#------------------------------------------------------------------------------
#$Date: 2021-11-06 22:41:53 +0200 (Sat, 06 Nov 2021) $
#$Revision: 270503 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/15/83/7158314.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_7158314
loop_
_publ_author_name
'Nawaz, Shah'
'Huang, Yue'
'Bao, Xiaoze'
'Wei, Shiqiang'
'Wei, Xingfu'
'Qu, Jingping'
'Wang, Baomin'
_publ_section_title
;
Construction of a spiro[pyrazolone-4,2'-pyridoindole] scaffold via
a [3 + 3] cycloaddition of 2-indolylmethanol with a
4-aminopyrazolone-derived azomethine ylide.
;
_journal_issue 39
_journal_name_full 'Organic & biomolecular chemistry'
_journal_page_first 8530
_journal_page_last 8538
_journal_paper_doi 10.1039/d1ob01631h
_journal_volume 19
_journal_year 2021
_chemical_formula_moiety 'C43 H32 N4 O'
_chemical_formula_sum 'C43 H34 N4 O'
_chemical_formula_weight 622.74
_space_group_crystal_system orthorhombic
_space_group_IT_number 61
_space_group_name_Hall '-P 2ac 2ab'
_space_group_name_H-M_alt 'P b c a'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_date 2020-09-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-06-02 deposited with the CCDC. 2021-09-09 downloaded from the CCDC.
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 18.8089(13)
_cell_length_b 17.8043(12)
_cell_length_c 21.9597(15)
_cell_measurement_reflns_used 9629
_cell_measurement_temperature 220.0
_cell_measurement_theta_max 25.691
_cell_measurement_theta_min 2.433
_cell_volume 7353.8(9)
_computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature 220.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0895
_diffrn_reflns_av_unetI/netI 0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 24
_diffrn_reflns_limit_h_min -24
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 148677
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.540
_diffrn_reflns_theta_min 2.148
_diffrn_source_current 50.0
_diffrn_source_power 2.5
_diffrn_source_voltage 50.0
_exptl_absorpt_coefficient_mu 0.068
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_correction_T_min 0.7094
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.0830 before and 0.0604 after correction.
The Ratio of minimum to maximum transmission is 0.9514.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour black
_exptl_crystal_colour_primary black
_exptl_crystal_density_diffrn 1.125
_exptl_crystal_description block
_exptl_crystal_F_000 2624
_exptl_crystal_size_max 0.26
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.22
_refine_diff_density_max 0.251
_refine_diff_density_min -0.244
_refine_diff_density_rms 0.046
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.069
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 441
_refine_ls_number_reflns 8472
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.069
_refine_ls_R_factor_all 0.0889
_refine_ls_R_factor_gt 0.0547
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1451
_refine_ls_wR_factor_ref 0.1645
_reflns_Friedel_coverage 0.000
_reflns_number_gt 5752
_reflns_number_total 8472
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file d1ob01631h2.cif
_cod_data_source_block 2
_cod_depositor_comments 'Adding full bibliography for 7158314.cif.'
_cod_database_code 7158314
_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.
;
_shelx_estimated_absorpt_t_max 0.985
_shelx_estimated_absorpt_t_min 0.982
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2.a Ternary CH refined with riding coordinates:
C00C(H00C)
2.b Aromatic/amide H refined with riding coordinates:
C00I(H00I), C00L(H00L), C00M(H00M), C00N(H00N), C00O(H00O), C00P(H00P),
C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V),
C00W(H00W), C00X(H00X), C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011),
C012(H012), C013(H013), C014(H014), C015(H015), C016(H016), C017(H017),
C018(H018), C01A(H01A), C01B(H01B), C01C(H01C), C01D(H01D)
;
_smtbx_masks_void_probe_radius 1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_file
;
TITL 2_a.res in Pbca
2.res
created by SHELXL-2018/3 at 09:07:45 on 25-Sep-2020
REM Old TITL 2_a.res in Pbca
REM SHELXT solution in Pbca: R1 0.183, Rweak 0.016, Alpha 0.032
REM 0.474 for 716 systematic absences, Orientation as input
REM Formula found by SHELXT: C47 N5 O2
CELL 0.71073 18.8089 17.8043 21.9597 90 90 90
ZERR 8 0.0013 0.0012 0.0015 0 0 0
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 N O
UNIT 344 272 32 8
L.S. 20
PLAN 10
SIZE 0.22 0.24 0.26
TEMP -53.15
CONF
BOND
list 4
MORE -1
BOND $H
ABIN
fmap 2
acta
OMIT 1 1 1
OMIT 0 0 4
REM
REM
REM
WGHT 0.100000
FVAR 0.28286
O001 4 0.710378 0.356769 0.820193 11.00000 0.04443 0.03586 =
0.04697 0.00688 -0.01344 -0.01276
N002 3 0.736863 0.527111 0.815760 11.00000 0.02671 0.03141 =
0.02417 -0.00295 -0.00114 0.00384
N003 3 0.825276 0.476650 0.653168 11.00000 0.03491 0.02882 =
0.02505 0.00300 0.00535 0.00526
N004 3 0.805195 0.370228 0.886564 11.00000 0.03801 0.03016 =
0.03012 0.00504 -0.00597 -0.00519
N005 3 0.855535 0.426153 0.900714 11.00000 0.03527 0.03210 =
0.02834 0.00015 -0.00345 -0.00285
C006 1 0.819554 0.460306 0.753422 11.00000 0.02774 0.02138 =
0.02634 0.00082 0.00042 -0.00102
C007 1 0.785736 0.490535 0.704744 11.00000 0.02954 0.02047 =
0.02616 -0.00047 0.00257 0.00011
C008 1 0.883260 0.424106 0.731877 11.00000 0.02807 0.01991 =
0.03225 -0.00068 0.00135 0.00002
