#------------------------------------------------------------------------------
#$Date: 2019-05-24 05:17:41 +0300 (Fri, 24 May 2019) $
#$Revision: 215468 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/16/2021644.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2021644
loop_
_publ_author_name
'Ren, Xiu-Hui'
'Li, Gang-Yuan'
'Du, Hua'
'Ma, Jian-Ping'
'Geng, Yan'
'Dong, Yu-bin'
_publ_section_title
;
Thermally activated delayed fluorescent (TADF) coordination polymer with
the generation of singlet oxygen
;
_journal_coeditor_code YP3184
_journal_issue 6
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2053229619006119
_journal_volume 75
_journal_year 2019
_chemical_formula_iupac '[Cd (C39 H24 N2 O4) (H2 O1)1.5]'
_chemical_formula_moiety 'C39 H27 Cd N2 O5.5'
_chemical_formula_sum 'C39 H27 Cd N2 O5.5'
_chemical_formula_weight 724.03
_chemical_name_systematic
;
catena-Poly[hemi-\m-aqua-aqua(\m~3~-4,4'-{9,9'-spirobi[10H-\
acridine]-10,10'-diyl}dibenzoato)cadmium(II)]
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-C 2yc'
_space_group_name_H-M_alt 'C 1 2/c 1'
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 1 2/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary iterative
_atom_sites_solution_secondary difmap
_audit_creation_method
;
Olex2 1.2
(compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha 90.00
_cell_angle_beta 108.581(7)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 27.4361(19)
_cell_length_b 9.0861(9)
_cell_length_c 40.473(2)
_cell_measurement_reflns_used 4113
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 70.7010
_cell_measurement_theta_min 7.0430
_cell_volume 9563.5(13)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
olex2.solve (Bourhis et al., 2015)
;
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 16.0793
_diffrn_measured_fraction_theta_full 0.9947
_diffrn_measured_fraction_theta_max 0.9679
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku OD SuperNova Dual source diffractometer with an Eos detector'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0568
_diffrn_reflns_av_unetI/netI 0.0566
_diffrn_reflns_limit_h_max 33
_diffrn_reflns_limit_h_min -30
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 49
_diffrn_reflns_limit_l_min -48
_diffrn_reflns_number 16822
_diffrn_reflns_theta_full 67.08
_diffrn_reflns_theta_max 71.25
_diffrn_reflns_theta_min 3.40
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 3.935
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.65971
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.006
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 2936
_exptl_crystal_size_max 0.29
_exptl_crystal_size_mid 0.23
_exptl_crystal_size_min 0.14
_refine_diff_density_max 0.624
_refine_diff_density_min -1.221
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.118
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 429
_refine_ls_number_reflns 8499
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.118
_refine_ls_R_factor_all 0.0855
_refine_ls_R_factor_gt 0.0671
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1147P)^2^+0.6298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1980
_refine_ls_wR_factor_ref 0.2269
_reflns_number_gt 5609
_reflns_number_total 8499
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file yp3184sup1.cif
_cod_data_source_block I
_cod_original_formula_sum 'C39 H27 Cd N2 O5.50'
_cod_database_code 2021644
_shelx_res_file
;
TITL CF solution in C2/c
CELL 1.54184 27.4361 9.08608 40.47299 90 108.5809 90
ZERR 8 0.00191 0.00089 0.00232 0 0.0072 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H Cd N O
UNIT 312 216 8 16 44
L.S. 4
PLAN 25
BOND $H
conf
htab 2
fmap 2
acta
SHEL 999 0.837
REM D:/data/20151119/2754/olex2_exp_2754/exp_2754_sqd-mask.hkl
WGHT 0.114700 0.629800
FVAR 9.48493
C1 1 0.558350 0.795614 0.298675 11.00000 0.15588 0.11773 =
0.02922 0.01147 0.00998 0.01719
C2 1 0.568242 0.694334 0.329099 11.00000 0.10100 0.07703 =
0.05483 0.01033 0.01856 0.01495
C3 1 0.532690 0.675468 0.346532 11.00000 0.08857 0.07554 =
0.05730 -0.00158 0.01609 0.02018
AFIX 43
