C91 117.9(5) . . ?
C91 C69 C70 121.1(5) . . ?
C69 C70 C71 117.5(5) . . ?
C69 C70 C75 115.2(5) . . ?
C75 C70 C71 127.3(5) . . ?
O14 C71 C70 120.7(6) . . ?
O14 C71 C72 114.9(6) . . ?
C70 C71 C72 123.9(6) . . ?
C71 C72 H72 111.6 . . ?
C71 C72 C74 105.0(8) . . ?
C73 C72 C71 111.0(7) . . ?
C73 C72 H72 111.6 . . ?
C73 C72 C74 105.6(7) . . ?
C74 C72 H72 111.6 . . ?
C72 C73 H73A 109.5 . . ?
C72 C73 H73B 109.5 . . ?
C72 C73 H73C 109.5 . . ?
H73A C73 H73B 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C72 C74 H74A 109.5 . . ?
C72 C74 H74B 109.5 . . ?
C72 C74 H74C 109.5 . . ?
H74A C74 H74B 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
O15 C75 C70 115.4(5) . . ?
C87 C75 O15 119.6(5) . . ?
C87 C75 C70 124.9(5) . . ?
O15 C76 C81 110.8(5) . . ?
C77 C76 O15 122.9(5) . . ?
C77 C76 C81 126.3(6) . . ?
C76 C77 C78 119.5(5) . . ?
C76 C77 C86 121.3(5) . . ?
C78 C77 C86 118.9(5) . . ?
O16 C78 C77 120.7(6) . . ?
O16 C78 C79 118.1(6) . . ?
C77 C78 C79 121.2(5) . . ?
C78 C79 C84 108.2(6) . . ?
C80 C79 C78 113.3(5) . . ?
C80 C79 C84 108.1(6) . . ?
C80 C79 C85 108.7(6) . . ?
C85 C79 C78 107.7(6) . . ?
C85 C79 C84 110.9(7) . . ?
O17 C80 C79 120.4(7) . . ?
O17 C80 C81 118.1(7) . . ?
C79 C80 C81 121.3(6) . . ?
C76 C81 C80 110.8(5) . . ?
C76 C81 C82 108.7(5) . . ?
C76 C81 C83 110.8(5) . . ?
C80 C81 C82 108.7(6) . . ?
C80 C81 C83 108.5(6) . . ?
C83 C81 C82 109.2(6) . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82B 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C81 C83 H83A 109.5 . . ?
C81 C83 H83B 109.5 . . ?
C81 C83 H83C 109.5 . . ?
H83A C83 H83B 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
C79 C84 H84A 109.5 . . ?
C79 C84 H84B 109.5 . . ?
C79 C84 H84C 109.5 . . ?
H84A C84 H84B 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
C79 C85 H85A 109.5 . . ?
C79 C85 H85B 109.5 . . ?
C79 C85 H85C 109.5 . . ?
H85A C85 H85B 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
C77 C86 H86 108.4 . . ?
C77 C86 C100 112.1(5) . . ?
C87 C86 C77 107.7(5) . . ?
C87 C86 H86 108.4 . . ?
C87 C86 C100 111.6(4) . . ?
C100 C86 H86 108.4 . . ?
C75 C87 C86 123.5(5) . . ?
C75 C87 C88 115.7(5) . . ?
C88 C87 C86 120.8(5) . . ?
O18 C88 C87 122.1(5) . . ?
O18 C88 C91 114.6(5) . . ?
C91 C88 C87 123.3(5) . . ?
O18 C89 C90 104.7(4) . . ?
O18 C89 C99 106.5(4) . . ?
C95 C89 O18 105.5(4) . . ?
C95 C89 C90 112.4(5) . . ?
C95 C89 C99 112.8(5) . . ?
C99 C89 C90 114.1(5) . . ?
C89 C90 H90 109.2 . . ?
C91 C90 C89 100.8(4) . . ?
C91 C90 H90 109.2 . . ?
C91 C90 C92 116.2(5) . . ?
C92 C90 C89 112.0(4) . . ?
C92 C90 H90 109.2 . . ?
C69 C91 C88 119.5(5) . . ?
C69 C91 C90 131.7(5) . . ?
C88 C91 C90 108.4(5) . . ?
C90 C92 H92A 108.8 . . ?
C90 C92 H92B 108.8 . . ?
H92A C92 H92B 107.7 . . ?
C93 C92 C90 113.8(5) . . ?
C93 C92 H92A 108.8 . . ?
C93 C92 H92B 108.8 . . ?
C92 C93 H93 106.5 . . ?
C92 C93 C96 115.4(5) . . ?
C94 C93 C92 109.4(5) . . ?
C94 C93 H93 106.5 . . ?
C94 C93 C96 111.8(5) . . ?
C96 C93 H93 106.5 . . ?
C93 C94 H94 117.8 . . ?
C95 C94 C93 124.4(5) . . ?
C95 C94 H94 117.8 . . ?
C89 C95 H95 117.7 . . ?
C94 C95 C89 124.6(5) . . ?
C94 C95 H95 117.7 . . ?
C93 C96 H96 107.0 . . ?
C93 C96 C97 112.4(5) . . ?
C97 C96 H96 107.0 . . ?
C98 C96 C93 112.4(6) . . ?
C98 C96 H96 107.0 . . ?
C98 C96 C97 110.8(6) . . ?
C96 C97 H97A 109.5 . . ?
C96 C97 H97B 109.5 . . ?
C96 C97 H97C 109.5 . . ?
H97A C97 H97B 109.5 . . ?
H97A C97 H97C 109.5 . . ?
H97B C97 H97C 109.5 . . ?
C96 C98 H98A 109.5 . . ?
C96 C98 H98B 109.5 . . ?
C96 C98 H98C 109.5 . . ?
H98A C98 H98B 109.5 . . ?
H98A C98 H98C 109.5 . . ?
H98B C98 H98C 109.5 . . ?
C89 C99 H99A 109.5 . . ?
C89 C99 H99B 109.5 . . ?
C89 C99 H99C 109.5 . . ?
H99A C99 H99B 109.5 . . ?
H99A C99 H99C 109.5 . . ?
H99B C99 H99C 109.5 . . ?
C86 C100 H100 107.4 . . ?
C101 C100 C86 112.1(5) . . ?
C101 C100 H100 107.4 . . ?
C101 C100 C102 110.7(6) . . ?
C102 C100 C86 111.7(5) . . ?
C102 C100 H100 107.4 . . ?
C100 C101 H10A 109.5 . . ?
C100 C101 H10B 109.5 . . ?
C100 C101 H10C 109.5 . . ?
H10A C101 H10B 109.5 . . ?
H10A C101 H10C 109.5 . . ?
H10B C101 H10C 109.5 . . ?
C100 C102 H10D 109.5 . . ?
C100 C102 H10E 109.5 . . ?
C100 C102 H10F 109.5 . . ?
H10D C102 H10E 109.5 . . ?
H10D C102 H10F 109.5 . . ?
H10E C102 H10F 109.5 . . ?
C103 O19 H19 109.5 . . ?
C110 O21 C109 119.0(4) . . ?
C122 O24 C123 106.7(4) . . ?
O19 C103 C104 121.6(5) . . ?
O19 C103 C125 118.4(5) . . ?
C125 C103 C104 120.0(5) . . ?
C103 C104 C105 116.8(5) . . ?
C109 C104 C103 116.1(5) . . ?
C109 C104 C105 127.0(5) . . ?
O20 C105 C104 119.8(6) . . ?
O20 C105 C106 115.3(6) . . ?
C104 C105 C106 124.6(5) . . ?
C105 C106 H106 110.1 . . ?
C105 C106 C107 108.5(6) . . ?
C105 C106 C108 109.3(7) . . ?
C107 C106 H106 110.1 . . ?
C107 C106 C108 108.8(7) . . ?
C108 C106 H106 110.1 . . ?
C106 C107 H10G 109.5 . . ?
C106 C107 H10H 109.5 . . ?
C106 C107 H10I 109.5 . . ?
H10G C107 H10H 109.5 . . ?
H10G C107 H10I 109.5 . . ?
H10H C107 H10I 109.5 . . ?
C106 C108 H10J 109.5 . . ?
C106 C108 H10K 109.5 . . ?
C106 C108 H10L 109.5 . . ?
H10J C108 H10K 109.5 . . ?
H10J C108 H10L 109.5 . . ?
H10K C108 H10L 109.5 . . ?
O21 C109 C104 116.6(5) . . ?
C121 C109 O21 118.8(5) . . ?
C121 C109 C104 124.5(5) . . ?
O21 C110 C115 110.9(5) . . ?
C111 C110 O21 123.0(5) . . ?
C111 C110 C115 126.0(5) . . ?
C110 C111 C112 118.8(5) . . ?
C110 C111 C120 121.4(5) . . ?
C112 C111 C120 119.3(5) . . ?
O22 C112 C111 120.3(5) . . ?
O22 C112 C113 121.3(6) . . ?
C111 C112 C113 118.4(5) . . ?
C112 C113 C118 109.2(6) . . ?
C112 C113 C119 106.1(5) . . ?
C114 C113 C112 114.7(5) . . ?
C114 C113 C118 109.6(6) . . ?
C114 C113 C119 107.9(6) . . ?
C118 C113 C119 109.1(6) . . ?
O23 C114 C113 120.4(6) . . ?
O23 C114 C115 118.7(6) . . ?
C113 C114 C115 120.8(5) . . ?
C110 C115 C114 110.2(5) . . ?
C110 C115 C116 110.1(5) . . ?
C110 C115 C117 110.4(6) . . ?
C114 C115 C116 107.7(5) . . ?
C114 C115 C117 108.7(5) . . ?
C117 C115 C116 109.7(6) . . ?
C115 C116 H11A 109.5 . . ?
C115 C116 H11B 109.5 . . ?
C115 C116 H11C 109.5 . . ?
H11A C116 H11B 109.5 . . ?
H11A C116 H11C 109.5 . . ?
H11B C116 H11C 109.5 . . ?
C115 C117 H11D 109.5 . . ?
C115 C117 H11E 109.5 . . ?
C115 C117 H11F 109.5 . . ?
H11D C117 H11E 109.5 . . ?
H11D C117 H11F 109.5 . . ?
H11E C117 H11F 109.5 . . ?
C113 C118 H11G 109.5 . . ?
C113 C118 H11H 109.5 . . ?
C113 C118 H11I 109.5 . . ?
H11G C118 H11H 109.5 . . ?
H11G C118 H11I 109.5 . . ?
H11H C118 H11I 109.5 . . ?
C113 C119 H11J 109.5 . . ?
C113 C119 H11K 109.5 . . ?
C113 C119 H11L 109.5 . . ?
H11J C119 H11K 109.5 . . ?
H11J C119 H11L 109.5 . . ?
H11K C119 H11L 109.5 . . ?
C111 C120 H120 107.8 . . ?
C111 C120 C121 108.1(4) . . ?
C111 C120 C134 113.8(4) . . ?
C121 C120 H120 107.8 . . ?
C121 C120 C134 111.5(5) . . ?
C134 C120 H120 107.8 . . ?
C109 C121 C120 124.0(5) . . ?
C109 C121 C122 115.1(5) . . ?
C122 C121 C120 120.9(5) . . ?
O24 C122 C121 122.0(5) . . ?
O24 C122 C125 114.3(5) . . ?
C125 C122 C121 123.7(5) . . ?
O24 C123 C124 103.8(4) . . ?
O24 C123 C129 105.0(4) . . ?
O24 C123 C133 106.9(5) . . ?
C129 C123 C124 111.7(5) . . ?
C133 C123 C124 115.0(5) . . ?
C133 C123 C129 113.3(5) . . ?
C123 C124 H124 108.6 . . ?
C125 C124 C123 101.7(4) . . ?
C125 C124 H124 108.6 . . ?
C125 C124 C126 117.1(5) . . ?
C126 C124 C123 111.8(5) . . ?
C126 C124 H124 108.6 . . ?
C103 C125 C124 131.3(5) . . ?
C122 C125 C103 120.4(5) . . ?
C122 C125 C124 108.1(5) . . ?
C124 C126 H12A 109.4 . . ?
C124 C126 H12B 109.4 . . ?
H12A C126 H12B 108.0 . . ?
C127 C126 C124 111.1(5) . . ?
C127 C126 H12A 109.4 . . ?
C127 C126 H12B 109.4 . . ?
C126 C127 H127 107.0 . . ?
C126 C127 C130 114.4(5) . . ?
C128 C127 C126 109.5(5) . . ?
C128 C127 H127 107.0 . . ?
C128 C127 C130 111.4(5) . . ?
C130 C127 H127 107.0 . . ?
C127 C128 H128 118.1 . . ?
C129 C128 C127 123.9(6) . . ?
C129 C128 H128 118.1 . . ?
C123 C129 H129 117.7 . . ?
C128 C129 C123 124.6(6) . . ?
C128 C129 H129 117.7 . . ?
C127 C130 H130 107.3 . . ?
C131 C130 C127 112.4(6) . . ?
C131 C130 H130 107.3 . . ?
C131 C130 C132 110.2(7) . . ?
C132 C130 C127 111.9(6) . . ?
C132 C130 H130 107.3 . . ?
C130 C131 H13A 109.5 . . ?
C130 C131 H13B 109.5 . . ?
C130 C131 H13C 109.5 . . ?
H13A C131 H13B 109.5 . . ?
H13A C131 H13C 109.5 . . ?
H13B C131 H13C 109.5 . . ?
C130 C132 H13D 109.5 . . ?
C130 C132 H13E 109.5 . . ?
C130 C132 H13F 109.5 . . ?
H13D C132 H13E 109.5 . . ?
H13D C132 H13F 109.5 . . ?
H13E C132 H13F 109.5 . . ?
C123 C133 H13G 109.5 . . ?
C123 C133 H13H 109.5 . . ?
C123 C133 H13I 109.5 . . ?
H13G C133 H13H 109.5 . . ?
H13G C133 H13I 109.5 . . ?
H13H C133 H13I 109.5 . . ?
C120 C134 H134 107.2 . . ?
C135 C134 C120 112.2(5) . . ?
C135 C134 H134 107.2 . . ?
C136 C134 C120 111.5(5) . . ?
C136 C134 H134 107.2 . . ?
C136 C134 C135 111.3(5) . . ?
C134 C135 H13J 109.5 . . ?
C134 C135 H13K 109.5 . . ?
C134 C135 H13L 109.5 . . ?
H13J C135 H13K 109.5 . . ?
H13J C135 H13L 109.5 . . ?
H13K C135 H13L 109.5 . . ?
C134 C136 H13M 109.5 . . ?
C134 C136 H13N 109.5 . . ?
C134 C136 H13O 109.5 . . ?
H13M C136 H13N 109.5 . . ?
H13M C136 H13O 109.5 . . ?
H13N C136 H13O 109.5 . . ?
C45 C51A H51D 109.5 . . ?
C45 C51A H51E 109.5 . . ?
C45 C51A H51F 109.5 . . ?
H51D C51A H51E 109.5 . . ?
H51D C51A H51F 109.5 . . ?
H51E C51A H51F 109.5 . . ?
C45 C50A H50D 109.5 . . ?
C45 C50A H50E 109.5 . . ?
C45 C50A H50F 109.5 . . ?
H50D C50A H50E 109.5 . . ?
H50D C50A H50F 109.5 . . ?
H50E C50A H50F 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -6.0(7) . . . . ?
O1 C1 C2 C7 176.2(5) . . . . ?
O1 C1 C23 C20 -178.4(5) . . . . ?
O1 C1 C23 C22 -2.9(8) . . . . ?
O2 C3 C4 C5 20.4(7) . . . . ?
O2 C3 C4 C6 -103.2(6) . . . . ?
O3 C7 C19 C18 -7.9(7) . . . . ?
O3 C7 C19 C20 175.7(4) . . . . ?
O3 C8 C9 C10 -170.0(5) . . . . ?
O3 C8 C9 C18 6.5(7) . . . . ?
O3 C8 C13 C12 175.8(4) . . . . ?
O3 C8 C13 C14 56.0(6) . . . . ?
O3 C8 C13 C15 -65.2(6) . . . . ?
O4 C10 C11 C12 -159.3(5) . . . . ?
O4 C10 C11 C16 84.6(7) . . . . ?
O4 C10 C11 C17 -33.9(8) . . . . ?
O5 C12 C13 C8 -174.4(5) . . . . ?
O5 C12 C13 C14 -51.4(7) . . . . ?
O5 C12 C13 C15 65.6(7) . . . . ?
O6 C20 C23 C1 178.8(5) . . . . ?
O6 C20 C23 C22 2.3(6) . . . . ?
O6 C21 C22 C23 10.8(5) . . . . ?
O6 C21 C22 C24 136.8(5) . . . . ?
O6 C21 C27 C26 -109.8(7) . . . . ?
C1 C2 C3 O2 7.1(8) . . . . ?
C1 C2 C3 C4 -167.8(5) . . . . ?
C1 C2 C7 O3 -175.1(4) . . . . ?
C1 C2 C7 C19 4.9(7) . . . . ?
C2 C1 C23 C20 0.9(8) . . . . ?
C2 C1 C23 C22 176.4(5) . . . . ?
C2 C3 C4 C5 -164.6(5) . . . . ?
C2 C3 C4 C6 71.8(7) . . . . ?
C2 C7 C19 C18 172.1(5) . . . . ?
C2 C7 C19 C20 -4.3(8) . . . . ?
C3 C2 C7 O3 7.3(7) . . . . ?
C3 C2 C7 C19 -172.7(5) . . . . ?
C7 O3 C8 C9 20.0(7) . . . . ?
C7 O3 C8 C13 -162.6(4) . . . . ?
C7 C2 C3 O2 -175.4(5) . . . . ?
C7 C2 C3 C4 9.7(8) . . . . ?
C7 C19 C20 O6 -177.1(5) . . . . ?
C7 C19 C20 C23 1.9(8) . . . . ?
C8 O3 C7 C2 160.9(4) . . . . ?
C8 O3 C7 C19 -19.1(7) . . . . ?
C8 C9 C10 O4 160.9(5) . . . . ?
C8 C9 C10 C11 -20.4(8) . . . . ?
C8 C9 C18 C19 -29.9(7) . . . . ?
C8 C9 C18 C32 94.1(6) . . . . ?
C9 C8 C13 C12 -7.0(7) . . . . ?
C9 C8 C13 C14 -126.7(6) . . . . ?
C9 C8 C13 C15 112.1(6) . . . . ?
C9 C10 C11 C12 22.0(7) . . . . ?
C9 C10 C11 C16 -94.1(6) . . . . ?
C9 C10 C11 C17 147.5(6) . . . . ?
C9 C18 C19 C7 30.7(7) . . . . ?
C9 C18 C19 C20 -153.1(5) . . . . ?
C9 C18 C32 C33 -66.8(6) . . . . ?
C9 C18 C32 C34 57.2(6) . . . . ?
C10 C9 C18 C19 146.7(5) . . . . ?
C10 C9 C18 C32 -89.3(6) . . . . ?
C10 C11 C12 O5 166.7(6) . . . . ?
C10 C11 C12 C13 -17.2(8) . . . . ?
C11 C12 C13 C8 9.3(7) . . . . ?
C11 C12 C13 C14 132.3(5) . . . . ?
C11 C12 C13 C15 -110.7(6) . . . . ?
C13 C8 C9 C10 13.0(8) . . . . ?
C13 C8 C9 C18 -170.5(5) . . . . ?
C16 C11 C12 O5 -76.6(7) . . . . ?
C16 C11 C12 C13 99.5(6) . . . . ?
C17 C11 C12 O5 40.4(8) . . . . ?
C17 C11 C12 C13 -143.5(6) . . . . ?
C18 C9 C10 O4 -15.7(8) . . . . ?
C18 C9 C10 C11 163.0(5) . . . . ?
C18 C19 C20 O6 6.5(8) . . . . ?
C18 C19 C20 C23 -174.5(5) . . . . ?
C19 C18 C32 C33 56.2(6) . . . . ?
C19 C18 C32 C34 -179.8(5) . . . . ?
C19 C20 C23 C1 -0.2(8) . . . . ?
C19 C20 C23 C22 -176.7(5) . . . . ?
C20 O6 C21 C22 -10.1(5) . . . . ?
C20 O6 C21 C27 111.1(5) . . . . ?
C20 O6 C21 C31 -130.5(5) . . . . ?
C21 O6 C20 C19 -175.9(5) . . . . ?
C21 O6 C20 C23 5.1(6) . . . . ?
C21 C22 C23 C1 175.8(5) . . . . ?
C21 C22 C23 C20 -8.3(6) . . . . ?
C21 C22 C24 C25 -52.1(7) . . . . ?
C22 C21 C27 C26 5.2(9) . . . . ?
C22 C24 C25 C26 53.6(7) . . . . ?
C22 C24 C25 C28 -179.4(6) . . . . ?
C23 C1 C2 C3 174.8(5) . . . . ?
C23 C1 C2 C7 -3.0(7) . . . . ?
C23 C22 C24 C25 66.0(7) . . . . ?
C24 C22 C23 C1 52.3(8) . . . . ?
C24 C22 C23 C20 -131.8(5) . . . . ?
C24 C25 C26 C27 -27.7(10) . . . . ?
C24 C25 C28 C29 -59.2(10) . . . . ?
C24 C25 C28 C30 67.3(10) . . . . ?
C25 C26 C27 C21 -1.7(11) . . . . ?
C26 C25 C28 C29 66.4(9) . . . . ?
C26 C25 C28 C30 -167.2(8) . . . . ?
C27 C21 C22 C23 -104.0(5) . . . . ?
C27 C21 C22 C24 22.1(7) . . . . ?
C28 C25 C26 C27 -158.0(7) . . . . ?
C31 C21 C22 C23 125.6(5) . . . . ?
C31 C21 C22 C24 -108.4(6) . . . . ?
C31 C21 C27 C26 136.4(7) . . . . ?
C32 C18 C19 C7 -95.0(6) . . . . ?
C32 C18 C19 C20 81.2(6) . . . . ?
O7 C35 C36 C37 -5.9(8) . . . . ?
O7 C35 C36 C41 176.9(5) . . . . ?
O7 C35 C57 C54 -179.5(5) . . . . ?
O7 C35 C57 C56 -3.1(9) . . . . ?
O8 C37 C38 C39 -105.1(6) . . . . ?
O8 C37 C38 C40 16.0(8) . . . . ?
O9 C41 C53 C52 -8.6(8) . . . . ?
O9 C41 C53 C54 175.1(5) . . . . ?
O9 C42 C43 C44 -170.8(5) . . . . ?
O9 C42 C43 C52 3.5(8) . . . . ?
O9 C42 C47 C46 179.8(4) . . . . ?
O9 C42 C47 C48 58.9(6) . . . . ?
O9 C42 C47 C49 -63.0(6) . . . . ?
O10 C44 C45 C46 -160.5(6) . . . . ?
O10 C44 C45 C50 -17.2(12) . . . . ?
O10 C44 C45 C51 93.3(10) . . . . ?
O10 C44 C45 C51A 57.6(13) . . . . ?
O10 C44 C45 C50A -50.7(12) . . . . ?
O11 C46 C47 C42 -176.7(6) . . . . ?
O11 C46 C47 C48 -52.9(8) . . . . ?
O11 C46 C47 C49 64.9(8) . . . . ?
O12 C54 C57 C35 179.6(5) . . . . ?
O12 C54 C57 C56 2.4(7) . . . . ?
O12 C55 C56 C57 20.7(5) . . . . ?
O12 C55 C56 C58 147.5(5) . . . . ?
O12 C55 C61 C60 -117.6(6) . . . . ?
C35 C36 C37 O8 7.7(8) . . . . ?
C35 C36 C37 C38 -168.2(5) . . . . ?
C35 C36 C41 O9 -174.7(5) . . . . ?
C35 C36 C41 C53 5.1(8) . . . . ?
C36 C35 C57 C54 -0.1(8) . . . . ?
C36 C35 C57 C56 176.3(6) . . . . ?