C009 1 0.847628 0.481438 0.863512 11.00000 0.02652 0.02949 =
0.02638 -0.00200 -0.00024 0.00344
C00A 1 0.726083 0.616224 0.692485 11.00000 0.02952 0.02528 =
0.02441 0.00057 0.00068 0.00158
C00B 1 0.621159 0.571992 0.784595 11.00000 0.02838 0.02757 =
0.02415 0.00205 0.00076 0.00087
C00C 1 0.681390 0.519224 0.768987 11.00000 0.02608 0.02482 =
0.02578 -0.00003 -0.00105 -0.00007
AFIX 13
H00C 2 0.663001 0.467163 0.770616 11.00000 -1.20000
AFIX 0
C00D 1 0.790225 0.467347 0.816688 11.00000 0.02602 0.02610 =
0.02503 0.00002 -0.00192 0.00063
C00E 1 0.885054 0.436547 0.668706 11.00000 0.03102 0.02097 =
0.03447 -0.00106 0.00438 -0.00003
C00F 1 0.671437 0.494302 0.652731 11.00000 0.03218 0.02467 =
0.02617 -0.00246 -0.00200 0.00512
C00G 1 0.715729 0.532271 0.703871 11.00000 0.02710 0.02385 =
0.02444 -0.00099 -0.00037 0.00132
C00H 1 0.893874 0.547548 0.867935 11.00000 0.02735 0.03199 =
0.02493 -0.00401 0.00214 -0.00166
C00I 1 0.668154 0.661584 0.678135 11.00000 0.02997 0.02772 =
0.03321 0.00224 -0.00349 0.00134
AFIX 43
H00I 2 0.623519 0.639387 0.671291 11.00000 -1.20000
AFIX 0
C00J 1 0.761362 0.391079 0.839320 11.00000 0.03254 0.03071 =
0.02582 0.00138 -0.00019 0.00016
C00K 1 0.800398 0.307640 0.926397 11.00000 0.05058 0.03150 =
0.02488 0.00191 0.00123 0.00116
C00L 1 0.938238 0.382875 0.758754 11.00000 0.03400 0.02608 =
0.03972 -0.00072 -0.00182 0.00333
AFIX 43
H00L 2 0.938011 0.373194 0.800833 11.00000 -1.20000
AFIX 0
C00M 1 0.551608 0.551004 0.771818 11.00000 0.02920 0.03382 =
0.04099 0.00372 -0.00014 -0.00034
AFIX 43
H00M 2 0.542574 0.504621 0.752891 11.00000 -1.20000
AFIX 0
C00N 1 0.957839 0.543028 0.899755 11.00000 0.02932 0.04231 =
0.03854 -0.00106 -0.00187 0.00057
AFIX 43
H00N 2 0.972068 0.497148 0.917078 11.00000 -1.20000
AFIX 0
C00O 1 0.675116 0.738531 0.673785 11.00000 0.04152 0.02709 =
0.04286 0.00238 -0.00427 0.00789
AFIX 43
H00O 2 0.635228 0.768124 0.664330 11.00000 -1.20000
AFIX 0
C00P 1 0.632776 0.640447 0.812839 11.00000 0.03447 0.03366 =
0.03532 -0.00423 -0.00125 0.00245
AFIX 43
H00P 2 0.679497 0.655629 0.821750 11.00000 -1.20000
AFIX 0
C00Q 1 0.633566 0.428573 0.661890 11.00000 0.04486 0.03356 =
0.03080 -0.00053 -0.00335 -0.00215
AFIX 43
H00Q 2 0.630180 0.408486 0.701370 11.00000 -1.20000
AFIX 0
C00R 1 0.791148 0.650942 0.700855 11.00000 0.03129 0.02928 =
0.04430 0.00252 0.00051 0.00161
AFIX 43
H00R 2 0.831397 0.621705 0.709909 11.00000 -1.20000
AFIX 0
C00S 1 0.676518 0.520553 0.593157 11.00000 0.04922 0.03243 =
0.02787 0.00120 -0.00116 0.00216
AFIX 43
H00S 2 0.702061 0.564888 0.585307 11.00000 -1.20000
AFIX 0
C00T 1 0.940350 0.410536 0.632276 11.00000 0.04192 0.03035 =
0.04176 -0.00170 0.01345 0.00182
AFIX 43
H00T 2 0.940948 0.419629 0.590113 11.00000 -1.20000
AFIX 0
C00U 1 0.994058 0.371074 0.660146 11.00000 0.03529 0.03275 =
0.05605 -0.00582 0.01307 0.00353
AFIX 43
H00U 2 1.032432 0.353423 0.636753 11.00000 -1.20000
AFIX 0
C00V 1 0.992543 0.356759 0.722731 11.00000 0.03289 0.02943 =
0.05833 -0.00139 0.00023 0.00654
AFIX 43
H00V 2 1.029439 0.328694 0.740504 11.00000 -1.20000
AFIX 0
C00W 1 0.874257 0.616112 0.842770 11.00000 0.03424 0.03451 =
0.04481 0.00075 -0.00486 -0.00398
AFIX 43
H00W 2 0.831209 0.620208 0.821282 11.00000 -1.20000
AFIX 0
C00X 1 0.739986 0.772285 0.683178 11.00000 0.04812 0.02360 =
0.06333 0.00055 -0.00295 -0.00074
AFIX 43
H00X 2 0.744644 0.824770 0.680796 11.00000 -1.20000
AFIX 0
C00Y 1 1.000370 0.605811 0.905893 11.00000 0.02799 0.05577 =
0.05014 -0.00495 -0.00305 -0.00633
AFIX 43
H00Y 2 1.043340 0.602427 0.927577 11.00000 -1.20000
AFIX 0
C00Z 1 0.980455 0.673094 0.880613 11.00000 0.03653 0.04283 =
0.05788 -0.00940 0.00523 -0.01334
AFIX 43
H00Z 2 1.009804 0.715504 0.884864 11.00000 -1.20000
AFIX 0
C010 1 0.606454 0.418532 0.555818 11.00000 0.06090 0.04415 =
0.03977 -0.01316 -0.01680 0.00660
AFIX 43
H010 2 0.584447 0.393082 0.523395 11.00000 -1.20000
AFIX 0
C011 1 0.644814 0.482825 0.545317 11.00000 0.06674 0.04475 =
0.02715 -0.00206 -0.00850 0.00797
AFIX 43
H011 2 0.649542 0.501278 0.505416 11.00000 -1.20000
AFIX 0
C012 1 0.576687 0.686588 0.828044 11.00000 0.05449 0.03649 =
0.04496 -0.00699 0.00204 0.01165
AFIX 43
H012 2 0.585378 0.732728 0.847472 11.00000 -1.20000
AFIX 0
C013 1 0.917630 0.678372 0.849120 11.00000 0.04197 0.03496 =
0.05583 0.00059 0.00003 -0.00529
AFIX 43
H013 2 0.904020 0.724463 0.831799 11.00000 -1.20000
AFIX 0
C014 1 0.600645 0.391931 0.614099 11.00000 0.05436 0.03660 =
0.04576 -0.00696 -0.00871 -0.00754
AFIX 43
H014 2 0.573979 0.348273 0.621697 11.00000 -1.20000
AFIX 0
C015 1 0.495664 0.597687 0.786682 11.00000 0.03018 0.05110 =
0.06099 0.00831 0.00054 0.00761
AFIX 43
H015 2 0.448824 0.583183 0.777489 11.00000 -1.20000
AFIX 0
C016 1 0.797786 0.728015 0.696087 11.00000 0.03457 0.03155 =
0.07315 0.00016 -0.00192 -0.00598
AFIX 43
H016 2 0.842539 0.750446 0.701767 11.00000 -1.20000
AFIX 0
C017 1 0.508241 0.665485 0.814954 11.00000 0.04005 0.04842 =
0.05814 0.00110 0.00602 0.01921
AFIX 43
H017 2 0.470081 0.697136 0.825226 11.00000 -1.20000
AFIX 0
C018 1 0.750472 0.252143 0.917139 11.00000 0.06169 0.04162 =
0.04460 0.01256 -0.00591 -0.00997
AFIX 43
H018 2 0.719286 0.255032 0.883772 11.00000 -1.20000
AFIX 0
C01A 1 0.847116 0.302155 0.974514 11.00000 0.08817 0.04639 =
0.04458 0.01183 -0.02538 -0.01252
AFIX 43
H01A 2 0.882086 0.339110 0.980628 11.00000 -1.20000
AFIX 0