H3 2 0.501077 0.723130 0.338751 11.00000 -1.20000
AFIX 0
C4 1 0.544437 0.585125 0.375667 11.00000 0.08256 0.06894 =
0.05666 0.00739 0.02195 0.00487
AFIX 43
H4 2 0.520366 0.571594 0.387187 11.00000 -1.20000
AFIX 0
C5 1 0.591139 0.515588 0.387657 11.00000 0.07978 0.06090 =
0.04769 0.00967 0.02168 0.00306
C6 1 0.626694 0.534093 0.370748 11.00000 0.08893 0.10621 =
0.07421 0.03513 0.03126 0.01973
AFIX 43
H6 2 0.658041 0.485107 0.378680 11.00000 -1.20000
AFIX 0
C7 1 0.616185 0.626291 0.341583 11.00000 0.08357 0.12704 =
0.06077 0.02751 0.03123 0.00879
AFIX 43
H7 2 0.640882 0.641941 0.330675 11.00000 -1.20000
AFIX 0
C8 1 0.624674 0.492289 0.450932 11.00000 0.04860 0.05079 =
0.05185 -0.00018 0.01896 0.00160
C9 1 0.643040 0.638271 0.453443 11.00000 0.06268 0.05134 =
0.06732 0.00652 0.02832 0.00351
AFIX 43
H9 2 0.640387 0.690888 0.433234 11.00000 -1.20000
AFIX 0
C10 1 0.664767 0.703568 0.485335 11.00000 0.05832 0.05171 =
0.07433 -0.00317 0.02384 -0.00391
AFIX 43
H10 2 0.676459 0.800103 0.486482 11.00000 -1.20000
AFIX 0
C11 1 0.669454 0.627856 0.515636 11.00000 0.05084 0.05569 =
0.07042 -0.01587 0.01208 -0.00116
AFIX 43
H11 2 0.684612 0.671793 0.537236 11.00000 -1.20000
AFIX 0
C12 1 0.651208 0.485404 0.513332 11.00000 0.05183 0.05351 =
0.05316 -0.00047 0.01829 0.00487
AFIX 43
H12 2 0.653742 0.434931 0.533803 11.00000 -1.20000
AFIX 0
C13 1 0.629162 0.414199 0.481604 11.00000 0.04134 0.04580 =
0.04751 0.00182 0.01819 0.00829
C14 1 0.607501 0.257997 0.480999 11.00000 0.04262 0.04904 =
0.04706 0.00507 0.01617 0.00393
C15 1 0.594635 0.190671 0.444735 11.00000 0.04468 0.05068 =
0.05133 -0.00106 0.01670 0.00442
C16 1 0.591393 0.275828 0.415525 11.00000 0.06070 0.05680 =
0.04948 -0.00608 0.01716 0.00564
C17 1 0.574508 0.209716 0.382400 11.00000 0.08985 0.07529 =
0.04974 -0.00593 0.01791 0.00621
AFIX 43
H17 2 0.571201 0.266379 0.362668 11.00000 -1.20000
AFIX 0
C18 1 0.562737 0.060971 0.378838 11.00000 0.08368 0.07282 =
0.06346 -0.02036 0.01537 0.00235
AFIX 43
H18 2 0.551769 0.018063 0.356833 11.00000 -1.20000
AFIX 0
C19 1 0.567393 -0.023923 0.408317 11.00000 0.08962 0.05788 =
0.06363 -0.01691 0.01882 -0.00421
AFIX 43
H19 2 0.559817 -0.123929 0.406178 11.00000 -1.20000
AFIX 0
C20 1 0.583327 0.041612 0.440678 11.00000 0.06466 0.05139 =
0.06869 -0.00452 0.02270 -0.00164
AFIX 43
H20 2 0.586593 -0.015540 0.460330 11.00000 -1.20000
AFIX 0
C21 1 0.647510 0.164748 0.507239 11.00000 0.04337 0.04456 =
0.05252 0.00398 0.01922 0.00348
C22 1 0.693885 0.134971 0.501276 11.00000 0.04806 0.05225 =
0.06502 0.00271 0.02354 0.00419
AFIX 43
H22 2 0.699161 0.171503 0.481220 11.00000 -1.20000
AFIX 0
C23 1 0.732401 0.052286 0.524454 11.00000 0.04479 0.06475 =
0.08179 0.00124 0.02649 0.01073
AFIX 43
H23 2 0.763324 0.035312 0.520239 11.00000 -1.20000
AFIX 0
C24 1 0.724175 -0.003439 0.553402 11.00000 0.05894 0.05977 =
0.07439 0.00310 0.01768 0.00725
AFIX 43
H24 2 0.749542 -0.060848 0.568690 11.00000 -1.20000
AFIX 0
C25 1 0.679144 0.023068 0.560654 11.00000 0.07007 0.08017 =
0.05461 0.01577 0.02348 0.00638
AFIX 43
H25 2 0.674563 -0.015008 0.580790 11.00000 -1.20000
AFIX 0
C26 1 0.639919 0.108456 0.537331 11.00000 0.05094 0.06384 =
0.05175 0.00521 0.02160 0.00358
C27 1 0.552969 0.208313 0.520739 11.00000 0.05014 0.06643 =
0.06781 0.00110 0.03036 0.00328
C28 1 0.505870 0.222495 0.527811 11.00000 0.06585 0.07959 =
0.08634 0.01396 0.04359 0.01485
AFIX 43
H28 2 0.502695 0.185523 0.548454 11.00000 -1.20000
AFIX 0
C29 1 0.465319 0.290298 0.504341 11.00000 0.04151 0.08947 =
0.10716 -0.00163 0.03733 0.00782
AFIX 43
H29 2 0.434064 0.295607 0.508691 11.00000 -1.20000
AFIX 0
C30 1 0.469539 0.350570 0.474603 11.00000 0.05044 0.07666 =
0.08713 0.00178 0.02283 0.01389
AFIX 43
H30 2 0.442022 0.400833 0.459275 11.00000 -1.20000
AFIX 0
C31 1 0.515457 0.335884 0.467523 11.00000 0.05129 0.06267 =
0.06718 0.00394 0.02117 0.01166
AFIX 43
H31 2 0.517886 0.373612 0.446744 11.00000 -1.20000
AFIX 0
C32 1 0.557634 0.267254 0.490240 11.00000 0.04176 0.05044 =
0.06129 -0.00072 0.02210 0.00415
C33 1 0.591787 0.107638 0.578990 11.00000 0.06051 0.08157 =