C36 C37 C38 C39 70.9(7) . . . . ?
C36 C37 C38 C40 -168.0(6) . . . . ?
C36 C41 C53 C52 171.6(5) . . . . ?
C36 C41 C53 C54 -4.7(8) . . . . ?
C37 C36 C41 O9 8.4(8) . . . . ?
C37 C36 C41 C53 -171.8(5) . . . . ?
C41 O9 C42 C43 20.5(7) . . . . ?
C41 O9 C42 C47 -162.8(4) . . . . ?
C41 C36 C37 O8 -175.4(6) . . . . ?
C41 C36 C37 C38 8.7(9) . . . . ?
C41 C53 C54 O12 -177.2(5) . . . . ?
C41 C53 C54 C57 1.8(8) . . . . ?
C42 O9 C41 C36 162.2(5) . . . . ?
C42 O9 C41 C53 -17.6(7) . . . . ?
C42 C43 C44 O10 160.0(6) . . . . ?
C42 C43 C44 C45 -22.5(8) . . . . ?
C42 C43 C52 C53 -26.2(7) . . . . ?
C42 C43 C52 C66 96.3(6) . . . . ?
C43 C42 C47 C46 -3.8(8) . . . . ?
C43 C42 C47 C48 -124.7(6) . . . . ?
C43 C42 C47 C49 113.4(6) . . . . ?
C43 C44 C45 C46 22.0(9) . . . . ?
C43 C44 C45 C50 165.3(10) . . . . ?
C43 C44 C45 C51 -84.3(10) . . . . ?
C43 C44 C45 C51A -119.9(11) . . . . ?
C43 C44 C45 C50A 131.8(11) . . . . ?
C43 C52 C53 C41 28.7(7) . . . . ?
C43 C52 C53 C54 -155.3(5) . . . . ?
C43 C52 C66 C67 -66.3(7) . . . . ?
C43 C52 C66 C68 58.9(6) . . . . ?
C44 C43 C52 C53 148.2(5) . . . . ?
C44 C43 C52 C66 -89.3(6) . . . . ?
C44 C45 C46 O11 167.5(7) . . . . ?
C44 C45 C46 C47 -13.3(9) . . . . ?
C45 C46 C47 C42 4.2(8) . . . . ?
C45 C46 C47 C48 128.0(6) . . . . ?
C45 C46 C47 C49 -114.2(6) . . . . ?
C47 C42 C43 C44 13.1(8) . . . . ?
C47 C42 C43 C52 -172.6(5) . . . . ?
C50 C45 C46 O11 25.7(13) . . . . ?
C50 C45 C46 C47 -155.2(10) . . . . ?
C51 C45 C46 O11 -85.0(10) . . . . ?
C51 C45 C46 C47 94.1(10) . . . . ?
C52 C43 C44 O10 -14.4(9) . . . . ?
C52 C43 C44 C45 163.0(5) . . . . ?
C52 C53 C54 O12 6.5(9) . . . . ?
C52 C53 C54 C57 -174.4(5) . . . . ?
C53 C52 C66 C67 55.2(7) . . . . ?
C53 C52 C66 C68 -179.6(5) . . . . ?
C53 C54 C57 C35 0.5(9) . . . . ?
C53 C54 C57 C56 -176.7(5) . . . . ?
C54 O12 C55 C56 -20.6(6) . . . . ?
C54 O12 C55 C61 96.2(5) . . . . ?
C54 O12 C55 C65 -141.8(5) . . . . ?
C55 O12 C54 C53 -168.9(5) . . . . ?
C55 O12 C54 C57 12.0(6) . . . . ?
C55 C56 C57 C35 168.6(6) . . . . ?
C55 C56 C57 C54 -14.7(6) . . . . ?
C55 C56 C58 C59 -58.0(7) . . . . ?
C56 C55 C61 C60 -5.3(8) . . . . ?
C56 C58 C59 C60 47.6(7) . . . . ?
C56 C58 C59 C62 172.5(5) . . . . ?
C57 C35 C36 C37 174.7(5) . . . . ?
C57 C35 C36 C41 -2.5(8) . . . . ?
C57 C56 C58 C59 59.3(7) . . . . ?
C58 C56 C57 C35 45.3(9) . . . . ?
C58 C56 C57 C54 -138.0(5) . . . . ?
C58 C59 C60 C61 -18.5(9) . . . . ?
C58 C59 C62 C63 56.6(7) . . . . ?
C58 C59 C62 C64 -69.6(8) . . . . ?
C59 C60 C61 C55 -2.6(10) . . . . ?
C60 C59 C62 C63 -180.0(5) . . . . ?
C60 C59 C62 C64 53.8(7) . . . . ?
C61 C55 C56 C57 -91.9(5) . . . . ?
C61 C55 C56 C58 34.8(6) . . . . ?
C62 C59 C60 C61 -144.4(6) . . . . ?
C65 C55 C56 C57 137.5(5) . . . . ?
C65 C55 C56 C58 -95.7(6) . . . . ?
C65 C55 C61 C60 124.9(7) . . . . ?
C66 C52 C53 C41 -95.2(6) . . . . ?
C66 C52 C53 C54 80.9(7) . . . . ?
O13 C69 C70 C71 -4.4(8) . . . . ?
O13 C69 C70 C75 175.5(5) . . . . ?
O13 C69 C91 C88 -176.6(5) . . . . ?
O13 C69 C91 C90 -5.4(9) . . . . ?
O14 C71 C72 C73 57.1(10) . . . . ?
O14 C71 C72 C74 -56.5(8) . . . . ?
O15 C75 C87 C86 -4.0(8) . . . . ?
O15 C75 C87 C88 176.8(4) . . . . ?
O15 C76 C77 C78 -165.1(5) . . . . ?
O15 C76 C77 C86 8.8(9) . . . . ?
O15 C76 C81 C80 -171.6(5) . . . . ?
O15 C76 C81 C82 -52.2(7) . . . . ?
O15 C76 C81 C83 67.8(7) . . . . ?
O16 C78 C79 C80 -178.2(6) . . . . ?
O16 C78 C79 C84 -58.3(9) . . . . ?
O16 C78 C79 C85 61.6(8) . . . . ?
O17 C80 C81 C76 156.3(7) . . . . ?
O17 C80 C81 C82 36.8(10) . . . . ?
O17 C80 C81 C83 -81.9(9) . . . . ?
O18 C88 C91 C69 178.0(5) . . . . ?
O18 C88 C91 C90 4.9(6) . . . . ?
O18 C89 C90 C91 20.9(5) . . . . ?
O18 C89 C90 C92 145.1(4) . . . . ?
O18 C89 C95 C94 -116.4(6) . . . . ?
C69 C70 C71 O14 12.8(8) . . . . ?
C69 C70 C71 C72 -158.6(7) . . . . ?
C69 C70 C75 O15 -174.0(4) . . . . ?
C69 C70 C75 C87 3.5(8) . . . . ?
C70 C69 C91 C88 4.0(8) . . . . ?
C70 C69 C91 C90 175.2(5) . . . . ?
C70 C71 C72 C73 -131.0(8) . . . . ?
C70 C71 C72 C74 115.3(7) . . . . ?
C70 C75 C87 C86 178.7(5) . . . . ?
C70 C75 C87 C88 -0.6(8) . . . . ?
C71 C70 C75 O15 5.8(8) . . . . ?
C71 C70 C75 C87 -176.7(5) . . . . ?
C75 O15 C76 C77 13.7(8) . . . . ?
C75 O15 C76 C81 -165.7(5) . . . . ?
C75 C70 C71 O14 -167.0(6) . . . . ?
C75 C70 C71 C72 21.6(10) . . . . ?
C75 C87 C88 O18 -179.6(5) . . . . ?
C75 C87 C88 C91 -0.9(7) . . . . ?
C76 O15 C75 C70 161.6(5) . . . . ?
C76 O15 C75 C87 -16.0(7) . . . . ?
C76 C77 C78 O16 159.6(6) . . . . ?
C76 C77 C78 C79 -19.7(9) . . . . ?
C76 C77 C86 C87 -25.3(7) . . . . ?
C76 C77 C86 C100 97.9(6) . . . . ?
C77 C76 C81 C80 9.0(9) . . . . ?
C77 C76 C81 C82 128.4(7) . . . . ?
C77 C76 C81 C83 -111.5(7) . . . . ?
C77 C78 C79 C80 1.1(9) . . . . ?
C77 C78 C79 C84 121.0(7) . . . . ?
C77 C78 C79 C85 -119.1(7) . . . . ?
C77 C86 C87 C75 23.0(7) . . . . ?
C77 C86 C87 C88 -157.8(5) . . . . ?
C77 C86 C100 C101 64.4(7) . . . . ?
C77 C86 C100 C102 -60.5(7) . . . . ?
C78 C77 C86 C87 148.7(5) . . . . ?
C78 C77 C86 C100 -88.1(6) . . . . ?
C78 C79 C80 O17 -161.2(8) . . . . ?
C78 C79 C80 C81 23.3(10) . . . . ?
C79 C80 C81 C76 -28.1(9) . . . . ?
C79 C80 C81 C82 -147.5(7) . . . . ?
C79 C80 C81 C83 93.7(8) . . . . ?
C81 C76 C77 C78 14.2(9) . . . . ?
C81 C76 C77 C86 -171.9(5) . . . . ?
C84 C79 C80 O17 78.9(10) . . . . ?
C84 C79 C80 C81 -96.6(8) . . . . ?
C85 C79 C80 O17 -41.5(10) . . . . ?
C85 C79 C80 C81 142.9(7) . . . . ?
C86 C77 C78 O16 -14.5(9) . . . . ?
C86 C77 C78 C79 166.2(6) . . . . ?
C86 C87 C88 O18 1.2(7) . . . . ?
C86 C87 C88 C91 179.9(5) . . . . ?
C87 C86 C100 C101 -174.6(5) . . . . ?
C87 C86 C100 C102 60.5(7) . . . . ?
C87 C88 C91 C69 -0.8(8) . . . . ?
C87 C88 C91 C90 -173.9(5) . . . . ?
C88 O18 C89 C90 -19.4(5) . . . . ?
C88 O18 C89 C95 99.3(5) . . . . ?
C88 O18 C89 C99 -140.6(5) . . . . ?
C89 O18 C88 C87 -171.6(4) . . . . ?
C89 O18 C88 C91 9.6(6) . . . . ?
C89 C90 C91 C69 171.9(6) . . . . ?
C89 C90 C91 C88 -16.2(5) . . . . ?
C89 C90 C92 C93 -56.1(6) . . . . ?
C90 C89 C95 C94 -2.9(8) . . . . ?
C90 C92 C93 C94 48.8(6) . . . . ?
C90 C92 C93 C96 175.9(5) . . . . ?
C91 C69 C70 C71 175.1(5) . . . . ?
C91 C69 C70 C75 -5.1(7) . . . . ?
C91 C90 C92 C93 59.0(7) . . . . ?
C92 C90 C91 C69 50.6(8) . . . . ?
C92 C90 C91 C88 -137.4(5) . . . . ?
C92 C93 C94 C95 -19.9(8) . . . . ?
C92 C93 C96 C97 -61.8(7) . . . . ?
C92 C93 C96 C98 63.9(8) . . . . ?
C93 C94 C95 C89 -2.9(9) . . . . ?
C94 C93 C96 C97 64.1(7) . . . . ?
C94 C93 C96 C98 -170.2(6) . . . . ?
C95 C89 C90 C91 -93.1(5) . . . . ?
C95 C89 C90 C92 31.1(6) . . . . ?
C96 C93 C94 C95 -149.1(6) . . . . ?
C99 C89 C90 C91 136.9(5) . . . . ?
C99 C89 C90 C92 -98.9(6) . . . . ?
C99 C89 C95 C94 127.8(6) . . . . ?
C100 C86 C87 C75 -100.5(6) . . . . ?
C100 C86 C87 C88 78.7(6) . . . . ?
O19 C103 C104 C105 -4.6(8) . . . . ?
O19 C103 C104 C109 176.3(5) . . . . ?
O19 C103 C125 C122 -177.2(5) . . . . ?
O19 C103 C125 C124 -2.8(10) . . . . ?
O20 C105 C106 C107 69.5(9) . . . . ?
O20 C105 C106 C108 -48.9(9) . . . . ?
O21 C109 C121 C120 -2.8(8) . . . . ?
O21 C109 C121 C122 -179.9(4) . . . . ?
O21 C110 C111 C112 -163.6(5) . . . . ?
O21 C110 C111 C120 9.0(9) . . . . ?
O21 C110 C115 C114 -166.4(5) . . . . ?
O21 C110 C115 C116 74.9(6) . . . . ?
O21 C110 C115 C117 -46.4(7) . . . . ?
O22 C112 C113 C114 -169.4(6) . . . . ?
O22 C112 C113 C118 -45.9(8) . . . . ?
O22 C112 C113 C119 71.6(8) . . . . ?
O23 C114 C115 C110 151.2(6) . . . . ?
O23 C114 C115 C116 -88.6(8) . . . . ?
O23 C114 C115 C117 30.1(9) . . . . ?
O24 C122 C125 C103 178.4(5) . . . . ?
O24 C122 C125 C124 2.8(6) . . . . ?
O24 C123 C124 C125 22.2(5) . . . . ?
O24 C123 C124 C126 147.9(4) . . . . ?
O24 C123 C129 C128 -117.6(6) . . . . ?
C103 C104 C105 O20 13.8(9) . . . . ?
C103 C104 C105 C106 -158.4(7) . . . . ?
C103 C104 C109 O21 -176.7(5) . . . . ?
C103 C104 C109 C121 2.0(8) . . . . ?
C104 C103 C125 C122 3.5(8) . . . . ?
C104 C103 C125 C124 177.9(6) . . . . ?
C104 C105 C106 C107 -118.0(8) . . . . ?
C104 C105 C106 C108 123.6(7) . . . . ?
C104 C109 C121 C120 178.6(5) . . . . ?
C104 C109 C121 C122 1.5(8) . . . . ?
C105 C104 C109 O21 4.3(9) . . . . ?
C105 C104 C109 C121 -177.1(6) . . . . ?
C109 O21 C110 C111 12.4(8) . . . . ?
C109 O21 C110 C115 -163.8(5) . . . . ?
C109 C104 C105 O20 -167.1(6) . . . . ?
C109 C104 C105 C106 20.7(11) . . . . ?
C109 C121 C122 O24 179.4(5) . . . . ?
C109 C121 C122 C125 -2.7(8) . . . . ?
C110 O21 C109 C104 163.5(5) . . . . ?
C110 O21 C109 C121 -15.2(7) . . . . ?
C110 C111 C112 O22 153.9(6) . . . . ?
C110 C111 C112 C113 -28.1(8) . . . . ?
C110 C111 C120 C121 -23.6(7) . . . . ?
C110 C111 C120 C134 100.8(6) . . . . ?
C111 C110 C115 C114 17.5(9) . . . . ?
C111 C110 C115 C116 -101.1(7) . . . . ?
C111 C110 C115 C117 137.6(7) . . . . ?
C111 C112 C113 C114 12.6(8) . . . . ?
C111 C112 C113 C118 136.2(6) . . . . ?
C111 C112 C113 C119 -106.4(7) . . . . ?
C111 C120 C121 C109 20.8(7) . . . . ?
C111 C120 C121 C122 -162.2(5) . . . . ?
C111 C120 C134 C135 62.6(6) . . . . ?
C111 C120 C134 C136 -63.0(7) . . . . ?
C112 C111 C120 C121 149.0(5) . . . . ?
C112 C111 C120 C134 -86.6(6) . . . . ?
C112 C113 C114 O23 -165.4(6) . . . . ?
C112 C113 C114 C115 18.3(9) . . . . ?
C113 C114 C115 C110 -32.4(8) . . . . ?
C113 C114 C115 C116 87.7(7) . . . . ?
C113 C114 C115 C117 -153.6(6) . . . . ?
C115 C110 C111 C112 12.0(9) . . . . ?
C115 C110 C111 C120 -175.4(5) . . . . ?
C118 C113 C114 O23 71.3(8) . . . . ?
C118 C113 C114 C115 -104.9(7) . . . . ?
C119 C113 C114 O23 -47.4(8) . . . . ?
C119 C113 C114 C115 136.3(6) . . . . ?
C120 C111 C112 O22 -18.9(8) . . . . ?
C120 C111 C112 C113 159.1(5) . . . . ?
C120 C121 C122 O24 2.1(8) . . . . ?
C120 C121 C122 C125 -180.0(5) . . . . ?
C121 C120 C134 C135 -174.9(5) . . . . ?
C121 C120 C134 C136 59.5(6) . . . . ?
C121 C122 C125 C103 0.3(8) . . . . ?
C121 C122 C125 C124 -175.3(5) . . . . ?
C122 O24 C123 C124 -21.7(5) . . . . ?
C122 O24 C123 C129 95.7(5) . . . . ?
C122 O24 C123 C133 -143.7(5) . . . . ?
C123 O24 C122 C121 -169.4(5) . . . . ?
C123 O24 C122 C125 12.5(6) . . . . ?
C123 C124 C125 C103 169.1(6) . . . . ?
C123 C124 C125 C122 -15.9(6) . . . . ?
C123 C124 C126 C127 -60.1(7) . . . . ?
C124 C123 C129 C128 -5.7(8) . . . . ?
C124 C126 C127 C128 51.4(7) . . . . ?
C124 C126 C127 C130 177.3(5) . . . . ?
C125 C103 C104 C105 174.7(6) . . . . ?
C125 C103 C104 C109 -4.4(8) . . . . ?
C125 C124 C126 C127 56.6(7) . . . . ?
C126 C124 C125 C103 47.0(9) . . . . ?
C126 C124 C125 C122 -138.1(5) . . . . ?
C126 C127 C128 C129 -22.3(8) . . . . ?
C126 C127 C130 C131 -58.1(8) . . . . ?
C126 C127 C130 C132 66.5(8) . . . . ?
C127 C128 C129 C123 -1.0(9) . . . . ?
C128 C127 C130 C131 66.8(7) . . . . ?
C128 C127 C130 C132 -168.6(6) . . . . ?
C129 C123 C124 C125 -90.5(5) . . . . ?
C129 C123 C124 C126 35.3(6) . . . . ?
C130 C127 C128 C129 -149.8(6) . . . . ?
C133 C123 C124 C125 138.6(5) . . . . ?
C133 C123 C124 C126 -95.6(6) . . . . ?
C133 C123 C129 C128 126.1(6) . . . . ?
C134 C120 C121 C109 -105.0(6) . . . . ?
C134 C120 C121 C122 72.0(6) . . . . ?
C51A C45 C46 O11 -51.4(13) . . . . ?
C51A C45 C46 C47 127.7(11) . . . . ?
C50A C45 C46 O11 54.7(12) . . . . ?
C50A C45 C46 C47 -126.1(11) . . . . ?