C01B 1 0.746344 0.192238 0.957003 11.00000 0.08204 0.04479 =
0.05877 0.01597 -0.00207 -0.01349
AFIX 43
H01B 2 0.712056 0.154621 0.950706 11.00000 -1.20000
AFIX 0
C01C 1 0.791735 0.187156 1.005596 11.00000 0.12136 0.04497 =
0.04917 0.02015 -0.00465 -0.00554
AFIX 43
H01C 2 0.788371 0.146733 1.032980 11.00000 -1.20000
AFIX 0
C01D 1 0.841924 0.241616 1.013699 11.00000 0.12777 0.06352 =
0.05113 0.02373 -0.03538 -0.01293
AFIX 43
H01D 2 0.873649 0.237884 1.046636 11.00000 -1.20000
AFIX 0
H002 2 0.718048 0.529858 0.852822 11.00000 0.04533
H003 2 0.813860 0.490342 0.615698 11.00000 0.05134
HKLF 4
REM 2_a.res in Pbca
REM wR2 = 0.1645, GooF = S = 1.069, Restrained GooF = 1.069 for all data
REM R1 = 0.0547 for 5752 Fo > 4sig(Fo) and 0.0889 for all 8472 data
REM 441 parameters refined using 0 restraints
END
WGHT 0.0625 2.5904
REM Highest difference peak 0.251, deepest hole -0.244, 1-sigma level 0.046
Q1 1 0.6928 0.5175 0.6799 11.00000 0.05 0.25
Q2 1 0.6964 0.5259 0.7323 11.00000 0.05 0.21
Q3 1 0.8023 0.4563 0.7825 11.00000 0.05 0.20
Q4 1 0.8184 0.4774 0.8413 11.00000 0.05 0.19
Q5 1 0.6979 0.6420 0.7032 11.00000 0.05 0.18
Q6 1 0.6958 0.5015 0.6232 11.00000 0.05 0.17
Q7 1 0.8213 0.6810 0.6185 11.00000 0.05 0.16
Q8 1 0.8484 0.4370 0.7506 11.00000 0.05 0.16
Q9 1 0.7184 0.5731 0.6982 11.00000 0.05 0.15
Q10 1 0.8166 0.4926 0.7361 11.00000 0.05 0.15
;
_shelx_res_checksum 9806
_shelx_fab_file
;
0 0 4 180.2615 0.0375
0 0 6 74.7391 0.0047
0 0 8 10.2969 -0.0121
0 0 10 -9.6049 -0.0096
0 0 12 -9.1888 -0.0010
0 0 14 -5.9192 0.0077
0 0 16 -2.9884 0.0076
0 0 18 -1.2034 -0.0032
0 0 20 -1.5131 -0.0097
0 0 22 -2.5566 -0.0046
0 0 24 -3.1815 0.0011
0 0 26 -3.2872 0.0005
0 0 28 -2.3184 -0.0012
0 2 1 16.4195 0.0008
0 2 2 105.2850 0.0151
0 2 3 39.9929 0.0136
0 2 4 51.7851 0.0182
0 2 5 42.8363 0.0115
0 2 6 7.3732 0.0109
0 2 7 28.7021 0.0033
0 2 8 -7.6618 0.0062
0 2 9 11.2802 0.0013
0 2 10 -3.9788 0.0055
0 2 11 0.6700 0.0022
0 2 12 0.8653 0.0048
0 2 13 -3.4505 -0.0002
0 2 14 3.8082 0.0067
0 2 15 -5.7876 -0.0013
0 2 16 7.5617 0.0073
0 2 17 -7.7676 0.0031
0 2 18 8.4371 -0.0016
0 2 19 -8.1915 0.0075
0 2 20 3.3965 -0.0116
0 2 21 -6.8865 0.0061
0 2 22 -2.6999 -0.0087
0 2 23 -4.7893 0.0011
0 2 24 -4.2249 0.0022
0 2 25 -2.8900 -0.0026
0 2 26 -2.0506 0.0069
0 2 27 -1.8081 -0.0031
0 2 28 -0.2453 0.0036
0 4 0 57.6434 -0.0142
0 4 1 -2.9053 -0.0025
0 4 2 46.2240 -0.0079
0 4 3 -10.1324 -0.0014
0 4 4 20.6463 -0.0039
0 4 5 -18.6346 0.0032
0 4 6 -1.9736 -0.0041
0 4 7 -24.5155 0.0075
0 4 8 -11.9679 -0.0009
0 4 9 -25.3480 0.0042
0 4 10 -11.5857 0.0018
0 4 11 -22.6121 -0.0053
0 4 12 -6.8714 -0.0024
0 4 13 -18.7785 -0.0128
0 4 14 -1.5307 -0.0041
0 4 15 -14.2002 -0.0143
0 4 16 2.0283 0.0034
0 4 17 -8.1846 -0.0107
0 4 18 2.1788 0.0074
0 4 19 -2.3007 -0.0038
0 4 20 -0.2292 0.0003
0 4 21 0.5935 0.0013
0 4 22 -2.6158 -0.0057
0 4 23 0.8092 0.0015
0 4 24 -3.1621 -0.0031
0 4 25 1.0515 0.0009
0 4 26 -1.9895 0.0009
0 4 27 1.6853 0.0026
0 4 28 -0.5644 0.0008
0 6 0 32.8127 -0.0016
0 6 1 5.0869 0.0000
0 6 2 25.4205 -0.0022
0 6 3 12.0479 0.0005
0 6 4 9.5739 -0.0036
0 6 5 12.8074 0.0077
0 6 6 -3.8084 -0.0054
0 6 7 9.3826 0.0110
0 6 8 -10.6868 0.0007
0 6 9 4.9423 0.0030
0 6 10 -13.0930 0.0096
0 6 11 1.7380 -0.0032
0 6 12 -12.5119 0.0083
0 6 13 0.2389 0.0026
0 6 14 -9.4991 0.0007
0 6 15 -0.8418 0.0087
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21 2 12 -0.4111 -0.0017
21 2 13 2.2310 0.0001
21 2 14 0.3292 -0.0028
21 3 1 -1.4788 -0.0017
21 3 2 -1.0126 -0.0041
21 3 3 -1.3443 0.0021
21 3 4 -1.0131 -0.0019
21 3 5 -1.4087 0.0030
21 3 6 -1.2149 -0.0000
21 3 7 -1.2845 0.0011
21 3 8 -2.6725 0.0013
21 3 9 -0.6798 -0.0004
21 3 10 -3.5292 0.0007
21 3 11 -0.2196 -0.0003
21 3 12 -1.7642 -0.0019
21 3 13 -0.0727 0.0010
21 3 14 0.8531 -0.0037
21 4 1 0.6492 0.0002
21 4 2 1.7235 -0.0021
21 4 3 1.4314 0.0012
21 4 4 2.3489 -0.0011
21 4 5 1.8263 0.0011
21 4 6 1.7482 0.0004
21 4 7 2.3010 -0.0011
21 4 8 0.3982 0.0006
21 4 9 3.3524 -0.0020
21 4 10 -0.9213 -0.0022
21 4 11 3.3451 0.0004
21 4 12 -1.3484 -0.0055
21 4 13 1.6535 0.0017
21 5 1 -1.9080 0.0036
21 5 2 0.2330 -0.0036
21 5 3 -2.3254 0.0025
21 5 4 0.3576 -0.0017
21 5 5 -3.3812 -0.0010
21 5 6 0.2755 0.0009
21 5 7 -3.8111 -0.0014
21 5 8 0.1170 0.0022
21 5 9 -2.9350 0.0006
21 5 10 0.3187 0.0018
21 5 11 -2.3274 0.0003
21 5 12 0.9746 0.0014
21 5 13 -2.5193 -0.0011
21 6 1 -0.4498 0.0006
21 6 2 2.3455 0.0006
21 6 3 0.2048 0.0001
21 6 4 3.1465 0.0004
21 6 5 0.8594 0.0016
21 6 6 2.6322 0.0012
21 6 7 1.0125 0.0012
21 6 8 1.6156 0.0012
21 6 9 0.8580 -0.0010
21 6 10 0.6881 0.0002
21 6 11 0.7763 -0.0015
21 6 12 0.4071 -0.0001
21 7 1 -3.3026 0.0061
21 7 2 0.1406 -0.0020
21 7 3 -0.9789 0.0041
21 7 4 0.5436 -0.0007
21 7 5 -0.2338 -0.0004
21 7 6 0.6238 -0.0012
21 7 7 -1.3015 -0.0016
21 7 8 0.4715 -0.0006
21 7 9 -1.0765 0.0006
21 7 10 0.7243 0.0012
21 7 11 0.6079 0.0023
21 8 1 -2.3354 0.0033
21 8 2 -0.1237 0.0009
21 8 3 -1.9496 0.0014
21 8 4 -1.1930 -0.0011
21 8 5 -0.3314 0.0006
21 8 6 -1.9988 -0.0012
21 8 7 1.3242 0.0006
21 8 8 -1.6758 -0.0010
21 8 9 1.2499 0.0004
21 8 10 -0.8533 -0.0013
21 9 1 1.3424 -0.0002
21 9 2 0.3869 -0.0024
21 9 3 1.3354 -0.0011
21 9 4 1.0208 -0.0005
21 9 5 1.1445 -0.0004
21 9 6 0.7222 -0.0013
21 9 7 1.0215 0.0007
21 9 8 -0.5149 -0.0022
21 9 9 1.0376 0.0011
21 10 1 0.5866 0.0019
21 10 2 0.0672 -0.0032
21 10 3 0.7780 -0.0020
21 10 4 0.2134 0.0011
21 10 5 1.6130 -0.0016