0.05461 -0.00238 0.02912 -0.00014
C34 1 0.571430 -0.018958 0.586604 11.00000 0.09072 0.08589 =
0.05145 -0.00239 0.03412 -0.00757
AFIX 43
H34 2 0.559591 -0.090489 0.569478 11.00000 -1.20000
AFIX 0
C35 1 0.568062 -0.043005 0.619833 11.00000 0.09453 0.08478 =
0.07241 0.00048 0.04654 -0.00875
AFIX 43
H35 2 0.554022 -0.130137 0.624799 11.00000 -1.20000
AFIX 0
C36 1 0.585273 0.060746 0.644841 11.00000 0.08333 0.09114 =
0.05041 -0.01199 0.02963 -0.00960
C37 1 0.605482 0.187683 0.637141 11.00000 0.15241 0.11426 =
0.07447 -0.02992 0.05901 -0.03896
AFIX 43
H37 2 0.617304 0.259045 0.654311 11.00000 -1.20000
AFIX 0
C38 1 0.608833 0.213017 0.603747 11.00000 0.13971 0.09276 =
0.09543 -0.01182 0.06590 -0.03042
AFIX 43
H38 2 0.622506 0.300554 0.598662 11.00000 -1.20000
AFIX 0
C39 1 0.579786 0.038252 0.680395 11.00000 0.09518 0.11097 =
0.05456 -0.01000 0.03151 -0.00123
CD1 3 0.559298 0.023983 0.741018 11.00000 0.11173 0.11008 =
0.04336 -0.00852 0.03215 0.00927
N1 4 0.602898 0.427563 0.418606 11.00000 0.09039 0.05189 =
0.04674 0.00054 0.02090 0.00043
N2 4 0.594254 0.134986 0.544623 11.00000 0.06312 0.09406 =
0.06091 0.01651 0.03515 0.01806
O1 5 0.560189 -0.074042 0.686976 11.00000 0.12221 0.10957 =
0.05674 -0.00146 0.04495 -0.00418
O2 5 0.594716 0.142403 0.702274 11.00000 0.17495 0.15842 =
0.07687 -0.04024 0.06818 -0.04847
O3 5 0.588898 0.812676 0.283456 11.00000 0.17529 0.17944 =
0.06799 0.06731 0.03302 0.01117
O4 5 0.517923 0.866465 0.290069 11.00000 0.18999 0.18541 =
0.07129 0.04762 0.02009 0.07944
O5 5 0.500000 -0.131820 0.750000 10.50000 0.33008 0.09862 =
0.30247 0.00000 0.25010 0.00000
AFIX 23
H5A 2 0.484915 -0.193729 0.729792 10.50000 -1.20000
H5B 2 0.515086 -0.193723 0.770209 10.50000 -1.20000
AFIX 0
O6 5 0.623983 -0.135543 0.768249 11.00000 0.36713 0.33378 =
0.12081 -0.04450 -0.04360 0.22937
AFIX 3
H6A 2 0.636773 -0.180293 0.751159 11.00000 -1.50000
H6B 2 0.651173 -0.081683 0.784669 11.00000 -1.50000
HKLF 4
REM CF solution in C2/c
REM R1 = 0.0671 for 5609 Fo > 4sig(Fo) and 0.0855 for all 8499 data
REM 429 parameters refined using 0 restraints
END
WGHT 0.1147 0.6448
REM Highest difference peak 0.624, deepest hole -1.221, 1-sigma level 0.075
Q1 1 0.5615 0.8230 0.2565 11.00000 0.05 0.62
Q2 1 0.5541 0.1602 0.7256 11.00000 0.05 0.54
Q3 1 0.5527 -0.1430 0.7251 11.00000 0.05 0.54
Q4 1 0.6093 -0.0198 0.7681 11.00000 0.05 0.49
Q5 1 0.5597 -0.1424 0.7576 11.00000 0.05 0.45
Q6 1 0.5000 -0.2646 0.7500 10.50000 0.05 0.43
Q7 1 0.4958 0.7851 0.2742 11.00000 0.05 0.43
Q8 1 0.5370 -0.2033 0.7911 11.00000 0.05 0.41
Q9 1 0.4890 -0.2343 0.7589 11.00000 0.05 0.41
Q10 1 0.5872 0.8883 0.2742 11.00000 0.05 0.38
Q11 1 0.5618 -0.0379 0.7134 11.00000 0.05 0.38
Q12 1 0.5072 -0.0300 0.7135 11.00000 0.05 0.36
Q13 1 0.5847 -0.1736 0.7792 11.00000 0.05 0.36
Q14 1 0.5653 0.7128 0.2700 11.00000 0.05 0.35
Q15 1 0.6090 0.0264 0.7100 11.00000 0.05 0.34
Q16 1 0.5420 -0.0528 0.7101 11.00000 0.05 0.33
Q17 1 0.5830 -0.1752 0.6795 11.00000 0.05 0.32
Q18 1 0.5104 0.9979 0.2737 11.00000 0.05 0.30
Q19 1 0.5567 -0.0013 0.7678 11.00000 0.05 0.30
Q20 1 0.5113 0.6756 0.4114 11.00000 0.05 0.28
Q21 1 0.5577 0.6299 0.3029 11.00000 0.05 0.28
Q22 1 0.5288 0.7392 0.2893 11.00000 0.05 0.28
Q23 1 0.5807 0.5241 0.4132 11.00000 0.05 0.28
Q24 1 0.5223 0.7964 0.3551 11.00000 0.05 0.27
Q25 1 0.5113 0.5512 0.3911 11.00000 0.05 0.27
REM The information below was added by Olex2.
REM
REM R1 = 0.0671 for 5609 Fo > 4sig(Fo) and 0.0855 for all 8499 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.62, deepest hole -1.22
REM Mean Shift 0, Max Shift 0.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0855
REM R1_gt = 0.0671
REM wR_ref = 0.2269
REM GOOF = 1.118
REM Shift_max = 0
REM Shift_mean = 0
REM Reflections_all = 8499
REM Reflections_gt = 5609
REM Parameters = n/a
REM Hole = 0.62
REM Peak = -1.22
REM Flack = n/a
;
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
C C1 0.5584(3) 0.7956(8) 0.29867(12) 0.106(2) Uani d . 1 1
C C2 0.5682(2) 0.6943(6) 0.32910(13) 0.0791(14) Uani d . 1 1
C C3 0.5327(2) 0.6755(6) 0.34653(12) 0.0755(13) Uani d . 1 1
