#------------------------------------------------------------------------------
#$Date: 2020-06-05 14:32:04 +0300 (Fri, 05 Jun 2020) $
#$Revision: 252928 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/15/74/7157499.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7157499
loop_
_publ_author_name
'Cui, Hai-Lei'
_publ_section_title
;
FeCl2 catalyzed direct modification of
dihydropyrrolo[2,1-a]isoquinolines with phenols.
;
_journal_issue 21
_journal_name_full 'Organic & biomolecular chemistry'
_journal_page_first 4085
_journal_page_last 4089
_journal_paper_doi 10.1039/d0ob00917b
_journal_volume 18
_journal_year 2020
_chemical_formula_moiety 'C30 H29 N O7'
_chemical_formula_sum 'C30 H29 N O7'
_chemical_formula_weight 515.54
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_date 2020-03-10
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-03-13 deposited with the CCDC. 2020-05-11 downloaded from the CCDC.
;
_cell_angle_alpha 90
_cell_angle_beta 107.486(5)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 11.6950(5)
_cell_length_b 14.5145(5)
_cell_length_c 15.6982(7)
_cell_measurement_reflns_used 4816
_cell_measurement_temperature 99.98(10)
_cell_measurement_theta_max 28.8290
_cell_measurement_theta_min 2.5840
_cell_volume 2541.59(19)
_computing_cell_refinement 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 99.98(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -15.00 11.00 1.00 5.00 -- -11.59 -99.00 60.00 26
2 \w -55.00 24.00 1.00 5.00 -- 11.74 -37.00 -90.00 79
3 \w -8.00 83.00 1.00 5.00 -- 11.74 37.00 90.00 91
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0236782000
_diffrn_orient_matrix_UB_12 -0.0429900000
_diffrn_orient_matrix_UB_13 -0.0187420000
_diffrn_orient_matrix_UB_21 0.0330756000
_diffrn_orient_matrix_UB_22 -0.0225565000
_diffrn_orient_matrix_UB_23 0.0398440000
_diffrn_orient_matrix_UB_31 -0.0489118000
_diffrn_orient_matrix_UB_32 0.0054879000
_diffrn_orient_matrix_UB_33 0.0174704000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0300
_diffrn_reflns_av_unetI/netI 0.0433
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 11091
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full 24.999
_diffrn_reflns_theta_max 24.999
_diffrn_reflns_theta_min 2.303
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu 0.096
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.70414
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.347
_exptl_crystal_description block
_exptl_crystal_F_000 1088
_exptl_crystal_size_max 0.14
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.12
_refine_diff_density_max 0.232
_refine_diff_density_min -0.232
_refine_diff_density_rms 0.045
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.010
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 349
_refine_ls_number_reflns 4476
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.010
_refine_ls_R_factor_all 0.0525
_refine_ls_R_factor_gt 0.0407
_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^)+(0.0530P)^2^+0.5240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0972
_refine_ls_wR_factor_ref 0.1054
_reflns_Friedel_coverage 0.000
_reflns_number_gt 3690
_reflns_number_total 4476
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file d0ob00917b3.cif
_cod_data_source_block c2001078
_cod_depositor_comments 'Adding full bibliography for 7157499.cif.'
_cod_database_code 7157499
_shelx_shelxl_version_number 2018/3
_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.
;
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_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.a Secondary CH2 refined with riding coordinates:
C7(H7A,H7B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
C4(H4), C18(H18), C20(H20), C14(H14), C1(H1), C24(H24), C23(H23), C22(H22),
C21(H21)
2.c Idealised Me refined as rotating group:
C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C27(H27A,H27B,
H27C), C30(H30A,H30B,H30C)
2.d Idealised tetrahedral OH refined as rotating group:
O6(H6)
;
_shelx_res_file
;
TITL c2001078_a.res in P2(1)/n
c2001078.res
created by SHELXL-2018/3 at 13:01:34 on 10-Mar-2020
REM Old TITL C2001078 in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.135, Rweak 0.154, Alpha 0.026
REM 0.687 for 220 systematic absences, Orientation as input
REM Formula found by SHELXT: C31 O7
CELL 0.71073 11.695 14.5145 15.6982 90 107.486 90
ZERR 4 0.0005 0.0005 0.0007 0 0.005 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N O
UNIT 120 116 4 28
L.S. 20
PLAN 5
CONF
BOND
list 4
MORE -1
BOND $H
fmap 2
acta
OMIT -3 50
REM
REM
REM
WGHT 0.053000 0.524000