21 10 6 0.3544 0.0030
21 10 7 1.9180 0.0010
21 11 1 2.1371 -0.0018
21 11 2 0.2351 -0.0012
21 11 3 0.9594 -0.0013
21 11 4 -0.2255 0.0018
21 11 5 -0.0776 0.0023
22 0 0 -1.1028 -0.0007
22 0 2 0.6430 0.0018
22 0 4 2.3465 0.0053
22 0 6 0.2455 0.0038
22 0 8 -2.4936 -0.0018
22 0 10 -1.7388 -0.0050
22 0 12 0.5765 -0.0032
22 1 0 -1.5184 0.0004
22 1 1 1.0382 0.0039
22 1 2 -0.6231 0.0014
22 1 3 1.7758 0.0058
22 1 4 0.4508 0.0014
22 1 5 0.5074 0.0014
22 1 6 0.1178 0.0012
22 1 7 -0.9908 -0.0030
22 1 8 -0.2048 0.0005
22 1 9 -1.4619 -0.0031
22 1 10 0.7840 -0.0008
22 1 11 -0.8522 -0.0016
22 1 12 1.8169 -0.0016
22 2 0 1.2147 -0.0059
22 2 1 -0.2215 -0.0055
22 2 2 0.5384 -0.0011
22 2 3 -0.0155 -0.0022
22 2 4 -0.9979 0.0031
22 2 5 0.6546 -0.0003
22 2 6 -2.0324 0.0014
22 2 7 -0.0115 0.0004
22 2 8 -1.4798 -0.0040
22 2 9 -2.0559 0.0010
22 2 10 -0.0259 -0.0056
22 2 11 -2.9622 0.0001
22 2 12 0.7503 -0.0015
22 3 0 -0.9538 -0.0020
22 3 1 0.6790 0.0093
22 3 2 -0.2000 -0.0008
22 3 3 1.5728 0.0035
22 3 4 0.5648 -0.0006
22 3 5 1.6657 -0.0004
22 3 6 0.3783 -0.0009
22 3 7 1.1779 0.0004
22 3 8 0.9988 -0.0009
22 3 9 0.2562 0.0006
22 3 10 2.4973 0.0001
22 3 11 -0.5008 -0.0028
22 4 0 1.2637 -0.0031
22 4 1 0.2174 -0.0040
22 4 2 0.4612 -0.0015
22 4 3 0.1736 -0.0014
22 4 4 -0.8875 -0.0010
22 4 5 -0.3884 0.0018
22 4 6 -1.2975 -0.0010
22 4 7 -0.6514 0.0027
22 4 8 -0.9315 -0.0001
22 4 9 -0.4618 0.0010
22 4 10 -0.8006 0.0006
22 4 11 -0.1660 -0.0008
22 5 0 -1.8819 0.0063
22 5 1 1.2563 0.0084
22 5 2 -0.4356 0.0048
22 5 3 2.2935 0.0033
22 5 4 1.7222 0.0012
22 5 5 1.0018 0.0009
22 5 6 1.9354 -0.0017
22 5 7 -0.5433 0.0004
22 5 8 1.0727 -0.0027
22 5 9 -0.6415 -0.0012
22 5 10 0.7171 -0.0015
22 6 0 -1.7988 0.0000
22 6 1 0.1745 0.0028
22 6 2 -1.8133 0.0008
22 6 3 0.2690 0.0016
22 6 4 -2.0400 -0.0009
22 6 5 0.0733 -0.0002
22 6 6 -2.4803 -0.0011
22 6 7 0.0936 -0.0007
22 6 8 -2.5059 0.0008
22 6 9 0.4629 0.0007
22 6 10 -1.7133 0.0012
22 7 0 -2.3756 0.0033
22 7 1 0.4605 0.0058
22 7 2 -1.8682 0.0006
22 7 3 0.8521 0.0022
22 7 4 -0.1818 -0.0005
22 7 5 0.4028 -0.0005
22 7 6 1.9740 0.0004
22 7 7 -0.4242 -0.0011
22 7 8 2.8034 0.0008
22 7 9 -1.1577 -0.0014
22 8 0 0.4356 -0.0022
22 8 1 0.4070 -0.0041
22 8 2 0.6166 -0.0000
22 8 3 1.4198 -0.0006
22 8 4 0.5483 -0.0008
22 8 5 1.8415 0.0007
22 8 6 -0.1908 -0.0018
22 8 7 0.7331 -0.0008
22 9 0 -0.0322 0.0007
22 9 1 0.3352 0.0002
22 9 2 -0.2004 -0.0007
22 9 3 0.1388 0.0013
22 9 4 0.1616 -0.0004
22 9 5 -0.6199 0.0020
22 10 0 1.3735 -0.0026
22 10 1 0.2022 -0.0081
22 10 2 1.0148 -0.0008
23 0 2 1.5120 0.0030
23 0 4 1.5531 0.0003
23 0 6 0.5852 -0.0050
23 0 8 -0.5226 -0.0062
23 1 1 0.3799 -0.0012
23 1 2 -1.2889 0.0011
23 1 3 0.7187 -0.0020
23 1 4 -0.4673 0.0010
23 1 5 -0.2341 -0.0011
23 1 6 1.3317 -0.0007
23 1 7 -1.6716 -0.0017
23 1 8 1.6342 -0.0004
23 1 9 -1.2923 -0.0036
23 2 1 -1.5523 -0.0004
23 2 2 0.8352 0.0030
23 2 3 -1.1712 0.0011
23 2 4 0.2502 -0.0006
23 2 5 -0.8987 0.0013
23 2 6 -0.7665 -0.0010
23 2 7 -0.3759 0.0015
23 2 8 -0.9058 0.0001
23 2 9 0.7174 0.0018
23 3 1 3.1102 0.0004
23 3 2 0.9276 0.0012
23 3 3 1.2967 0.0004
23 3 4 0.2527 -0.0001
23 3 5 0.1680 -0.0013
23 3 6 -1.1740 -0.0009
23 3 7 0.5906 -0.0034
23 3 8 -1.7235 -0.0012
23 3 9 1.0122 -0.0036
23 4 1 -1.4426 0.0017
23 4 2 -0.1622 0.0056
23 4 3 -0.1697 -0.0016
23 4 4 -0.9340 -0.0009
23 4 5 0.3436 -0.0043
23 4 6 -1.5603 -0.0014
23 4 7 0.0584 -0.0033
23 4 8 -1.1411 -0.0000
23 5 1 -0.4265 -0.0033
23 5 2 1.4678 0.0011
23 5 3 -1.9958 -0.0060
23 5 4 1.5302 0.0024
23 5 5 -2.8429 -0.0039
23 5 6 0.8895 0.0014
23 5 7 -2.4032 -0.0006
23 6 1 -2.6846 0.0040
23 6 2 0.2965 0.0019
23 6 3 -0.5103 0.0003
23 6 4 0.7002 -0.0008
23 6 5 1.1057 -0.0027
23 6 6 0.6116 -0.0008
23 7 1 0.1389 -0.0010
23 7 2 0.0687 0.0020
23 7 3 -0.7011 0.0017
23 7 4 -0.3153 0.0005
24 0 0 -0.5224 0.0041
24 0 2 0.2467 0.0032
24 0 4 1.0981 0.0017
24 1 0 -0.1690 -0.0006
24 1 1 0.3748 0.0018
24 1 2 -0.8251 -0.0010
24 1 3 0.5232 -0.0002
24 1 4 -1.6140 -0.0024
24 1 5 -0.0746 -0.0009
24 2 0 3.3675 0.0028
24 2 1 -0.3203 0.0017
24 2 2 2.3571 -0.0002
24 2 3 -0.7719 -0.0032
24 2 4 0.4393 -0.0018
24 2 5 -0.7790 -0.0054
24 3 0 -0.7156 0.0011
24 3 1 0.1267 -0.0038
24 3 2 -0.6108 -0.0010
24 3 3 -0.0230 -0.0044
24 3 4 -0.4713 -0.0032
24 4 0 0.4092 0.0029
24 4 1 0.6096 0.0006
24 4 2 -0.0333 -0.0013
0 0 0 0.0 0.0
;
_shelx_fab_checksum 92540
_olex2_submission_special_instructions 'No special instructions were received'
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'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
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
O001 O 0.71038(7) 0.35677(7) 0.82019(6) 0.0424(3) Uani 1 1 d . . . . .
N002 N 0.73686(7) 0.52711(7) 0.81576(6) 0.0274(3) Uani 1 1 d . . . . .
N003 N 0.82528(7) 0.47665(7) 0.65317(6) 0.0296(3) Uani 1 1 d . . . . .
N004 N 0.80520(7) 0.37023(7) 0.88656(6) 0.0328(3) Uani 1 1 d . . . . .
N005 N 0.85553(7) 0.42615(7) 0.90071(6) 0.0319(3) Uani 1 1 d . . . . .
C006 C 0.81955(8) 0.46031(8) 0.75342(7) 0.0252(3) Uani 1 1 d . . . . .
C007 C 0.78574(8) 0.49053(8) 0.70474(7) 0.0254(3) Uani 1 1 d . . . . .
C008 C 0.88326(8) 0.42411(8) 0.73188(7) 0.0267(3) Uani 1 1 d . . . . .
C009 C 0.84763(8) 0.48144(9) 0.86351(7) 0.0275(3) Uani 1 1 d . . . . .
C00A C 0.72608(8) 0.61622(8) 0.69249(7) 0.0264(3) Uani 1 1 d . . . . .
C00B C 0.62116(8) 0.57199(8) 0.78460(7) 0.0267(3) Uani 1 1 d . . . . .