H H3 0.5011 0.7231 0.3388 0.091 Uiso calc R 1 1
C C4 0.5444(2) 0.5851(6) 0.37567(12) 0.0694(12) Uani d . 1 1
H H4 0.5204 0.5716 0.3872 0.083 Uiso calc R 1 1
C C5 0.5911(2) 0.5156(5) 0.38766(12) 0.0625(11) Uani d . 1 1
C C6 0.6267(2) 0.5341(7) 0.37075(16) 0.0885(17) Uani d . 1 1
H H6 0.6580 0.4851 0.3787 0.106 Uiso calc R 1 1
C C7 0.6162(2) 0.6263(7) 0.34158(13) 0.0885(17) Uani d . 1 1
H H7 0.6409 0.6419 0.3307 0.106 Uiso calc R 1 1
C C8 0.62467(15) 0.4923(4) 0.45093(11) 0.0497(9) Uani d . 1 1
C C9 0.64304(16) 0.6383(5) 0.45344(12) 0.0586(10) Uani d . 1 1
H H9 0.6404 0.6909 0.4332 0.070 Uiso calc R 1 1
C C10 0.66477(16) 0.7036(5) 0.48533(12) 0.0608(10) Uani d . 1 1
H H10 0.6765 0.8001 0.4865 0.073 Uiso calc R 1 1
C C11 0.66945(15) 0.6279(5) 0.51564(13) 0.0607(11) Uani d . 1 1
H H11 0.6846 0.6718 0.5372 0.073 Uiso calc R 1 1
C C12 0.65121(16) 0.4854(4) 0.51333(12) 0.0525(9) Uani d . 1 1
H H12 0.6537 0.4349 0.5338 0.063 Uiso calc R 1 1
C C13 0.62916(13) 0.4142(4) 0.48160(10) 0.0439(8) Uani d . 1 1
C C14 0.60750(13) 0.2580(4) 0.48100(10) 0.0458(8) Uani d . 1 1
C C15 0.59464(13) 0.1907(4) 0.44474(10) 0.0486(8) Uani d . 1 1
C C16 0.59139(16) 0.2758(5) 0.41552(10) 0.0558(9) Uani d . 1 1
C C17 0.5745(2) 0.2097(6) 0.38240(12) 0.0726(13) Uani d . 1 1
H H17 0.5712 0.2664 0.3627 0.087 Uiso calc R 1 1
C C18 0.5627(2) 0.0610(6) 0.37884(14) 0.0752(14) Uani d . 1 1
H H18 0.5518 0.0181 0.3568 0.090 Uiso calc R 1 1
C C19 0.5674(2) -0.0239(5) 0.40832(14) 0.0717(13) Uani d . 1 1
H H19 0.5598 -0.1239 0.4062 0.086 Uiso calc R 1 1
C C20 0.58333(18) 0.0416(5) 0.44068(13) 0.0612(11) Uani d . 1 1
H H20 0.5866 -0.0155 0.4603 0.073 Uiso calc R 1 1
C C21 0.64751(13) 0.1647(4) 0.50724(10) 0.0459(8) Uani d . 1 1
C C22 0.69388(14) 0.1350(4) 0.50128(12) 0.0538(9) Uani d . 1 1
H H22 0.6992 0.1715 0.4812 0.065 Uiso calc R 1 1
C C23 0.73240(16) 0.0523(5) 0.52445(14) 0.0623(11) Uani d . 1 1
H H23 0.7633 0.0353 0.5202 0.075 Uiso calc R 1 1
C C24 0.72417(18) -0.0034(5) 0.55340(15) 0.0652(12) Uani d . 1 1
H H24 0.7495 -0.0608 0.5687 0.078 Uiso calc R 1 1
C C25 0.6791(2) 0.0231(6) 0.56065(14) 0.0674(12) Uani d . 1 1
H H25 0.6746 -0.0150 0.5808 0.081 Uiso calc R 1 1
C C26 0.63992(15) 0.1085(5) 0.53733(11) 0.0543(9) Uani d . 1 1
C C27 0.55297(16) 0.2083(5) 0.52074(12) 0.0587(10) Uani d . 1 1
C C28 0.50587(18) 0.2225(6) 0.52781(14) 0.0727(13) Uani d . 1 1
H H28 0.5027 0.1855 0.5485 0.087 Uiso calc R 1 1
C C29 0.46532(16) 0.2903(6) 0.50434(15) 0.0762(14) Uani d . 1 1
H H29 0.4341 0.2956 0.5087 0.091 Uiso calc R 1 1
C C30 0.46954(17) 0.3506(6) 0.47460(14) 0.0712(13) Uani d . 1 1
H H30 0.4420 0.4008 0.4593 0.085 Uiso calc R 1 1
C C31 0.51546(15) 0.3359(5) 0.46752(12) 0.0598(10) Uani d . 1 1
H H31 0.5179 0.3736 0.4467 0.072 Uiso calc R 1 1
C C32 0.55763(13) 0.2673(4) 0.49024(10) 0.0498(9) Uani d . 1 1
C C33 0.59179(17) 0.1076(6) 0.57899(12) 0.0630(11) Uani d . 1 1
C C34 0.5714(2) -0.0190(6) 0.58660(14) 0.0733(14) Uani d . 1 1
H H34 0.5596 -0.0905 0.5695 0.088 Uiso calc R 1 1
C C35 0.5681(2) -0.0430(6) 0.61983(15) 0.0792(14) Uani d . 1 1
H H35 0.5540 -0.1301 0.6248 0.095 Uiso calc R 1 1
C C36 0.5853(2) 0.0607(6) 0.64484(13) 0.0730(13) Uani d . 1 1
C C37 0.6055(3) 0.1877(8) 0.63714(16) 0.108(2) Uani d . 1 1
H H37 0.6173 0.2590 0.6543 0.130 Uiso calc R 1 1
C C38 0.6088(3) 0.2130(7) 0.60375(16) 0.103(2) Uani d . 1 1
H H38 0.6225 0.3006 0.5987 0.123 Uiso calc R 1 1
C C39 0.5798(3) 0.0383(8) 0.68039(15) 0.0851(16) Uani d . 1 1
Cd Cd1 0.559298(17) 0.02398(6) 0.741018(9) 0.0866(2) Uani d . 1 1
N N1 0.60290(16) 0.4276(4) 0.41861(9) 0.0632(9) Uani d . 1 1
N N2 0.59425(14) 0.1350(5) 0.54462(10) 0.0691(10) Uani d . 1 1
O O1 0.56019(18) -0.0740(5) 0.68698(10) 0.0923(11) Uani d . 1 1
O O2 0.5947(2) 0.1424(7) 0.70227(12) 0.1301(19) Uani d . 1 1
O O3 0.5889(2) 0.8127(7) 0.28346(12) 0.142(2) Uani d . 1 1
O O4 0.5179(3) 0.8665(8) 0.29007(13) 0.154(3) Uani d . 1 1
O O5 0.5000 -0.1318(9) 0.7500 0.208(6) Uani d S 1 2
H H5A 0.4849 -0.1937 0.7298 0.250 Uiso calc PR 0.50 1
H H5B 0.5151 -0.1937 0.7702 0.250 Uiso calc PR 0.50 1
O O6 0.6240(4) -0.1355(13) 0.76825(19) 0.303(7) Uani d . 1 1