FVAR 0.53016
O1 4 -0.093592 0.616107 0.242894 11.00000 0.01995 0.02472 =
0.01716 0.00470 0.00036 0.00244
O4 4 0.568227 0.392982 0.793908 11.00000 0.01998 0.02532 =
0.01645 -0.00117 0.00002 0.00262
O6 4 0.498254 0.648627 1.055073 11.00000 0.03003 0.02480 =
0.01382 -0.00438 0.00440 -0.00373
AFIX 147
H6 2 0.456326 0.624343 1.082249 11.00000 -1.50000
AFIX 0
O2 4 0.087842 0.521716 0.226414 11.00000 0.02586 0.02702 =
0.01327 0.00032 0.00580 0.00172
O5 4 0.641533 0.683214 0.959209 11.00000 0.02041 0.02677 =
0.02107 -0.00750 0.00273 -0.00460
O7 4 0.289119 0.559140 0.988815 11.00000 0.02509 0.03226 =
0.01491 -0.00250 0.00722 -0.00490
O3 4 0.479723 0.294454 0.684289 11.00000 0.03504 0.01614 =
0.02446 -0.00107 -0.00614 0.00649
N1 3 0.276933 0.555104 0.632559 11.00000 0.01580 0.01518 =
0.01355 -0.00177 0.00347 0.00167
C5 1 0.173829 0.537775 0.472920 11.00000 0.01554 0.01368 =
0.01500 -0.00043 0.00475 -0.00301
C6 1 0.079955 0.593020 0.481131 11.00000 0.01812 0.01256 =
0.01798 0.00008 0.00623 -0.00251
C10 1 0.348440 0.436896 0.572979 11.00000 0.01353 0.01745 =
0.01306 0.00037 0.00432 -0.00203
C11 1 0.414546 0.445878 0.665643 11.00000 0.01441 0.01684 =
0.01493 0.00059 0.00470 -0.00114
C12 1 0.369293 0.520951 0.700270 11.00000 0.01399 0.01686 =
0.01409 0.00004 0.00274 -0.00175
C2 1 -0.007726 0.593830 0.320858 11.00000 0.01727 0.01546 =
0.01573 0.00462 0.00101 -0.00331
C13 1 0.400759 0.557743 0.792568 11.00000 0.02003 0.01386 =
0.01415 0.00016 0.00242 0.00373
C29 1 0.496324 0.378757 0.721543 11.00000 0.01662 0.01948 =
0.01549 -0.00060 0.00697 -0.00102
C19 1 0.370178 0.367662 0.509646 11.00000 0.01713 0.01509 =
0.01074 0.00179 0.00177 0.00309
C9 1 0.264327 0.506489 0.554005 11.00000 0.01660 0.01537 =
0.01233 -0.00177 0.00544 -0.00304
C15 1 0.355843 0.572205 0.931385 11.00000 0.02189 0.01730 =
0.01471 0.00289 0.00570 0.00261
C4 1 0.178510 0.514026 0.387245 11.00000 0.01638 0.01343 =
0.01853 -0.00098 0.00648 -0.00001
AFIX 43
H4 2 0.242332 0.479151 0.381203 11.00000 -1.20000
AFIX 0
C17 1 0.538709 0.635644 0.916479 11.00000 0.01643 0.01582 =
0.01880 -0.00400 0.00132 0.00131
C18 1 0.507525 0.605282 0.828586 11.00000 0.01712 0.01830 =
0.01778 0.00011 0.00506 0.00260
AFIX 43
H18 2 0.557978 0.616738 0.793921 11.00000 -1.20000
AFIX 0
C20 1 0.474127 0.372641 0.484113 11.00000 0.01852 0.01755 =
0.02382 -0.00250 0.00664 -0.00211
AFIX 43
H20 2 0.529783 0.418944 0.507197 11.00000 -1.20000
AFIX 0
C14 1 0.323876 0.542045 0.843677 11.00000 0.01893 0.01743 =
0.01608 -0.00001 0.00250 -0.00047
AFIX 43
H14 2 0.251536 0.511511 0.819090 11.00000 -1.20000
AFIX 0
C3 1 0.089800 0.541770 0.312261 11.00000 0.02161 0.01590 =
0.01224 0.00118 0.00577 -0.00348
C7 1 0.077795 0.621923 0.572672 11.00000 0.01728 0.01584 =
0.01906 0.00089 0.00757 0.00084
AFIX 23
H7A 2 0.038796 0.574651 0.597703 11.00000 -1.20000
H7B 2 0.032068 0.678417 0.568256 11.00000 -1.20000
AFIX 0
C8 1 0.204076 0.637044 0.633593 11.00000 0.02165 0.01367 =
0.01638 -0.00172 0.00708 0.00235
AFIX 23
H8A 2 0.239186 0.690229 0.613569 11.00000 -1.20000
H8B 2 0.202158 0.648825 0.693972 11.00000 -1.20000
AFIX 0
C1 1 -0.009804 0.619925 0.404869 11.00000 0.01616 0.01304 =
0.02108 0.00110 0.00672 0.00043
AFIX 43
H1 2 -0.072559 0.656275 0.410611 11.00000 -1.20000
AFIX 0
C16 1 0.463684 0.618460 0.968822 11.00000 0.02572 0.01473 =
0.01240 -0.00198 0.00223 0.00354
C24 1 0.289892 0.297102 0.475180 11.00000 0.01595 0.02230 =
0.01972 -0.00210 0.00692 -0.00198
AFIX 43
H24 2 0.219853 0.292849 0.491399 11.00000 -1.20000
AFIX 0
C23 1 0.312145 0.232827 0.417017 11.00000 0.02303 0.02035 =
0.02107 -0.00462 0.00245 -0.00166
AFIX 43
H23 2 0.257782 0.185361 0.395282 11.00000 -1.20000
AFIX 0
C22 1 0.415063 0.238921 0.391056 11.00000 0.03009 0.02146 =
0.01766 -0.00424 0.00843 0.00631
AFIX 43
H22 2 0.429848 0.196173 0.351504 11.00000 -1.20000
AFIX 0
C21 1 0.495527 0.309323 0.424659 11.00000 0.02368 0.02518 =
0.02923 -0.00238 0.01605 -0.00053
AFIX 43
H21 2 0.564574 0.314228 0.407223 11.00000 -1.20000
AFIX 0
C26 1 -0.193505 0.667498 0.251757 11.00000 0.02185 0.01964 =
0.03271 0.00503 0.00179 0.00342
AFIX 137
H26A 2 -0.252341 0.673612 0.194315 11.00000 -1.50000
H26B 2 -0.167121 0.727528 0.275204 11.00000 -1.50000
H26C 2 -0.228228 0.635907 0.291711 11.00000 -1.50000
AFIX 0
C25 1 0.198661 0.492236 0.215603 11.00000 0.03312 0.03582 =
0.01913 0.00054 0.01293 0.00119
AFIX 137
H25A 2 0.190785 0.487273 0.153116 11.00000 -1.50000
H25B 2 0.219927 0.433287 0.243618 11.00000 -1.50000
H25C 2 0.260053 0.536253 0.242779 11.00000 -1.50000
AFIX 0
C28 1 0.712768 0.714448 0.905823 11.00000 0.02107 0.03245 =