C00C C 0.68139(8) 0.51922(8) 0.76899(7) 0.0256(3) Uani 1 1 d . . . . .
H00C H 0.663001 0.467163 0.770616 0.031 Uiso 1 1 calc R U . . .
C00D C 0.79023(8) 0.46735(9) 0.81669(7) 0.0257(3) Uani 1 1 d . . . . .
C00E C 0.88505(8) 0.43655(8) 0.66871(7) 0.0288(4) Uani 1 1 d . . . . .
C00F C 0.67144(8) 0.49430(8) 0.65273(7) 0.0277(4) Uani 1 1 d . . . . .
C00G C 0.71573(8) 0.53227(8) 0.70387(7) 0.0251(3) Uani 1 1 d . . . . .
C00H C 0.89387(8) 0.54755(9) 0.86794(7) 0.0281(4) Uani 1 1 d . . . . .
C00I C 0.66815(9) 0.66158(9) 0.67814(7) 0.0303(4) Uani 1 1 d . . . . .
H00I H 0.623519 0.639387 0.671291 0.036 Uiso 1 1 calc R U . . .
C00J C 0.76136(9) 0.39108(9) 0.83932(7) 0.0297(4) Uani 1 1 d . . . . .
C00K C 0.80040(10) 0.30764(9) 0.92640(7) 0.0357(4) Uani 1 1 d . . . . .
C00L C 0.93824(9) 0.38287(9) 0.75875(8) 0.0333(4) Uani 1 1 d . . . . .
H00L H 0.938011 0.373194 0.800833 0.040 Uiso 1 1 calc R U . . .
C00M C 0.55161(9) 0.55100(10) 0.77182(8) 0.0347(4) Uani 1 1 d . . . . .
H00M H 0.542574 0.504621 0.752891 0.042 Uiso 1 1 calc R U . . .
C00N C 0.95784(9) 0.54303(10) 0.89975(8) 0.0367(4) Uani 1 1 d . . . . .
H00N H 0.972068 0.497148 0.917078 0.044 Uiso 1 1 calc R U . . .
C00O C 0.67512(10) 0.73853(9) 0.67379(8) 0.0372(4) Uani 1 1 d . . . . .
H00O H 0.635228 0.768124 0.664330 0.045 Uiso 1 1 calc R U . . .
C00P C 0.63278(9) 0.64045(9) 0.81284(7) 0.0345(4) Uani 1 1 d . . . . .
H00P H 0.679497 0.655629 0.821750 0.041 Uiso 1 1 calc R U . . .
C00Q C 0.63357(9) 0.42857(9) 0.66189(8) 0.0364(4) Uani 1 1 d . . . . .
H00Q H 0.630180 0.408486 0.701370 0.044 Uiso 1 1 calc R U . . .
C00R C 0.79115(9) 0.65094(9) 0.70085(8) 0.0350(4) Uani 1 1 d . . . . .
H00R H 0.831397 0.621705 0.709909 0.042 Uiso 1 1 calc R U . . .
C00S C 0.67652(10) 0.52055(10) 0.59316(8) 0.0365(4) Uani 1 1 d . . . . .
H00S H 0.702061 0.564888 0.585307 0.044 Uiso 1 1 calc R U . . .
C00T C 0.94035(9) 0.41054(9) 0.63228(8) 0.0380(4) Uani 1 1 d . . . . .
H00T H 0.940948 0.419629 0.590113 0.046 Uiso 1 1 calc R U . . .
C00U C 0.99406(10) 0.37107(9) 0.66015(9) 0.0414(4) Uani 1 1 d . . . . .
H00U H 1.032432 0.353423 0.636753 0.050 Uiso 1 1 calc R U . . .
C00V C 0.99254(9) 0.35676(9) 0.72273(9) 0.0402(4) Uani 1 1 d . . . . .
H00V H 1.029439 0.328694 0.740504 0.048 Uiso 1 1 calc R U . . .
C00W C 0.87426(9) 0.61611(9) 0.84277(8) 0.0379(4) Uani 1 1 d . . . . .
H00W H 0.831209 0.620208 0.821282 0.045 Uiso 1 1 calc R U . . .
C00X C 0.73999(10) 0.77229(10) 0.68318(9) 0.0450(5) Uani 1 1 d . . . . .
H00X H 0.744644 0.824770 0.680796 0.054 Uiso 1 1 calc R U . . .
C00Y C 1.00037(9) 0.60581(11) 0.90589(9) 0.0446(5) Uani 1 1 d . . . . .
H00Y H 1.043340 0.602427 0.927577 0.054 Uiso 1 1 calc R U . . .
C00Z C 0.98045(10) 0.67309(11) 0.88061(9) 0.0457(5) Uani 1 1 d . . . . .
H00Z H 1.009804 0.715504 0.884864 0.055 Uiso 1 1 calc R U . . .
C010 C 0.60645(11) 0.41853(11) 0.55582(9) 0.0483(5) Uani 1 1 d . . . . .
H010 H 0.584447 0.393082 0.523395 0.058 Uiso 1 1 calc R U . . .
C011 C 0.64481(11) 0.48283(11) 0.54532(8) 0.0462(5) Uani 1 1 d . . . . .
H011 H 0.649542 0.501278 0.505416 0.055 Uiso 1 1 calc R U . . .
C012 C 0.57669(10) 0.68659(10) 0.82804(9) 0.0453(5) Uani 1 1 d . . . . .
H012 H 0.585378 0.732728 0.847472 0.054 Uiso 1 1 calc R U . . .
C013 C 0.91763(10) 0.67837(10) 0.84912(9) 0.0443(5) Uani 1 1 d . . . . .
H013 H 0.904020 0.724463 0.831799 0.053 Uiso 1 1 calc R U . . .
C014 C 0.60065(11) 0.39193(10) 0.61410(8) 0.0456(5) Uani 1 1 d . . . . .
H014 H 0.573979 0.348273 0.621697 0.055 Uiso 1 1 calc R U . . .
C015 C 0.49566(10) 0.59769(11) 0.78668(9) 0.0474(5) Uani 1 1 d . . . . .
H015 H 0.448824 0.583183 0.777489 0.057 Uiso 1 1 calc R U . . .
C016 C 0.79779(10) 0.72801(10) 0.69609(9) 0.0464(5) Uani 1 1 d . . . . .
H016 H 0.842539 0.750446 0.701767 0.056 Uiso 1 1 calc R U . . .
C017 C 0.50824(10) 0.66549(11) 0.81495(9) 0.0489(5) Uani 1 1 d . . . . .
H017 H 0.470081 0.697136 0.825226 0.059 Uiso 1 1 calc R U . . .
C018 C 0.75047(11) 0.25214(11) 0.91714(9) 0.0493(5) Uani 1 1 d . . . . .
H018 H 0.719286 0.255032 0.883772 0.059 Uiso 1 1 calc R U . . .
C01A C 0.84712(13) 0.30215(11) 0.97451(9) 0.0597(6) Uani 1 1 d . . . . .
H01A H 0.882086 0.339110 0.980628 0.072 Uiso 1 1 calc R U . . .
C01B C 0.74634(13) 0.19224(12) 0.95700(10) 0.0619(6) Uani 1 1 d . . . . .
H01B H 0.712056 0.154621 0.950706 0.074 Uiso 1 1 calc R U . . .
C01C C 0.79173(16) 0.18716(13) 1.00560(11) 0.0718(7) Uani 1 1 d . . . . .
H01C H 0.788371 0.146733 1.032980 0.086 Uiso 1 1 calc R U . . .
C01D C 0.84192(16) 0.24162(14) 1.01370(11) 0.0808(9) Uani 1 1 d . . . . .
H01D H 0.873649 0.237884 1.046636 0.097 Uiso 1 1 calc R U . . .
H002 H 0.7180(10) 0.5299(10) 0.8528(9) 0.045(5) Uiso 1 1 d . . . . .