H H6A 0.6368 -0.1803 0.7512 0.454 Uiso d R 1 1
H H6B 0.6512 -0.0817 0.7847 0.454 Uiso d R 1 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.156(6) 0.118(5) 0.029(2) 0.017(5) 0.010(3) 0.011(3)
C2 0.101(4) 0.077(3) 0.055(3) 0.015(3) 0.019(3) 0.010(2)
C3 0.089(3) 0.076(3) 0.057(3) 0.020(3) 0.016(2) -0.002(2)
C4 0.083(3) 0.069(3) 0.057(3) 0.005(3) 0.022(2) 0.007(2)
C5 0.080(3) 0.061(2) 0.048(2) 0.003(2) 0.022(2) 0.0097(19)
C6 0.089(4) 0.106(4) 0.074(4) 0.020(3) 0.031(3) 0.035(3)
C7 0.084(3) 0.127(5) 0.061(3) 0.009(3) 0.031(3) 0.028(3)
C8 0.049(2) 0.051(2) 0.052(2) 0.0016(16) 0.0190(17) -0.0002(17)
C9 0.063(2) 0.051(2) 0.067(3) 0.0035(19) 0.028(2) 0.007(2)
C10 0.058(2) 0.052(2) 0.074(3) -0.0039(19) 0.024(2) -0.003(2)
C11 0.051(2) 0.056(2) 0.070(3) -0.0012(19) 0.0121(19) -0.016(2)
C12 0.052(2) 0.054(2) 0.053(2) 0.0049(17) 0.0183(18) -0.0005(17)
C13 0.0413(17) 0.0458(19) 0.048(2) 0.0083(15) 0.0182(15) 0.0018(16)
C14 0.0426(18) 0.049(2) 0.0471(19) 0.0039(16) 0.0162(15) 0.0051(16)
C15 0.0447(18) 0.051(2) 0.051(2) 0.0044(17) 0.0167(16) -0.0011(17)
C16 0.061(2) 0.057(2) 0.049(2) 0.0056(19) 0.0172(18) -0.0061(18)
C17 0.090(3) 0.075(3) 0.050(2) 0.006(3) 0.018(2) -0.006(2)
C18 0.084(3) 0.073(3) 0.063(3) 0.002(3) 0.015(2) -0.020(3)
C19 0.090(3) 0.058(3) 0.064(3) -0.004(2) 0.019(3) -0.017(2)
C20 0.065(2) 0.051(2) 0.069(3) -0.002(2) 0.023(2) -0.005(2)
C21 0.0434(18) 0.0446(19) 0.053(2) 0.0035(16) 0.0192(15) 0.0040(16)
C22 0.048(2) 0.052(2) 0.065(2) 0.0042(18) 0.0235(18) 0.0027(19)
C23 0.045(2) 0.065(3) 0.082(3) 0.011(2) 0.026(2) 0.001(2)
C24 0.059(2) 0.060(3) 0.074(3) 0.007(2) 0.018(2) 0.003(2)
C25 0.070(3) 0.080(3) 0.055(3) 0.006(2) 0.023(2) 0.016(2)
C26 0.051(2) 0.064(2) 0.052(2) 0.0036(19) 0.0216(17) 0.0052(19)
C27 0.050(2) 0.066(3) 0.068(3) 0.003(2) 0.0304(19) 0.001(2)
C28 0.066(3) 0.080(3) 0.086(3) 0.015(2) 0.044(3) 0.014(3)
C29 0.042(2) 0.089(3) 0.107(4) 0.008(2) 0.037(2) -0.002(3)
C30 0.050(2) 0.077(3) 0.087(3) 0.014(2) 0.023(2) 0.002(3)
C31 0.051(2) 0.063(2) 0.067(3) 0.012(2) 0.0212(19) 0.004(2)
C32 0.0418(18) 0.050(2) 0.061(2) 0.0042(16) 0.0221(17) -0.0007(18)
C33 0.061(2) 0.082(3) 0.055(2) 0.000(2) 0.029(2) -0.002(2)
C34 0.091(4) 0.086(3) 0.051(3) -0.008(3) 0.034(3) -0.002(2)
C35 0.095(4) 0.085(3) 0.072(3) -0.009(3) 0.047(3) 0.000(3)
C36 0.083(3) 0.091(3) 0.050(3) -0.010(3) 0.030(2) -0.012(2)
C37 0.152(6) 0.114(5) 0.074(4) -0.039(5) 0.059(4) -0.030(4)
C38 0.140(6) 0.093(4) 0.095(4) -0.030(4) 0.066(4) -0.012(4)
C39 0.095(4) 0.111(5) 0.055(3) -0.001(3) 0.032(3) -0.010(3)
Cd1 0.1117(4) 0.1101(4) 0.0434(3) 0.0093(2) 0.0321(2) -0.00852(17)
N1 0.090(3) 0.0519(19) 0.0467(19) 0.0004(19) 0.0209(18) 0.0005(16)
N2 0.063(2) 0.094(3) 0.061(2) 0.018(2) 0.0351(18) 0.017(2)
O1 0.122(3) 0.110(3) 0.057(2) -0.004(3) 0.045(2) -0.001(2)
O2 0.175(5) 0.158(5) 0.077(3) -0.048(4) 0.068(3) -0.040(3)
O3 0.175(5) 0.179(5) 0.068(3) 0.011(4) 0.033(3) 0.067(3)
O4 0.190(6) 0.185(6) 0.071(3) 0.079(5) 0.020(3) 0.048(4)
O5 0.330(14) 0.099(5) 0.302(14) 0.000 0.250(13) 0.000
O6 0.367(13) 0.334(13) 0.121(6) 0.229(12) -0.044(7) -0.045(7)
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'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 C1 C2 . . 122.1(7) ?
O3 C1 O4 . . 120.1(6) ?
O4 C1 C2 . . 117.8(7) ?
C3 C2 C1 . . 121.7(6) ?
C3 C2 C7 . . 119.8(5) ?
C7 C2 C1 . . 118.4(6) ?
C2 C3 H3 . . 120.1 ?
C2 C3 C4 . . 119.7(5) ?
C4 C3 H3 . . 120.1 ?
C3 C4 H4 . . 119.6 ?
C5 C4 C3 . . 120.7(5) ?
C5 C4 H4 . . 119.6 ?
C4 C5 N1 . . 119.4(4) ?
C6 C5 C4 . . 120.1(4) ?
C6 C5 N1 . . 120.5(4) ?
C5 C6 H6 . . 119.8 ?
C5 C6 C7 . . 120.4(5) ?
C7 C6 H6 . . 119.8 ?
C2 C7 C6 . . 119.2(5) ?
C2 C7 H7 . . 120.4 ?
C6 C7 H7 . . 120.4 ?
C13 C8 C9 . . 118.9(4) ?
N1 C8 C9 . . 120.3(4) ?
N1 C8 C13 . . 120.8(4) ?
C8 C9 H9 . . 119.6 ?
C10 C9 C8 . . 120.8(4) ?
C10 C9 H9 . . 119.6 ?
C9 C10 H10 . . 119.6 ?
C9 C10 C11 . . 120.8(4) ?
C11 C10 H10 . . 119.6 ?
C10 C11 H11 . . 120.7 ?
C10 C11 C12 . . 118.7(4) ?
C12 C11 H11 . . 120.7 ?
C11 C12 H12 . . 118.7 ?
C11 C12 C13 . . 122.7(4) ?
C13 C12 H12 . . 118.7 ?
C8 C13 C14 . . 122.0(3) ?
C12 C13 C8 . . 118.1(4) ?