_shelx_res_file
;
3+2_1f_tw_sq.res created by SHELXL-2014/7
TITL 3+2_1f P 1 21 1 R = 0.09
CELL 1.54184 11.541 16.4653 32.9338 90 95.72 90
ZERR 8 0.0002 0.0003 0.0005 0 0.001 0
LATT -1
SYMM -X,0.5+Y,-Z
SFAC C H O
UNIT 272 352 48
DFIX 1.5 0.001 C51 C45
DFIX 1.5 0.001 C45 C50A
RIGU C45 C50 C51 C51A C50A
RIGU C25 C28 C29 C30
ISOR 0.001 0.002 C50A
ISOR 0.001 0.002 C30 C28 C29
ISOR 0.001 0.002 C50 C51A C51
L.S. 5 0 12
PLAN -20
TEMP -173
BOND $H
CONF
MORE -1
list 8
ABIN
fmap 2
acta
SHEL 999 0.83
REM
REM
REM
WGHT 0.082700 11.235999
BASF 0.11324
FVAR 3.33450 0.54274
O1 3 0.713933 0.120209 0.315854 11.00000 0.03136 0.02078 =
0.02304 -0.00191 0.00584 0.00344
AFIX 147
H1 2 0.730924 0.070590 0.316218 11.00000 -1.50000
AFIX 0
O2 3 0.707840 -0.023041 0.337201 11.00000 0.04460 0.02060 =
0.02589 -0.00244 0.00473 0.00824
O3 3 0.592430 0.051363 0.447744 11.00000 0.02253 0.01278 =
0.01741 0.00268 -0.00110 0.00034
O4 3 0.578819 0.260248 0.543701 11.00000 0.04617 0.01945 =
0.02344 -0.00095 0.00650 -0.00019
O5 3 0.639530 -0.006621 0.588953 11.00000 0.06829 0.03002 =
0.02249 0.01004 0.01062 0.01906
O6 3 0.584825 0.324122 0.397155 11.00000 0.02987 0.01272 =
0.01865 0.00485 0.00448 -0.00067
C1 1 0.668831 0.140101 0.350766 11.00000 0.01892 0.01992 =
0.01690 0.00241 -0.00121 -0.00006
C2 1 0.647005 0.079226 0.380113 11.00000 0.01604 0.01438 =
0.02106 -0.00277 -0.00395 0.00010
C3 1 0.663772 -0.006321 0.369705 11.00000 0.02081 0.01819 =
0.02052 -0.00109 -0.00154 0.00334
C4 1 0.622502 -0.076559 0.393976 11.00000 0.03270 0.01268 =
0.02164 -0.00225 -0.00198 0.00462
AFIX 13
H4 2 0.644928 -0.065654 0.423588 11.00000 -1.20000
AFIX 0
C5 1 0.681886 -0.156894 0.382410 11.00000 0.04531 0.01438 =
0.02903 0.00022 0.00033 0.00910
AFIX 137
H5A 2 0.653033 -0.172295 0.354478 11.00000 -1.50000
H5B 2 0.663655 -0.200012 0.401276 11.00000 -1.50000
H5C 2 0.766408 -0.149019 0.384186 11.00000 -1.50000
AFIX 0
C6 1 0.490685 -0.082302 0.387125 11.00000 0.03374 0.02675 =
0.03562 0.00032 0.00258 -0.00447
AFIX 137
H6A 2 0.456457 -0.029565 0.392848 11.00000 -1.50000
H6B 2 0.463142 -0.123477 0.405384 11.00000 -1.50000
H6C 2 0.467384 -0.097568 0.358721 11.00000 -1.50000
AFIX 0
C7 1 0.605914 0.108341 0.417057 11.00000 0.01613 0.01063 =
0.01574 0.00335 -0.00547 -0.00071
C8 1 0.587298 0.078622 0.486996 11.00000 0.01442 0.01270 =
0.01882 -0.00084 -0.00151 -0.00498
C9 1 0.560161 0.156669 0.494993 11.00000 0.01913 0.01203 =
0.01614 0.00090 0.00021 -0.00156
C10 1 0.573587 0.187865 0.537077 11.00000 0.02226 0.01842 =
0.01465 -0.00238 0.00240 -0.00123
C11 1 0.578105 0.127583 0.572085 11.00000 0.03535 0.01345 =
0.02202 0.00184 0.00590 0.00055
C12 1 0.613095 0.042240 0.562079 11.00000 0.02296 0.01453 =
0.02148 0.00233 0.00363 0.00035
C13 1 0.609415 0.011707 0.517326 11.00000 0.01764 0.01574 =
0.02138 0.00403 0.00431 0.00115
C14 1 0.728234 -0.031332 0.513532 11.00000 0.01934 0.01681 =
0.02109 0.00509 0.00037 0.00118
AFIX 137
H14A 2 0.730047 -0.051952 0.485689 11.00000 -1.50000
H14B 2 0.737460 -0.076652 0.532874 11.00000 -1.50000
H14C 2 0.791856 0.007565 0.519650 11.00000 -1.50000
AFIX 0
C15 1 0.510961 -0.050531 0.510862 11.00000 0.02055 0.01601 =
0.03292 0.00323 0.00007 -0.00229
AFIX 137
H15A 2 0.435759 -0.022471 0.509265 11.00000 -1.50000
H15B 2 0.516457 -0.088783 0.533771 11.00000 -1.50000
H15C 2 0.517572 -0.080226 0.485408 11.00000 -1.50000
AFIX 0
C16 1 0.451913 0.120345 0.583730 11.00000 0.04894 0.02445 =
0.04685 0.01842 0.02580 0.00912
AFIX 137
H16A 2 0.423189 0.174261 0.590377 11.00000 -1.50000
H16B 2 0.450649 0.084609 0.607477 11.00000 -1.50000
H16C 2 0.401968 0.097579 0.560710 11.00000 -1.50000
AFIX 0
C17 1 0.657194 0.158502 0.609221 11.00000 0.07882 0.02701 =
0.02777 0.00547 -0.00769 -0.01400
AFIX 137
H17A 2 0.738068 0.159944 0.602574 11.00000 -1.50000
H17B 2 0.651058 0.121988 0.632408 11.00000 -1.50000
H17C 2 0.632848 0.213273 0.616343 11.00000 -1.50000
AFIX 0
C18 1 0.522557 0.213365 0.460866 11.00000 0.01765 0.01198 =
0.01901 -0.00019 -0.00042 -0.00219
AFIX 13
H18 2 0.551559 0.268830 0.469004 11.00000 -1.20000
AFIX 0
C19 1 0.579164 0.188671 0.423983 11.00000 0.01701 0.01169 =
0.01915 -0.00026 -0.00298 0.00158
C20 1 0.602201 0.243880 0.393303 11.00000 0.01832 0.01006 =
0.01675 0.00160 -0.00230 -0.00193
C21 1 0.609863 0.363693 0.357477 11.00000 0.02973 0.01874 =
0.01384 0.00910 0.00171 0.00123
C22 1 0.665906 0.296353 0.333075 11.00000 0.02324 0.01549 =
0.02148 0.00132 0.00176 -0.00119
AFIX 13
H22 2 0.751676 0.306531 0.334779 11.00000 -1.20000
AFIX 0
C23 1 0.645701 0.221418 0.357375 11.00000 0.01331 0.01538 =
0.01951 0.00056 -0.00264 0.00176
C24 1 0.618431 0.295072 0.287976 11.00000 0.05432 0.01927 =
0.01686 0.00410 0.00094 0.00280
AFIX 23
H24A 2 0.649939 0.247081 0.274681 11.00000 -1.20000
H24B 2 0.645434 0.344242 0.274406 11.00000 -1.20000
AFIX 0
C25 1 0.484037 0.292035 0.282202 11.00000 0.05713 0.02664 =
0.04251 0.00762 -0.02061 -0.01158
AFIX 13
H25 2 0.460825 0.240836 0.295578 11.00000 -1.20000
AFIX 0
C26 1 0.438080 0.360409 0.305687 11.00000 0.02314 0.04534 =
0.03654 0.00766 -0.00183 -0.00615
AFIX 43
H26 2 0.363846 0.382001 0.296345 11.00000 -1.20000
AFIX 0
C27 1 0.494159 0.392537 0.338520 11.00000 0.02749 0.03938 =
0.02405 0.01074 0.00667 0.00901
AFIX 43
H27 2 0.458851 0.436937 0.350989 11.00000 -1.20000
AFIX 0
C28 1 0.426077 0.289597 0.238266 11.00000 0.05785 0.05611 =
0.05599 -0.00013 0.00262 0.00032
AFIX 13
H28 2 0.339913 0.291455 0.239552 11.00000 -1.20000
AFIX 0
C29 1 0.459723 0.364320 0.214495 11.00000 0.06048 0.05746 =
0.04975 0.00297 0.00337 0.00914
AFIX 137
H29A 2 0.432721 0.413459 0.227455 11.00000 -1.50000
H29B 2 0.423439 0.361019 0.186346 11.00000 -1.50000
H29C 2 0.544574 0.366375 0.214451 11.00000 -1.50000
AFIX 0
C30 1 0.454583 0.208880 0.218815 11.00000 0.08420 0.07881 =
0.07855 -0.00518 0.00360 -0.00163
AFIX 137
H30A 2 0.535461 0.209618 0.212151 11.00000 -1.50000
H30B 2 0.402363 0.200619 0.193821 11.00000 -1.50000
H30C 2 0.444239 0.164546 0.237977 11.00000 -1.50000
AFIX 0
C31 1 0.691399 0.433534 0.369685 11.00000 0.03026 0.01604 =
0.02804 -0.00446 0.00408 -0.00032
AFIX 137
H31A 2 0.650209 0.474371 0.384444 11.00000 -1.50000
H31B 2 0.718150 0.458118 0.345176 11.00000 -1.50000
H31C 2 0.758593 0.413302 0.387336 11.00000 -1.50000
AFIX 0
C32 1 0.388309 0.218609 0.451101 11.00000 0.02082 0.01845 =
0.02836 0.00504 -0.00002 0.00465
AFIX 13
H32 2 0.372083 0.261386 0.429735 11.00000 -1.20000
AFIX 0
C33 1 0.334401 0.139405 0.433817 11.00000 0.01628 0.02373 =
0.03897 0.00099 -0.00436 -0.00222
AFIX 137
H33A 2 0.366592 0.126293 0.408174 11.00000 -1.50000
H33B 2 0.249776 0.145802 0.428731 11.00000 -1.50000
H33C 2 0.352307 0.095392 0.453476 11.00000 -1.50000
AFIX 0
C34 1 0.325828 0.244373 0.488530 11.00000 0.03233 0.02272 =
0.03890 0.00710 0.01618 0.00308
AFIX 137
H34A 2 0.328349 0.199528 0.508163 11.00000 -1.50000
H34B 2 0.244564 0.257977 0.479667 11.00000 -1.50000
H34C 2 0.365019 0.291925 0.501455 11.00000 -1.50000
AFIX 0
O7 3 0.328969 0.881662 0.187225 11.00000 0.02946 0.02671 =
0.02377 -0.00329 -0.00979 -0.00550
AFIX 147
H7 2 0.341150 0.931964 0.187411 11.00000 -1.50000
AFIX 0
O8 3 0.310793 1.024913 0.163564 11.00000 0.04352 0.02742 =
0.03562 -0.00327 -0.00731 -0.00859
O9 3 0.127537 0.945076 0.055477 11.00000 0.02274 0.01119 =
0.02030 -0.00040 -0.00052 0.00052
O10 3 0.038667 0.735448 -0.038293 11.00000 0.05285 0.01857 =
0.02589 -0.00015 -0.00527 -0.00500
O11 3 0.069645 0.999087 -0.085934 11.00000 0.08837 0.03614 =
0.02855 0.01148 -0.00327 -0.02319
O12 3 0.146619 0.675505 0.109895 11.00000 0.02718 0.01289 =
0.02256 0.00508 -0.00069 0.00062
C35 1 0.262632 0.861179 0.152715 11.00000 0.02024 0.02592 =
0.01643 -0.00489 -0.00107 -0.00018
C36 1 0.222655 0.919319 0.122509 11.00000 0.02007 0.01947 =
0.02090 -0.00105 -0.00089 0.00058
C37 1 0.246876 1.005733 0.132151 11.00000 0.02288 0.02337 =
0.02393 -0.00344 0.00156 -0.00357
C38 1 0.190874 1.075771 0.106807 11.00000 0.03289 0.02218 =
0.02967 -0.00276 0.00250 -0.00473
AFIX 13
H38 2 0.197093 1.064588 0.077259 11.00000 -1.20000
AFIX 0
C39 1 0.060912 1.080281 0.114088 11.00000 0.02960 0.03356 =
0.03348 -0.00280 0.00243 0.00491
AFIX 137
H39A 2 0.022538 1.029032 0.105681 11.00000 -1.50000
H39B 2 0.023660 1.125010 0.098067 11.00000 -1.50000
H39C 2 0.054057 1.089664 0.143136 11.00000 -1.50000
AFIX 0
C40 1 0.250109 1.156617 0.118148 11.00000 0.05362 0.02400 =
0.03476 -0.00316 -0.00180 -0.00682
AFIX 137
H40A 2 0.229277 1.174168 0.144911 11.00000 -1.50000
H40B 2 0.224342 1.197554 0.097605 11.00000 -1.50000
H40C 2 0.334755 1.150057 0.119214 11.00000 -1.50000
AFIX 0
C41 1 0.158581 0.890219 0.086602 11.00000 0.01217 0.00781 =
0.02187 0.00028 -0.00095 -0.00020
C42 1 0.094664 0.916039 0.016735 11.00000 0.01353 0.01265 =
0.02150 -0.00092 -0.00567 0.00330
C43 1 0.058201 0.839782 0.010331 11.00000 0.01569 0.01470 =
0.02537 0.00028 -0.00436 0.00110
C44 1 0.040816 0.807688 -0.031809 11.00000 0.03345 0.01759 =
0.02695 0.00062 -0.00482 -0.00668
C45 1 0.020318 0.866803 -0.067529 11.00000 0.06443 0.03001 =
0.02689 0.00551 -0.02143 -0.01106
C46 1 0.064384 0.953262 -0.058055 11.00000 0.03248 0.01987 =
0.02437 0.00824 -0.00452 -0.00100
C47 1 0.100010 0.983136 -0.014435 11.00000 0.02001 0.01347 =
0.02524 0.00545 -0.00197 0.00023
C48 1 0.223501 1.020349 -0.013907 11.00000 0.01983 0.01912 =
0.03446 0.00660 -0.00056 0.00132
AFIX 137
H48A 2 0.247024 1.043233 0.013130 11.00000 -1.50000
H48B 2 0.222755 1.063367 -0.034496 11.00000 -1.50000
H48C 2 0.278811 0.977976 -0.020023 11.00000 -1.50000
AFIX 0
C49 1 0.011786 1.049214 -0.005669 11.00000 0.02580 0.01917 =
0.03940 0.00511 -0.00481 0.00560
AFIX 137
H49A 2 -0.063357 1.023942 -0.002023 11.00000 -1.50000
H49B 2 0.002240 1.087276 -0.028636 11.00000 -1.50000
H49C 2 0.040222 1.078555 0.019240 11.00000 -1.50000
AFIX 0
PART 1
C50 1 0.032391 0.834105 -0.105265 21.00000 0.05566 0.05164 =
0.04915 -0.00115 0.00064 -0.00302
AFIX 137
H50A 2 0.115203 0.825899 -0.108276 21.00000 -1.50000
H50B 2 -0.001137 0.871258 -0.126530 21.00000 -1.50000
H50C 2 -0.008284 0.781837 -0.107902 21.00000 -1.50000
AFIX 0
C51 1 -0.108495 0.881240 -0.068930 21.00000 0.05801 0.05348 =
0.05575 0.00404 -0.00179 -0.00305
AFIX 137
H51A 2 -0.149373 0.828995 -0.070160 21.00000 -1.50000
H51B 2 -0.134574 0.913413 -0.093166 21.00000 -1.50000
H51C 2 -0.125603 0.910735 -0.044380 21.00000 -1.50000
AFIX 0
PART 0
C52 1 0.044783 0.782975 0.045268 11.00000 0.01854 0.00886 =
0.02497 -0.00180 -0.00389 -0.00313
AFIX 13
H52 2 0.067909 0.727222 0.037132 11.00000 -1.20000
AFIX 0
C53 1 0.125608 0.809305 0.080968 11.00000 0.01549 0.01525 =
0.02234 0.00309 -0.00148 0.00005
C54 1 0.167294 0.755949 0.111935 11.00000 0.01733 0.01191 =
0.02253 0.00113 -0.00216 0.00202
C55 1 0.182841 0.640534 0.150987 11.00000 0.02375 0.01802 =
0.02217 0.01000 -0.00610 -0.00066
C56 1 0.268616 0.704621 0.171947 11.00000 0.01372 0.02374 =
0.02740 0.00533 0.00029 0.00365
AFIX 13
H56 2 0.349544 0.689061 0.166701 11.00000 -1.20000
AFIX 0
C57 1 0.234361 0.779968 0.146951 11.00000 0.01509 0.02119 =
0.02094 0.00195 -0.00132 0.00255
C58 1 0.263562 0.708889 0.217856 11.00000 0.02876 0.02154 =
0.02254 0.00794 -0.00074 0.00592
AFIX 23
H58A 2 0.318725 0.750906 0.229394 11.00000 -1.20000
H58B 2 0.288641 0.656080 0.230138 11.00000 -1.20000
AFIX 0
C59 1 0.140700 0.729049 0.229420 11.00000 0.03818 0.02967 =
0.02358 0.00974 0.00687 0.00917
AFIX 13
H59 2 0.123098 0.786454 0.221018 11.00000 -1.20000
AFIX 0
C60 1 0.053749 0.675420 0.205218 11.00000 0.02227 0.04400 =
0.03465 0.01614 0.00166 0.00462
AFIX 43
H60 2 -0.020670 0.669557 0.214872 11.00000 -1.20000
AFIX 0
C61 1 0.072451 0.636101 0.171852 11.00000 0.02352 0.03165 =
0.03189 0.01557 -0.00178 -0.00123
AFIX 43
H61 2 0.011748 0.602194 0.159898 11.00000 -1.20000
AFIX 0
C62 1 0.129743 0.722770 0.275657 11.00000 0.03940 0.03352 =
0.02270 -0.00002 0.00593 0.01312
AFIX 13
H62 2 0.050737 0.743771 0.280166 11.00000 -1.20000
AFIX 0
C63 1 0.217403 0.776897 0.299957 11.00000 0.05370 0.02948 =
0.03071 0.00327 0.00924 0.01075
AFIX 137
H63A 2 0.296166 0.756055 0.297951 11.00000 -1.50000
H63B 2 0.201368 0.777388 0.328623 11.00000 -1.50000
H63C 2 0.211359 0.832248 0.289012 11.00000 -1.50000
AFIX 0
C64 1 0.136732 0.636496 0.291874 11.00000 0.05141 0.04382 =
0.02161 0.00755 0.00716 -0.00062
AFIX 137
H64A 2 0.071697 0.604689 0.278724 11.00000 -1.50000
H64B 2 0.132507 0.637156 0.321445 11.00000 -1.50000
H64C 2 0.210506 0.611907 0.285931 11.00000 -1.50000
AFIX 0
C65 1 0.237989 0.559628 0.144598 11.00000 0.04010 0.02092 =
0.03847 0.00191 -0.00635 0.00397
AFIX 137
H65A 2 0.178134 0.521084 0.133646 11.00000 -1.50000
H65B 2 0.275121 0.539396 0.170705 11.00000 -1.50000
H65C 2 0.296736 0.565554 0.125271 11.00000 -1.50000
AFIX 0
C66 1 -0.082794 0.779436 0.056961 11.00000 0.01646 0.01908 =
0.04130 0.00770 0.00213 -0.00034
AFIX 13
H66 2 -0.084494 0.737591 0.078901 11.00000 -1.20000
AFIX 0
C67 1 -0.123907 0.858577 0.074254 11.00000 0.01954 0.02368 =
0.05045 -0.00982 0.00495 -0.00034
AFIX 137
H67A 2 -0.073182 0.872869 0.098864 11.00000 -1.50000
H67B 2 -0.204056 0.852223 0.081169 11.00000 -1.50000
H67C 2 -0.121044 0.901762 0.053902 11.00000 -1.50000
AFIX 0
C68 1 -0.169972 0.752050 0.021349 11.00000 0.01653 0.02762 =
0.06619 -0.00240 -0.00632 -0.00165
AFIX 137
H68A 2 -0.184613 0.796935 0.001974 11.00000 -1.50000
H68B 2 -0.243192 0.735998 0.031801 11.00000 -1.50000
H68C 2 -0.137773 0.705732 0.007534 11.00000 -1.50000
AFIX 0
O13 3 0.889119 0.066859 0.457082 11.00000 0.03784 0.02421 =
0.02397 0.00514 -0.00090 -0.00997
AFIX 147
H13 2 0.946560 0.035905 0.462235 11.00000 -1.50000
AFIX 0
O14 3 0.943151 -0.029212 0.404322 11.00000 0.05796 0.02165 =
0.03075 0.00321 0.00392 -0.00579
O15 3 1.013280 0.164135 0.330401 11.00000 0.02517 0.02575 =
0.01855 0.00235 0.00317 0.00561
O16 3 0.892109 0.423099 0.287203 11.00000 0.04294 0.03573 =
0.02800 0.01185 0.00081 0.01662
O17 3 1.056969 0.246051 0.196967 11.00000 0.10390 0.06486 =
0.02905 0.00966 0.03235 0.02219
O18 3 0.908839 0.343464 0.435757 11.00000 0.02524 0.02018 =
0.01602 0.00102 0.00187 0.00218
C69 1 0.918067 0.127583 0.432570 11.00000 0.02078 0.01805 =
0.02092 0.00402 -0.00770 -0.00881
C70 1 0.962052 0.110733 0.394203 11.00000 0.02190 0.01870 =
0.01897 -0.00144 -0.00683 -0.00062
C71 1 0.982084 0.025943 0.384250 11.00000 0.03055 0.01683 =
0.03169 0.00028 -0.00337 -0.00413
C72 1 1.062823 -0.001305 0.353651 11.00000 0.06936 0.01735 =
0.09093 -0.00351 0.05071 -0.00373
AFIX 13
H72 2 1.094358 0.045824 0.339072 11.00000 -1.20000
AFIX 0
C73 1 1.004593 -0.061246 0.324606 11.00000 0.03877 0.13021 =
0.04678 -0.04506 -0.00634 0.01884
AFIX 137
H73A 2 0.990553 -0.111648 0.339167 11.00000 -1.50000
H73B 2 1.054663 -0.072583 0.302934 11.00000 -1.50000
H73C 2 0.930199 -0.038999 0.312581 11.00000 -1.50000
AFIX 0
C74 1 1.164940 -0.050825 0.379957 11.00000 0.05284 0.05196 =
0.08257 -0.00854 -0.01245 0.00457
AFIX 137
H74A 2 1.198304 -0.017012 0.402671 11.00000 -1.50000
H74B 2 1.225843 -0.064994 0.362480 11.00000 -1.50000
H74C 2 1.132728 -0.100562 0.390706 11.00000 -1.50000
AFIX 0
C75 1 0.981098 0.180760 0.369733 11.00000 0.01538 0.01606 =
0.01871 -0.00019 -0.00177 -0.00077
C76 1 1.000377 0.224665 0.301711 11.00000 0.02202 0.02874 =
0.01934 0.00259 -0.00118 0.00056
C77 1 0.981201 0.302618 0.311150 11.00000 0.01718 0.02661 =
0.01913 0.00495 -0.00068 0.00140
C78 1 0.940865 0.359025 0.279103 11.00000 0.03083 0.02812 =
0.02111 0.00178 -0.00009 0.00697
C79 1 0.955961 0.340829 0.234172 11.00000 0.05230 0.03917 =
0.01744 0.00514 0.00510 0.00931
C80 1 1.013152 0.259796 0.227953 11.00000 0.05290 0.04348 =
0.02169 0.00260 0.00954 0.00492
C81 1 1.009480 0.190804 0.259236 11.00000 0.03569 0.02902 =
0.02210 -0.00367 0.00791 0.00403
C82 1 1.123368 0.140631 0.259766 11.00000 0.04171 0.05258 =
0.03369 0.00210 0.01396 0.01735
AFIX 137
H82A 2 1.189387 0.173810 0.271037 11.00000 -1.50000
H82B 2 1.135180 0.124205 0.231875 11.00000 -1.50000
H82C 2 1.117493 0.092177 0.276720 11.00000 -1.50000
AFIX 0
C83 1 0.904123 0.135330 0.245830 11.00000 0.04950 0.04544 =
0.01846 -0.00979 0.00172 -0.00206
AFIX 137
H83A 2 0.905353 0.087922 0.263859 11.00000 -1.50000