H003 H 0.8139(10) 0.4903(11) 0.6157(10) 0.051(6) 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
O001 0.0444(7) 0.0359(7) 0.0470(8) 0.0069(6) -0.0134(6) -0.0128(6)
N002 0.0267(7) 0.0314(7) 0.0242(7) -0.0029(6) -0.0011(6) 0.0038(6)
N003 0.0349(8) 0.0288(7) 0.0251(8) 0.0030(6) 0.0053(6) 0.0053(6)
N004 0.0380(8) 0.0302(7) 0.0301(8) 0.0050(6) -0.0060(6) -0.0052(6)
N005 0.0353(8) 0.0321(8) 0.0283(7) 0.0002(6) -0.0035(6) -0.0029(6)
C006 0.0277(8) 0.0214(7) 0.0263(8) 0.0008(6) 0.0004(6) -0.0010(6)
C007 0.0295(9) 0.0205(8) 0.0262(8) -0.0005(6) 0.0026(6) 0.0001(6)
C008 0.0281(8) 0.0199(7) 0.0322(9) -0.0007(6) 0.0013(7) 0.0000(6)
C009 0.0265(8) 0.0295(8) 0.0264(8) -0.0020(7) -0.0002(6) 0.0034(7)
C00A 0.0295(9) 0.0253(8) 0.0244(8) 0.0006(6) 0.0007(6) 0.0016(6)
C00B 0.0284(8) 0.0276(8) 0.0241(8) 0.0021(6) 0.0008(6) 0.0009(7)
C00C 0.0261(8) 0.0248(8) 0.0258(8) 0.0000(6) -0.0011(6) -0.0001(6)
C00D 0.0260(8) 0.0261(8) 0.0250(8) 0.0000(6) -0.0019(6) 0.0006(6)
C00E 0.0310(9) 0.0210(8) 0.0345(9) -0.0011(7) 0.0044(7) 0.0000(7)
C00F 0.0322(9) 0.0247(8) 0.0262(8) -0.0025(6) -0.0020(7) 0.0051(7)
C00G 0.0271(8) 0.0238(8) 0.0244(8) -0.0010(6) -0.0004(6) 0.0013(6)
C00H 0.0273(9) 0.0320(8) 0.0249(8) -0.0040(7) 0.0021(6) -0.0017(7)
C00I 0.0300(9) 0.0277(8) 0.0332(9) 0.0022(7) -0.0035(7) 0.0013(7)
C00J 0.0325(9) 0.0307(9) 0.0258(8) 0.0014(7) -0.0002(7) 0.0002(7)
C00K 0.0506(11) 0.0315(9) 0.0249(9) 0.0019(7) 0.0012(7) 0.0012(8)
C00L 0.0340(9) 0.0261(8) 0.0397(10) -0.0007(7) -0.0018(7) 0.0033(7)
C00M 0.0292(9) 0.0338(9) 0.0410(10) 0.0037(8) -0.0001(8) -0.0003(7)
C00N 0.0293(9) 0.0423(10) 0.0385(10) -0.0011(8) -0.0019(7) 0.0006(8)
C00O 0.0415(10) 0.0271(9) 0.0429(10) 0.0024(8) -0.0043(8) 0.0079(8)
C00P 0.0345(10) 0.0337(9) 0.0353(10) -0.0042(7) -0.0013(7) 0.0025(7)
C00Q 0.0449(11) 0.0336(9) 0.0308(9) -0.0005(7) -0.0034(8) -0.0022(8)
C00R 0.0313(9) 0.0293(9) 0.0443(10) 0.0025(8) 0.0005(7) 0.0016(7)
C00S 0.0492(11) 0.0324(9) 0.0279(9) 0.0012(7) -0.0012(8) 0.0022(8)
C00T 0.0419(11) 0.0304(9) 0.0418(10) -0.0017(8) 0.0134(8) 0.0018(8)
C00U 0.0353(10) 0.0327(9) 0.0560(12) -0.0058(8) 0.0131(8) 0.0035(8)
C00V 0.0329(10) 0.0294(9) 0.0583(12) -0.0014(8) 0.0002(8) 0.0065(7)
C00W 0.0342(10) 0.0345(9) 0.0448(11) 0.0008(8) -0.0049(8) -0.0040(8)
C00X 0.0481(12) 0.0236(9) 0.0633(13) 0.0006(8) -0.0029(10) -0.0007(8)
C00Y 0.0280(9) 0.0558(12) 0.0501(12) -0.0050(9) -0.0031(8) -0.0063(9)
C00Z 0.0365(11) 0.0428(11) 0.0579(12) -0.0094(9) 0.0052(9) -0.0133(8)
C010 0.0609(13) 0.0442(11) 0.0398(11) -0.0132(9) -0.0168(10) 0.0066(10)
C011 0.0667(13) 0.0447(11) 0.0271(10) -0.0021(8) -0.0085(9) 0.0080(10)
C012 0.0545(13) 0.0365(10) 0.0450(11) -0.0070(9) 0.0020(9) 0.0117(9)
C013 0.0420(11) 0.0350(10) 0.0558(12) 0.0006(9) 0.0000(9) -0.0053(8)
C014 0.0544(12) 0.0366(10) 0.0458(11) -0.0070(9) -0.0087(9) -0.0075(9)
C015 0.0302(10) 0.0511(12) 0.0610(13) 0.0083(10) 0.0005(9) 0.0076(9)
C016 0.0346(10) 0.0316(10) 0.0732(14) 0.0002(9) -0.0019(9) -0.0060(8)
C017 0.0400(11) 0.0484(12) 0.0581(13) 0.0011(10) 0.0060(9) 0.0192(9)
C018 0.0617(13) 0.0416(11) 0.0446(11) 0.0126(9) -0.0059(9) -0.0100(10)
C01A 0.0882(17) 0.0464(12) 0.0446(12) 0.0118(9) -0.0254(11) -0.0125(11)
C01B 0.0820(17) 0.0448(12) 0.0588(15) 0.0160(11) -0.0021(12) -0.0135(11)
C01C 0.121(2) 0.0450(13) 0.0492(14) 0.0201(11) -0.0047(14) -0.0055(14)
C01D 0.128(2) 0.0635(16) 0.0511(15) 0.0237(12) -0.0354(15) -0.0129(16)
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
C00C N002 H002 111.2(12) . . ?
C00D N002 C00C 115.28(12) . . ?
C00D N002 H002 107.5(12) . . ?
C007 N003 H003 125.8(13) . . ?
C00E N003 C007 109.31(13) . . ?
C00E N003 H003 124.9(13) . . ?
N005 N004 C00K 117.50(13) . . ?
C00J N004 N005 112.23(13) . . ?
C00J N004 C00K 129.66(14) . . ?
C009 N005 N004 108.83(13) . . ?
C007 C006 C008 108.00(13) . . ?
C007 C006 C00D 121.65(14) . . ?
C008 C006 C00D 130.35(14) . . ?
N003 C007 C00G 123.23(14) . . ?
C006 C007 N003 108.90(14) . . ?
C006 C007 C00G 127.87(14) . . ?
C00E C008 C006 105.88(13) . . ?
C00L C008 C006 135.33(15) . . ?
C00L C008 C00E 118.79(14) . . ?
N005 C009 C00D 112.77(14) . . ?
N005 C009 C00H 120.19(14) . . ?
C00H C009 C00D 126.99(14) . . ?
C00I C00A C00G 120.31(14) . . ?
C00R C00A C00G 121.88(14) . . ?
C00R C00A C00I 117.59(15) . . ?
C00M C00B C00C 119.53(14) . . ?
C00P C00B C00C 122.04(14) . . ?
C00P C00B C00M 118.41(15) . . ?
N002 C00C C00B 108.30(12) . . ?
N002 C00C H00C 108.2 . . ?
N002 C00C C00G 109.07(12) . . ?
C00B C00C H00C 108.2 . . ?
C00B C00C C00G 114.75(12) . . ?
C00G C00C H00C 108.2 . . ?
N002 C00D C006 107.47(12) . . ?
N002 C00D C009 112.26(12) . . ?
N002 C00D C00J 113.75(13) . . ?
C006 C00D C009 112.40(13) . . ?
C006 C00D C00J 110.72(13) . . ?
C009 C00D C00J 100.26(12) . . ?
N003 C00E C008 107.89(13) . . ?
N003 C00E C00T 129.90(16) . . ?
C00T C00E C008 122.21(15) . . ?
C00Q C00F C00G 122.60(14) . . ?
C00Q C00F C00S 117.09(15) . . ?
C00S C00F C00G 119.76(14) . . ?
C007 C00G C00A 111.83(13) . . ?
C007 C00G C00C 105.74(12) . . ?
C007 C00G C00F 105.21(12) . . ?
C00A C00G C00C 110.04(12) . . ?
C00A C00G C00F 112.08(12) . . ?
C00F C00G C00C 111.70(12) . . ?
C00N C00H C009 119.92(15) . . ?