C12 C13 C14 . . 119.8(3) ?
C15 C14 C13 . . 110.9(3) ?
C15 C14 C32 . . 107.8(3) ?
C21 C14 C13 . . 108.3(3) ?
C21 C14 C15 . . 110.1(3) ?
C21 C14 C32 . . 111.3(3) ?
C32 C14 C13 . . 108.5(3) ?
C16 C15 C14 . . 121.8(3) ?
C20 C15 C14 . . 118.7(4) ?
C20 C15 C16 . . 119.4(4) ?
C15 C16 C17 . . 119.0(4) ?
C15 C16 N1 . . 121.1(4) ?
C17 C16 N1 . . 119.9(4) ?
C16 C17 H17 . . 119.6 ?
C18 C17 C16 . . 120.7(5) ?
C18 C17 H17 . . 119.6 ?
C17 C18 H18 . . 120.1 ?
C17 C18 C19 . . 119.8(5) ?
C19 C18 H18 . . 120.1 ?
C18 C19 H19 . . 120.3 ?
C20 C19 C18 . . 119.4(4) ?
C20 C19 H19 . . 120.3 ?
C15 C20 H20 . . 119.1 ?
C19 C20 C15 . . 121.7(5) ?
C19 C20 H20 . . 119.1 ?
C22 C21 C14 . . 118.9(3) ?
C22 C21 C26 . . 118.5(4) ?
C26 C21 C14 . . 122.6(3) ?
C21 C22 H22 . . 119.1 ?
C23 C22 C21 . . 121.8(4) ?
C23 C22 H22 . . 119.1 ?
C22 C23 H23 . . 120.5 ?
C24 C23 C22 . . 118.9(4) ?
C24 C23 H23 . . 120.5 ?
C23 C24 H24 . . 119.2 ?
C23 C24 C25 . . 121.6(4) ?
C25 C24 H24 . . 119.2 ?
C24 C25 H25 . . 120.1 ?
C24 C25 C26 . . 119.7(4) ?
C26 C25 H25 . . 120.1 ?
C21 C26 C25 . . 119.3(4) ?
C21 C26 N2 . . 120.9(4) ?
N2 C26 C25 . . 119.8(4) ?
C32 C27 C28 . . 119.6(4) ?
C32 C27 N2 . . 120.9(3) ?
N2 C27 C28 . . 119.5(4) ?
C27 C28 H28 . . 120.1 ?
C29 C28 C27 . . 119.8(4) ?
C29 C28 H28 . . 120.1 ?
C28 C29 H29 . . 119.4 ?
C28 C29 C30 . . 121.3(4) ?
C30 C29 H29 . . 119.4 ?
C29 C30 H30 . . 120.5 ?
C29 C30 C31 . . 118.9(4) ?
C31 C30 H30 . . 120.5 ?
C30 C31 H31 . . 118.9 ?
C32 C31 C30 . . 122.1(4) ?
C32 C31 H31 . . 118.9 ?
C27 C32 C14 . . 122.6(3) ?
C31 C32 C14 . . 119.2(4) ?
C31 C32 C27 . . 118.2(3) ?
C34 C33 C38 . . 120.0(5) ?
C34 C33 N2 . . 121.1(5) ?
C38 C33 N2 . . 118.8(5) ?
C33 C34 H34 . . 119.6 ?
C33 C34 C35 . . 120.7(5) ?
C35 C34 H34 . . 119.6 ?
C34 C35 H35 . . 120.1 ?
C36 C35 C34 . . 119.8(5) ?
C36 C35 H35 . . 120.1 ?
C35 C36 C37 . . 119.4(5) ?
C35 C36 C39 . . 120.1(5) ?
C37 C36 C39 . . 120.4(5) ?
C36 C37 H37 . . 119.4 ?
C36 C37 C38 . . 121.2(6) ?
C38 C37 H37 . . 119.4 ?
C33 C38 C37 . . 118.9(6) ?
C33 C38 H38 . . 120.6 ?
C37 C38 H38 . . 120.6 ?
C36 C39 Cd1 . . 172.2(5) ?
O1 C39 C36 . . 120.4(5) ?
O1 C39 Cd1 . . 61.7(3) ?
O1 C39 O2 . . 122.4(5) ?
O2 C39 C36 . . 117.1(6) ?
O2 C39 Cd1 . . 61.0(3) ?
O1 Cd1 C39 . . 27.01(16) ?
O2 Cd1 C39 . . 28.21(17) ?
O2 Cd1 O1 . . 55.14(16) y
O3 Cd1 C39 6_566 . 122.9(2) ?
O3 Cd1 O1 6_566 . 149.0(2) ?
O3 Cd1 O2 6_566 . 94.8(2) y
O3 Cd1 O4 6_566 5_666 100.3(2) ?
O3 Cd1 O5 6_566 . 113.4(2) y
O3 Cd1 O6 6_566 . 90.8(3) y
O4 Cd1 C39 5_666 . 84.5(2) ?
O4 Cd1 O1 5_666 . 86.37(19) ?
O4 Cd1 O2 5_666 . 86.7(2) ?
O5 Cd1 C39 . . 123.00(17) ?
O5 Cd1 O1 . . 97.59(15) y
O5 Cd1 O2 . . 149.42(13) ?
O5 Cd1 O4 . 5_666 77.1(2) ?
O5 Cd1 O6 . . 90.8(4) y
O6 Cd1 C39 . . 96.6(3) ?
O6 Cd1 O1 . . 88.4(2) y
O6 Cd1 O2 . . 100.9(4) y
O6 Cd1 O4 . 5_666 166.0(4) y
C8 N1 C5 . . 119.9(4) ?
C8 N1 C16 . . 121.0(4) ?
C16 N1 C5 . . 119.1(4) ?
C26 N2 C27 . . 121.2(3) ?
C26 N2 C33 . . 119.8(4) ?
C27 N2 C33 . . 118.3(3) ?
C39 O1 Cd1 . . 91.3(3) ?
C39 O2 Cd1 . . 90.8(4) ?
C1 O3 Cd1 . 6_565 109.9(5) ?
C1 O4 Cd1 . 5_666 164.3(5) ?
Cd1 O5 Cd1 2_656 . 102.9(3) ?
Cd1 O5 H5A . . 111.2 ?
Cd1 O5 H5A 2_656 . 111.2 ?
Cd1 O5 H5B . . 111.2 ?
Cd1 O5 H5B 2_656 . 111.2 ?