H83B 2 0.908694 0.117316 0.217673 11.00000 -1.50000
H83C 2 0.831684 0.165666 0.247478 11.00000 -1.50000
AFIX 0
C84 1 0.834252 0.340155 0.210021 11.00000 0.06860 0.06962 =
0.01958 0.00187 -0.00991 0.02458
AFIX 137
H84A 2 0.784624 0.300479 0.222164 11.00000 -1.50000
H84B 2 0.841596 0.325293 0.181578 11.00000 -1.50000
H84C 2 0.799270 0.394267 0.210991 11.00000 -1.50000
AFIX 0
C85 1 1.032010 0.408016 0.218710 11.00000 0.09051 0.05273 =
0.04185 0.01158 0.03211 -0.00005
AFIX 137
H85A 2 0.991893 0.460301 0.219857 11.00000 -1.50000
H85B 2 1.046530 0.396456 0.190469 11.00000 -1.50000
H85C 2 1.106301 0.410312 0.235903 11.00000 -1.50000
AFIX 0
C86 1 0.989549 0.331036 0.355043 11.00000 0.01972 0.01548 =
0.01822 0.00558 -0.00163 0.00302
AFIX 13
H86 2 0.927297 0.372393 0.357696 11.00000 -1.20000
AFIX 0
C87 1 0.966205 0.258719 0.381269 11.00000 0.01477 0.01600 =
0.02036 0.00237 -0.00336 -0.00663
C88 1 0.927887 0.269458 0.420513 11.00000 0.01498 0.01516 =
0.02108 0.00093 -0.00515 -0.00196
C89 1 0.887367 0.331655 0.479556 11.00000 0.02088 0.02231 =
0.01611 0.00241 0.00034 0.00017
C90 1 0.853858 0.240134 0.482647 11.00000 0.01582 0.02147 =
0.01667 0.00010 -0.00073 -0.00502
AFIX 13
H90 2 0.767159 0.234754 0.478698 11.00000 -1.20000
AFIX 0
C91 1 0.905084 0.205961 0.445638 11.00000 0.01961 0.02433 =
0.01421 0.00185 -0.00269 -0.00835
C92 1 0.898878 0.203471 0.523784 11.00000 0.02075 0.02440 =
0.01586 0.00169 -0.00057 -0.00439
AFIX 23
H92A 2 0.858923 0.230145 0.545446 11.00000 -1.20000
H92B 2 0.878383 0.145084 0.523732 11.00000 -1.20000
AFIX 0
C93 1 1.028749 0.211988 0.533955 11.00000 0.02197 0.02759 =
0.01865 -0.00188 -0.00002 0.00206
AFIX 13
H93 2 1.066113 0.178193 0.513655 11.00000 -1.20000
AFIX 0
C94 1 1.064021 0.298368 0.527091 11.00000 0.01613 0.02819 =
0.01784 -0.00144 -0.00115 -0.00309
AFIX 43
H94 2 1.136464 0.316386 0.540245 11.00000 -1.20000
AFIX 0
C95 1 1.000803 0.351181 0.503894 11.00000 0.02535 0.01997 =
0.02010 -0.00306 0.00255 -0.00337
AFIX 43
H95 2 1.029382 0.405133 0.502610 11.00000 -1.20000
AFIX 0
C96 1 1.076405 0.181270 0.576267 11.00000 0.02857 0.03314 =
0.02200 0.00270 -0.00658 0.00341
AFIX 13
H96 2 1.162247 0.191475 0.579103 11.00000 -1.20000
AFIX 0
C97 1 1.025819 0.228105 0.610908 11.00000 0.03402 0.05336 =
0.02022 0.00137 -0.00209 -0.00708
AFIX 137
H97A 2 1.035487 0.286573 0.606814 11.00000 -1.50000
H97B 2 1.066945 0.212127 0.637164 11.00000 -1.50000
H97C 2 0.942821 0.215430 0.610798 11.00000 -1.50000
AFIX 0
C98 1 1.059446 0.090039 0.581079 11.00000 0.06275 0.03918 =
0.05516 0.01052 -0.01344 -0.00198
AFIX 137
H98A 2 0.976681 0.076702 0.575334 11.00000 -1.50000
H98B 2 1.086464 0.073862 0.609065 11.00000 -1.50000
H98C 2 1.104297 0.060931 0.561931 11.00000 -1.50000
AFIX 0
C99 1 0.791720 0.389464 0.487663 11.00000 0.03364 0.03304 =
0.02607 0.00189 0.00578 0.00607
AFIX 137
H99A 2 0.819679 0.445431 0.485902 11.00000 -1.50000
H99B 2 0.768286 0.379574 0.515027 11.00000 -1.50000
H99C 2 0.724768 0.381117 0.467351 11.00000 -1.50000
AFIX 0
C100 1 1.109377 0.370527 0.368729 11.00000 0.02809 0.02293 =
0.02684 0.00700 -0.00916 -0.00924
AFIX 13
H100 2 1.109261 0.385702 0.398126 11.00000 -1.20000
AFIX 0
C101 1 1.128794 0.447766 0.345264 11.00000 0.04251 0.02534 =
0.03748 0.01011 -0.00198 -0.01049
AFIX 137
H10A 2 1.140750 0.434116 0.317020 11.00000 -1.50000
H10B 2 1.197682 0.476036 0.358097 11.00000 -1.50000
H10C 2 1.060497 0.483064 0.345511 11.00000 -1.50000
AFIX 0
C102 1 1.209897 0.310791 0.365660 11.00000 0.01961 0.04568 =
0.05895 0.02957 -0.00877 -0.00359
AFIX 137
H10D 2 1.200390 0.264106 0.383486 11.00000 -1.50000
H10E 2 1.283958 0.337915 0.374138 11.00000 -1.50000
H10F 2 1.209648 0.292139 0.337394 11.00000 -1.50000
AFIX 0
O19 3 0.414224 0.919134 0.043979 11.00000 0.04213 0.02877 =
0.02462 0.00370 -0.00085 0.01576
AFIX 147
H19 2 0.438060 0.964082 0.053556 11.00000 -1.50000
AFIX 0
O20 3 0.508091 1.016205 0.094256 11.00000 0.05685 0.02379 =
0.03970 0.00359 -0.00530 0.01480
O21 3 0.623728 0.823520 0.168820 11.00000 0.02166 0.02521 =
0.01692 -0.00212 -0.00847 -0.00002
O22 3 0.517287 0.574620 0.220421 11.00000 0.03970 0.03649 =
0.03025 0.00936 0.00603 -0.00060
O23 3 0.784930 0.745376 0.297565 11.00000 0.06860 0.04750 =
0.03802 -0.01193 -0.03324 0.01773
O24 3 0.433680 0.644030 0.068592 11.00000 0.02013 0.02407 =
0.01788 -0.00247 -0.00770 -0.00279
C103 1 0.456130 0.859118 0.068964 11.00000 0.02268 0.02365 =
0.01740 0.00218 -0.00132 0.01143
C104 1 0.527431 0.875845 0.106607 11.00000 0.02119 0.02031 =
0.02176 0.00124 0.00088 0.00752
C105 1 0.559591 0.961211 0.114824 11.00000 0.03681 0.01443 =
0.04078 0.00407 0.00370 0.00845
C106 1 0.660815 0.988103 0.143144 11.00000 0.04087 0.01963 =
0.06669 0.00035 -0.01696 -0.00375
AFIX 13
H106 2 0.705386 0.939883 0.154663 11.00000 -1.20000
AFIX 0
C107 1 0.615912 1.036972 0.177090 11.00000 0.03030 0.11887 =
0.04375 -0.00152 -0.00654 -0.01487
AFIX 137
H10G 2 0.563942 1.079814 0.165359 11.00000 -1.50000
H10H 2 0.681644 1.061576 0.193837 11.00000 -1.50000
H10I 2 0.573016 1.001234 0.194098 11.00000 -1.50000
AFIX 0
C108 1 0.740439 1.042950 0.119772 11.00000 0.04374 0.04364 =
0.09436 0.00249 0.01160 0.00080
AFIX 137
H10J 2 0.761533 1.014302 0.095484 11.00000 -1.50000
H10K 2 0.811195 1.056119 0.137521 11.00000 -1.50000
H10L 2 0.699026 1.093171 0.111505 11.00000 -1.50000
AFIX 0
C109 1 0.560210 0.807695 0.131430 11.00000 0.00897 0.02195 =
0.01672 0.00047 -0.00369 0.00196
C110 1 0.632214 0.764120 0.198244 11.00000 0.02096 0.02342 =
0.02034 -0.00147 -0.00517 0.00139
C111 1 0.600367 0.686359 0.190542 11.00000 0.02150 0.01893 =
0.01767 0.00118 -0.00213 0.00499
C112 1 0.582276 0.632301 0.225236 11.00000 0.02846 0.02623 =
0.01866 0.00454 0.00281 0.00612
C113 1 0.650457 0.649548 0.266487 11.00000 0.04355 0.03506 =
0.01924 0.00744 0.00071 0.01341
C114 1 0.710166 0.731228 0.269627 11.00000 0.03676 0.03363 =
0.02063 -0.01094 -0.01027 0.01101
C115 1 0.673245 0.799247 0.239555 11.00000 0.03294 0.02368 =
0.02365 -0.00532 -0.00951 0.00814
C116 1 0.572740 0.846915 0.256810 11.00000 0.04040 0.03642 =
0.02022 -0.00907 -0.00672 0.00699
AFIX 137
H11A 2 0.547608 0.891358 0.238184 11.00000 -1.50000
H11B 2 0.600160 0.869229 0.283644 11.00000 -1.50000
H11C 2 0.507080 0.810214 0.259480 11.00000 -1.50000
AFIX 0
C117 1 0.777995 0.856137 0.236355 11.00000 0.04025 0.05295 =
0.04001 -0.00692 -0.01585 -0.01249
AFIX 137
H11D 2 0.839794 0.826566 0.224282 11.00000 -1.50000
H11E 2 0.807263 0.875238 0.263648 11.00000 -1.50000
H11F 2 0.753533 0.902779 0.219102 11.00000 -1.50000
AFIX 0
C118 1 0.568452 0.641538 0.300346 11.00000 0.06448 0.06341 =
0.02423 0.00544 0.01823 0.00678
AFIX 137
H11G 2 0.507671 0.683192 0.296609 11.00000 -1.50000
H11H 2 0.613042 0.648730 0.327019 11.00000 -1.50000
H11I 2 0.532407 0.587588 0.298977 11.00000 -1.50000
AFIX 0
C119 1 0.746570 0.582411 0.272479 11.00000 0.06276 0.03405 =
0.03878 0.00450 -0.01638 0.02172
AFIX 137
H11J 2 0.709872 0.528688 0.270627 11.00000 -1.50000
H11K 2 0.790318 0.588777 0.299357 11.00000 -1.50000
H11L 2 0.799723 0.587713 0.251207 11.00000 -1.50000
AFIX 0
C120 1 0.569325 0.656557 0.147723 11.00000 0.01433 0.01785 =
0.01946 -0.00097 -0.00124 0.00174
AFIX 13
H120 2 0.500886 0.619394 0.148032 11.00000 -1.20000
AFIX 0
C121 1 0.531629 0.728756 0.121395 11.00000 0.01353 0.01926 =
0.01543 -0.00143 -0.00584 0.00322
C122 1 0.467269 0.718238 0.082914 11.00000 0.00927 0.02499 =
0.01508 -0.00378 -0.00285 0.00188
C123 1 0.388804 0.654978 0.024685 11.00000 0.01934 0.03360 =
0.01714 -0.00135 -0.00495 -0.00272
C124 1 0.356918 0.746153 0.021529 11.00000 0.01595 0.03078 =
0.02122 0.00155 -0.00452 0.00724
AFIX 13
H124 2 0.273072 0.752533 0.026155 11.00000 -1.20000
AFIX 0
C125 1 0.430843 0.780825 0.057787 11.00000 0.01860 0.02763 =
0.01632 0.00312 -0.00202 0.00728
C126 1 0.375113 0.781328 -0.020794 11.00000 0.02765 0.03622 =
0.02110 0.00215 -0.00408 0.00767
AFIX 23
H12A 2 0.324453 0.752178 -0.042037 11.00000 -1.20000
H12B 2 0.352479 0.839344 -0.021775 11.00000 -1.20000
AFIX 0
C127 1 0.501413 0.773308 -0.029640 11.00000 0.02845 0.03339 =
0.01911 -0.00267 0.00227 -0.00262
AFIX 13
H127 2 0.548886 0.807640 -0.009184 11.00000 -1.20000
AFIX 0
C128 1 0.540852 0.686960 -0.022578 11.00000 0.02409 0.02790 =
0.02602 -0.00866 0.00129 0.00019
AFIX 43
H128 2 0.605435 0.668514 -0.035811 11.00000 -1.20000
AFIX 0
C129 1 0.490658 0.634904 0.001099 11.00000 0.02190 0.02652 =
0.02323 -0.00746 -0.00253 0.00042
AFIX 43
H129 2 0.521073 0.581298 0.003319 11.00000 -1.20000
AFIX 0
C130 1 0.526069 0.803715 -0.072546 11.00000 0.04938 0.03295 =
0.02661 0.00223 0.00504 0.00228
AFIX 13
H130 2 0.609666 0.791832 -0.075710 11.00000 -1.20000
AFIX 0
C131 1 0.453132 0.759645 -0.106719 11.00000 0.05762 0.05526 =
0.01668 0.00007 0.00349 0.00045
AFIX 137
H13A 2 0.455691 0.701069 -0.101428 11.00000 -1.50000
H13B 2 0.484330 0.770829 -0.132756 11.00000 -1.50000
H13C 2 0.372375 0.778637 -0.107994 11.00000 -1.50000
AFIX 0
C132 1 0.509265 0.895311 -0.076995 11.00000 0.08873 0.03908 =
0.04198 0.00561 0.01251 0.00057
AFIX 137
H13D 2 0.429104 0.909469 -0.072440 11.00000 -1.50000
H13E 2 0.524427 0.911999 -0.104535 11.00000 -1.50000
H13F 2 0.563471 0.923296 -0.056869 11.00000 -1.50000
AFIX 0
C133 1 0.287723 0.597483 0.016153 11.00000 0.02956 0.04881 =
0.02426 -0.00489 -0.00561 -0.01206
AFIX 137
H13G 2 0.315095 0.541437 0.020146 11.00000 -1.50000
H13H 2 0.253513 0.604565 -0.012072 11.00000 -1.50000
H13I 2 0.228821 0.609056 0.034836 11.00000 -1.50000
AFIX 0
C134 1 0.668969 0.608320 0.129892 11.00000 0.01956 0.02256 =
0.02080 -0.00509 0.00097 0.00335
AFIX 13
H134 2 0.639314 0.591511 0.101572 11.00000 -1.20000
AFIX 0
C135 1 0.700557 0.531466 0.153784 11.00000 0.03763 0.02655 =
0.03637 0.00170 0.00693 0.00870
AFIX 137
H13J 2 0.725567 0.545428 0.182238 11.00000 -1.50000
H13K 2 0.764057 0.503588 0.141826 11.00000 -1.50000
H13L 2 0.632474 0.495679 0.152738 11.00000 -1.50000
AFIX 0
C136 1 0.774316 0.660833 0.126585 11.00000 0.02329 0.02421 =
0.04800 -0.00225 0.00971 -0.00179
AFIX 137
H13M 2 0.751182 0.710194 0.111238 11.00000 -1.50000
H13N 2 0.831567 0.630869 0.112381 11.00000 -1.50000
H13O 2 0.808811 0.675639 0.153981 11.00000 -1.50000
AFIX 0
PART 2
C51A 1 -0.085276 0.857996 -0.091915 -21.00000 0.04475 0.04246 =
0.04103 0.00080 0.00003 -0.00169
AFIX 137
H51D 2 -0.094172 0.801494 -0.101050 -21.00000 -1.50000
H51E 2 -0.085900 0.893796 -0.115708 -21.00000 -1.50000
H51F 2 -0.149746 0.872528 -0.076074 -21.00000 -1.50000
AFIX 0
C50A 1 0.101695 0.840584 -0.097855 -21.00000 0.06385 0.06058 =
0.05992 0.00174 0.00549 -0.00005
AFIX 137
H50D 2 0.182054 0.842451 -0.085075 -21.00000 -1.50000
H50E 2 0.093518 0.877171 -0.121438 -21.00000 -1.50000
H50F 2 0.082644 0.785012 -0.106853 -21.00000 -1.50000
AFIX 0
HKLF 5
REM 3+2_1f P 1 21 1 R = 0.09
REM R1 = 0.0714 for 19521 Fo > 4sig(Fo) and 0.0732 for all 20250 data
REM 1511 parameters refined using 81 restraints
END
WGHT 0.0827 11.2359
REM Highest difference peak 0.921, deepest hole -0.618, 1-sigma level 0.076
Q1 1 1.1662 0.0140 0.3500 11.00000 0.05 0.92
Q2 1 -0.1433 0.8933 -0.0605 11.00000 0.05 0.88
Q3 1 0.7638 0.9801 0.1536 11.00000 0.05 0.75
Q4 1 0.1433 0.8403 -0.1015 11.00000 0.05 0.68
Q5 1 0.4847 0.3002 0.2273 11.00000 0.05 0.63
Q6 1 0.3499 0.2787 0.2166 11.00000 0.05 0.60
Q7 1 0.5007 0.3986 0.2170 11.00000 0.05 0.41
Q8 1 0.6216 0.9796 0.1639 11.00000 0.05 0.37
Q9 1 0.6846 0.7202 0.2242 11.00000 0.05 0.32
Q10 1 0.0625 0.8652 -0.0714 11.00000 0.05 0.32
Q11 1 1.0158 0.0176 0.3321 11.00000 0.05 0.31
Q12 1 0.3249 0.4586 0.1712 11.00000 0.05 0.30
Q13 1 -0.1479 0.9458 -0.0392 11.00000 0.05 0.29
Q14 1 0.6062 0.7787 0.0457 11.00000 0.05 0.28
Q15 1 0.8563 0.1330 0.3762 11.00000 0.05 0.28
Q16 1 0.6709 0.7781 0.1412 11.00000 0.05 0.27
Q17 1 1.2193 0.0936 0.3765 11.00000 0.05 0.27
Q18 1 -0.2165 0.8977 -0.0451 11.00000 0.05 0.27
Q19 1 0.6613 0.3072 0.5273 11.00000 0.05 0.27
Q20 1 0.4898 0.3441 0.4378 11.00000 0.05 0.26
;
_shelx_res_checksum 79272
_shelx_fab_checksum 56811
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8 8 0 0.26 1.00
9 8 0 -0.01 0.60
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8 6 0 0.07 0.55
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11 3 0 0.25 0.90
12 3 0 0.03 -0.19
13 3 0 -0.24 0.11
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3 2 0 0.09 0.59
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11 2 0 -0.19 0.05
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13 2 0 0.16 0.09
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4 1 0 0.00 0.56
5 1 0 -0.04 1.21
6 1 0 0.53 1.24
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9 1 0 -0.35 0.01
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-5 6 36 -0.17 -0.01
-4 6 36 0.10 -0.04
-3 6 36 -0.31 0.07
-2 6 36 -0.32 0.39
-1 6 36 -0.08 -0.05
0 6 36 -0.37 0.24
-5 5 36 0.01 0.02
-4 5 36 -0.16 -0.06
-3 5 36 0.22 0.46
-2 5 36 -0.32 0.09
-1 5 36 0.19 0.12
-6 4 36 -0.18 -0.27
-5 4 36 -0.07 0.15
-4 4 36 -0.21 -0.12
-3 4 36 -0.43 -0.38
-2 4 36 -0.59 0.13
-1 4 36 -0.19 -0.22
-6 3 36 -0.16 -0.15
-5 3 36 0.28 -0.22
-4 3 36 -0.12 0.30
-3 3 36 0.37 0.14
-2 3 36 -0.46 0.20
-1 3 36 0.46 -0.11
-6 2 36 -0.33 -0.57
-5 2 36 0.39 -0.11
-4 2 36 -0.09 -0.22
-3 2 36 0.08 -0.92
-2 2 36 -0.14 -0.14
-1 2 36 -0.17 -0.54
1 2 36 -0.38 -0.16
2 2 36 0.06 0.00
3 2 36 0.14 0.07
4 2 36 0.08 0.17
-7 1 36 -0.12 -0.03
-6 1 36 -0.11 -0.10
-5 1 36 0.30 -0.62
-4 1 36 0.01 1.11
-3 1 36 0.23 -0.08
-2 1 36 -0.21 0.27
-1 1 36 0.20 0.13
0 1 36 -0.05 -0.10
1 1 36 -0.04 0.44
2 1 36 0.59 0.40
3 1 36 0.14 0.16
4 1 36 0.01 0.54
-7 0 36 0.07 0.00
-6 0 36 -0.32 0.01
-5 0 36 0.75 -0.03
-4 0 36 0.30 -0.01
-3 0 36 0.57 0.01
-2 0 36 0.51 0.05
-1 0 36 -0.03 0.01
0 0 36 1.01 -0.08
1 0 36 -0.44 0.05
2 0 36 0.03 0.03
3 0 36 0.48 0.02
4 0 36 -0.13 -0.01
0 2 36 0.43 -0.17
0 3 36 -0.29 -0.03
1 3 36 -0.13 0.06
2 3 36 0.82 0.14
3 3 36 0.31 -0.23
4 3 36 -0.09 0.23
0 4 36 -0.29 0.27
2 4 36 0.25 0.12
3 4 36 -0.23 -0.05
0 5 36 -0.42 -0.18
2 5 36 0.15 0.03
3 5 36 0.20 -0.13
-2 7 37 -0.27 -0.06
-1 7 37 0.05 -0.21
-4 6 37 -0.04 -0.02
-3 6 37 -0.59 0.24
-2 6 37 0.00 -0.15
-1 6 37 -0.25 -0.11
0 6 37 0.22 -0.12
1 6 37 0.10 0.02
-4 5 37 0.14 -0.13
-3 5 37 -0.11 -0.24
-2 5 37 -0.20 -0.16
-1 5 37 0.11 -0.40
0 5 37 -0.41 -0.09
-5 4 37 0.04 0.08
-4 4 37 -0.09 -0.18
-3 4 37 -0.51 0.17
-2 4 37 -0.19 -0.24
-1 4 37 0.00 0.21
0 4 37 -0.04 -0.45
-5 3 37 -0.21 0.03
-4 3 37 0.55 -0.28
-3 3 37 0.46 -0.19
-2 3 37 0.01 -0.25
-1 3 37 0.56 -0.24
0 3 37 -0.22 -0.06
-6 2 37 0.21 -0.14
-5 2 37 0.20 0.32
-4 2 37 -0.61 -0.31
-3 2 37 0.18 0.05
-2 2 37 -0.44 -0.28
-1 2 37 0.20 0.10
0 2 37 -0.08 -0.40
-6 1 37 0.38 -0.36
-5 1 37 0.01 0.66
-4 1 37 0.42 0.29
-3 1 37 0.44 0.33
-2 1 37 0.06 0.43
-1 1 37 0.52 0.21
0 1 37 0.06 0.42
1 1 37 0.14 -0.22
2 1 37 0.12 0.39
3 1 37 -0.02 0.20
-6 0 37 0.36 0.01
-5 0 37 0.40 0.03
-4 0 37 -0.99 0.01
-3 0 37 0.71 -0.02
-2 0 37 -0.55 -0.01
-1 0 37 0.28 -0.02
0 0 37 0.14 -0.05
1 0 37 -0.47 0.08
2 0 37 -0.21 0.06
3 0 37 -0.19 -0.02
2 2 37 -0.15 0.48
3 2 37 0.05 0.07
2 3 37 0.09 0.01
3 3 37 -0.10 0.02
2 4 37 -0.07 0.24
-3 5 38 -0.27 -0.50
-2 5 38 0.21 -0.05
-1 5 38 -0.08 -0.22
0 5 38 0.09 0.24
-4 4 38 0.19 0.36
-3 4 38 0.01 -0.08
-2 4 38 0.22 0.08
-1 4 38 0.35 0.06
0 4 38 -0.09 -0.24
1 4 38 0.05 0.26
-4 3 38 0.50 -0.35
-3 3 38 -0.19 -0.26
-2 3 38 0.33 -0.28
-1 3 38 0.13 0.00
0 3 38 0.21 -0.21
1 3 38 -0.45 0.13
-5 2 38 -0.34 -0.04
-4 2 38 0.11 0.67
-3 2 38 -0.12 0.21
-2 2 38 -0.25 0.27
-1 2 38 0.11 0.43
0 2 38 -0.06 -0.09
1 2 38 0.01 0.37
2 2 38 -0.10 0.03
-5 1 38 -0.10 0.12
-4 1 38 0.42 -0.45
-3 1 38 -0.02 0.61
-2 1 38 0.27 -0.42
-1 1 38 0.24 0.54
0 1 38 0.15 -0.16
1 1 38 -0.25 0.00
2 1 38 -0.02 -0.08
-4 0 38 -0.16 0.00
-3 0 38 -0.35 -0.05
-2 0 38 -0.79 -0.02
-1 0 38 -0.10 0.02
0 0 38 -0.19 -0.01
2 0 38 -0.36 0.01
-2 3 39 -0.21 0.03
-1 3 39 0.04 0.11
0 3 39 -0.11 -0.06
-3 2 39 -0.20 -0.17
-2 2 39 0.23 0.64
-1 2 39 -0.10 0.24
0 2 39 0.16 0.04
-3 1 39 -0.04 -0.44
-2 1 39 -0.17 -0.50
-1 1 39 -0.04 0.21
0 1 39 -0.06 -0.11
5 0 0 -1.20 0.06
13 7 0 -0.06 0.28
12 10 0 -0.47 -0.26
6 18 0 0.15 -0.06
4 19 0 0.07 -0.12
0 0 1 0.33 -0.03
0 1 1 -1.29 19.65
-13 7 1 -0.03 -0.07
13 7 1 0.05 -0.03