0.03238 -0.01247 0.01042 -0.00657
AFIX 137
H28A 2 0.664033 0.749981 0.856688 11.00000 -1.50000
H28B 2 0.745387 0.662387 0.883368 11.00000 -1.50000
H28C 2 0.776981 0.752065 0.941366 11.00000 -1.50000
AFIX 0
C27 1 0.175104 0.516418 0.952288 11.00000 0.03046 0.05694 =
0.02331 -0.00359 0.01186 -0.01397
AFIX 137
H27A 2 0.130402 0.549053 0.899616 11.00000 -1.50000
H27B 2 0.131983 0.517764 0.995544 11.00000 -1.50000
H27C 2 0.186139 0.453664 0.937104 11.00000 -1.50000
AFIX 0
C30 1 0.555435 0.222833 0.734287 11.00000 0.04532 0.01940 =
0.03560 0.00175 -0.00461 0.00908
AFIX 137
H30A 2 0.534134 0.165144 0.703719 11.00000 -1.50000
H30B 2 0.545148 0.218655 0.792576 11.00000 -1.50000
H30C 2 0.637628 0.236831 0.739983 11.00000 -1.50000
AFIX 0
HKLF 4
REM c2001078_a.res in P2(1)/n
REM wR2 = 0.1054, GooF = S = 1.010, Restrained GooF = 1.010 for all data
REM R1 = 0.0407 for 3690 Fo > 4sig(Fo) and 0.0525 for all 4476 data
REM 349 parameters refined using 0 restraints
END
WGHT 0.0432 0.5922
REM Highest difference peak 0.232, deepest hole -0.232, 1-sigma level 0.045
Q1 1 0.4335 0.5658 0.9573 11.00000 0.05 0.23
Q2 1 0.2815 0.4418 0.5725 11.00000 0.05 0.21
Q3 1 0.1108 0.5473 0.4824 11.00000 0.05 0.19
Q4 1 0.3772 0.4606 0.6935 11.00000 0.05 0.19
Q5 1 0.1407 0.5939 0.4737 11.00000 0.05 0.19
;
_shelx_res_checksum 97823
_shelx_hkl_file
;
0 0 -2 460.11 9.90
0 0 -2 457.92 10.35
0 0 -3 0.08 0.42
0 0 3 0.75 0.74
0 0 4 2909.59 45.33
0 0 -4 2973.90 44.60
0 0 5 0.74 0.77
0 0 -5 3.08 1.43
0 0 -6 421.87 15.17
0 0 6 408.15 15.46
0 0 -7 3.56 1.67
0 0 7 0.20 1.28
0 0 -8 434.68 17.95
0 0 -9 1.92 1.96
0 0 10 108.88 9.97
0 0 -10 99.12 9.46
0 0 11 3.27 2.31
0 0 -11 4.33 2.69
0 0 -12 19.25 4.93
0 0 -13 5.84 4.35
0 0 -14 1.92 2.25
0 0 -14 8.70 4.46
0 0 -15 2.70 3.15
0 0 -15 0.91 1.57
0 0 -16 8.22 3.04
0 0 -16 2.97 3.78
0 0 -17 -0.39 1.90
0 0 -17 -2.63 2.82
0 0 -18 11.05 4.75
0 0 -19 -2.11 2.88
0 0 -20 69.20 12.13
0 -1 -2 141.43 4.92
0 1 -2 132.41 5.41
0 1 2 138.82 4.92
0 -1 2 143.03 4.83
0 1 -2 158.28 5.07
0 1 -3 55.89 3.41
0 1 3 55.51 3.63
0 -1 -3 56.42 3.65
0 1 -3 56.73 4.16
0 -1 4 752.39 18.42
0 1 -4 755.51 16.40
0 1 4 770.23 17.48
0 1 -4 790.16 19.43
0 -1 -4 756.13 17.42
0 1 5 632.10 17.07
0 1 5 627.43 18.08
0 -1 5 610.22 17.78
0 1 -5 642.47 18.99
0 -1 -5 634.38 17.35
0 1 6 661.82 20.14
0 -1 -6 682.72 19.47
0 1 -6 676.68 20.53
0 1 -6 684.76 21.44
0 -1 6 659.54 20.05
0 -1 7 934.26 26.18
0 1 7 952.14 26.54
0 1 -7 924.52 27.50
0 -1 -7 930.22 25.21
0 1 -7 1000.81 26.99
0 -1 -8 137.69 9.67
0 1 -8 142.74 10.28
0 1 8 153.15 10.63
0 -1 9 10.22 3.19
0 -1 -9 10.53 3.03
0 1 -9 7.69 2.61
0 1 -10 23.73 4.88
0 -1 -10 35.95 5.81
0 1 -10 28.83 4.53
0 -1 10 26.66 4.88
0 1 10 23.95 4.69
0 -1 -11 383.39 19.53
0 1 -11 408.83 21.05
0 1 11 396.29 20.52
0 -1 11 399.35 20.23
0 1 12 163.44 13.48
0 1 -12 153.42 13.38
0 -1 -12 151.39 12.71
0 1 -13 145.35 11.93
0 1 -13 152.37 14.09
0 -1 -13 133.05 12.55
0 1 -14 135.47 13.78
0 1 -14 125.47 11.48
0 -1 -14 121.53 12.48
0 -1 -15 60.73 9.01
0 1 -15 53.26 9.18
0 1 -15 62.35 8.35
0 1 -16 65.79 10.57
0 1 -16 47.04 7.58
0 -1 -16 58.00 9.47
0 1 -17 3.68 2.82
0 1 -17 8.51 3.90
0 -1 -17 13.07 4.45
0 -1 -17 9.45 5.18
0 1 -18 0.30 3.03
0 -1 -18 1.49 3.47
0 1 -19 153.15 17.64
0 -1 -19 148.24 16.76
0 -1 -20 16.97 6.01
0 1 -20 6.88 4.66
0 -2 0 4607.63 55.38
0 2 0 4620.32 55.35
0 2 -1 725.69 13.53
0 -2 -2 487.58 10.27
0 2 -2 469.36 11.71
0 2 2 471.62 10.44
0 2 -3 4676.86 64.66
0 -2 -3 4772.74 60.96
0 2 3 4616.87 61.83
0 2 -4 325.29 12.33
0 -2 4 301.02 10.23
0 2 -4 329.76 11.53
0 -2 -4 332.30 10.64
0 2 4 338.67 11.03
0 2 -5 167.66 7.89
0 2 -5 153.70 9.19
0 2 5 147.25 7.86
0 -2 -5 163.49 8.10
0 2 6 1000.31 24.28
0 2 -6 1013.42 22.85
0 -2 6 935.92 24.98
0 -2 -6 996.98 24.04
0 2 -6 975.29 26.94
0 2 -7 89.45 6.64
0 -2 -7 96.25 7.30
0 2 -7 96.38 8.38
0 2 7 94.13 7.30
0 -2 7 99.99 8.04
0 2 8 27.41 4.21
0 2 8 23.87 4.26
0 -2 -8 19.45 3.61
0 2 -8 26.53 3.94
0 2 -8 29.63 5.04
0 -2 9 102.47 9.08
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10 4 -14 7.14 5.64
10 4 -14 9.73 3.77
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10 4 -12 21.53 4.76
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10 5 -17 2.46 3.38
10 5 -16 6.73 4.83
10 5 -16 7.05 3.47
10 5 -15 17.04 8.45
10 5 -15 20.63 5.52
10 5 -14 18.76 7.49
10 5 -14 15.01 4.42
10 5 -13 1.23 3.32
10 5 -13 6.19 2.39
10 5 -12 39.42 9.65
10 5 -12 58.90 7.98
10 5 -11 14.64 5.72
10 5 -11 30.97 5.87
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10 5 -10 7.50 3.24
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10 6 -16 10.27 5.13
10 6 -15 79.10 10.86
10 6 -15 38.00 9.35