H5A O5 H5B . . 109.1 ?
Cd1 O6 H6A . . 109.1 ?
Cd1 O6 H6B . . 108.9 ?
H6A O6 H6B . . 109.4 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 . 1.491(7) ?
C1 O3 . 1.198(9) ?
C1 O4 . 1.233(9) ?
C2 C3 . 1.385(7) ?
C2 C7 . 1.394(8) ?
C3 H3 . 0.9300 ?
C3 C4 . 1.388(7) ?
C4 H4 . 0.9300 ?
C4 C5 . 1.371(7) ?
C5 C6 . 1.369(8) ?
C5 N1 . 1.434(6) ?
C6 H6 . 0.9300 ?
C6 C7 . 1.400(7) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.411(6) ?
C8 C13 . 1.401(6) ?
C8 N1 . 1.384(6) ?
C9 H9 . 0.9300 ?
C9 C10 . 1.372(6) ?
C10 H10 . 0.9300 ?
C10 C11 . 1.376(6) ?
C11 H11 . 0.9300 ?
C11 C12 . 1.380(6) ?
C12 H12 . 0.9300 ?
C12 C13 . 1.392(6) ?
C13 C14 . 1.536(5) ?
C14 C15 . 1.524(5) ?
C14 C21 . 1.519(5) ?
C14 C32 . 1.531(5) ?
C15 C16 . 1.392(6) ?
C15 C20 . 1.387(6) ?
C16 C17 . 1.406(6) ?
C16 N1 . 1.411(6) ?
C17 H17 . 0.9300 ?
C17 C18 . 1.386(7) ?
C18 H18 . 0.9300 ?
C18 C19 . 1.392(8) ?
C19 H19 . 0.9300 ?
C19 C20 . 1.377(7) ?
C20 H20 . 0.9300 ?
C21 C22 . 1.395(5) ?
C21 C26 . 1.396(5) ?
C22 H22 . 0.9300 ?
C22 C23 . 1.389(6) ?
C23 H23 . 0.9300 ?
C23 C24 . 1.360(7) ?
C24 H24 . 0.9300 ?
C24 C25 . 1.379(7) ?
C25 H25 . 0.9300 ?
C25 C26 . 1.416(6) ?
C26 N2 . 1.397(5) ?
C27 C28 . 1.416(5) ?
C27 C32 . 1.388(6) ?
C27 N2 . 1.401(6) ?
C28 H28 . 0.9300 ?
C28 C29 . 1.359(7) ?
C29 H29 . 0.9300 ?
C29 C30 . 1.360(7) ?
C30 H30 . 0.9300 ?
C30 C31 . 1.385(6) ?
C31 H31 . 0.9300 ?
C31 C32 . 1.377(5) ?
C33 C34 . 1.356(7) ?
C33 C38 . 1.357(7) ?
C33 N2 . 1.436(5) ?
C34 H34 . 0.9300 ?
C34 C35 . 1.394(7) ?
C35 H35 . 0.9300 ?
C35 C36 . 1.353(7) ?
C36 C37 . 1.358(8) ?
C36 C39 . 1.508(7) ?
C37 H37 . 0.9300 ?
C37 C38 . 1.403(8) ?
C38 H38 . 0.9300 ?
C39 Cd1 . 2.689(6) ?
C39 O1 . 1.222(7) ?
C39 O2 . 1.271(7) ?
Cd1 O1 . 2.369(4) y
Cd1 O2 . 2.352(5) y
Cd1 O3 6_566 2.219(4) y
Cd1 O4 5_666 2.316(6) y
Cd1 O5 . 2.272(5) y
Cd1 O6 . 2.284(7) y
O3 Cd1 6_565 2.219(4) ?
O4 Cd1 5_666 2.316(6) ?
O5 Cd1 2_656 2.272(5) ?
O5 H5A . 0.9700 ?
O5 H5B . 0.9700 ?
O6 H6A . 0.9600 ?
O6 H6B . 0.9600 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C23 H23 Cg1 2_656 0.93 2.66 3.5712(4) 168
C29 H29 Cg1 3_666 0.93 2.69 3.5457(4) 154
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
C1 C2 C3 C4 . . -177.1(5)
C1 C2 C7 C6 . . 178.2(6)
C2 C1 O3 Cd1 . 6_565 -178.7(5)
C2 C1 O4 Cd1 . 5_666 -132(2)
C2 C3 C4 C5 . . 0.8(8)
C3 C2 C7 C6 . . 3.0(9)
C3 C4 C5 C6 . . -0.4(8)
C3 C4 C5 N1 . . 177.6(4)
C4 C5 C6 C7 . . 1.3(9)
C4 C5 N1 C8 . . -87.5(6)
C4 C5 N1 C16 . . 91.7(6)
C5 C6 C7 C2 . . -2.6(10)
C6 C5 N1 C8 . . 90.5(6)
C6 C5 N1 C16 . . -90.3(6)
C7 C2 C3 C4 . . -2.1(8)
C8 C9 C10 C11 . . 0.4(6)
C8 C13 C14 C15 . . 14.7(5)
C8 C13 C14 C21 . . 135.6(3)
C8 C13 C14 C32 . . -103.5(4)
C9 C8 C13 C12 . . 0.7(5)
C9 C8 C13 C14 . . 176.7(3)
C9 C8 N1 C5 . . -10.4(6)
C9 C8 N1 C16 . . 170.4(4)
C9 C10 C11 C12 . . -0.9(6)
C10 C11 C12 C13 . . 1.3(6)
C11 C12 C13 C8 . . -1.2(6)
C11 C12 C13 C14 . . -177.3(3)
C12 C13 C14 C15 . . -169.3(3)
C12 C13 C14 C21 . . -48.5(4)
C12 C13 C14 C32 . . 72.4(4)
C13 C8 C9 C10 . . -0.3(6)
C13 C8 N1 C5 . . 170.0(4)
C13 C8 N1 C16 . . -9.2(6)
C13 C14 C15 C16 . . -14.6(5)
C13 C14 C15 C20 . . 168.7(3)
C13 C14 C21 C22 . . -65.9(4)
C13 C14 C21 C26 . . 113.6(4)
C13 C14 C32 C27 . . -113.3(4)
C13 C14 C32 C31 . . 67.0(5)