-12 10 1 0.32 -0.06
12 10 1 -0.25 0.06
11 12 1 0.08 0.13
-6 18 1 -0.12 0.01
6 18 1 -0.02 0.00
-4 19 1 -0.01 -0.09
4 19 1 -0.07 -0.10
0 0 2 -14.80 0.05
-13 7 2 0.21 0.10
-12 10 2 0.24 0.19
11 12 2 0.07 0.22
-10 14 2 -0.06 0.17
9 15 2 -0.04 0.22
-6 18 2 -0.35 0.37
-4 19 2 0.08 0.05
4 19 2 0.17 0.18
11 12 3 0.09 -0.17
-10 14 3 0.27 -0.06
9 15 3 -0.32 0.06
7 17 3 0.05 0.16
-6 18 3 0.08 0.12
-4 19 3 0.03 -0.04
4 19 3 0.24 0.07
2 0 4 2.68 0.06
5 0 4 0.02 -0.05
13 6 4 0.47 0.02
-10 14 4 0.11 -0.02
8 16 4 0.04 0.01
7 17 4 0.15 0.06
-6 18 4 0.16 -0.46
-4 19 4 -0.22 -0.16
13 6 5 0.49 -0.28
-12 10 5 0.23 -0.35
8 16 5 0.18 -0.20
-4 19 5 -0.23 0.06
-13 7 6 0.22 0.23
12 9 6 0.20 0.06
-12 10 6 -0.23 0.14
-4 19 6 0.31 0.03
2 0 7 2.08 -0.01
13 5 7 -0.34 -0.31
-13 7 7 -0.29 0.23
-12 10 7 0.05 0.31
-11 12 7 0.18 0.27
10 13 7 -0.34 -0.12
-9 15 7 -0.10 -0.32
-7 17 7 -0.23 -0.30
-5 18 7 -0.03 -0.40
3 19 7 0.44 0.06
13 4 8 0.15 -0.37
-13 7 8 0.06 -0.27
-12 10 8 0.25 0.02
11 11 8 0.14 0.04
-11 12 8 -0.20 -0.10
-9 15 8 0.30 -0.13
-8 16 8 -0.21 0.21
-7 17 8 -0.46 -0.08
-6 17 8 0.03 0.49
-5 18 8 -0.11 0.30
-4 18 8 0.09 0.17
5 18 8 0.35 0.14
3 19 8 -0.25 -0.03
13 3 9 0.22 0.18
12 8 9 0.19 -0.05
-11 12 9 -0.03 -0.16
9 14 9 0.10 -0.27
-8 16 9 -0.04 -0.17
-6 16 9 -0.43 0.16
-5 16 9 0.03 -0.05
-6 17 9 0.22 0.00
-5 17 9 -0.48 0.27
-4 17 9 -0.06 -0.25
-5 18 9 0.03 -0.05
-4 18 9 -0.03 -0.39
-3 19 9 0.18 0.09
-9 0 10 0.09 0.01
13 2 10 -0.41 0.18
-5 15 10 -0.14 -0.12
-7 16 10 -0.27 0.02
-6 16 10 -0.20 -0.04
-5 16 10 -0.37 -0.37
-6 17 10 -0.10 -0.26
-5 17 10 0.08 0.04
-4 17 10 -0.05 -0.28
6 17 10 -0.02 -0.05
-5 18 10 -0.01 -0.57
-4 18 10 0.15 0.25
2 19 10 -0.44 0.01
13 0 11 -0.23 0.00
13 1 11 -0.12 -0.46
12 7 11 0.24 0.30
11 10 11 0.06 -0.06
10 12 11 0.16 -0.05
-5 14 11 0.34 -0.38
-6 15 11 0.31 -0.36
-5 15 11 0.05 -0.23
8 15 11 0.02 -0.05
-7 16 11 0.05 0.01
-6 16 11 -0.04 -0.04
-5 16 11 0.30 -0.15
7 16 11 -0.11 -0.03
-6 17 11 0.14 -0.21
-5 17 11 0.45 -0.05
-4 17 11 -0.43 0.20
-5 18 11 0.08 0.11
-4 18 11 0.03 0.18
4 18 11 -0.36 -0.24
-2 19 11 0.46 0.33
1 19 11 -0.16 0.11
-13 6 12 0.37 0.18
-7 9 12 -0.26 0.23
-10 13 12 -0.32 0.33
-5 14 12 0.38 0.00
-6 15 12 0.12 -0.13
-5 15 12 0.29 0.50
-7 16 12 0.25 -0.02
-6 16 12 0.23 0.24
-5 16 12 0.12 0.08
-6 17 12 0.10 0.01
-5 17 12 -0.09 0.32
-4 17 12 -0.01 -0.22
-4 18 12 0.01 -0.37
-1 19 12 -0.33 -0.28
0 19 12 -0.19 0.13
12 6 13 -0.12 0.06
-12 9 13 -0.10 -0.01
-7 9 13 -0.74 0.06
-10 13 13 -0.08 -0.03
9 13 13 -0.01 0.27
-5 14 13 -0.10 0.16
-6 15 13 0.03 0.21
-5 15 13 -0.12 0.29
-7 16 13 0.17 0.06
-6 16 13 -0.06 0.15
-5 16 13 -0.36 -0.02
-6 17 13 -0.25 0.18
-5 17 13 -0.11 -0.03
-4 18 13 0.19 0.11
-13 5 14 -0.22 -0.47
12 5 14 0.01 -0.03
-7 9 14 0.00 -0.11
-6 10 14 -0.70 -0.21
-11 11 14 0.16 0.08
10 11 14 -0.05 0.15
-9 14 14 -0.14 -0.12
-8 15 14 0.09 -0.09
-7 15 14 -0.13 0.20
-6 15 14 -0.08 -0.10
-5 15 14 -0.10 -0.06
-7 16 14 -0.12 -0.13
-6 16 14 -0.26 -0.02
-5 16 14 0.13 -0.15
-5 17 14 0.12 -0.09
5 17 14 0.29 0.55
-4 18 14 -0.04 0.23
3 18 14 0.24 0.38
12 4 15 -0.27 0.02
-6 10 15 -0.47 -0.78
-9 14 15 0.14 0.15
-6 14 15 -0.28 -0.14
-8 15 15 0.09 -0.03
-7 15 15 0.08 -0.07
-6 15 15 -0.04 -0.29
-5 15 15 0.29 0.13
7 15 15 0.29 -0.11
-7 16 15 -0.13 -0.10
-6 16 15 0.21 -0.01
-5 16 15 0.04 0.00
6 16 15 0.00 0.23
-5 17 15 0.02 0.26
12 3 16 0.09 -0.21
-13 4 16 0.14 0.31
-12 8 16 0.08 -0.26
-6 10 16 0.17 -0.03
9 12 16 -0.01 -0.02
-6 14 16 0.06 0.07
-7 15 16 -0.08 0.02
-6 15 16 0.17 -0.08
-6 16 16 0.16 0.03
-5 16 16 -0.24 0.05
-5 17 16 0.04 -0.02
4 17 16 -0.33 -0.12
12 0 17 -0.20 0.00
12 1 17 -0.03 -0.41
-13 3 17 -0.05 0.15
11 7 17 0.25 0.47
-11 10 17 -0.15 0.01
-10 12 17 -0.07 0.12
-7 14 17 -0.03 -0.13
-6 14 17 0.33 0.33
-7 15 17 -0.18 0.12
-6 15 17 0.00 0.05
-6 16 17 -0.10 0.07
-5 16 17 0.04 -0.13
-1 18 17 -0.12 -0.22
0 18 17 -0.33 -0.10
-13 0 18 -0.46 0.06
-13 1 18 0.08 0.16
-13 2 18 -0.35 -0.07
11 6 18 -0.34 0.05
-12 7 18 -0.23 -0.03
10 9 18 -0.25 0.12
-9 13 18 -0.30 -0.18
-6 13 18 -0.19 0.50
-8 14 18 0.01 -0.24
-7 14 18 0.18 -0.12
-6 14 18 -0.16 -0.04
7 14 18 0.17 -0.19
-7 15 18 0.01 -0.02
-6 15 18 -0.10 0.05
6 15 18 -0.06 0.06
-6 16 18 0.01 0.05
-5 16 18 -0.11 -0.15
-4 17 18 -0.07 -0.07
3 17 18 0.16 -0.04
11 5 19 0.10 -0.12
-6 13 19 0.24 -0.31
-8 14 19 -0.04 -0.15
-7 14 19 0.09 -0.03
-6 14 19 -0.27 -0.15
-7 15 19 0.06 0.08
-6 15 19 0.09 -0.16
-5 16 19 -0.21 -0.05
2 17 19 0.31 -0.22
11 4 20 0.09 0.05
-12 6 20 0.13 -0.25
10 8 20 -0.01 -0.23
-11 9 20 0.03 -0.10
-10 11 20 0.12 0.15
8 12 20 -0.26 -0.20
-7 13 20 0.06 0.14
-6 13 20 0.43 -0.30
-7 14 20 -0.35 -0.03
-6 14 20 0.35 0.20
-6 15 20 0.14 -0.08
-5 16 20 0.06 0.06
-3 17 20 0.24 0.16
1 17 20 -0.03 -0.29
11 1 21 0.07 0.05
11 2 21 -0.43 0.01
-12 5 21 0.33 0.38
10 7 21 0.00 0.06
-9 12 21 -0.06 0.22
-8 13 21 0.05 0.19
-7 13 21 0.06 -0.55
-7 14 21 -0.09 0.01
-6 14 21 0.12 0.40
6 14 21 -0.12 0.23
-6 15 21 0.04 0.25
3 16 21 0.25 0.00
-1 17 21 -0.06 0.37
-12 4 22 -0.55 -0.03
10 6 22 -0.20 -0.10
9 9 22 0.27 -0.24
-10 10 22 -0.24 -0.15
-8 13 22 0.19 -0.36
-7 13 22 -0.27 0.00
-7 14 22 0.18 -0.01
-6 14 22 -0.28 0.12
-4 16 22 -0.33 -0.21
-12 2 23 -0.17 -0.16
-12 3 23 0.29 -0.19
10 5 23 0.14 -0.32
-11 7 23 -0.25 0.14
9 8 23 0.14 -0.06
-7 12 23 -0.10 -0.33
-7 13 23 -0.23 0.19
6 13 23 0.01 0.53
-6 14 23 0.05 -0.31
5 14 23 -0.02 -0.19
-3 16 23 0.30 -0.19
1 16 23 -0.42 -0.18
10 3 24 0.04 -0.02
-10 9 24 0.15 -0.18
-8 12 24 0.00 -0.23
-7 12 24 -0.01 -0.41
-7 13 24 0.21 -0.28
-6 14 24 -0.02 -0.04
3 15 24 -0.01 -0.33
10 0 25 -0.22 0.03
8 9 25 0.05 0.20
-7 12 25 0.26 0.11
6 12 25 -0.12 -0.13
5 13 25 -0.05 -0.29
2 15 25 -0.08 -0.27
-11 4 26 0.30 0.02
9 5 26 -0.14 0.29
8 8 26 -0.11 0.25
7 10 26 0.28 -0.15
-8 11 26 0.18 0.17
-7 11 26 -0.09 0.06
-7 12 26 -0.17 0.30
-6 13 26 -0.43 -0.20
-5 14 26 0.19 -0.23
3 14 26 -0.07 -0.15
-2 15 26 -0.06 0.06
-1 15 26 0.01 0.10
0 15 26 0.06 -0.16
-11 2 27 0.27 0.09
-11 3 27 -0.26 0.19
9 3 27 -0.03 0.18
-10 7 27 0.07 0.16
8 7 27 -0.14 -0.03
-9 9 27 0.11 0.00
-7 11 27 -0.38 -0.37
5 12 27 0.00 0.00
-4 14 27 0.21 -0.03
2 14 27 0.02 -0.15
-10 6 28 0.13 0.29
8 6 28 -0.03 -0.10
-8 10 28 -0.08 -0.22
6 10 28 -0.29 0.05
-7 11 28 0.14 -0.01
-5 13 28 0.04 0.22
3 13 28 0.04 -0.18
-2 14 28 -0.07 0.26
0 14 28 -0.50 0.16
1 14 28 0.04 0.28
-4 13 29 0.04 -0.27
2 13 29 0.23 -0.52
8 1 30 0.05 -0.13
-10 2 30 -0.13 -0.27
8 2 30 -0.07 -0.13
-10 3 30 0.13 -0.15
7 6 30 0.29 0.11
-7 10 30 0.02 0.09
-6 11 30 0.26 -0.03
4 11 30 0.03 0.03
2 12 30 0.57 0.28
-2 13 30 -0.04 0.12
-1 13 30 -0.29 -0.25
0 13 30 -0.23 0.01
-9 5 31 0.18 0.06
7 5 31 -0.25 0.05
5 9 31 -0.06 -0.33
2 10 31 0.25 -0.15
3 11 31 0.27 -0.41
7 2 32 0.19 0.12
-9 4 32 -0.18 0.08
6 6 32 -0.15 -0.01
5 8 32 0.37 0.05
2 9 32 0.10 0.23
2 10 32 -0.04 -0.01
3 10 32 -0.05 0.27
-4 11 32 -0.19 -0.19
2 11 32 0.15 0.00
-1 12 32 -0.01 -0.02
-9 0 33 -0.02 -0.01
-9 1 33 -0.01 -0.07
-8 5 33 -0.01 -0.09
5 7 33 0.05 0.05
2 9 33 -0.13 -0.20
-2 11 33 0.19 0.06
0 11 33 0.24 0.20
6 0 34 0.28 0.02
6 1 34 -0.18 0.27
6 2 34 0.01 -0.06
1 5 34 0.47 0.20
-7 6 34 0.02 0.07
1 6 34 0.14 0.44
1 7 34 0.18 -0.09
1 8 34 -0.18 0.05
2 8 34 0.25 -0.11
-5 9 34 -0.02 -0.04
2 9 34 -0.31 -0.24
-3 10 34 -0.26 -0.33
1 10 34 -0.19 -0.11
5 3 35 -0.14 0.06
-7 5 35 -0.10 -0.14
1 5 35 -0.30 0.03
1 6 35 0.09 0.15
4 6 35 0.09 -0.22
1 7 35 -0.11 -0.23
2 7 35 0.14 -0.04
-5 8 35 -0.02 -0.11
1 8 35 0.34 0.03
2 8 35 0.23 -0.12
-3 9 35 0.28 -0.21
1 9 35 0.11 -0.17
-7 2 36 -0.04 0.26
1 4 36 0.05 -0.12
4 4 36 0.30 0.36
-6 5 36 -0.12 0.27
1 5 36 -0.04 -0.06
1 6 36 0.45 -0.11
2 6 36 0.14 0.15
3 6 36 -0.19 -0.33
2 7 36 -0.20 0.07
-3 8 36 0.05 0.14
1 8 36 0.24 -0.02
4 0 37 -0.60 -0.02
1 2 37 -0.21 0.35
-6 3 37 0.38 -0.25
1 3 37 0.24 -0.09
1 4 37 0.18 0.35
3 4 37 0.23 0.27
-5 5 37 -0.11 -0.09
1 5 37 0.13 0.32
2 5 37 -0.07 -0.05
-3 7 37 -0.13 -0.04
0 7 37 -0.24 0.01
-5 0 38 -0.94 0.02
1 0 38 -0.16 0.00
3 0 38 -0.15 -0.02
-5 3 38 -0.11 -0.02
2 3 38 -0.06 -0.14
2 4 38 0.09 -0.06
1 5 38 -0.18 0.19
-2 6 38 0.05 -0.14
-1 6 38 0.31 -0.02
-4 0 39 0.14 0.00
-3 0 39 -0.76 -0.01
-2 0 39 0.08 0.02
-1 0 39 -0.54 0.08
0 0 39 0.09 -0.05
1 0 39 -0.38 -0.06
-4 1 39 -0.29 0.24
1 1 39 -0.12 -0.13
-4 2 39 0.29 0.58
1 2 39 -0.23 -0.12
-3 3 39 0.02 -0.15
-2 4 39 0.22 0.35
-1 4 39 0.16 -0.10
0 4 39 -0.08 0.00
0 0 0 0.00 0.00
# SQUEEZE RESULTS (Version = 191016)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.238 1.000 0.258 130 10 ' '
2 -0.238 0.500 0.742 130 10 ' '
3 0.336 0.432 0.972 13 1 ' '
4 0.663 0.932 0.028 13 1 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
5 0 0 19.613
0 0 1 1.348
0 1 1 3.004
0 0 2 2.697
2 0 4 9.873
5 0 4 20.948
2 0 7 12.862
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details
)
TITL 3+2_1f_tw P 1 21 1 R = 0.07
CELL 11.5410 16.4653 32.9338 90.00 95.72 90.00
SPGR P21
# Solvent Accessible Volume = 287
# Electrons Found in S.A.V. = 21
# Note: Atoms in Void as Cxxx and Qxxx all others
Q101 0.832 0.518 0.647 ! 1.01 eA-3
Q102 0.236 0.490 0.841 ! 0.74 eA-3
Q103 0.521 0.512 0.662 ! 0.68 eA-3
Q104 0.486 0.299 0.228 ! 0.67 eA-3
Q105 0.653 0.791 0.779 ! 0.60 eA-3
Q106 0.969 1.003 0.236 ! 0.59 eA-3
Q107 0.889 0.391 0.749 ! 0.53 eA-3
Q108 0.269 0.439 0.944 ! 0.52 eA-3
C109 0.656 0.566 0.668 ! 0.51 eA-3
)
;
_shelx_SHELXL_version_number 2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.887(4)
2 0.113(4)
#######################################################################
#
# 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_3_2_hy
_database_code_depnum_ccdc_archive 'CCDC 1582657'
_audit_update_record
;
2017-10-28 deposited with the CCDC.
2017-11-27 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2016/4
_shelx_SHELXL_version_number 2016/4
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C34 H45 O7'
_chemical_formula_weight 565.70
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
_cell_length_a 6.38280(10)
_cell_length_b 14.89930(10)
_cell_length_c 32.6050(2)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 3100.71(6)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 22524
_cell_measurement_theta_min 4.1520
_cell_measurement_theta_max 73.4790
_exptl_crystal_description blocks
_exptl_crystal_colour colorless
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.212
_exptl_crystal_F_000 1220
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.41
_exptl_crystal_size_mid 0.32
_exptl_crystal_size_min 0.21
_exptl_absorpt_coefficient_mu 0.673
_shelx_estimated_absorpt_T_min ?
_shelx_estimated_absorpt_T_max ?
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.65065
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_process_details ?
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 1.54178
_diffrn_radiation_type CuK\a
_diffrn_source ?
_diffrn_measurement_device_type 'Oxford Gemini S ultra'
_diffrn_measurement_method ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 29525
_diffrn_reflns_av_unetI/netI 0.0184
_diffrn_reflns_av_R_equivalents 0.0270
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_l_min -40
_diffrn_reflns_limit_l_max 40
_diffrn_reflns_theta_min 4.019
_diffrn_reflns_theta_max 73.670
_diffrn_reflns_theta_full 67.679
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total 6184
_reflns_number_gt 6103
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.731
_reflns_Friedel_fraction_max 0.978
_reflns_Friedel_fraction_full 1.000
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'CrysAlis PRO '
_computing_cell_refinement 'CrysAlis PRO '
_computing_data_reduction 'CrysAlis PRO '
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics ?
_computing_publication_material ?
_refine_special_details ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+0.5352P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method 'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_extinction_coef 0.0052(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details
;
Flack x determined using 2537 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.04(3)
_chemical_absolute_configuration ad
_refine_ls_number_reflns 6184
_refine_ls_number_parameters 383
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0283
_refine_ls_R_factor_gt 0.0278
_refine_ls_wR_factor_ref 0.0727
_refine_ls_wR_factor_gt 0.0723
_refine_ls_goodness_of_fit_ref 1.044
_refine_ls_restrained_S_all 1.044
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.0282(2) 0.35452(8) 0.01658(3) 0.0282(3) Uani 1 1 d . . . . .
O2 O 0.3717(4) 0.57166(10) -0.05636(4) 0.0605(6) Uani 1 1 d . . . . .
O3 O 0.5870(2) 0.71910(7) 0.18630(3) 0.0240(3) Uani 1 1 d . . . . .
O4 O 0.36654(19) 0.62000(7) 0.23015(3) 0.0201(2) Uani 1 1 d . . . . .
H4 H 0.440472 0.663255 0.224462 0.030 Uiso 1 1 calc R U . . .
O5 O 0.46751(17) 0.55559(7) 0.08663(3) 0.0166(2) Uani 1 1 d . . . . .
O6 O -0.37324(18) 0.40194(9) 0.21365(3) 0.0264(3) Uani 1 1 d . . . . .
O12 O 0.03982(17) 0.37249(7) 0.17421(3) 0.0156(2) Uani 1 1 d . . . . .
C1 C 0.1730(3) 0.40751(10) 0.01529(4) 0.0184(3) Uani 1 1 d . . . . .
C2 C 0.2705(3) 0.43460(11) -0.02576(4) 0.0216(3) Uani 1 1 d . . . . .
C3 C 0.3573(3) 0.52961(11) -0.02504(5) 0.0282(4) Uani 1 1 d . . . . .
C4 C 0.4393(3) 0.57272(10) 0.01475(5) 0.0207(3) Uani 1 1 d . . . . .
C6 C 0.4364(2) 0.58993(10) 0.15793(4) 0.0151(3) Uani 1 1 d . . . . .
C7 C 0.3382(2) 0.56923(9) 0.19635(4) 0.0152(3) Uani 1 1 d . . . . .
C8 C -0.0951(3) 0.52445(10) 0.24723(5) 0.0208(3) Uani 1 1 d . . . . .
H8A H -0.170613 0.541602 0.222633 0.025 Uiso 1 1 calc R U . . .
H8B H -0.038170 0.578513 0.259504 0.025 Uiso 1 1 calc R U . . .
C9 C -0.2470(3) 0.47993(11) 0.27745(5) 0.0205(3) Uani 1 1 d . . . . .
H9 H -0.362863 0.521700 0.282442 0.025 Uiso 1 1 calc R U . . .
C10 C -0.3359(3) 0.39672(11) 0.25745(4) 0.0217(3) Uani 1 1 d . . . . .
H10 H -0.439977 0.363378 0.273456 0.026 Uiso 1 1 calc R U . . .
C11 C -0.2104(3) 0.34361(11) 0.22818(4) 0.0190(3) Uani 1 1 d . . . . .
H11 H -0.242560 0.279330 0.227264 0.023 Uiso 1 1 calc R U . . .
C13 C 0.2397(2) 0.39070(9) 0.09243(4) 0.0156(3) Uani 1 1 d . . . . .
H13 H 0.096500 0.367041 0.093087 0.019 Uiso 1 1 calc R U . . .
C1' C 0.4589(3) 0.37092(12) -0.03247(5) 0.0307(4) Uani 1 1 d . . . . .
H1'1 H 0.524952 0.384731 -0.058161 0.046 Uiso 1 1 calc R U . . .
H1'2 H 0.410717 0.309892 -0.032821 0.046 Uiso 1 1 calc R U . . .
H1'3 H 0.557955 0.378646 -0.010598 0.046 Uiso 1 1 calc R U . . .
C2' C 0.1123(3) 0.42407(12) -0.06047(5) 0.0308(4) Uani 1 1 d . . . . .
H2'1 H -0.000235 0.466033 -0.056705 0.046 Uiso 1 1 calc R U . . .
H2'2 H 0.057463 0.364067 -0.060325 0.046 Uiso 1 1 calc R U . . .
H2'3 H 0.179967 0.435481 -0.086242 0.046 Uiso 1 1 calc R U . . .
C3' C 0.6793(3) 0.58090(12) 0.01066(5) 0.0278(4) Uani 1 1 d . . . . .
H3'1 H 0.733580 0.614643 0.033382 0.042 Uiso 1 1 calc R U . . .
H3'2 H 0.712950 0.611077 -0.014501 0.042 Uiso 1 1 calc R U . . .
H3'3 H 0.740629 0.522076 0.010566 0.042 Uiso 1 1 calc R U . . .
C4' C 0.3405(3) 0.66667(11) 0.01828(5) 0.0277(4) Uani 1 1 d . . . . .
H4'1 H 0.191258 0.661029 0.020913 0.042 Uiso 1 1 calc R U . . .
H4'2 H 0.372828 0.700870 -0.005862 0.042 Uiso 1 1 calc R U . . .
H4'3 H 0.395747 0.696707 0.041972 0.042 Uiso 1 1 calc R U . . .
C5' C 0.5789(2) 0.66729(10) 0.15638(4) 0.0168(3) Uani 1 1 d . . . . .
C6' C 0.7304(2) 0.68463(10) 0.12121(4) 0.0177(3) Uani 1 1 d . . . . .
H6' H 0.651373 0.686370 0.095454 0.021 Uiso 1 1 calc R U . . .
C7' C 0.8897(3) 0.60776(11) 0.11911(5) 0.0221(3) Uani 1 1 d . . . . .
H7'1 H 0.969717 0.606192 0.144031 0.033 Uiso 1 1 calc R U . . .
H7'2 H 0.982058 0.617130 0.096272 0.033 Uiso 1 1 calc R U . . .
H7'3 H 0.817056 0.551835 0.115718 0.033 Uiso 1 1 calc R U . . .
C8' C 0.8445(3) 0.77375(11) 0.12668(5) 0.0278(4) Uani 1 1 d . . . . .
H8'1 H 0.743985 0.821502 0.128516 0.042 Uiso 1 1 calc R U . . .
H8'2 H 0.934927 0.783952 0.103614 0.042 Uiso 1 1 calc R U . . .
H8'3 H 0.926507 0.771903 0.151350 0.042 Uiso 1 1 calc R U . . .
C9' C -0.1491(3) 0.45525(11) 0.31936(4) 0.0218(3) Uani 1 1 d . . . . .
H9' H -0.054119 0.404454 0.314990 0.026 Uiso 1 1 calc R U . . .
C10' C -0.0217(4) 0.53171(13) 0.33772(6) 0.0349(4) Uani 1 1 d . . . . .
H10A H -0.107860 0.584327 0.339830 0.052 Uiso 1 1 calc R U . . .