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13 5 -10 60.99 8.81
13 5 -9 -1.35 1.91
13 5 -8 8.13 3.91
13 5 -7 -2.69 1.95
13 5 -6 37.45 7.14
13 5 -5 21.95 5.98
13 5 -4 25.80 6.62
-13 5 4 17.91 4.82
13 5 -3 82.93 11.59
-13 5 3 84.06 10.38
-13 5 2 305.37 20.90
-13 5 1 49.65 8.77
-13 5 0 106.59 13.38
-13 -5 -1 -1.03 2.50
-13 5 -1 8.23 4.89
-13 -5 -2 23.04 7.03
-13 5 -2 32.80 7.97
-13 5 -3 114.73 15.58
-13 5 -4 3.98 3.25
13 6 -14 116.24 13.78
13 6 -13 17.62 5.48
13 6 -12 65.00 9.83
13 6 -11 76.03 10.27
13 6 -10 16.68 4.46
13 6 -9 23.50 6.16
13 6 -8 1.29 2.87
13 6 -7 36.62 7.59
13 6 -6 46.82 8.74
13 6 -5 2.43 2.37
13 6 -4 4.23 3.72
13 6 -3 55.85 9.98
-13 6 3 43.66 7.74
-13 6 2 39.21 7.63
-13 6 1 79.85 11.28
-13 6 0 278.09 21.69
-13 6 -1 9.71 4.49
-13 6 -2 9.69 5.04
-13 6 -3 33.98 8.65
13 7 -14 19.93 5.22
13 7 -13 189.64 17.30
13 7 -12 19.48 5.51
13 7 -11 52.98 9.05
13 7 -10 3.11 2.57
13 7 -9 3.59 2.67
13 7 -8 89.23 11.66
13 7 -7 12.80 5.30
13 7 -6 55.49 9.56
13 7 -5 13.26 5.60
13 7 -4 25.53 6.89
13 7 -3 94.83 12.84
13 7 -2 8.67 4.98
-13 7 2 2.21 2.37
-13 7 1 -0.42 2.75
-13 7 0 15.09 4.86
-13 7 -1 -2.20 3.59
-13 7 -2 59.80 10.91
-13 7 -3 4.82 3.15
13 8 -14 33.56 7.48
13 8 -13 27.56 7.03
13 8 -12 17.94 6.05
13 8 -11 -0.54 2.22
13 8 -10 31.22 7.23
13 8 -9 35.80 7.36
13 8 -8 14.65 4.79
13 8 -7 39.00 8.39
13 8 -6 0.60 2.04
13 8 -5 17.22 5.40
13 8 -4 26.28 6.93
13 8 -3 13.01 5.11
13 8 -2 12.68 4.92
13 8 -1 0.40 3.60
-13 8 1 3.42 3.14
-13 8 0 42.78 9.06
-13 8 -1 15.33 5.40
-13 8 -2 7.29 4.67
-13 8 -3 4.63 4.22
13 9 -12 31.00 7.15
13 9 -11 59.11 10.23
13 9 -10 49.63 9.26
13 9 -9 -2.32 3.72
13 9 -8 26.33 6.86
13 9 -7 26.76 6.97
13 9 -6 6.47 3.24
13 9 -5 53.01 9.96
13 9 -4 4.09 3.78
13 9 -3 23.27 6.80
-13 9 -1 0.63 3.25
-13 9 -2 12.18 4.56
14 0 -13 -2.62 4.45
14 0 -12 82.78 15.04
14 0 -11 -1.46 3.27
14 0 -10 17.49 7.12
14 0 -9 -1.68 2.71
14 0 -8 189.42 20.37
14 0 -7 1.58 2.94
14 0 -6 3.75 1.70
14 0 -6 12.15 4.97
14 0 -5 -1.54 2.61
14 0 -5 0.22 4.37
14 0 -4 0.31 4.94
-14 0 3 -1.55 2.01
-14 0 2 -1.16 2.93
-14 0 1 -1.97 1.95
-14 0 0 206.06 19.53
-14 0 -1 2.50 3.57
-14 0 -2 51.98 10.04
14 -1 -13 125.61 19.26
14 -1 -12 24.18 8.50
14 1 -12 11.90 6.91
14 -1 -11 -2.95 4.37
14 1 -11 4.83 4.01
14 1 -10 0.73 3.72
14 -1 -10 -4.77 6.05
14 1 -9 35.33 9.84
14 -1 -9 18.16 7.18
14 1 -8 12.20 6.51
14 -1 -8 10.72 6.41
14 1 -7 19.98 5.37
14 -1 -7 16.01 6.61
14 1 -7 28.75 8.84
14 1 -6 -1.04 3.29
14 1 -6 8.42 5.35
14 -1 -6 6.17 3.88
14 -1 -5 -0.92 2.94
14 1 -5 0.57 1.69
14 -1 -5 -2.24 2.58
-14 1 4 4.81 3.53
14 -1 -4 8.50 5.26
-14 -1 3 56.46 9.32
-14 1 3 56.48 9.12
-14 -1 2 24.82 6.46
-14 1 2 21.62 6.30
-14 -1 1 1.34 3.43
-14 1 1 5.50 3.32
-14 -1 0 5.97 4.69
-14 1 0 4.82 4.13
-14 -1 -1 50.95 10.18
-14 1 -1 46.54 9.26
-14 -1 -2 10.08 5.97
-14 1 -2 1.03 3.38
14 -2 -12 38.22 10.73
14 2 -12 53.19 11.89
14 -2 -11 35.94 10.10
14 2 -11 47.82 12.33
14 -2 -10 24.40 8.38
14 2 -10 23.25 8.52
14 -2 -9 28.64 9.09
14 2 -9 38.16 10.69
14 2 -9 41.38 7.16
14 2 -8 40.67 7.50
14 2 -8 41.36 10.73
14 -2 -8 34.17 8.09
14 2 -7 11.15 3.87
14 -2 -7 5.26 4.35
14 2 -7 3.23 5.30
14 2 -6 7.69 3.86
14 -2 -6 13.15 6.45
14 2 -5 17.95 4.95
-14 2 5 9.07 3.99
14 -2 -5 22.37 7.07
-14 2 4 15.41 4.74
14 -2 -4 26.55 7.70
-14 2 3 -1.27 3.73
-14 2 2 96.14 12.23
-14 -2 2 75.07 11.49
-14 -2 1 21.53 6.70
-14 2 1 11.81 3.77
-14 -2 0 23.04 7.13
-14 2 0 25.91 7.08
-14 -2 -1 -0.78 2.88
-14 2 -1 5.03 3.56
-14 2 -2 3.57 4.61
14 -3 -12 38.63 10.44
14 3 -12 22.52 8.25
14 3 -11 6.62 5.15
14 -3 -11 19.24 7.56
14 3 -10 4.45 6.32
14 3 -10 1.71 2.37
14 -3 -10 3.11 3.70
14 3 -9 48.27 12.31
14 -3 -9 72.35 13.73
14 3 -9 74.10 9.71
14 3 -8 -4.36 10.49
14 -3 -8 5.28 3.72
14 3 -7 11.96 4.38
14 -3 -7 10.12 5.74
14 3 -6 46.65 8.39
14 -3 -6 49.51 10.34
14 3 -5 0.11 2.93
14 -3 -5 -3.97 4.19
14 3 -4 9.32 3.72
-14 3 4 16.05 4.77
-14 3 3 77.28 10.43
-14 3 2 1.97 2.57
-14 -3 1 51.68 9.76
-14 3 1 53.55 9.42
-14 -3 0 5.04 4.44
-14 3 0 2.57 2.50
-14 -3 -1 6.62 4.85
-14 3 -1 7.10 4.17
-14 3 -2 32.67 8.01
14 4 -12 -39.42 12.62
14 4 -11 -14.40 10.32
14 4 -10 -7.44 8.07
14 4 -10 49.54 8.42
14 4 -9 10.01 4.57
14 4 -8 14.49 4.98
14 4 -7 13.77 4.16
14 4 -6 28.52 6.87
14 -4 -6 24.23 7.17
14 -4 -5 54.66 10.85
14 4 -5 38.63 7.92
14 4 -4 16.77 5.19
-14 4 3 -0.29 2.11
-14 4 2 5.31 3.35
-14 4 1 47.91 9.08
-14 4 0 135.22 15.65
-14 4 -1 6.25 3.99
-14 4 -2 5.80 2.90
14 5 -11 20.58 5.16
14 5 -10 72.74 10.42
14 5 -9 70.68 10.22
14 5 -8 16.48 5.57
14 5 -7 -0.97 2.73
14 5 -6 6.41 3.98
14 5 -5 0.20 2.21
14 5 -4 121.95 14.40
14 5 -3 3.26 3.44
-14 5 2 -0.75 3.03
-14 5 1 65.69 10.60
-14 5 0 63.41 10.80