C00W C00H C009 121.40(15) . . ?
C00W C00H C00N 118.64(15) . . ?
C00A C00I H00I 119.4 . . ?
C00O C00I C00A 121.16(16) . . ?
C00O C00I H00I 119.4 . . ?
O001 C00J N004 126.82(15) . . ?
O001 C00J C00D 127.56(15) . . ?
N004 C00J C00D 105.62(13) . . ?
C018 C00K N004 121.01(16) . . ?
C01A C00K N004 119.19(16) . . ?
C01A C00K C018 119.79(17) . . ?
C008 C00L H00L 120.5 . . ?
C00V C00L C008 118.98(16) . . ?
C00V C00L H00L 120.5 . . ?
C00B C00M H00M 119.7 . . ?
C015 C00M C00B 120.55(17) . . ?
C015 C00M H00M 119.7 . . ?
C00H C00N H00N 119.9 . . ?
C00Y C00N C00H 120.15(17) . . ?
C00Y C00N H00N 119.9 . . ?
C00I C00O H00O 119.7 . . ?
C00X C00O C00I 120.51(16) . . ?
C00X C00O H00O 119.7 . . ?
C00B C00P H00P 119.6 . . ?
C012 C00P C00B 120.82(16) . . ?
C012 C00P H00P 119.6 . . ?
C00F C00Q H00Q 119.4 . . ?
C014 C00Q C00F 121.27(17) . . ?
C014 C00Q H00Q 119.4 . . ?
C00A C00R H00R 119.5 . . ?
C016 C00R C00A 120.90(16) . . ?
C016 C00R H00R 119.5 . . ?
C00F C00S H00S 119.3 . . ?
C011 C00S C00F 121.42(17) . . ?
C011 C00S H00S 119.3 . . ?
C00E C00T H00T 121.2 . . ?
C00U C00T C00E 117.62(17) . . ?
C00U C00T H00T 121.2 . . ?
C00T C00U H00U 119.5 . . ?
C00T C00U C00V 121.06(16) . . ?
C00V C00U H00U 119.5 . . ?
C00L C00V C00U 121.32(17) . . ?
C00L C00V H00V 119.3 . . ?
C00U C00V H00V 119.3 . . ?
C00H C00W H00W 119.8 . . ?
C013 C00W C00H 120.48(17) . . ?
C013 C00W H00W 119.8 . . ?
C00O C00X H00X 120.6 . . ?
C016 C00X C00O 118.86(16) . . ?
C016 C00X H00X 120.6 . . ?
C00N C00Y H00Y 119.7 . . ?
C00Z C00Y C00N 120.59(17) . . ?
C00Z C00Y H00Y 119.7 . . ?
C00Y C00Z H00Z 120.0 . . ?
C013 C00Z C00Y 119.91(17) . . ?
C013 C00Z H00Z 120.0 . . ?
C011 C010 H010 120.4 . . ?
C014 C010 H010 120.4 . . ?
C014 C010 C011 119.18(17) . . ?
C00S C011 H011 119.9 . . ?
C010 C011 C00S 120.29(17) . . ?
C010 C011 H011 119.9 . . ?
C00P C012 H012 119.9 . . ?
C017 C012 C00P 120.30(18) . . ?
C017 C012 H012 119.9 . . ?
C00W C013 H013 119.9 . . ?
C00Z C013 C00W 120.24(18) . . ?
C00Z C013 H013 119.9 . . ?
C00Q C014 H014 119.6 . . ?
C010 C014 C00Q 120.72(18) . . ?
C010 C014 H014 119.6 . . ?
C00M C015 H015 119.9 . . ?
C017 C015 C00M 120.22(18) . . ?
C017 C015 H015 119.9 . . ?
C00R C016 H016 119.5 . . ?
C00X C016 C00R 120.96(17) . . ?
C00X C016 H016 119.5 . . ?
C012 C017 C015 119.71(17) . . ?
C012 C017 H017 120.1 . . ?
C015 C017 H017 120.1 . . ?
C00K C018 H018 120.1 . . ?
C00K C018 C01B 119.88(19) . . ?
C01B C018 H018 120.1 . . ?
C00K C01A H01A 120.4 . . ?
C00K C01A C01D 119.2(2) . . ?
C01D C01A H01A 120.4 . . ?
C018 C01B H01B 119.7 . . ?
C01C C01B C018 120.6(2) . . ?
C01C C01B H01B 119.7 . . ?
C01B C01C H01C 120.5 . . ?
C01D C01C C01B 119.1(2) . . ?
C01D C01C H01C 120.5 . . ?
C01A C01D H01D 119.3 . . ?
C01C C01D C01A 121.4(2) . . ?
C01C C01D H01D 119.3 . . ?
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
O001 C00J 1.2121(19) . ?
N002 C00C 1.4708(19) . ?
N002 C00D 1.463(2) . ?
N002 H002 0.889(19) . ?
N003 C007 1.377(2) . ?
N003 C00E 1.375(2) . ?
N003 H003 0.88(2) . ?
N004 N005 1.4087(18) . ?
N004 C00J 1.376(2) . ?
N004 C00K 1.420(2) . ?
N005 C009 1.2878(19) . ?
C006 C007 1.355(2) . ?
C006 C008 1.441(2) . ?
C006 C00D 1.500(2) . ?
C007 C00G 1.512(2) . ?
C008 C00E 1.405(2) . ?
C008 C00L 1.399(2) . ?
C009 C00D 1.512(2) . ?
C009 C00H 1.467(2) . ?
C00A C00G 1.528(2) . ?
C00A C00I 1.392(2) . ?
C00A C00R 1.383(2) . ?
C00B C00C 1.511(2) . ?
C00B C00M 1.389(2) . ?
C00B C00P 1.385(2) . ?
C00C H00C 0.9900 . ?
C00C C00G 1.586(2) . ?
C00D C00J 1.545(2) . ?
C00E C00T 1.391(2) . ?
C00F C00G 1.553(2) . ?
C00F C00Q 1.385(2) . ?
C00F C00S 1.392(2) . ?
C00H C00N 1.394(2) . ?
C00H C00W 1.390(2) . ?
C00I H00I 0.9400 . ?
C00I C00O 1.380(2) . ?
C00K C018 1.378(2) . ?
C00K C01A 1.378(3) . ?
C00L H00L 0.9400 . ?
C00L C00V 1.373(2) . ?
C00M H00M 0.9400 . ?
C00M C015 1.380(2) . ?
C00N H00N 0.9400 . ?
C00N C00Y 1.381(2) . ?
C00O H00O 0.9400 . ?
C00O C00X 1.376(2) . ?
C00P H00P 0.9400 . ?
C00P C012 1.378(2) . ?
C00Q H00Q 0.9400 . ?
C00Q C014 1.382(2) . ?
C00R H00R 0.9400 . ?
C00R C016 1.382(2) . ?
C00S H00S 0.9400 . ?
C00S C011 1.382(2) . ?
C00T H00T 0.9400 . ?
C00T C00U 1.374(3) . ?
C00U H00U 0.9400 . ?
C00U C00V 1.398(3) . ?
C00V H00V 0.9400 . ?
C00W H00W 0.9400 . ?
C00W C013 1.383(2) . ?
C00X H00X 0.9400 . ?
C00X C016 1.372(2) . ?
C00Y H00Y 0.9400 . ?
C00Y C00Z 1.372(3) . ?
C00Z H00Z 0.9400 . ?
C00Z C013 1.372(3) . ?
C010 H010 0.9400 . ?
C010 C011 1.373(3) . ?
C010 C014 1.369(3) . ?
C011 H011 0.9400 . ?
C012 H012 0.9400 . ?
C012 C017 1.372(3) . ?
C013 H013 0.9400 . ?
C014 H014 0.9400 . ?
C015 H015 0.9400 . ?
C015 C017 1.378(3) . ?
C016 H016 0.9400 . ?
C017 H017 0.9400 . ?
C018 H018 0.9400 . ?
C018 C01B 1.382(3) . ?
C01A H01A 0.9400 . ?
C01A C01D 1.383(3) . ?
C01B H01B 0.9400 . ?
C01B C01C 1.370(3) . ?
C01C H01C 0.9400 . ?
C01C C01D 1.365(3) . ?
C01D H01D 0.9400 . ?
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
N002 C00C C00G C007 42.72(15) . . . . ?
N002 C00C C00G C00A -78.21(15) . . . . ?