H10B H 0.096391 0.544222 0.320410 0.052 Uiso 1 1 calc R U . . .
H10C H 0.026681 0.514818 0.364512 0.052 Uiso 1 1 calc R U . . .
C11' C -0.3176(3) 0.42544(14) 0.34990(5) 0.0343(4) Uani 1 1 d . . . . .
H11A H -0.253144 0.410811 0.375645 0.051 Uiso 1 1 calc R U . . .
H11B H -0.388824 0.373588 0.339355 0.051 Uiso 1 1 calc R U . . .
H11C H -0.416459 0.473227 0.353825 0.051 Uiso 1 1 calc R U . . .
C12' C 0.1544(3) 0.29288(10) 0.23438(4) 0.0188(3) Uani 1 1 d . . . . .
H12A H 0.117375 0.238001 0.220754 0.028 Uiso 1 1 calc R U . . .
H12B H 0.137465 0.285626 0.263447 0.028 Uiso 1 1 calc R U . . .
H12C H 0.297626 0.307491 0.228391 0.028 Uiso 1 1 calc R U . . .
C13' C 0.3959(3) 0.31010(10) 0.09326(5) 0.0196(3) Uani 1 1 d . . . . .
H13' H 0.377970 0.277008 0.067523 0.023 Uiso 1 1 calc R U . . .
C14' C 0.6249(3) 0.33961(11) 0.09555(5) 0.0253(3) Uani 1 1 d . . . . .
H14A H 0.648496 0.371244 0.120774 0.038 Uiso 1 1 calc R U . . .
H14B H 0.655988 0.378361 0.072826 0.038 Uiso 1 1 calc R U . . .
H14C H 0.713957 0.287750 0.094472 0.038 Uiso 1 1 calc R U . . .
C15' C 0.3463(3) 0.24543(11) 0.12823(5) 0.0288(4) Uani 1 1 d . . . . .
H15A H 0.431255 0.192581 0.125574 0.043 Uiso 1 1 calc R U . . .
H15B H 0.200959 0.228994 0.127126 0.043 Uiso 1 1 calc R U . . .
H15C H 0.375444 0.274015 0.153992 0.043 Uiso 1 1 calc R U . . .
C4A C 0.3839(3) 0.51725(10) 0.05194(4) 0.0161(3) Uani 1 1 d . . . . .
C5A C 0.3896(2) 0.53057(9) 0.12486(4) 0.0144(3) Uani 1 1 d . . . . .
C7A C 0.2094(2) 0.49532(10) 0.19987(4) 0.0148(3) Uani 1 1 d . . . . .
C11A C 0.0132(3) 0.36795(10) 0.21944(4) 0.0155(3) Uani 1 1 d . . . . .
C12A C 0.1747(2) 0.44058(9) 0.16648(4) 0.0140(3) Uani 1 1 d . . . . .
C13A C 0.2692(2) 0.44226(10) 0.05309(4) 0.0163(3) Uani 1 1 d . . . . .
C7B C 0.0847(2) 0.46140(9) 0.23566(4) 0.0152(3) Uani 1 1 d . . . . .
H7B H 0.177339 0.453296 0.259342 0.018 Uiso 1 1 calc R U . . .
C12B C 0.2675(2) 0.45432(9) 0.12802(4) 0.0142(3) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0340(7) 0.0314(6) 0.0194(5) -0.0017(5) -0.0017(5) -0.0152(6)
O2 0.1246(17) 0.0385(8) 0.0184(6) 0.0095(5) -0.0142(8) -0.0412(10)
O3 0.0318(7) 0.0201(5) 0.0202(5) -0.0058(4) 0.0005(5) -0.0072(5)
O4 0.0256(6) 0.0190(5) 0.0156(5) -0.0043(4) -0.0001(4) -0.0045(5)
O5 0.0203(6) 0.0172(5) 0.0124(5) -0.0006(4) -0.0006(4) -0.0054(4)
O6 0.0171(6) 0.0445(7) 0.0177(5) 0.0030(5) -0.0029(4) 0.0051(5)
O12 0.0182(6) 0.0167(5) 0.0120(5) 0.0009(4) 0.0013(4) -0.0024(4)
C1 0.0226(8) 0.0169(7) 0.0156(6) -0.0001(5) -0.0013(6) -0.0023(6)
C2 0.0293(9) 0.0210(7) 0.0143(7) -0.0006(6) -0.0011(6) -0.0067(7)
C3 0.0443(11) 0.0242(8) 0.0161(7) 0.0015(6) -0.0029(7) -0.0110(8)
C4 0.0298(9) 0.0173(7) 0.0151(7) 0.0009(6) -0.0006(6) -0.0064(6)
C6 0.0147(7) 0.0140(6) 0.0166(6) 0.0004(5) -0.0019(6) 0.0014(6)
C7 0.0158(7) 0.0149(6) 0.0150(6) -0.0012(5) -0.0025(6) 0.0016(6)
C8 0.0235(8) 0.0192(7) 0.0197(7) 0.0029(6) 0.0040(6) 0.0051(6)
C9 0.0201(8) 0.0221(7) 0.0194(7) 0.0023(6) 0.0043(6) 0.0069(7)
C10 0.0164(8) 0.0325(8) 0.0160(7) 0.0039(6) 0.0014(6) 0.0021(7)
C11 0.0176(8) 0.0239(7) 0.0155(7) 0.0022(6) -0.0007(6) -0.0024(6)
C13 0.0186(7) 0.0145(6) 0.0136(6) -0.0004(5) 0.0003(6) -0.0029(6)
C1' 0.0378(11) 0.0311(9) 0.0231(8) -0.0017(7) 0.0069(7) 0.0002(8)
C2' 0.0426(11) 0.0344(9) 0.0155(7) 0.0006(6) -0.0057(7) -0.0119(9)
C3' 0.0318(10) 0.0294(8) 0.0223(7) 0.0008(6) 0.0069(7) -0.0093(7)
C4' 0.0397(11) 0.0188(7) 0.0248(8) 0.0053(6) -0.0054(8) -0.0012(7)
C5' 0.0168(8) 0.0159(7) 0.0177(7) 0.0006(5) -0.0036(6) 0.0007(6)
C6' 0.0184(7) 0.0168(7) 0.0180(7) 0.0006(5) -0.0021(6) -0.0030(6)
C7' 0.0177(8) 0.0245(8) 0.0240(7) 0.0011(6) -0.0010(6) 0.0014(7)
C8' 0.0322(10) 0.0231(8) 0.0282(8) -0.0003(6) 0.0027(7) -0.0114(7)
C9' 0.0256(9) 0.0232(7) 0.0165(7) -0.0006(6) 0.0034(6) 0.0028(7)
C10' 0.0442(12) 0.0343(10) 0.0262(8) -0.0069(7) 0.0017(8) -0.0041(9)
C11' 0.0384(11) 0.0453(11) 0.0192(7) 0.0033(7) 0.0081(7) -0.0022(9)
C12' 0.0214(8) 0.0165(7) 0.0185(7) 0.0011(5) -0.0018(6) 0.0014(6)
C13' 0.0276(8) 0.0151(6) 0.0160(6) -0.0009(5) 0.0033(6) 0.0000(6)
C14' 0.0254(9) 0.0233(7) 0.0270(8) -0.0011(6) -0.0001(7) 0.0059(7)
C15' 0.0433(11) 0.0177(7) 0.0256(8) 0.0045(6) 0.0112(8) 0.0082(8)
C4A 0.0183(8) 0.0178(7) 0.0124(6) -0.0008(5) -0.0012(6) -0.0008(6)
C5A 0.0139(7) 0.0162(6) 0.0130(6) 0.0009(5) 0.0007(5) 0.0011(6)
C7A 0.0143(7) 0.0163(6) 0.0136(6) 0.0008(5) -0.0006(5) 0.0026(6)
C11A 0.0186(8) 0.0169(7) 0.0111(6) 0.0009(5) 0.0000(5) -0.0005(6)
C12A 0.0133(7) 0.0123(6) 0.0162(6) 0.0017(5) -0.0004(5) 0.0011(6)
C13A 0.0187(8) 0.0165(6) 0.0136(6) -0.0002(5) -0.0004(6) -0.0001(6)
C7B 0.0161(7) 0.0157(6) 0.0139(6) 0.0003(5) -0.0002(6) 0.0003(6)
C12B 0.0147(7) 0.0145(6) 0.0134(6) -0.0002(5) -0.0005(5) 0.0011(6)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.216(2) . ?
O2 C3 1.202(2) . ?
O3 C5' 1.2451(18) . ?
O4 C7 1.3489(17) . ?
O5 C4A 1.3749(17) . ?
O5 C5A 1.3929(16) . ?
O6 C11 1.435(2) . ?
O6 C10 1.4498(17) . ?
O12 C12A 1.3541(18) . ?
O12 C11A 1.4861(16) . ?
C1 C13A 1.4713(19) . ?
C1 C2 1.530(2) . ?
C2 C3 1.521(2) . ?
C2 C2' 1.525(2) . ?
C2 C1' 1.547(3) . ?
C3 C4 1.539(2) . ?
C4 C4A 1.5092(19) . ?
C4 C4' 1.540(2) . ?
C4 C3' 1.542(3) . ?
C6 C5A 1.4262(19) . ?
C6 C7 1.4342(19) . ?
C6 C5' 1.469(2) . ?
C7 C7A 1.379(2) . ?
C8 C7B 1.530(2) . ?
C8 C9 1.534(2) . ?
C9 C10 1.511(2) . ?
C9 C9' 1.547(2) . ?
C10 C11 1.476(2) . ?
C11 C11A 1.500(2) . ?
C13 C13A 1.5070(19) . ?
C13 C12B 1.5088(18) . ?
C13 C13' 1.561(2) . ?
C5' C6' 1.522(2) . ?
C6' C8' 1.525(2) . ?
C6' C7' 1.533(2) . ?
C9' C10' 1.522(2) . ?
C9' C11' 1.531(2) . ?
C12' C11A 1.517(2) . ?
C13' C15' 1.526(2) . ?
C13' C14' 1.528(2) . ?
C4A C13A 1.336(2) . ?
C5A C12B 1.382(2) . ?
C7A C12A 1.3784(19) . ?
C7A C7B 1.5003(19) . ?
C11A C7B 1.558(2) . ?
C12A C12B 1.4018(19) . ?
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
C4A O5 C5A 119.10(11) . . ?
C11 O6 C10 61.54(10) . . ?
C12A O12 C11A 106.95(11) . . ?
O1 C1 C13A 121.11(13) . . ?
O1 C1 C2 120.70(13) . . ?
C13A C1 C2 118.04(13) . . ?
C3 C2 C2' 110.41(14) . . ?
C3 C2 C1 112.36(13) . . ?
C2' C2 C1 110.66(14) . . ?
C3 C2 C1' 106.83(15) . . ?
C2' C2 C1' 110.28(14) . . ?
C1 C2 C1' 106.15(13) . . ?
O2 C3 C2 120.01(14) . . ?
O2 C3 C4 118.23(15) . . ?
C2 C3 C4 121.69(13) . . ?
C4A C4 C3 111.66(12) . . ?
C4A C4 C4' 110.01(13) . . ?
C3 C4 C4' 107.64(14) . . ?
C4A C4 C3' 110.19(14) . . ?
C3 C4 C3' 107.30(14) . . ?
C4' C4 C3' 109.96(14) . . ?
C5A C6 C7 115.81(13) . . ?
C5A C6 C5' 126.17(13) . . ?
C7 C6 C5' 117.99(12) . . ?
O4 C7 C7A 117.37(13) . . ?
O4 C7 C6 122.30(13) . . ?
C7A C7 C6 120.34(12) . . ?
C7B C8 C9 111.54(12) . . ?
C10 C9 C8 108.35(12) . . ?
C10 C9 C9' 109.75(13) . . ?
C8 C9 C9' 114.51(14) . . ?
O6 C10 C11 58.74(10) . . ?
O6 C10 C9 116.28(13) . . ?
C11 C10 C9 120.99(14) . . ?
O6 C11 C10 59.71(10) . . ?
O6 C11 C11A 118.69(13) . . ?
C10 C11 C11A 120.65(14) . . ?
C13A C13 C12B 108.64(11) . . ?
C13A C13 C13' 109.10(12) . . ?
C12B C13 C13' 113.28(12) . . ?
O3 C5' C6 119.02(13) . . ?
O3 C5' C6' 117.31(13) . . ?
C6 C5' C6' 123.53(13) . . ?
C5' C6' C8' 111.29(13) . . ?
C5' C6' C7' 109.16(12) . . ?
C8' C6' C7' 109.81(14) . . ?
C10' C9' C11' 109.67(14) . . ?
C10' C9' C9 112.66(14) . . ?
C11' C9' C9 111.05(15) . . ?
C15' C13' C14' 110.09(15) . . ?
C15' C13' C13 111.49(13) . . ?
C14' C13' C13 112.97(12) . . ?
C13A C4A O5 122.47(13) . . ?
C13A C4A C4 127.49(13) . . ?
O5 C4A C4 110.03(12) . . ?
C12B C5A O5 119.22(12) . . ?
C12B C5A C6 124.88(13) . . ?
O5 C5A C6 115.84(12) . . ?
C12A C7A C7 120.16(13) . . ?
C12A C7A C7B 109.26(13) . . ?
C7 C7A C7B 130.55(13) . . ?
O12 C11A C11 107.97(12) . . ?
O12 C11A C12' 106.52(12) . . ?
C11 C11A C12' 109.03(12) . . ?
O12 C11A C7B 105.24(11) . . ?
C11 C11A C7B 115.48(13) . . ?
C12' C11A C7B 112.09(12) . . ?
O12 C12A C7A 113.48(12) . . ?
O12 C12A C12B 122.99(13) . . ?
C7A C12A C12B 123.53(13) . . ?
C4A C13A C1 119.96(13) . . ?
C4A C13A C13 121.24(13) . . ?
C1 C13A C13 118.78(13) . . ?
C7A C7B C8 112.51(12) . . ?
C7A C7B C11A 101.09(11) . . ?
C8 C7B C11A 114.38(13) . . ?
C5A C12B C12A 115.16(12) . . ?
C5A C12B C13 121.71(12) . . ?
C12A C12B C13 123.13(13) . . ?
_refine_diff_density_max 0.212
_refine_diff_density_min -0.161
_refine_diff_density_rms 0.036
_shelx_res_file
;
TITL 3_2_hy in P2(1)2(1)2(1)
3_2_hy.res created by SHELXL-2016/4 at 15:18:35 on 09-Jan-2017
CELL 1.54178 6.3828 14.8993 32.6050 90.000 90.000 90.000
ZERR 4.00 0.0001 0.0001 0.0002 0.000 0.000 0.000
LATT -1
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM 0.5+X, 0.5-Y, -Z
SFAC C H O
UNIT 136 180 28
L.S. 4
ACTA
BOND
FMAP 2
PLAN 20
WGHT 0.040900 0.535200
EXTI 0.005161
FVAR 0.54524
MOLE 1
O1 3 0.028157 0.354519 0.016585 11.00000 0.03396 0.03138 =
0.01937 -0.00174 -0.00172 -0.01518
O2 3 0.371694 0.571661 -0.056364 11.00000 0.12459 0.03848 =
0.01844 0.00954 -0.01421 -0.04117
O3 3 0.586997 0.719105 0.186298 11.00000 0.03175 0.02014 =
0.02022 -0.00576 0.00049 -0.00718
O4 3 0.366542 0.619998 0.230145 11.00000 0.02561 0.01903 =
0.01555 -0.00434 -0.00007 -0.00454
AFIX 147
H4 2 0.440472 0.663255 0.224462 11.00000 -1.50000
AFIX 0
O5 3 0.467510 0.555587 0.086629 11.00000 0.02034 0.01719 =
0.01241 -0.00056 -0.00061 -0.00538
O6 3 -0.373237 0.401936 0.213651 11.00000 0.01715 0.04448 =
0.01769 0.00304 -0.00285 0.00507
O12 3 0.039823 0.372488 0.174206 11.00000 0.01818 0.01671 =
0.01197 0.00086 0.00126 -0.00244
C1 1 0.172979 0.407511 0.015289 11.00000 0.02262 0.01686 =
0.01565 -0.00013 -0.00135 -0.00226
C2 1 0.270460 0.434596 -0.025760 11.00000 0.02933 0.02103 =
0.01432 -0.00064 -0.00107 -0.00669
C3 1 0.357342 0.529615 -0.025042 11.00000 0.04434 0.02418 =
0.01611 0.00150 -0.00294 -0.01097
C4 1 0.439262 0.572720 0.014754 11.00000 0.02976 0.01733 =
0.01514 0.00095 -0.00064 -0.00638
C6 1 0.436397 0.589926 0.157929 11.00000 0.01468 0.01404 =
0.01657 0.00044 -0.00192 0.00144
C7 1 0.338188 0.569229 0.196345 11.00000 0.01577 0.01488 =
0.01504 -0.00117 -0.00254 0.00155
C8 1 -0.095065 0.524450 0.247228 11.00000 0.02351 0.01922 =
0.01973 0.00289 0.00395 0.00510
AFIX 23
H8A 2 -0.170613 0.541602 0.222633 11.00000 -1.20000
H8B 2 -0.038170 0.578513 0.259504 11.00000 -1.20000
AFIX 0
C9 1 -0.247021 0.479934 0.277452 11.00000 0.02012 0.02210 =
0.01943 0.00232 0.00427 0.00688
AFIX 13
H9 2 -0.362863 0.521700 0.282442 11.00000 -1.20000
AFIX 0
C10 1 -0.335923 0.396725 0.257447 11.00000 0.01644 0.03251 =
0.01600 0.00388 0.00136 0.00211
AFIX 13
H10 2 -0.439977 0.363378 0.273456 11.00000 -1.20000
AFIX 0
C11 1 -0.210385 0.343613 0.228180 11.00000 0.01764 0.02388 =
0.01554 0.00220 -0.00071 -0.00238
AFIX 13
H11 2 -0.242560 0.279330 0.227264 11.00000 -1.20000
AFIX 0
C13 1 0.239726 0.390695 0.092429 11.00000 0.01864 0.01446 =
0.01362 -0.00044 0.00027 -0.00288
AFIX 13
H13 2 0.096500 0.367041 0.093087 11.00000 -1.20000
AFIX 0
C1' 1 0.458906 0.370923 -0.032472 11.00000 0.03784 0.03115 =
0.02312 -0.00171 0.00685 0.00019
AFIX 137
H1'1 2 0.524952 0.384731 -0.058161 11.00000 -1.50000
H1'2 2 0.410717 0.309892 -0.032821 11.00000 -1.50000
H1'3 2 0.557955 0.378646 -0.010598 11.00000 -1.50000
AFIX 0
C2' 1 0.112264 0.424069 -0.060473 11.00000 0.04261 0.03443 =
0.01547 0.00065 -0.00571 -0.01194
AFIX 137
H2'1 2 -0.000235 0.466033 -0.056705 11.00000 -1.50000
H2'2 2 0.057463 0.364067 -0.060325 11.00000 -1.50000
H2'3 2 0.179967 0.435481 -0.086242 11.00000 -1.50000
AFIX 0
C3' 1 0.679263 0.580902 0.010664 11.00000 0.03180 0.02945 =
0.02226 0.00079 0.00691 -0.00931
AFIX 137
H3'1 2 0.733580 0.614643 0.033382 11.00000 -1.50000
H3'2 2 0.712950 0.611077 -0.014501 11.00000 -1.50000
H3'3 2 0.740629 0.522076 0.010566 11.00000 -1.50000
AFIX 0
C4' 1 0.340477 0.666674 0.018276 11.00000 0.03966 0.01882 =
0.02476 0.00532 -0.00535 -0.00121
AFIX 137
H4'1 2 0.191258 0.661029 0.020913 11.00000 -1.50000
H4'2 2 0.372828 0.700870 -0.005862 11.00000 -1.50000
H4'3 2 0.395747 0.696707 0.041972 11.00000 -1.50000
AFIX 0
C5' 1 0.578914 0.667295 0.156377 11.00000 0.01681 0.01591 =
0.01768 0.00056 -0.00359 0.00065
C6' 1 0.730413 0.684627 0.121210 11.00000 0.01841 0.01682 =
0.01801 0.00063 -0.00213 -0.00297
AFIX 13
H6' 2 0.651373 0.686370 0.095454 11.00000 -1.20000
AFIX 0
C7' 1 0.889693 0.607765 0.119112 11.00000 0.01766 0.02454 =
0.02400 0.00113 -0.00097 0.00135
AFIX 137
H7'1 2 0.969717 0.606192 0.144031 11.00000 -1.50000
H7'2 2 0.982058 0.617130 0.096272 11.00000 -1.50000
H7'3 2 0.817056 0.551835 0.115718 11.00000 -1.50000
AFIX 0
C8' 1 0.844527 0.773750 0.126679 11.00000 0.03215 0.02310 =
0.02816 -0.00030 0.00267 -0.01143
AFIX 137
H8'1 2 0.743985 0.821502 0.128516 11.00000 -1.50000
H8'2 2 0.934927 0.783952 0.103614 11.00000 -1.50000
H8'3 2 0.926507 0.771903 0.151350 11.00000 -1.50000
AFIX 0
C9' 1 -0.149066 0.455250 0.319363 11.00000 0.02563 0.02322 =
0.01651 -0.00055 0.00340 0.00280
AFIX 13
H9' 2 -0.054119 0.404454 0.314990 11.00000 -1.20000
AFIX 0
C10' 1 -0.021704 0.531714 0.337724 11.00000 0.04420 0.03434 =
0.02616 -0.00688 0.00173 -0.00412
AFIX 137
H10A 2 -0.107860 0.584327 0.339830 11.00000 -1.50000
H10B 2 0.096391 0.544222 0.320410 11.00000 -1.50000
H10C 2 0.026681 0.514818 0.364512 11.00000 -1.50000
AFIX 0
C11' 1 -0.317595 0.425438 0.349895 11.00000 0.03841 0.04528 =
0.01917 0.00334 0.00810 -0.00215
AFIX 137
H11A 2 -0.253144 0.410811 0.375645 11.00000 -1.50000
H11B 2 -0.388824 0.373588 0.339355 11.00000 -1.50000
H11C 2 -0.416459 0.473227 0.353825 11.00000 -1.50000
AFIX 0
C12' 1 0.154369 0.292878 0.234378 11.00000 0.02137 0.01646 =
0.01855 0.00111 -0.00175 0.00144
AFIX 137
H12A 2 0.117375 0.238001 0.220754 11.00000 -1.50000
H12B 2 0.137465 0.285626 0.263447 11.00000 -1.50000
H12C 2 0.297626 0.307491 0.228391 11.00000 -1.50000
AFIX 0
C13' 1 0.395854 0.310105 0.093260 11.00000 0.02756 0.01512 =
0.01603 -0.00089 0.00330 -0.00001
AFIX 13
H13' 2 0.377970 0.277008 0.067523 11.00000 -1.20000
AFIX 0
C14' 1 0.624860 0.339607 0.095546 11.00000 0.02543 0.02333 =
0.02704 -0.00110 -0.00011 0.00590
AFIX 137
H14A 2 0.648496 0.371244 0.120774 11.00000 -1.50000
H14B 2 0.655988 0.378361 0.072826 11.00000 -1.50000
H14C 2 0.713957 0.287750 0.094472 11.00000 -1.50000
AFIX 0
C15' 1 0.346281 0.245426 0.128231 11.00000 0.04325 0.01768 =
0.02556 0.00453 0.01123 0.00822
AFIX 137
H15A 2 0.431255 0.192581 0.125574 11.00000 -1.50000
H15B 2 0.200959 0.228994 0.127126 11.00000 -1.50000
H15C 2 0.375444 0.274015 0.153992 11.00000 -1.50000
AFIX 0
C4A 1 0.383923 0.517245 0.051939 11.00000 0.01832 0.01776 =
0.01235 -0.00084 -0.00123 -0.00080
C5A 1 0.389554 0.530574 0.124859 11.00000 0.01390 0.01616 =
0.01302 0.00094 0.00069 0.00110
C7A 1 0.209389 0.495321 0.199871 11.00000 0.01433 0.01633 =
0.01362 0.00078 -0.00063 0.00265
C11A 1 0.013191 0.367949 0.219437 11.00000 0.01858 0.01694 =
0.01106 0.00093 -0.00001 -0.00047
C12A 1 0.174687 0.440577 0.166476 11.00000 0.01333 0.01233 =
0.01621 0.00169 -0.00039 0.00107
C13A 1 0.269241 0.442259 0.053090 11.00000 0.01873 0.01647 =
0.01355 -0.00016 -0.00038 -0.00009
C7B 1 0.084679 0.461405 0.235664 11.00000 0.01607 0.01570 =
0.01388 0.00033 -0.00025 0.00030
AFIX 13
H7B 2 0.177339 0.453296 0.259342 11.00000 -1.20000
AFIX 0
C12B 1 0.267458 0.454325 0.128016 11.00000 0.01473 0.01450 =
0.01338 -0.00018 -0.00050 0.00107
HKLF 4
REM 3_2_hy in P2(1)2(1)2(1)
REM R1 = 0.0278 for 6103 Fo > 4sig(Fo) and 0.0283 for all 6184 data
REM 383 parameters refined using 0 restraints
END
WGHT 0.0409 0.5351
REM Highest difference peak 0.212, deepest hole -0.161, 1-sigma level 0.036
Q1 1 0.3024 0.4791 -0.0237 11.00000 0.05 0.21
Q2 1 0.4064 0.5491 0.0311 11.00000 0.05 0.21
Q3 1 0.0503 0.4160 0.2272 11.00000 0.05 0.20
Q4 1 0.3876 0.5832 0.1753 11.00000 0.05 0.20
Q5 1 0.2791 0.5014 0.1245 11.00000 0.05 0.20
Q6 1 0.3959 0.6148 0.0180 11.00000 0.05 0.20
Q7 1 0.3779 0.4659 0.0508 11.00000 0.05 0.19
Q8 1 0.3694 0.4825 0.1283 11.00000 0.05 0.19
Q9 1 0.5062 0.6202 0.1571 11.00000 0.05 0.19
Q10 1 0.3866 0.5549 -0.0014 11.00000 0.05 0.18
Q11 1 0.2550 0.4251 0.1114 11.00000 0.05 0.18
Q12 1 0.1899 0.4758 0.1837 11.00000 0.05 0.18
Q13 1 0.2485 0.4241 0.0718 11.00000 0.05 0.17
Q14 1 0.3326 0.3528 0.0937 11.00000 0.05 0.17
Q15 1 0.4699 0.6355 0.1540 11.00000 0.05 0.17
Q16 1 0.6410 0.6783 0.1358 11.00000 0.05 0.17
Q17 1 -0.0907 0.3652 0.2250 11.00000 0.05 0.17
Q18 1 0.2285 0.4295 0.0345 11.00000 0.05 0.16
Q19 1 0.2453 0.5355 0.1962 11.00000 0.05 0.16
Q20 1 0.2946 0.5246 0.2000 11.00000 0.05 0.16
;
_shelx_res_checksum 23577
#######################################################################
#
# 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_caojiaqing_bii41-53xi
_database_code_depnum_ccdc_archive 'CCDC 1526146'
_audit_update_record
;
2017-11-21 deposited with the CCDC.