-14 5 -1 -1.71 3.09
-14 5 -2 8.67 3.93
14 6 -12 11.87 5.23
14 6 -11 11.64 4.63
14 6 -10 10.91 4.79
14 6 -9 64.51 9.71
14 6 -8 6.18 4.89
14 6 -7 5.91 4.09
14 6 -6 1.33 2.55
14 6 -5 70.27 11.09
14 6 -4 2.94 3.80
14 6 -3 273.64 22.66
14 6 -2 3.54 3.82
-14 6 1 3.95 2.21
-14 6 0 44.23 9.25
-14 6 -1 44.32 9.27
-14 6 -2 4.67 4.28
14 7 -12 4.57 3.18
14 7 -11 65.42 10.12
14 7 -10 -1.65 3.11
14 7 -9 -3.28 3.37
14 7 -8 15.19 6.09
14 7 -7 5.05 3.75
14 7 -6 13.19 4.91
14 7 -5 5.33 3.71
14 7 -4 43.96 9.30
14 7 -3 12.55 5.35
-14 7 -1 7.50 3.67
14 8 -12 22.69 5.77
14 8 -11 22.06 6.15
14 8 -10 10.44 4.25
14 8 -9 37.87 8.34
14 8 -8 2.46 2.37
14 8 -7 5.76 3.75
14 8 -6 0.56 3.66
14 8 -5 35.07 8.85
15 0 -11 130.59 19.29
15 0 -10 8.46 6.10
15 0 -9 238.18 24.81
15 0 -8 -1.57 3.25
15 0 -7 26.27 7.94
15 0 -6 3.87 4.39
-15 0 3 19.29 5.99
-15 0 2 0.78 2.69
-15 0 1 37.44 8.35
-15 0 0 2.20 3.78
15 1 -11 32.09 10.14
15 -1 -11 29.62 9.01
15 1 -10 37.59 11.67
15 -1 -10 29.27 9.35
15 1 -9 64.88 13.68
15 -1 -9 47.82 11.14
15 1 -8 1.50 5.27
15 -1 -8 12.25 7.67
15 -1 -7 0.34 2.67
15 1 -7 7.13 4.79
15 1 -6 2.90 7.21
15 -1 -6 5.33 3.91
-15 1 3 4.74 2.75
-15 -1 2 106.50 13.76
-15 1 2 130.72 14.99
-15 -1 1 14.92 5.57
-15 1 1 14.99 6.09
-15 1 0 4.40 4.18
15 -2 -11 10.59 6.65
15 2 -11 16.99 8.99
15 2 -10 13.71 7.27
15 -2 -10 11.49 5.10
15 -2 -9 -13.47 6.39
15 2 -9 -6.34 8.43
15 -2 -8 4.99 3.46
15 2 -8 -8.51 10.03
15 -2 -7 4.65 3.95
15 2 -6 3.41 3.56
15 2 -5 15.98 5.05
15 2 -4 -5.54 4.48
-15 2 3 196.77 17.67
-15 2 2 3.16 2.63
-15 -2 1 8.89 4.34
-15 2 1 11.29 4.90
-15 2 0 8.78 5.65
15 -3 -11 72.67 14.46
15 3 -10 -20.29 12.78
15 -3 -10 -5.75 5.65
15 -3 -9 9.05 3.67
15 -3 -8 -2.73 2.96
15 3 -7 47.15 8.55
15 -3 -7 47.68 10.57
15 3 -6 16.68 5.97
15 3 -5 12.10 4.88
15 3 -4 16.59 6.07
-15 3 2 2.28 3.41
-15 3 1 96.85 13.17
-15 3 0 -0.73 3.54
15 -4 -10 52.91 12.20
15 -4 -9 19.26 6.90
15 -4 -8 -0.26 3.14
15 4 -8 2.29 3.51
15 4 -7 31.17 7.08
15 -4 -7 21.26 7.11
15 4 -6 7.55 3.95
15 4 -5 22.26 6.64
15 4 -4 7.36 3.90
15 4 -3 41.81 9.03
-15 4 1 48.56 9.41
-15 4 0 3.92 3.18
15 5 -9 -1.20 2.27
15 5 -8 6.71 4.37
15 5 -7 -5.90 4.29
15 -5 -7 1.25 3.38
15 5 -6 4.54 3.50
15 5 -5 3.99 3.41
15 5 -4 37.78 8.77
15 5 -3 6.62 4.03
15 6 -10 7.72 4.95
15 6 -9 -0.01 2.43
15 6 -8 19.82 6.38
15 6 -7 7.99 4.35
15 6 -6 1.08 2.36
15 6 -5 87.50 12.95
15 6 -4 13.88 5.40
15 7 -9 8.25 4.27
15 7 -8 6.95 4.05
16 0 -9 4.47 5.17
16 1 -9 125.92 20.36
0 0 0 0.00 0.00
TITL C2001078 in P2(1)/n
REM P2(1)/n (#14 in standard setting)
CELL 0.71073 11.694961 14.514447 15.698237 90.0000 107.4859 90.0000
ZERR 11.00 0.000519 0.000536 0.000695 0.0000 0.0050 0.0000
LATT 1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC C H N O
UNIT 121.00 110.00 11.00 11.00
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 83024
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.906
_oxdiff_exptl_absorpt_empirical_full_min 0.749
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 -0.09359(10) 0.61611(8) 0.24289(7) 0.0218(3) Uani 1 1 d . . . . .
O4 O 0.56823(10) 0.39298(8) 0.79391(7) 0.0218(3) Uani 1 1 d . . . . .
O6 O 0.49825(10) 0.64863(8) 1.05507(7) 0.0234(3) Uani 1 1 d . . . . .
H6 H 0.456326 0.624343 1.082249 0.035 Uiso 1 1 calc R U . . .
O2 O 0.08784(10) 0.52172(8) 0.22641(7) 0.0221(3) Uani 1 1 d . . . . .
O5 O 0.64153(10) 0.68321(8) 0.95921(8) 0.0235(3) Uani 1 1 d . . . . .
O7 O 0.28912(10) 0.55914(8) 0.98881(7) 0.0238(3) Uani 1 1 d . . . . .
O3 O 0.47972(11) 0.29445(8) 0.68429(8) 0.0285(3) Uani 1 1 d . . . . .
N1 N 0.27693(11) 0.55510(9) 0.63256(8) 0.0151(3) Uani 1 1 d . . . . .
C5 C 0.17383(14) 0.53778(11) 0.47292(10) 0.0147(4) Uani 1 1 d . . . . .
C6 C 0.07996(14) 0.59302(11) 0.48113(11) 0.0160(4) Uani 1 1 d . . . . .
C10 C 0.34844(14) 0.43690(11) 0.57298(10) 0.0146(4) Uani 1 1 d . . . . .
C11 C 0.41455(14) 0.44588(11) 0.66564(11) 0.0153(4) Uani 1 1 d . . . . .
C12 C 0.36929(14) 0.52095(11) 0.70027(10) 0.0153(4) Uani 1 1 d . . . . .
C2 C -0.00773(14) 0.59383(11) 0.32086(11) 0.0170(4) Uani 1 1 d . . . . .
C13 C 0.40076(14) 0.55774(11) 0.79257(11) 0.0166(4) Uani 1 1 d . . . . .
C29 C 0.49632(14) 0.37876(11) 0.72154(11) 0.0167(4) Uani 1 1 d . . . . .
C19 C 0.37018(14) 0.36766(11) 0.50965(10) 0.0149(4) Uani 1 1 d . . . . .
C9 C 0.26433(14) 0.50649(11) 0.55401(10) 0.0145(4) Uani 1 1 d . . . . .
C15 C 0.35584(14) 0.57220(11) 0.93138(11) 0.0179(4) Uani 1 1 d . . . . .
C4 C 0.17851(14) 0.51403(11) 0.38725(10) 0.0158(4) Uani 1 1 d . . . . .
H4 H 0.242332 0.479151 0.381203 0.019 Uiso 1 1 calc R U . . .
C17 C 0.53871(14) 0.63564(11) 0.91648(11) 0.0179(4) Uani 1 1 d . . . . .