N002 C00C C00G C00F 156.65(12) . . . . ?
N002 C00D C00J O001 54.0(2) . . . . ?
N002 C00D C00J N004 -125.30(14) . . . . ?
N003 C007 C00G C00A -72.65(18) . . . . ?
N003 C007 C00G C00C 167.59(14) . . . . ?
N003 C007 C00G C00F 49.25(18) . . . . ?
N003 C00E C00T C00U -179.72(16) . . . . ?
N004 N005 C009 C00D -2.02(18) . . . . ?
N004 N005 C009 C00H -179.67(13) . . . . ?
N004 C00K C018 C01B -179.23(19) . . . . ?
N004 C00K C01A C01D 179.3(2) . . . . ?
N005 N004 C00J O001 -174.56(17) . . . . ?
N005 N004 C00J C00D 4.73(17) . . . . ?
N005 N004 C00K C018 177.24(16) . . . . ?
N005 N004 C00K C01A -3.6(2) . . . . ?
N005 C009 C00D N002 125.66(15) . . . . ?
N005 C009 C00D C006 -113.04(15) . . . . ?
N005 C009 C00D C00J 4.57(17) . . . . ?
N005 C009 C00H C00N 17.9(2) . . . . ?
N005 C009 C00H C00W -159.76(16) . . . . ?
C006 C007 C00G C00A 108.25(18) . . . . ?
C006 C007 C00G C00C -11.5(2) . . . . ?
C006 C007 C00G C00F -129.85(16) . . . . ?
C006 C008 C00E N003 -1.03(16) . . . . ?
C006 C008 C00E C00T 178.83(15) . . . . ?
C006 C008 C00L C00V -179.38(17) . . . . ?
C006 C00D C00J O001 -67.2(2) . . . . ?
C006 C00D C00J N004 113.56(14) . . . . ?
C007 N003 C00E C008 0.42(17) . . . . ?
C007 N003 C00E C00T -179.43(16) . . . . ?
C007 C006 C008 C00E 1.29(17) . . . . ?
C007 C006 C008 C00L -178.53(17) . . . . ?
C007 C006 C00D N002 -16.3(2) . . . . ?
C007 C006 C00D C009 -140.31(15) . . . . ?
C007 C006 C00D C00J 108.47(16) . . . . ?
C008 C006 C007 N003 -1.06(17) . . . . ?
C008 C006 C007 C00G 178.15(14) . . . . ?
C008 C006 C00D N002 163.56(15) . . . . ?
C008 C006 C00D C009 39.6(2) . . . . ?
C008 C006 C00D C00J -71.7(2) . . . . ?
C008 C00E C00T C00U 0.5(2) . . . . ?
C008 C00L C00V C00U 0.5(2) . . . . ?
C009 C00D C00J O001 173.99(17) . . . . ?
C009 C00D C00J N004 -5.29(15) . . . . ?
C009 C00H C00N C00Y -177.70(16) . . . . ?
C009 C00H C00W C013 177.95(16) . . . . ?
C00A C00I C00O C00X 0.5(3) . . . . ?
C00A C00R C016 C00X 0.3(3) . . . . ?
C00B C00C C00G C007 164.41(13) . . . . ?
C00B C00C C00G C00A 43.48(17) . . . . ?
C00B C00C C00G C00F -81.67(16) . . . . ?
C00B C00M C015 C017 -0.6(3) . . . . ?
C00B C00P C012 C017 -0.5(3) . . . . ?
C00C N002 C00D C006 52.75(17) . . . . ?
C00C N002 C00D C009 176.84(13) . . . . ?
C00C N002 C00D C00J -70.19(17) . . . . ?
C00C C00B C00M C015 178.81(16) . . . . ?
C00C C00B C00P C012 -178.23(16) . . . . ?
C00D N002 C00C C00B 165.02(13) . . . . ?
C00D N002 C00C C00G -69.46(16) . . . . ?
C00D C006 C007 N003 178.84(13) . . . . ?
C00D C006 C007 C00G -2.0(2) . . . . ?
C00D C006 C008 C00E -178.60(15) . . . . ?
C00D C006 C008 C00L 1.6(3) . . . . ?
C00D C009 C00H C00N -159.34(15) . . . . ?
C00D C009 C00H C00W 23.0(2) . . . . ?
C00E N003 C007 C006 0.42(18) . . . . ?
C00E N003 C007 C00G -178.84(14) . . . . ?
C00E C008 C00L C00V 0.8(2) . . . . ?
C00E C00T C00U C00V 0.9(3) . . . . ?
C00F C00Q C014 C010 2.0(3) . . . . ?
C00F C00S C011 C010 0.9(3) . . . . ?
C00G C00A C00I C00O 173.34(15) . . . . ?
C00G C00A C00R C016 -173.62(16) . . . . ?
C00G C00F C00Q C014 -173.27(16) . . . . ?
C00G C00F C00S C011 172.08(16) . . . . ?
C00H C009 C00D N002 -56.9(2) . . . . ?
C00H C009 C00D C006 64.4(2) . . . . ?
C00H C009 C00D C00J -177.98(15) . . . . ?
C00H C00N C00Y C00Z -0.3(3) . . . . ?
C00H C00W C013 C00Z -0.3(3) . . . . ?
C00I C00A C00G C007 167.27(14) . . . . ?
C00I C00A C00G C00C -75.53(17) . . . . ?
C00I C00A C00G C00F 49.40(19) . . . . ?
C00I C00A C00R C016 1.1(2) . . . . ?
C00I C00O C00X C016 0.9(3) . . . . ?
C00J N004 N005 C009 -1.89(18) . . . . ?
C00J N004 C00K C018 7.0(3) . . . . ?
C00J N004 C00K C01A -173.78(18) . . . . ?
C00K N004 N005 C009 -173.75(14) . . . . ?
C00K N004 C00J O001 -3.9(3) . . . . ?
C00K N004 C00J C00D 175.34(16) . . . . ?
C00K C018 C01B C01C -0.4(4) . . . . ?
C00K C01A C01D C01C 0.2(4) . . . . ?
C00L C008 C00E N003 178.83(14) . . . . ?
C00L C008 C00E C00T -1.3(2) . . . . ?
C00M C00B C00C N002 -145.40(15) . . . . ?
C00M C00B C00C C00G 92.49(17) . . . . ?
C00M C00B C00P C012 0.1(3) . . . . ?
C00M C015 C017 C012 0.3(3) . . . . ?
C00N C00H C00W C013 0.2(3) . . . . ?
C00N C00Y C00Z C013 0.3(3) . . . . ?
C00O C00X C016 C00R -1.3(3) . . . . ?
C00P C00B C00C N002 33.0(2) . . . . ?
C00P C00B C00C C00G -89.14(18) . . . . ?
C00P C00B C00M C015 0.4(2) . . . . ?
C00P C012 C017 C015 0.2(3) . . . . ?
C00Q C00F C00G C007 82.18(18) . . . . ?
C00Q C00F C00G C00A -156.07(15) . . . . ?
C00Q C00F C00G C00C -32.1(2) . . . . ?
C00Q C00F C00S C011 0.3(3) . . . . ?
C00R C00A C00G C007 -18.2(2) . . . . ?
C00R C00A C00G C00C 99.01(17) . . . . ?
C00R C00A C00G C00F -136.06(15) . . . . ?
C00R C00A C00I C00O -1.4(2) . . . . ?
C00S C00F C00G C007 -89.10(17) . . . . ?
C00S C00F C00G C00A 32.6(2) . . . . ?
C00S C00F C00G C00C 156.65(14) . . . . ?
C00S C00F C00Q C014 -1.8(2) . . . . ?
C00T C00U C00V C00L -1.4(3) . . . . ?
C00W C00H C00N C00Y 0.1(2) . . . . ?
C00Y C00Z C013 C00W 0.0(3) . . . . ?
C011 C010 C014 C00Q -0.8(3) . . . . ?
C014 C010 C011 C00S -0.7(3) . . . . ?
C018 C00K C01A C01D -1.5(3) . . . . ?
C018 C01B C01C C01D -0.9(4) . . . . ?
C01A C00K C018 C01B 1.6(3) . . . . ?
C01B C01C C01D C01A 1.0(4) . . . . ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 378.8 101.7 ?
2 0.000 0.500 0.500 378.8 101.7 ?
3 0.500 0.000 0.500 378.8 101.7 ?
4 0.500 0.500 0.000 378.8 101.7 ?