2017-11-27 downloaded from the CCDC.
;
_audit_creation_date 2017-11-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C34 H46 O7'
_chemical_formula_sum 'C34 H46 O7'
_chemical_formula_weight 566.71
_chemical_absolute_configuration ad
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
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 orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
_symmetry_space_group_name_H-M_alt 'P 21 21 21'
_cell_length_a 12.4836(2)
_cell_length_b 12.5791(2)
_cell_length_c 20.1204(3)
_cell_angle_alpha 90.0
_cell_angle_beta 90.0
_cell_angle_gamma 90.0
_cell_volume 3159.58(9)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 23514
_cell_measurement_temperature 173.00(10)
_cell_measurement_theta_max 62.8160
_cell_measurement_theta_min 3.5280
_cell_oxdiff_angle_alpha 90.004(2)
_cell_oxdiff_angle_beta 89.988(2)
_cell_oxdiff_angle_gamma 90.035(3)
_cell_oxdiff_length_a 12.4785(4)
_cell_oxdiff_length_b 12.5787(4)
_cell_oxdiff_length_c 20.1295(6)
_cell_oxdiff_measurement_reflns_used 23515
_cell_oxdiff_volume 3159.58(17)
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.660
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.74933
_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.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.191
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description blocks
_exptl_crystal_F_000 1224
_exptl_crystal_size_max 0.43
_exptl_crystal_size_mid 0.33
_exptl_crystal_size_min 0.21
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0485
_diffrn_reflns_av_unetI/netI 0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 50336
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full 62.813
_diffrn_reflns_theta_max 62.813
_diffrn_reflns_theta_min 4.145
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 173.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 16.0288
_diffrn_detector_type Sapphire3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega 13.00 102.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 33.2434 57.0000 30.0000 89
#__ type_ start__ end____ width___ exp.time_
2 omega 32.00 110.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 33.2434 -178.0000 -120.0000 78
#__ type_ start__ end____ width___ exp.time_
3 omega 13.00 102.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 33.2434 57.0000 -60.0000 89
#__ type_ start__ end____ width___ exp.time_
4 omega 13.00 102.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 33.2434 57.0000 -120.0000 89
#__ type_ start__ end____ width___ exp.time_
5 omega 3.00 103.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 33.2434 77.0000 -180.0000 100
#__ type_ start__ end____ width___ exp.time_
6 omega 13.00 102.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 33.2434 57.0000 120.0000 89
#__ type_ start__ end____ width___ exp.time_
7 omega 19.00 129.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 -93.0000 -134.8622 110
#__ type_ start__ end____ width___ exp.time_
8 omega 19.00 129.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 -92.0000 133.6550 110
#__ type_ start__ end____ width___ exp.time_
9 omega 19.00 129.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 -93.0000 45.5231 110
#__ type_ start__ end____ width___ exp.time_
10 omega 37.00 164.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 15.0000 -150.0000 127
#__ type_ start__ end____ width___ exp.time_
11 omega 22.00 112.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 -61.0000 60.0000 90
#__ type_ start__ end____ width___ exp.time_
12 omega 18.00 69.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 -30.0000 30.0000 51
#__ type_ start__ end____ width___ exp.time_
13 omega 22.00 112.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 -61.0000 150.0000 90
#__ type_ start__ end____ width___ exp.time_
14 omega 19.00 127.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 -88.0000 80.3267 108
#__ type_ start__ end____ width___ exp.time_
15 omega 19.00 129.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 -93.0000 -153.6529 110
#__ type_ start__ end____ width___ exp.time_
16 omega 79.00 163.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 111.0000 -180.0000 84
#__ type_ start__ end____ width___ exp.time_
17 omega 19.00 77.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 -45.0000 -60.0000 58
#__ type_ start__ end____ width___ exp.time_
18 omega 19.00 77.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 -45.0000 -180.0000 58
#__ type_ start__ end____ width___ exp.time_
19 omega 22.00 112.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 -61.0000 120.0000 90
#__ type_ start__ end____ width___ exp.time_
20 omega 19.00 77.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 -45.0000 150.0000 58
#__ type_ start__ end____ width___ exp.time_
21 omega 61.00 163.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 30.0000 -90.0000 102
#__ type_ start__ end____ width___ exp.time_
22 omega 18.00 163.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 0.0000 60.0000 145
#__ type_ start__ end____ width___ exp.time_
23 omega 60.00 161.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 77.0000 -150.0000 101
#__ type_ start__ end____ width___ exp.time_
24 omega 60.00 161.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 77.0000 150.0000 101
#__ type_ start__ end____ width___ exp.time_
25 omega 69.00 159.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 61.0000 -180.0000 90
#__ type_ start__ end____ width___ exp.time_
26 omega 69.00 159.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 61.0000 -150.0000 90
#__ type_ start__ end____ width___ exp.time_
27 omega 19.00 129.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 -92.0000 141.5751 110
#__ type_ start__ end____ width___ exp.time_
28 omega 61.00 163.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 30.0000 -180.0000 102
#__ type_ start__ end____ width___ exp.time_
29 omega 18.00 90.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 -111.0000 120.0000 72
#__ type_ start__ end____ width___ exp.time_
30 omega 79.00 163.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 111.0000 -90.0000 84
#__ type_ start__ end____ width___ exp.time_
31 omega 19.00 71.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 -45.0000 -150.0000 52
#__ type_ start__ end____ width___ exp.time_
32 omega 39.00 66.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 15.0000 150.0000 27
#__ type_ start__ end____ width___ exp.time_
33 omega 124.00 150.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 15.0000 150.0000 26
#__ type_ start__ end____ width___ exp.time_
34 omega 58.00 114.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 27.0000 -6.0000 56
#__ type_ start__ end____ width___ exp.time_
35 omega 21.00 68.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 -30.0000 120.0000 47
#__ type_ start__ end____ width___ exp.time_
36 omega 66.00 92.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 -92.0000 6.4979 26
#__ type_ start__ end____ width___ exp.time_
37 omega 20.00 45.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 -95.0000 -90.0000 25
#__ type_ start__ end____ width___ exp.time_
38 omega 54.00 80.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 -95.0000 -90.0000 26
#__ type_ start__ end____ width___ exp.time_
39 omega 62.00 89.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 -111.0000 -120.0000 27
#__ type_ start__ end____ width___ exp.time_
40 omega 90.00 118.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 -93.0000 -71.9672 28
#__ type_ start__ end____ width___ exp.time_
41 omega 33.00 76.00 1.0000 1.3450
omega____ theta____ kappa____ phi______ frames
- 90.5000 -93.0000 -71.9672 43
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 -0.0350818000
_diffrn_orient_matrix_UB_12 0.1173896000
_diffrn_orient_matrix_UB_13 -0.0011997000
_diffrn_orient_matrix_UB_21 -0.1109208000
_diffrn_orient_matrix_UB_22 -0.0319700000
_diffrn_orient_matrix_UB_23 0.0270634000
_diffrn_orient_matrix_UB_31 0.0413261000
_diffrn_orient_matrix_UB_32 0.0140658000
_diffrn_orient_matrix_UB_33 0.0715763000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'sealed X-ray tube'
_diffrn_source_type 'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage 0.766
_reflns_Friedel_fraction_full 0.993
_reflns_Friedel_fraction_max 0.993
_reflns_number_gt 4934
_reflns_number_total 5062
_reflns_odcompleteness_completeness 97.24
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 63.60
_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 'XH (Sheldrick, 2008)'
_computing_structure_solution 'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max 0.492
_refine_diff_density_min -0.369
_refine_diff_density_rms 0.040
_refine_ls_abs_structure_details
;
Flack x determined using 2087 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack -0.10(10)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.043
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 391
_refine_ls_number_reflns 5062
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0464
_refine_ls_R_factor_gt 0.0456
_refine_ls_restrained_S_all 1.043
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+1.0445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1213
_refine_ls_wR_factor_ref 0.1222
_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,H,H) groups, All O(H) groups
2. Others
Sof(H13A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(H14D)=Sof(H14E)=Sof(H14F)=
Sof(C13")=Sof(H13")=1-FVAR(1)
Sof(H13)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
Sof(C13')=Sof(H13')=FVAR(1)
3.a Riding coordinates:
O3(H3)
3.b Ternary CH refined with riding coordinates:
C6'(H6'), C7B(H7B), C13(H13), C13(H13A), C9(H9), C9'(H9'), C13'(H13'),
C13"(H13")
3.c Secondary CH2 refined with riding coordinates:
C8(H8A,H8B)
3.d Me refined with riding coordinates:
C15'(H15A,H15B,H15C), C15'(H15D,H15E,H15F), C14'(H14A,H14B,H14C), C14'(H14D,
H14E,H14F)
3.e Aromatic/amide H refined with riding coordinates:
C11(H11), C10(H10)
3.f Idealised Me refined as rotating group:
C7'(H7'A,H7'B,H7'C), C10'(H10A,H10B,H10C), C8'(H8'A,H8'B,H8'C), C12'(H12A,
H12B,H12C), C2'(H2'A,H2'B,H2'C), C4'(H4'A,H4'B,H4'C), C1'(H1'A,H1'B,H1'C),
C3'(H3'A,H3'B,H3'C), C11'(H11A,H11B,H11C)
3.g Idealised tetrahedral OH refined as rotating group:
O4(H4), O6(H6)
;
_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
O4 O 0.68147(16) 0.75411(19) 0.19988(11) 0.0447(5) Uani 1 1 d . . . . .
H4 H 0.665621 0.745408 0.239056 0.067 Uiso 1 1 calc GR . . . .
O6 O 0.99633(18) 0.6824(2) 0.07107(11) 0.0510(6) Uani 1 1 d . . . . .
H6 H 0.980514 0.739954 0.054682 0.077 Uiso 1 1 calc GR . . . .
O7 O 0.88443(17) 0.43260(16) 0.22323(10) 0.0395(5) Uani 1 1 d . . . . .
O3 O 0.83032(19) 0.42968(18) 0.35497(11) 0.0510(6) Uani 1 1 d . . . . .
H3 H 0.866643 0.407778 0.321721 0.076 Uiso 1 1 d R . . . .
O5 O 0.8956(2) 0.8497(2) 0.05580(13) 0.0599(7) Uani 1 1 d . . . . .
O1 O 0.6223(2) 0.7348(2) 0.32460(12) 0.0670(8) Uani 1 1 d . . . . .
O2 O 0.6991(4) 0.6117(4) 0.53854(14) 0.1181(17) Uani 1 1 d . . . . .
C7A C 0.9383(2) 0.5611(2) 0.15041(14) 0.0343(6) Uani 1 1 d . . . . .
C7 C 0.9240(2) 0.6565(2) 0.11770(13) 0.0337(6) Uani 1 1 d . . . . .
C5A C 0.7629(2) 0.6878(2) 0.18343(13) 0.0325(6) Uani 1 1 d . . . . .
C12A C 0.8621(2) 0.5308(2) 0.19657(13) 0.0318(6) Uani 1 1 d . . . . .
C6 C 0.8350(2) 0.7237(2) 0.13287(13) 0.0323(6) Uani 1 1 d . . . . .
C6' C 0.7259(3) 0.8937(2) 0.09766(15) 0.0398(7) Uani 1 1 d . . . . .
H6' H 0.706039 0.905640 0.144185 0.048 Uiso 1 1 calc R . . . .
C2 C 0.6464(3) 0.6832(3) 0.43625(15) 0.0445(7) Uani 1 1 d . . . . .
C12B C 0.7726(2) 0.5895(2) 0.21453(13) 0.0315(6) Uani 1 1 d . . . . .
C11 C 1.0626(3) 0.4499(3) 0.26415(17) 0.0478(8) Uani 1 1 d . . . . .
H11 H 1.049993 0.419876 0.305661 0.057 Uiso 1 1 calc R . . . .
C5' C 0.8238(2) 0.8226(3) 0.09526(15) 0.0389(7) Uani 1 1 d . . . . .
C10 C 1.1349(3) 0.5257(3) 0.25995(17) 0.0487(8) Uani 1 1 d . . . . .
H10 H 1.165678 0.549331 0.299349 0.058 Uiso 1 1 calc R . . . .
C13A C 0.7090(2) 0.5705(2) 0.33573(13) 0.0333(6) Uani 1 1 d . . . . .
C1 C 0.6598(2) 0.6659(3) 0.36174(15) 0.0417(7) Uani 1 1 d . . . . .
C4A C 0.7715(2) 0.5117(2) 0.37577(14) 0.0367(7) Uani 1 1 d . . . . .
C7B C 1.0204(2) 0.4745(3) 0.14311(15) 0.0408(7) Uani 1 1 d . . . . .
H7B H 1.002473 0.431466 0.104035 0.049 Uiso 1 1 calc R . . . .
C4 C 0.7866(3) 0.5269(3) 0.44989(15) 0.0434(7) Uani 1 1 d . . . . .
C7' C 0.6336(3) 0.8375(3) 0.06231(17) 0.0502(8) Uani 1 1 d . . . . .
H7'A H 0.652736 0.824881 0.016780 0.075 Uiso 1 1 calc GR . . . .
H7'B H 0.570770 0.881467 0.064032 0.075 Uiso 1 1 calc GR . . . .
H7'C H 0.619261 0.770983 0.083890 0.075 Uiso 1 1 calc GR . . . .
C13 C 0.6904(3) 0.5430(3) 0.26262(15) 0.0510(9) Uani 1 1 d . . . . .
H13 H 0.631848 0.592950 0.253843 0.061 Uiso 0.497(10) 1 calc R . P A 1
H13A H 0.716693 0.469625 0.263412 0.061 Uiso 0.503(10) 1 calc R . P A 2
C8 C 1.1367(3) 0.5090(3) 0.13817(17) 0.0463(8) Uani 1 1 d . . . . .
H8A H 1.181938 0.446398 0.135933 0.056 Uiso 1 1 calc R . . . .
H8B H 1.146761 0.548969 0.097411 0.056 Uiso 1 1 calc R . . . .
C9 C 1.1714(2) 0.5769(3) 0.19669(17) 0.0457(7) Uani 1 1 d . . . . .
H9 H 1.134210 0.645301 0.192927 0.055 Uiso 1 1 calc R . . . .
C10' C 1.3278(4) 0.6542(5) 0.1338(3) 0.0857(15) Uani 1 1 d . . . . .
H10A H 1.319707 0.605917 0.097158 0.129 Uiso 1 1 calc GR . . . .
H10B H 1.401526 0.675003 0.137508 0.129 Uiso 1 1 calc GR . . . .
H10C H 1.284348 0.716058 0.126275 0.129 Uiso 1 1 calc GR . . . .
C8' C 0.7486(4) 1.0005(3) 0.06491(19) 0.0582(9) Uani 1 1 d . . . . .
H8'A H 0.812183 1.030908 0.083853 0.087 Uiso 1 1 calc GR . . . .
H8'B H 0.689149 1.047515 0.072202 0.087 Uiso 1 1 calc GR . . . .
H8'C H 0.758743 0.990469 0.018034 0.087 Uiso 1 1 calc GR . . . .
C12' C 1.0071(4) 0.2889(3) 0.1975(2) 0.0704(12) Uani 1 1 d . . . . .
H12A H 0.992053 0.254601 0.239052 0.106 Uiso 1 1 calc GR . . . .
H12B H 1.078181 0.270550 0.183233 0.106 Uiso 1 1 calc GR . . . .
H12C H 0.956305 0.265810 0.164690 0.106 Uiso 1 1 calc GR . . . .
C11A C 0.9990(3) 0.4085(2) 0.20601(17) 0.0448(7) Uani 1 1 d . . . . .
C3 C 0.7108(3) 0.6076(4) 0.47908(16) 0.0580(10) Uani 1 1 d . . . . .
C15' C 0.5871(4) 0.4580(5) 0.17139(19) 0.0803(16) Uani 1 1 d . . . . .
H15A H 0.549509 0.393979 0.160008 0.120 Uiso 0.497(10) 1 calc R . P A 1
H15B H 0.538838 0.517268 0.169262 0.120 Uiso 0.497(10) 1 calc R . P A 1
H15C H 0.644959 0.468818 0.140663 0.120 Uiso 0.497(10) 1 calc R . P A 1
H15D H 0.515996 0.444256 0.155459 0.120 Uiso 0.503(10) 1 calc R . P A 2
H15E H 0.625745 0.498752 0.138931 0.120 Uiso 0.503(10) 1 calc R . P A 2
H15F H 0.623460 0.391796 0.178898 0.120 Uiso 0.503(10) 1 calc R . P A 2
C2' C 0.5275(4) 0.6618(5) 0.4509(2) 0.0787(14) Uani 1 1 d . . . . .
H2'A H 0.483875 0.706243 0.423152 0.118 Uiso 1 1 calc GR . . . .
H2'B H 0.512794 0.677266 0.496776 0.118 Uiso 1 1 calc GR . . . .
H2'C H 0.511447 0.588496 0.442096 0.118 Uiso 1 1 calc GR . . . .
C4' C 0.9025(3) 0.5633(4) 0.4631(2) 0.0704(12) Uani 1 1 d . . . . .
H4'A H 0.915528 0.629120 0.440442 0.106 Uiso 1 1 calc GR . . . .
H4'B H 0.951391 0.510178 0.447221 0.106 Uiso 1 1 calc GR . . . .
H4'C H 0.912689 0.573133 0.510029 0.106 Uiso 1 1 calc GR . . . .
C14' C 0.5267(4) 0.4401(4) 0.28942(19) 0.0773(14) Uani 1 1 d . . . . .
H14A H 0.490073 0.375279 0.278661 0.116 Uiso 0.497(10) 1 calc R . P A 1
H14B H 0.543345 0.441044 0.335999 0.116 Uiso 0.497(10) 1 calc R . P A 1
H14C H 0.481663 0.499623 0.278860 0.116 Uiso 0.497(10) 1 calc R . P A 1
H14D H 0.455048 0.424481 0.275159 0.116 Uiso 0.503(10) 1 calc R . P A 2
H14E H 0.567849 0.375677 0.290696 0.116 Uiso 0.503(10) 1 calc R . P A 2
H14F H 0.524817 0.471265 0.332963 0.116 Uiso 0.503(10) 1 calc R . P A 2
C9' C 1.2927(3) 0.6001(3) 0.1973(2) 0.0610(10) Uani 1 1 d . . . . .
H9' H 1.330822 0.532261 0.200881 0.073 Uiso 1 1 calc R . . . .
C1' C 0.6705(6) 0.7978(4) 0.4540(3) 0.107(2) Uani 1 1 d . . . . .
H1'A H 0.746368 0.809563 0.452078 0.161 Uiso 1 1 calc GR . . . .
H1'B H 0.645039 0.812325 0.498069 0.161 Uiso 1 1 calc GR . . . .
H1'C H 0.635188 0.844052 0.422970 0.161 Uiso 1 1 calc GR . . . .
C3' C 0.7677(5) 0.4215(3) 0.48551(19) 0.0745(13) Uani 1 1 d . . . . .
H3'A H 0.773101 0.432101 0.532649 0.112 Uiso 1 1 calc GR . . . .
H3'B H 0.820650 0.370878 0.471532 0.112 Uiso 1 1 calc GR . . . .
H3'C H 0.697624 0.395332 0.474776 0.112 Uiso 1 1 calc GR . . . .
C11' C 1.3238(4) 0.6690(5) 0.2570(3) 0.0889(16) Uani 1 1 d . . . . .
H11A H 1.315122 0.628741 0.297193 0.133 Uiso 1 1 calc GR . . . .
H11B H 1.278639 0.730703 0.258531 0.133 Uiso 1 1 calc GR . . . .
H11C H 1.397217 0.690727 0.252759 0.133 Uiso 1 1 calc GR . . . .