C18 C 0.50753(14) 0.60528(11) 0.82859(11) 0.0178(4) Uani 1 1 d . . . . .
H18 H 0.557978 0.616738 0.793921 0.021 Uiso 1 1 calc R U . . .
C20 C 0.47413(14) 0.37264(11) 0.48411(11) 0.0199(4) Uani 1 1 d . . . . .
H20 H 0.529783 0.418944 0.507197 0.024 Uiso 1 1 calc R U . . .
C14 C 0.32388(15) 0.54204(11) 0.84368(11) 0.0181(4) Uani 1 1 d . . . . .
H14 H 0.251536 0.511511 0.819090 0.022 Uiso 1 1 calc R U . . .
C3 C 0.08980(15) 0.54177(11) 0.31226(10) 0.0164(4) Uani 1 1 d . . . . .
C7 C 0.07780(14) 0.62192(11) 0.57267(11) 0.0169(4) Uani 1 1 d . . . . .
H7A H 0.038796 0.574651 0.597703 0.020 Uiso 1 1 calc R U . . .
H7B H 0.032068 0.678417 0.568256 0.020 Uiso 1 1 calc R U . . .
C8 C 0.20408(14) 0.63704(11) 0.63359(11) 0.0169(4) Uani 1 1 d . . . . .
H8A H 0.239186 0.690229 0.613569 0.020 Uiso 1 1 calc R U . . .
H8B H 0.202158 0.648825 0.693972 0.020 Uiso 1 1 calc R U . . .
C1 C -0.00980(14) 0.61993(11) 0.40487(11) 0.0165(4) Uani 1 1 d . . . . .
H1 H -0.072559 0.656275 0.410611 0.020 Uiso 1 1 calc R U . . .
C16 C 0.46368(15) 0.61846(11) 0.96882(10) 0.0184(4) Uani 1 1 d . . . . .
C24 C 0.28989(14) 0.29710(12) 0.47518(11) 0.0190(4) Uani 1 1 d . . . . .
H24 H 0.219853 0.292849 0.491399 0.023 Uiso 1 1 calc R U . . .
C23 C 0.31214(15) 0.23283(12) 0.41702(11) 0.0224(4) Uani 1 1 d . . . . .
H23 H 0.257782 0.185361 0.395282 0.027 Uiso 1 1 calc R U . . .
C22 C 0.41506(16) 0.23892(12) 0.39106(11) 0.0228(4) Uani 1 1 d . . . . .
H22 H 0.429848 0.196173 0.351504 0.027 Uiso 1 1 calc R U . . .
C21 C 0.49553(15) 0.30932(12) 0.42466(12) 0.0242(4) Uani 1 1 d . . . . .
H21 H 0.564574 0.314228 0.407223 0.029 Uiso 1 1 calc R U . . .
C26 C -0.19350(15) 0.66750(12) 0.25176(12) 0.0261(4) Uani 1 1 d . . . . .
H26A H -0.252341 0.673612 0.194315 0.039 Uiso 1 1 calc R U . . .
H26B H -0.167121 0.727528 0.275204 0.039 Uiso 1 1 calc R U . . .
H26C H -0.228228 0.635907 0.291711 0.039 Uiso 1 1 calc R U . . .
C25 C 0.19866(16) 0.49224(14) 0.21560(12) 0.0282(4) Uani 1 1 d . . . . .
H25A H 0.190785 0.487273 0.153116 0.042 Uiso 1 1 calc R U . . .
H25B H 0.219927 0.433287 0.243618 0.042 Uiso 1 1 calc R U . . .
H25C H 0.260053 0.536253 0.242779 0.042 Uiso 1 1 calc R U . . .
C28 C 0.71277(16) 0.71445(13) 0.90582(13) 0.0281(4) Uani 1 1 d . . . . .
H28A H 0.664033 0.749981 0.856688 0.042 Uiso 1 1 calc R U . . .
H28B H 0.745387 0.662387 0.883368 0.042 Uiso 1 1 calc R U . . .
H28C H 0.776981 0.752065 0.941366 0.042 Uiso 1 1 calc R U . . .
C27 C 0.17510(17) 0.51642(16) 0.95229(13) 0.0361(5) Uani 1 1 d . . . . .
H27A H 0.130402 0.549053 0.899616 0.054 Uiso 1 1 calc R U . . .
H27B H 0.131983 0.517764 0.995544 0.054 Uiso 1 1 calc R U . . .
H27C H 0.186139 0.453664 0.937104 0.054 Uiso 1 1 calc R U . . .
C30 C 0.55544(19) 0.22283(13) 0.73429(14) 0.0371(5) Uani 1 1 d . . . . .
H30A H 0.534134 0.165144 0.703719 0.056 Uiso 1 1 calc R U . . .
H30B H 0.545148 0.218655 0.792576 0.056 Uiso 1 1 calc R U . . .
H30C H 0.637628 0.236831 0.739983 0.056 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0200(6) 0.0247(7) 0.0172(6) 0.0047(5) 0.0004(5) 0.0024(5)
O4 0.0200(6) 0.0253(7) 0.0165(6) -0.0012(5) 0.0000(5) 0.0026(5)
O6 0.0300(7) 0.0248(7) 0.0138(6) -0.0044(5) 0.0044(5) -0.0037(5)
O2 0.0259(7) 0.0270(7) 0.0133(6) 0.0003(5) 0.0058(5) 0.0017(5)
O5 0.0204(6) 0.0268(7) 0.0211(6) -0.0075(5) 0.0027(5) -0.0046(5)
O7 0.0251(7) 0.0323(7) 0.0149(6) -0.0025(5) 0.0072(5) -0.0049(5)
O3 0.0350(7) 0.0161(6) 0.0245(7) -0.0011(5) -0.0061(6) 0.0065(5)
N1 0.0158(7) 0.0152(7) 0.0135(7) -0.0018(6) 0.0035(6) 0.0017(6)
C5 0.0155(8) 0.0137(8) 0.0150(8) -0.0004(7) 0.0048(7) -0.0030(7)
C6 0.0181(8) 0.0126(8) 0.0180(9) 0.0001(7) 0.0062(7) -0.0025(7)
C10 0.0135(8) 0.0174(8) 0.0131(8) 0.0004(7) 0.0043(7) -0.0020(7)
C11 0.0144(8) 0.0168(8) 0.0149(8) 0.0006(7) 0.0047(7) -0.0011(7)
C12 0.0140(8) 0.0169(8) 0.0141(8) 0.0000(7) 0.0027(7) -0.0017(7)
C2 0.0173(8) 0.0155(8) 0.0157(8) 0.0046(7) 0.0010(7) -0.0033(7)
C13 0.0200(9) 0.0139(8) 0.0141(8) 0.0002(7) 0.0024(7) 0.0037(7)
C29 0.0166(8) 0.0195(9) 0.0155(9) -0.0006(7) 0.0070(7) -0.0010(7)
C19 0.0171(8) 0.0151(8) 0.0107(8) 0.0018(7) 0.0018(7) 0.0031(7)
C9 0.0166(8) 0.0154(8) 0.0123(8) -0.0018(7) 0.0054(7) -0.0030(7)
C15 0.0219(9) 0.0173(9) 0.0147(8) 0.0029(7) 0.0057(7) 0.0026(7)
C4 0.0164(8) 0.0134(8) 0.0185(9) -0.0010(7) 0.0065(7) 0.0000(7)
C17 0.0164(8) 0.0158(8) 0.0188(9) -0.0040(7) 0.0013(7) 0.0013(7)
C18 0.0171(8) 0.0183(9) 0.0178(9) 0.0001(7) 0.0051(7) 0.0026(7)
C20 0.0185(9) 0.0176(9) 0.0238(9) -0.0025(8) 0.0066(8) -0.0021(7)
C14 0.0189(9) 0.0174(9) 0.0161(9) 0.0000(7) 0.0025(7) -0.0005(7)
C3 0.0216(9) 0.0159(8) 0.0122(8) 0.0012(7) 0.0058(7) -0.0035(7)
C7 0.0173(8) 0.0158(8) 0.0191(9) 0.0009(7) 0.0076(7) 0.0008(7)
C8 0.0216(9) 0.0137(8) 0.0164(8) -0.0017(7) 0.0071(7) 0.0023(7)
C1 0.0162(8) 0.0130(8) 0.0211(9) 0.0011(7) 0.0067(7) 0.0004(7)
C16 0.0257(9) 0.0147(8) 0.0124(8) -0.0020(7) 0.0022(7) 0.0035(7)
C24 0.0160(8) 0.0223(9) 0.0197(9) -0.0021(7) 0.0069(7) -0.0020(7)
C23 0.0230(9) 0.0204(9) 0.0211(9) -0.0046(8) 0.0024(8) -0.0017(7)
C22 0.0301(10) 0.0215(9) 0.0177(9) -0.0042(8) 0.0084(8) 0.0063(8)
C21 0.0237(10) 0.0252(10) 0.0292(10) -0.0024(8) 0.0161(8) -0.0005(8)
C26 0.0219(9) 0.0196(9) 0.0327(11) 0.0050(8) 0.0018(8) 0.0034(8)
C25 0.0331(11) 0.0358(11) 0.0191(9) 0.0005(8) 0.0129(9) 0.0012(9)
C28 0.0211(9) 0.0324(11) 0.0324(11) -0.0125(9) 0.0104(8) -0.0066(8)
C27 0.0305(11) 0.0569(14) 0.0233(10) -0.0036(10) 0.0119(9) -0.0140(10)
C30 0.0453(12) 0.0194(10) 0.0356(12) 0.0018(9) -0.0046(10) 0.0091(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C2 O1 C26 116.00(13) . . ?
C16 O6 H6 109.5 . . ?
C3 O2 C25 115.72(13) . . ?
C17 O5 C28 117.02(13) . . ?
C15 O7 C27 116.36(13) . . ?
C29 O3 C30 115.86(14) . . ?
C12 N1 C9 110.84(13) . . ?
C12 N1 C8 127.91(13) . . ?
C9 N1 C8 120.98(13) . . ?
C6 C5 C9 118.79(14) . . ?
C6 C5 C4 119.14(15) . . ?
C4 C5 C9 122.07(14) . . ?
C5 C6 C7 119.18(14) . . ?
C1 C6 C5 119.54(14) . . ?
C1 C6 C7 121.28(14) . . ?
C11 C10 C19 126.23(14) . . ?
C9 C10 C11 106.55(14) . . ?
C9 C10 C19 127.19(14) . . ?
C10 C11 C29 127.28(14) . . ?
C12 C11 C10 108.37(14) . . ?
C12 C11 C29 123.05(15) . . ?
N1 C12 C11 106.61(14) . . ?
N1 C12 C13 122.52(14) . . ?
C11 C12 C13 130.68(15) . . ?
O1 C2 C3 116.04(14) . . ?
O1 C2 C1 124.84(14) . . ?
C1 C2 C3 119.11(15) . . ?
C18 C13 C12 120.35(14) . . ?
C14 C13 C12 119.38(14) . . ?
C14 C13 C18 120.26(15) . . ?
O4 C29 O3 122.14(15) . . ?
O4 C29 C11 126.53(15) . . ?
O3 C29 C11 111.28(14) . . ?
C20 C19 C10 119.78(14) . . ?
C24 C19 C10 121.90(14) . . ?
C24 C19 C20 118.31(14) . . ?
N1 C9 C5 118.10(13) . . ?
C10 C9 N1 107.56(14) . . ?
C10 C9 C5 134.32(14) . . ?
O7 C15 C14 124.96(15) . . ?
O7 C15 C16 114.27(14) . . ?
C14 C15 C16 120.76(15) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 C5 120.74(15) . . ?
C3 C4 H4 119.6 . . ?
O5 C17 C18 125.07(14) . . ?
O5 C17 C16 114.58(14) . . ?
C18 C17 C16 120.35(15) . . ?
C13 C18 H18 120.1 . . ?
C17 C18 C13 119.83(15) . . ?
C17 C18 H18 120.1 . . ?
C19 C20 H20 119.7 . . ?
C21 C20 C19 120.66(15) . . ?
C21 C20 H20 119.7 . . ?
C13 C14 H14 120.2 . . ?
C15 C14 C13 119.55(15) . . ?
C15 C14 H14 120.2 . . ?
O2 C3 C2 115.66(14) . . ?
O2 C3 C4 124.36(14) . . ?
C4 C3 C2 119.98(14) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 C8 110.51(13) . . ?
H7A C7 H7B 108.1 . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
N1 C8 C7 109.58(13) . . ?
N1 C8 H8A 109.8 . . ?
N1 C8 H8B 109.8 . . ?
C7 C8 H8A 109.8 . . ?
C7 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
C6 C1 H1 119.3 . . ?
C2 C1 C6 121.37(14) . . ?
C2 C1 H1 119.3 . . ?
O6 C16 C15 122.29(14) . . ?
O6 C16 C17 118.48(15) . . ?
C15 C16 C17 119.22(14) . . ?
C19 C24 H24 119.4 . . ?
C19 C24 C23 121.10(15) . . ?
C23 C24 H24 119.4 . . ?
C24 C23 H23 119.9 . . ?
C24 C23 C22 120.24(16) . . ?
C22 C23 H23 119.9 . . ?
C23 C22 H22 120.4 . . ?
C21 C22 C23 119.16(15) . . ?
C21 C22 H22 120.4 . . ?
C20 C21 H21 119.7 . . ?
C22 C21 C20 120.51(15) . . ?
C22 C21 H21 119.7 . . ?
O1 C26 H26A 109.5 . . ?
O1 C26 H26B 109.5 . . ?
O1 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O2 C25 H25A 109.5 . . ?
O2 C25 H25B 109.5 . . ?
O2 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O5 C28 H28A 109.5 . . ?
O5 C28 H28B 109.5 . . ?
O5 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O7 C27 H27A 109.5 . . ?
O7 C27 H27B 109.5 . . ?
O7 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O3 C30 H30A 109.5 . . ?
O3 C30 H30B 109.5 . . ?
O3 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
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 C2 1.3683(19) . ?
O1 C26 1.428(2) . ?
O4 C29 1.2109(19) . ?
O6 H6 0.8200 . ?
O6 C16 1.3636(19) . ?
O2 C3 1.3722(19) . ?
O2 C25 1.423(2) . ?
O5 C17 1.3740(19) . ?
O5 C28 1.422(2) . ?
O7 C15 1.3713(19) . ?
O7 C27 1.425(2) . ?
O3 C29 1.345(2) . ?