C13' C 0.6354(5) 0.4475(5) 0.2472(3) 0.039(2) Uani 0.497(10) 1 d . . P A 1
H13' H 0.680675 0.384518 0.252756 0.047 Uiso 0.497(10) 1 calc R . P A 1
C13" C 0.5810(4) 0.5221(5) 0.2383(3) 0.0322(18) Uani 0.503(10) 1 d . . P A 2
H13" H 0.539141 0.587537 0.233616 0.039 Uiso 0.503(10) 1 calc R . P A 2
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
O4 0.0338(10) 0.0658(14) 0.0345(11) 0.0107(11) 0.0096(9) 0.0145(10)
O6 0.0364(11) 0.0754(16) 0.0413(12) 0.0214(12) 0.0168(10) 0.0103(11)
O7 0.0427(11) 0.0378(10) 0.0381(11) 0.0016(9) 0.0069(9) 0.0015(9)
O3 0.0637(15) 0.0512(13) 0.0380(12) 0.0031(10) 0.0110(10) 0.0146(11)
O5 0.0442(13) 0.0752(16) 0.0603(15) 0.0325(13) 0.0137(12) 0.0075(12)
O1 0.0783(18) 0.0828(18) 0.0397(13) 0.0171(13) 0.0173(12) 0.0372(16)
O2 0.139(3) 0.178(4) 0.0368(16) -0.007(2) 0.0031(18) 0.080(3)
C7A 0.0304(13) 0.0472(16) 0.0252(13) -0.0017(12) 0.0017(11) 0.0003(12)
C7 0.0244(13) 0.0535(17) 0.0233(13) 0.0030(12) 0.0028(10) 0.0002(12)
C5A 0.0219(12) 0.0488(15) 0.0269(13) -0.0009(12) -0.0006(10) 0.0017(12)
C12A 0.0337(14) 0.0375(14) 0.0240(13) -0.0023(11) 0.0002(12) -0.0050(12)
C6 0.0258(13) 0.0468(16) 0.0243(13) 0.0034(12) -0.0013(10) -0.0002(11)
C6' 0.0409(16) 0.0459(16) 0.0325(14) 0.0020(13) -0.0047(13) 0.0064(13)
C2 0.0560(19) 0.0436(16) 0.0339(16) -0.0005(13) 0.0125(14) -0.0025(15)
C12B 0.0262(13) 0.0446(15) 0.0238(13) -0.0003(11) 0.0011(10) -0.0052(12)
C11 0.0474(18) 0.0560(19) 0.0401(17) 0.0137(15) -0.0010(14) 0.0145(16)
C5' 0.0326(14) 0.0538(18) 0.0303(15) 0.0050(13) -0.0031(12) -0.0022(13)
C10 0.0418(17) 0.062(2) 0.0425(17) 0.0042(15) -0.0057(14) 0.0127(16)
C13A 0.0290(13) 0.0436(15) 0.0274(14) 0.0017(12) 0.0058(11) -0.0077(12)
C1 0.0388(16) 0.0551(18) 0.0312(15) 0.0062(14) 0.0098(13) 0.0049(14)
C4A 0.0369(15) 0.0405(15) 0.0328(15) 0.0016(12) 0.0060(12) -0.0067(13)
C7B 0.0407(16) 0.0481(16) 0.0335(15) -0.0066(13) 0.0052(13) 0.0075(13)
C4 0.0429(17) 0.0572(18) 0.0300(15) 0.0046(14) -0.0009(13) 0.0003(15)
C7' 0.0416(17) 0.069(2) 0.0402(17) -0.0039(16) -0.0119(14) 0.0089(16)
C13 0.0398(16) 0.085(3) 0.0282(15) -0.0018(16) 0.0042(13) -0.0282(17)
C8 0.0349(15) 0.060(2) 0.0436(17) 0.0022(15) 0.0063(14) 0.0127(14)
C9 0.0361(15) 0.0528(18) 0.0481(18) 0.0050(15) -0.0026(13) 0.0096(14)
C10' 0.049(2) 0.113(4) 0.096(4) 0.026(3) 0.006(2) -0.013(2)
C8' 0.072(2) 0.054(2) 0.049(2) 0.0096(16) 0.0030(18) 0.0067(18)
C12' 0.084(3) 0.0411(19) 0.086(3) -0.0054(19) 0.020(3) 0.0116(19)
C11A 0.0465(17) 0.0399(16) 0.0482(18) 0.0015(14) 0.0107(14) 0.0118(14)
C3 0.065(2) 0.082(3) 0.0273(16) -0.0021(16) 0.0029(15) 0.009(2)
C15' 0.068(2) 0.134(4) 0.039(2) -0.023(2) 0.0086(18) -0.052(3)
C2' 0.064(3) 0.122(4) 0.050(2) 0.008(2) 0.024(2) 0.004(3)
C4' 0.054(2) 0.107(3) 0.050(2) -0.008(2) -0.0095(17) -0.010(2)
C14' 0.071(3) 0.113(4) 0.048(2) -0.009(2) 0.0156(19) -0.060(3)
C9' 0.0379(18) 0.072(2) 0.073(3) 0.011(2) -0.0056(18) 0.0033(17)
C1' 0.199(7) 0.061(3) 0.063(3) -0.007(2) 0.013(4) -0.042(4)
C3' 0.113(4) 0.072(3) 0.0386(19) 0.0170(18) 0.002(2) -0.009(3)
C11' 0.059(3) 0.107(4) 0.100(4) -0.002(3) -0.015(3) -0.017(3)
C13' 0.032(3) 0.042(4) 0.042(3) -0.005(3) 0.000(3) -0.007(3)
C13" 0.021(3) 0.043(3) 0.034(3) 0.000(2) -0.003(2) -0.002(2)
_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
O4 C5A 1.356(3) . ?
O6 C7 1.342(3) . ?
O7 C12A 1.375(3) . ?
O7 C11A 1.503(4) . ?
O3 C4A 1.334(4) . ?
O5 C5' 1.245(4) . ?
O1 C1 1.236(4) . ?
O2 C3 1.206(5) . ?
C7A C7 1.380(4) . ?
C7A C12A 1.384(4) . ?
C7A C7B 1.503(4) . ?
C7 C6 1.429(4) . ?
C5A C6 1.432(4) . ?
C5A C12B 1.391(4) . ?
C12A C12B 1.387(4) . ?
C6 C5' 1.463(4) . ?
C6' C5' 1.515(4) . ?
C6' C7' 1.527(5) . ?
C6' C8' 1.523(5) . ?
C2 C1 1.524(4) . ?
C2 C3 1.514(5) . ?
C2 C2' 1.538(6) . ?
C2 C1' 1.515(5) . ?
C12B C13 1.526(4) . ?
C11 C10 1.315(5) . ?
C11 C11A 1.506(5) . ?
C10 C9 1.498(5) . ?
C13A C1 1.446(4) . ?
C13A C4A 1.344(4) . ?
C13A C13 1.529(4) . ?
C4A C4 1.515(4) . ?
C7B C8 1.519(5) . ?
C7B C11A 1.537(5) . ?
C4 C3 1.507(5) . ?
C4 C4' 1.541(5) . ?
C4 C3' 1.525(5) . ?
C13 C13' 1.418(7) . ?
C13 C13" 1.475(6) . ?
C8 C9 1.518(5) . ?
C9 C9' 1.543(5) . ?
C10' C9' 1.514(6) . ?
C12' C11A 1.518(5) . ?
C15' C13' 1.646(7) . ?
C15' C13" 1.570(7) . ?
C14' C13' 1.603(7) . ?
C14' C13" 1.606(7) . ?
C9' C11' 1.531(7) . ?
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
C12A O7 C11A 106.5(2) . . ?
C7 C7A C12A 118.1(3) . . ?
C7 C7A C7B 132.2(3) . . ?
C12A C7A C7B 109.5(3) . . ?
O6 C7 C7A 117.2(3) . . ?
O6 C7 C6 121.9(3) . . ?
C7A C7 C6 120.9(2) . . ?
O4 C5A C6 116.8(3) . . ?
O4 C5A C12B 120.2(2) . . ?
C12B C5A C6 123.1(3) . . ?
O7 C12A C7A 111.7(2) . . ?
O7 C12A C12B 122.7(2) . . ?
C7A C12A C12B 125.6(3) . . ?
C7 C6 C5A 117.0(3) . . ?
C7 C6 C5' 117.9(2) . . ?
C5A C6 C5' 125.1(3) . . ?
C5' C6' C7' 108.7(3) . . ?
C5' C6' C8' 110.9(3) . . ?
C8' C6' C7' 110.3(3) . . ?
C1 C2 C2' 105.7(3) . . ?
C3 C2 C1 114.4(3) . . ?
C3 C2 C2' 107.1(3) . . ?
C3 C2 C1' 111.0(4) . . ?
C1' C2 C1 110.2(3) . . ?
C1' C2 C2' 108.2(4) . . ?
C5A C12B C13 124.6(3) . . ?
C12A C12B C5A 115.2(2) . . ?
C12A C12B C13 120.1(3) . . ?
C10 C11 C11A 124.2(3) . . ?
O5 C5' C6 119.5(3) . . ?
O5 C5' C6' 116.1(3) . . ?
C6 C5' C6' 124.3(3) . . ?
C11 C10 C9 125.1(3) . . ?
C1 C13A C13 118.1(3) . . ?
C4A C13A C1 119.1(3) . . ?
C4A C13A C13 122.7(3) . . ?
O1 C1 C2 117.0(3) . . ?
O1 C1 C13A 121.6(3) . . ?
C13A C1 C2 121.4(3) . . ?
O3 C4A C13A 123.9(3) . . ?
O3 C4A C4 109.8(3) . . ?
C13A C4A C4 126.4(3) . . ?
C7A C7B C8 116.8(3) . . ?
C7A C7B C11A 101.1(2) . . ?
C8 C7B C11A 112.0(3) . . ?
C4A C4 C4' 108.9(3) . . ?
C4A C4 C3' 109.5(3) . . ?
C3 C4 C4A 113.0(3) . . ?
C3 C4 C4' 108.8(3) . . ?
C3 C4 C3' 107.8(3) . . ?
C3' C4 C4' 108.7(4) . . ?
C12B C13 C13A 114.9(2) . . ?
C13' C13 C12B 120.8(4) . . ?
C13' C13 C13A 118.4(4) . . ?
C13" C13 C12B 118.7(3) . . ?
C13" C13 C13A 120.0(3) . . ?
C9 C8 C7B 112.5(3) . . ?
C10 C9 C8 109.3(3) . . ?
C10 C9 C9' 111.9(3) . . ?
C8 C9 C9' 113.1(3) . . ?
O7 C11A C11 104.7(2) . . ?
O7 C11A C7B 104.2(2) . . ?
O7 C11A C12' 106.8(3) . . ?
C11 C11A C7B 111.2(3) . . ?
C11 C11A C12' 113.3(3) . . ?
C12' C11A C7B 115.5(3) . . ?
O2 C3 C2 118.3(4) . . ?
O2 C3 C4 119.4(4) . . ?
C4 C3 C2 122.3(3) . . ?
C10' C9' C9 111.2(3) . . ?
C10' C9' C11' 109.6(4) . . ?
C11' C9' C9 111.3(4) . . ?
C13 C13' C15' 108.2(5) . . ?
C13 C13' C14' 110.1(4) . . ?
C14' C13' C15' 100.7(4) . . ?
C13 C13" C15' 109.3(4) . . ?
C13 C13" C14' 107.0(4) . . ?
C15' C13" C14' 103.9(4) . . ?
_iucr_refine_instructions_details
;
TITL CAOJIAQING_BII41-53xi in P212121 #19
caojiaqing_bii41-53xi.res
created by SHELXL-2017/1 at 13:56:42 on 19-Nov-2017
REM reset to P212121 #19
CELL 1.54184 12.483645 12.579134 20.120412 90 90 90
ZERR 4 0.000198 0.000212 0.000305 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,-Z
SYMM -X,0.5+Y,0.5-Z
SFAC C H O
UNIT 136 184 28
L.S. 20
PLAN 10
BOND
fmap 2
acta
REM
REM
REM
WGHT 0.071200 1.044500
FVAR 7.61756 0.49661
O4 3 0.681472 0.754114 0.199882 11.00000 0.03380 0.06582 =
0.03449 0.01069 0.00955 0.01453
AFIX 147
H4 2 0.665621 0.745408 0.239056 11.00000 -1.50000
AFIX 0
O6 3 0.996329 0.682368 0.071067 11.00000 0.03637 0.07540 =
0.04128 0.02136 0.01682 0.01029
AFIX 147
H6 2 0.980514 0.739954 0.054682 11.00000 -1.50000
AFIX 0
O7 3 0.884432 0.432601 0.223226 11.00000 0.04266 0.03776 =
0.03815 0.00164 0.00694 0.00146
O3 3 0.830323 0.429678 0.354971 11.00000 0.06371 0.05117 =
0.03798 0.00315 0.01099 0.01459
AFIX 3
H3 2 0.866643 0.407778 0.321721 11.00000 -1.50000
AFIX 0
O5 3 0.895607 0.849657 0.055798 11.00000 0.04421 0.07516 =
0.06033 0.03251 0.01371 0.00747
O1 3 0.622325 0.734784 0.324603 11.00000 0.07831 0.08279 =
0.03975 0.01714 0.01729 0.03716
O2 3 0.699098 0.611660 0.538539 11.00000 0.13915 0.17843 =
0.03684 -0.00680 0.00312 0.07973
C7A 1 0.938319 0.561144 0.150412 11.00000 0.03044 0.04721 =
0.02518 -0.00168 0.00166 0.00033
C7 1 0.924040 0.656514 0.117703 11.00000 0.02441 0.05355 =
0.02329 0.00304 0.00284 0.00019
C5A 1 0.762863 0.687773 0.183429 11.00000 0.02190 0.04877 =
0.02689 -0.00091 -0.00060 0.00167
C12A 1 0.862058 0.530791 0.196574 11.00000 0.03374 0.03751 =
0.02403 -0.00226 0.00021 -0.00504
C6 1 0.835042 0.723746 0.132874 11.00000 0.02585 0.04683 =
0.02429 0.00335 -0.00131 -0.00015
C6' 1 0.725894 0.893694 0.097657 11.00000 0.04087 0.04594 =
0.03249 0.00204 -0.00471 0.00638
AFIX 13
H6' 2 0.706039 0.905640 0.144185 11.00000 -1.20000
AFIX 0
C2 1 0.646398 0.683166 0.436254 11.00000 0.05603 0.04365 =
0.03389 -0.00053 0.01248 -0.00252
C12B 1 0.772579 0.589518 0.214534 11.00000 0.02615 0.04462 =
0.02377 -0.00027 0.00108 -0.00524
C11 1 1.062621 0.449868 0.264146 11.00000 0.04736 0.05600 =
0.04009 0.01374 -0.00096 0.01448
AFIX 43
H11 2 1.049993 0.419876 0.305661 11.00000 -1.20000
AFIX 0
C5' 1 0.823755 0.822627 0.095256 11.00000 0.03256 0.05376 =
0.03025 0.00502 -0.00310 -0.00221
C10 1 1.134855 0.525688 0.259951 11.00000 0.04182 0.06183 =
0.04252 0.00420 -0.00566 0.01271
AFIX 43
H10 2 1.165678 0.549331 0.299349 11.00000 -1.20000
AFIX 0
C13A 1 0.709022 0.570515 0.335728 11.00000 0.02897 0.04363 =
0.02735 0.00175 0.00578 -0.00765
C1 1 0.659762 0.665920 0.361736 11.00000 0.03879 0.05511 =
0.03120 0.00621 0.00977 0.00494
C4A 1 0.771520 0.511710 0.375771 11.00000 0.03686 0.04049 =
0.03280 0.00158 0.00604 -0.00668
C7B 1 1.020372 0.474454 0.143108 11.00000 0.04065 0.04812 =
0.03349 -0.00663 0.00522 0.00747
AFIX 13
H7B 2 1.002473 0.431466 0.104035 11.00000 -1.20000
AFIX 0
C4 1 0.786567 0.526912 0.449894 11.00000 0.04290 0.05724 =
0.03000 0.00460 -0.00091 0.00028
C7' 1 0.633595 0.837542 0.062308 11.00000 0.04162 0.06865 =
0.04023 -0.00394 -0.01186 0.00889
AFIX 137
H7'A 2 0.652736 0.824881 0.016780 11.00000 -1.50000
H7'B 2 0.570770 0.881467 0.064032 11.00000 -1.50000
H7'C 2 0.619261 0.770983 0.083890 11.00000 -1.50000
AFIX 0
C13 1 0.690437 0.543034 0.262618 11.00000 0.03976 0.08509 =
0.02816 -0.00178 0.00416 -0.02820
PART 1
AFIX 13
H13 2 0.631848 0.592950 0.253843 21.00000 -1.20000
AFIX 13
PART 0
PART 2
H13A 2 0.716693 0.469625 0.263412 -21.00000 -1.20000
AFIX 0
PART 0
C8 1 1.136715 0.509002 0.138166 11.00000 0.03493 0.06032 =
0.04358 0.00217 0.00633 0.01273
AFIX 23
H8A 2 1.181938 0.446398 0.135933 11.00000 -1.20000
H8B 2 1.146761 0.548969 0.097411 11.00000 -1.20000
AFIX 0
C9 1 1.171358 0.576933 0.196687 11.00000 0.03608 0.05285 =
0.04809 0.00501 -0.00259 0.00956
AFIX 13
H9 2 1.134210 0.645301 0.192927 11.00000 -1.20000
AFIX 0
C10' 1 1.327778 0.654224 0.133755 11.00000 0.04895 0.11271 =
0.09554 0.02586 0.00645 -0.01253
AFIX 137
H10A 2 1.319707 0.605917 0.097158 11.00000 -1.50000
H10B 2 1.401526 0.675003 0.137508 11.00000 -1.50000
H10C 2 1.284348 0.716058 0.126275 11.00000 -1.50000
AFIX 0
C8' 1 0.748590 1.000521 0.064909 11.00000 0.07171 0.05353 =
0.04930 0.00958 0.00296 0.00673
AFIX 137
H8'A 2 0.812183 1.030908 0.083853 11.00000 -1.50000
H8'B 2 0.689149 1.047515 0.072202 11.00000 -1.50000
H8'C 2 0.758743 0.990469 0.018034 11.00000 -1.50000
AFIX 0
C12' 1 1.007138 0.288872 0.197460 11.00000 0.08406 0.04111 =
0.08607 -0.00544 0.01951 0.01165
AFIX 137
H12A 2 0.992053 0.254601 0.239052 11.00000 -1.50000
H12B 2 1.078181 0.270550 0.183233 11.00000 -1.50000
H12C 2 0.956305 0.265810 0.164690 11.00000 -1.50000
AFIX 0
C11A 1 0.999036 0.408503 0.206008 11.00000 0.04646 0.03986 =
0.04818 0.00145 0.01073 0.01176
C3 1 0.710789 0.607609 0.479083 11.00000 0.06501 0.08185 =
0.02726 -0.00208 0.00287 0.00878
C15' 1 0.587150 0.457990 0.171391 11.00000 0.06756 0.13395 =
0.03931 -0.02254 0.00855 -0.05173
PART 1
AFIX 33
H15A 2 0.549509 0.393979 0.160008 21.00000 -1.50000
H15B 2 0.538838 0.517268 0.169262 21.00000 -1.50000
H15C 2 0.644959 0.468818 0.140663 21.00000 -1.50000
AFIX 33
PART 0
PART 2
H15D 2 0.515996 0.444256 0.155459 -21.00000 -1.50000
H15E 2 0.625745 0.498752 0.138931 -21.00000 -1.50000
H15F 2 0.623460 0.391796 0.178898 -21.00000 -1.50000
AFIX 0
PART 0
C2' 1 0.527457 0.661784 0.450950 11.00000 0.06389 0.12180 =
0.05039 0.00778 0.02405 0.00395
AFIX 137
H2'A 2 0.483875 0.706243 0.423152 11.00000 -1.50000
H2'B 2 0.512794 0.677266 0.496776 11.00000 -1.50000
H2'C 2 0.511447 0.588496 0.442096 11.00000 -1.50000
AFIX 0
C4' 1 0.902463 0.563260 0.463145 11.00000 0.05386 0.10729 =
0.05012 -0.00807 -0.00949 -0.00982
AFIX 137
H4'A 2 0.915528 0.629120 0.440442 11.00000 -1.50000
H4'B 2 0.951391 0.510178 0.447221 11.00000 -1.50000
H4'C 2 0.912689 0.573133 0.510029 11.00000 -1.50000
AFIX 0
C14' 1 0.526720 0.440128 0.289418 11.00000 0.07071 0.11339 =
0.04787 -0.00884 0.01563 -0.05996
PART 1
AFIX 33
H14A 2 0.490073 0.375279 0.278661 21.00000 -1.50000
H14B 2 0.543345 0.441044 0.335999 21.00000 -1.50000
H14C 2 0.481663 0.499623 0.278860 21.00000 -1.50000
AFIX 33
PART 0
PART 2
H14D 2 0.455048 0.424481 0.275159 -21.00000 -1.50000
H14E 2 0.567849 0.375677 0.290696 -21.00000 -1.50000
H14F 2 0.524817 0.471265 0.332963 -21.00000 -1.50000
AFIX 0
PART 0
C9' 1 1.292702 0.600130 0.197336 11.00000 0.03788 0.07249 =
0.07268 0.01082 -0.00564 0.00332
AFIX 13
H9' 2 1.330822 0.532261 0.200881 11.00000 -1.20000
AFIX 0
C1' 1 0.670452 0.797774 0.453965 11.00000 0.19868 0.06081 =
0.06272 -0.00659 0.01307 -0.04201
AFIX 137
H1'A 2 0.746368 0.809563 0.452078 11.00000 -1.50000
H1'B 2 0.645039 0.812325 0.498069 11.00000 -1.50000
H1'C 2 0.635188 0.844052 0.422970 11.00000 -1.50000
AFIX 0
C3' 1 0.767742 0.421547 0.485511 11.00000 0.11287 0.07205 =
0.03863 0.01697 0.00176 -0.00871
AFIX 137
H3'A 2 0.773101 0.432101 0.532649 11.00000 -1.50000
H3'B 2 0.820650 0.370878 0.471532 11.00000 -1.50000
H3'C 2 0.697624 0.395332 0.474776 11.00000 -1.50000
AFIX 0
C11' 1 1.323821 0.668995 0.257018 11.00000 0.05922 0.10709 =
0.10028 -0.00174 -0.01546 -0.01659
AFIX 137
H11A 2 1.315122 0.628741 0.297193 11.00000 -1.50000
H11B 2 1.278639 0.730703 0.258531 11.00000 -1.50000
H11C 2 1.397217 0.690727 0.252759 11.00000 -1.50000
AFIX 0
PART 1
C13' 1 0.635395 0.447541 0.247226 21.00000 0.03227 0.04229 =
0.04171 -0.00452 -0.00020 -0.00652
AFIX 13
H13' 2 0.680675 0.384518 0.252756 21.00000 -1.20000
AFIX 0
PART 0
PART 2
C13" 1 0.581014 0.522060 0.238272 -21.00000 0.02051 0.04252 =
0.03356 0.00041 -0.00307 -0.00153
AFIX 13
H13" 2 0.539141 0.587537 0.233616 -21.00000 -1.20000
AFIX 0
HKLF 4
REM CAOJIAQING_BII41-53xi in P212121 #19
REM R1 = 0.0456 for 4934 Fo > 4sig(Fo) and 0.0464 for all 5062 data
REM 391 parameters refined using 0 restraints
END
WGHT 0.0713 1.0365
REM Highest difference peak 0.492, deepest hole -0.369, 1-sigma level 0.040
Q1 1 0.7663 0.6748 0.5255 11.00000 0.05 0.49
Q2 1 0.7830 0.7753 0.4431 11.00000 0.05 0.19
Q3 1 0.5604 0.4082 0.3199 11.00000 0.05 0.15
Q4 1 0.8282 0.4374 0.3047 11.00000 0.05 0.15
Q5 1 0.7136 0.4269 0.2582 11.00000 0.05 0.13
Q6 1 0.7622 0.6598 0.4694 11.00000 0.05 0.12
Q7 1 0.5900 0.6114 0.2467 11.00000 0.05 0.12
Q8 1 0.4949 0.4687 0.1564 11.00000 0.05 0.12
Q9 1 0.7830 0.6528 0.2225 11.00000 0.05 0.12
Q10 1 0.8259 0.5828 0.2862 11.00000 0.05 0.12
REM The information below was added by Olex2.
REM
REM R1 = 0.0456 for 4934 Fo > 4sig(Fo) and 0.0464 for all 50435 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.49, deepest hole -0.37
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0464
REM R1_gt = 0.0456
REM wR_ref = 0.1222
REM GOOF = 1.043
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 50435
REM Reflections_gt = 4934
REM Parameters = n/a
REM Hole = -0.37
REM Peak = 0.49
REM Flack = -0.1(1)
;
_olex2_submission_special_instructions 'No special instructions were received'