O3 C30 1.436(2) . ?
N1 C12 1.361(2) . ?
N1 C9 1.390(2) . ?
N1 C8 1.466(2) . ?
C5 C6 1.396(2) . ?
C5 C9 1.462(2) . ?
C5 C4 1.405(2) . ?
C6 C7 1.504(2) . ?
C6 C1 1.390(2) . ?
C10 C11 1.433(2) . ?
C10 C19 1.488(2) . ?
C10 C9 1.379(2) . ?
C11 C12 1.391(2) . ?
C11 C29 1.459(2) . ?
C12 C13 1.483(2) . ?
C2 C3 1.408(2) . ?
C2 C1 1.379(2) . ?
C13 C18 1.389(2) . ?
C13 C14 1.392(2) . ?
C19 C20 1.392(2) . ?
C19 C24 1.385(2) . ?
C15 C14 1.385(2) . ?
C15 C16 1.393(2) . ?
C4 H4 0.9300 . ?
C4 C3 1.375(2) . ?
C17 C18 1.389(2) . ?
C17 C16 1.393(2) . ?
C18 H18 0.9300 . ?
C20 H20 0.9300 . ?
C20 C21 1.385(2) . ?
C14 H14 0.9300 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.515(2) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C1 H1 0.9300 . ?
C24 H24 0.9300 . ?
C24 C23 1.384(2) . ?
C23 H23 0.9300 . ?
C23 C22 1.385(2) . ?
C22 H22 0.9300 . ?
C22 C21 1.382(2) . ?
C21 H21 0.9300 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
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 C2 C3 O2 1.5(2) . . . . ?
O1 C2 C3 C4 -178.12(14) . . . . ?
O1 C2 C1 C6 178.80(14) . . . . ?
O5 C17 C18 C13 -179.95(15) . . . . ?
O5 C17 C16 O6 -0.5(2) . . . . ?
O5 C17 C16 C15 178.77(14) . . . . ?
O7 C15 C14 C13 -178.53(15) . . . . ?
O7 C15 C16 O6 -0.6(2) . . . . ?
O7 C15 C16 C17 -179.92(14) . . . . ?
N1 C12 C13 C18 -111.83(17) . . . . ?
N1 C12 C13 C14 69.9(2) . . . . ?
C5 C6 C7 C8 34.5(2) . . . . ?
C5 C6 C1 C2 -0.6(2) . . . . ?
C5 C4 C3 O2 179.84(14) . . . . ?
C5 C4 C3 C2 -0.6(2) . . . . ?
C6 C5 C9 N1 -20.6(2) . . . . ?
C6 C5 C9 C10 161.34(17) . . . . ?
C6 C5 C4 C3 -2.4(2) . . . . ?
C6 C7 C8 N1 -53.02(17) . . . . ?
C10 C11 C12 N1 1.70(17) . . . . ?
C10 C11 C12 C13 176.72(15) . . . . ?
C10 C11 C29 O4 165.06(15) . . . . ?
C10 C11 C29 O3 -17.5(2) . . . . ?
C10 C19 C20 C21 -179.45(15) . . . . ?
C10 C19 C24 C23 -179.38(15) . . . . ?
C11 C10 C19 C20 -68.4(2) . . . . ?
C11 C10 C19 C24 111.14(19) . . . . ?
C11 C10 C9 N1 -1.12(16) . . . . ?
C11 C10 C9 C5 177.07(16) . . . . ?
C11 C12 C13 C18 73.8(2) . . . . ?
C11 C12 C13 C14 -104.4(2) . . . . ?
C12 N1 C9 C5 -176.25(13) . . . . ?
C12 N1 C9 C10 2.28(17) . . . . ?
C12 N1 C8 C7 -147.76(15) . . . . ?
C12 C11 C29 O4 -29.5(2) . . . . ?
C12 C11 C29 O3 148.00(15) . . . . ?
C12 C13 C18 C17 -176.97(15) . . . . ?
C12 C13 C14 C15 176.73(15) . . . . ?
C29 C11 C12 N1 -166.14(14) . . . . ?
C29 C11 C12 C13 8.9(3) . . . . ?
C19 C10 C11 C12 177.71(14) . . . . ?
C19 C10 C11 C29 -15.1(3) . . . . ?
C19 C10 C9 N1 -179.16(14) . . . . ?
C19 C10 C9 C5 -1.0(3) . . . . ?
C19 C20 C21 C22 -1.3(3) . . . . ?
C19 C24 C23 C22 -1.0(3) . . . . ?
C9 N1 C12 C11 -2.46(17) . . . . ?
C9 N1 C12 C13 -177.98(14) . . . . ?
C9 N1 C8 C7 38.79(19) . . . . ?
C9 C5 C6 C7 2.6(2) . . . . ?
C9 C5 C6 C1 -177.10(14) . . . . ?
C9 C5 C4 C3 177.68(14) . . . . ?
C9 C10 C11 C12 -0.35(17) . . . . ?
C9 C10 C11 C29 166.84(15) . . . . ?
C9 C10 C19 C20 109.24(19) . . . . ?
C9 C10 C19 C24 -71.2(2) . . . . ?
C4 C5 C6 C7 -177.34(14) . . . . ?
C4 C5 C6 C1 2.9(2) . . . . ?
C4 C5 C9 N1 159.35(14) . . . . ?
C4 C5 C9 C10 -18.7(3) . . . . ?
C18 C13 C14 C15 -1.5(2) . . . . ?
C18 C17 C16 O6 179.33(15) . . . . ?
C18 C17 C16 C15 -1.4(2) . . . . ?
C20 C19 C24 C23 0.2(2) . . . . ?
C14 C13 C18 C17 1.3(2) . . . . ?
C14 C15 C16 O6 -179.62(15) . . . . ?
C14 C15 C16 C17 1.1(2) . . . . ?
C3 C2 C1 C6 -2.4(2) . . . . ?
C7 C6 C1 C2 179.72(14) . . . . ?
C8 N1 C12 C11 -176.46(14) . . . . ?
C8 N1 C12 C13 8.0(2) . . . . ?
C8 N1 C9 C5 -1.8(2) . . . . ?
C8 N1 C9 C10 176.75(13) . . . . ?
C1 C6 C7 C8 -145.75(15) . . . . ?
C1 C2 C3 O2 -177.42(14) . . . . ?
C1 C2 C3 C4 3.0(2) . . . . ?
C16 C15 C14 C13 0.3(2) . . . . ?
C16 C17 C18 C13 0.2(2) . . . . ?
C24 C19 C20 C21 1.0(2) . . . . ?
C24 C23 C22 C21 0.6(3) . . . . ?
C23 C22 C21 C20 0.5(3) . . . . ?
C26 O1 C2 C3 178.93(14) . . . . ?
C26 O1 C2 C1 -2.2(2) . . . . ?
C25 O2 C3 C2 163.39(14) . . . . ?
C25 O2 C3 C4 -17.0(2) . . . . ?
C28 O5 C17 C18 9.1(2) . . . . ?
C28 O5 C17 C16 -171.06(14) . . . . ?
C27 O7 C15 C14 -4.2(2) . . . . ?
C27 O7 C15 C16 176.82(16) . . . . ?
C30 O3 C29 O4 -2.0(2) . . . . ?
C30 O3 C29 C11 -179.63(14) . . . . ?