C14 C15 C16 C17 . . -173.9(4)
C14 C15 C16 N1 . . 3.8(6)
C14 C15 C20 C19 . . 174.7(4)
C14 C21 C22 C23 . . 179.1(4)
C14 C21 C26 C25 . . -179.7(4)
C14 C21 C26 N2 . . 0.5(6)
C15 C14 C21 C22 . . 55.5(5)
C15 C14 C21 C26 . . -125.1(4)
C15 C14 C32 C27 . . 126.6(4)
C15 C14 C32 C31 . . -53.1(5)
C15 C16 C17 C18 . . -2.0(7)
C15 C16 N1 C5 . . -170.0(4)
C15 C16 N1 C8 . . 9.3(6)
C16 C15 C20 C19 . . -2.0(7)
C16 C17 C18 C19 . . 0.3(8)
C17 C16 N1 C5 . . 7.6(7)
C17 C16 N1 C8 . . -173.1(4)
C17 C18 C19 C20 . . 0.5(8)
C18 C19 C20 C15 . . 0.4(8)
C20 C15 C16 C17 . . 2.8(6)
C20 C15 C16 N1 . . -179.6(4)
C21 C14 C15 C16 . . -134.5(4)
C21 C14 C15 C20 . . 48.9(5)
C21 C14 C32 C27 . . 5.7(5)
C21 C14 C32 C31 . . -174.0(4)
C21 C22 C23 C24 . . 1.3(7)
C21 C26 N2 C27 . . 5.3(7)
C21 C26 N2 C33 . . -165.0(4)
C22 C21 C26 C25 . . -0.2(6)
C22 C21 C26 N2 . . 179.9(4)
C22 C23 C24 C25 . . -1.5(7)
C23 C24 C25 C26 . . 0.9(8)
C24 C25 C26 C21 . . 0.0(7)
C24 C25 C26 N2 . . 179.8(5)
C25 C26 N2 C27 . . -174.5(5)
C25 C26 N2 C33 . . 15.1(7)
C26 C21 C22 C23 . . -0.4(6)
C27 C28 C29 C30 . . -2.7(8)
C28 C27 C32 C14 . . 179.2(4)
C28 C27 C32 C31 . . -1.1(7)
C28 C27 N2 C26 . . 174.8(5)
C28 C27 N2 C33 . . -14.6(7)
C28 C29 C30 C31 . . 3.1(8)
C29 C30 C31 C32 . . -2.6(7)
C30 C31 C32 C14 . . -178.7(4)
C30 C31 C32 C27 . . 1.6(7)
C32 C14 C15 C16 . . 104.0(4)
C32 C14 C15 C20 . . -72.7(4)
C32 C14 C21 C22 . . 175.0(3)
C32 C14 C21 C26 . . -5.6(5)
C32 C27 C28 C29 . . 1.6(8)
C32 C27 N2 C26 . . -5.2(7)
C32 C27 N2 C33 . . 165.3(4)
C33 C34 C35 C36 . . 0.0(9)
C34 C33 C38 C37 . . 0.7(10)
C34 C33 N2 C26 . . -98.3(6)
C34 C33 N2 C27 . . 91.1(6)
C34 C35 C36 C37 . . 0.3(9)
C34 C35 C36 C39 . . 177.5(6)
C35 C36 C37 C38 . . 0.0(11)
C35 C36 C39 Cd1 . . -103(3)
C35 C36 C39 O1 . . 0.6(9)
C35 C36 C39 O2 . . -177.1(6)
C36 C37 C38 C33 . . -0.5(11)
C36 C39 Cd1 O1 . . 108(4)
C36 C39 Cd1 O2 . . -78(3)
C36 C39 Cd1 O3 . 6_566 -84(3)
C36 C39 Cd1 O4 . 5_666 15(3)
C36 C39 Cd1 O5 . . 86(3)
C36 C39 Cd1 O6 . . -18E1(10)
C36 C39 O1 Cd1 . . -171.4(5)
C36 C39 O2 Cd1 . . 171.4(5)
C37 C36 C39 Cd1 . . 74(4)
C37 C36 C39 O1 . . 177.8(6)
C37 C36 C39 O2 . . 0.1(10)
C38 C33 C34 C35 . . -0.4(9)
C38 C33 N2 C26 . . 83.7(7)
C38 C33 N2 C27 . . -86.9(6)
C39 C36 C37 C38 . . -177.2(6)
C39 Cd1 O5 Cd1 . 2_656 -116.36(19)
N1 C5 C6 C7 . . -176.6(5)
N1 C8 C9 C10 . . -179.9(4)
N1 C8 C13 C12 . . -179.7(4)
N1 C8 C13 C14 . . -3.7(6)
N1 C16 C17 C18 . . -179.6(5)
N2 C27 C28 C29 . . -178.4(5)
N2 C27 C32 C14 . . -0.8(7)
N2 C27 C32 C31 . . 178.9(4)
N2 C33 C34 C35 . . -178.4(5)
N2 C33 C38 C37 . . 178.7(6)
O1 C39 Cd1 O2 . . 174.1(7)
O1 C39 Cd1 O3 . 6_566 168.5(4)
O1 C39 Cd1 O4 . 5_666 -92.8(4)
O1 C39 Cd1 O5 . . -22.0(5)
O1 C39 Cd1 O6 . . 73.2(5)
O1 C39 O2 Cd1 . . -6.2(7)
O1 Cd1 O2 C39 . . 3.3(4)
O1 Cd1 O5 Cd1 . 2_656 -126.24(11)
O2 C39 Cd1 O1 . . -174.1(7)
O2 C39 Cd1 O3 . 6_566 -5.6(5)
O2 C39 Cd1 O4 . 5_666 93.2(5)
O2 C39 Cd1 O5 . . 163.9(4)
O2 C39 Cd1 O6 . . -100.8(6)
O2 C39 O1 Cd1 . . 6.1(7)
O2 Cd1 O1 C39 . . -3.4(4)
O2 Cd1 O5 Cd1 . 2_656 -101.5(4)
O3 C1 C2 C3 . . 180.0(7)
O3 C1 C2 C7 . . 4.8(10)
O3 C1 O4 Cd1 . 5_666 50(3)
O3 Cd1 O1 C39 6_566 . -19.0(6)
O3 Cd1 O2 C39 6_566 . 175.3(4)
O3 Cd1 O5 Cd1 6_566 2_656 54.05(19)
O4 C1 C2 C3 . . 2.3(10)
O4 C1 C2 C7 . . -172.8(7)
O4 C1 O3 Cd1 . 6_565 -1.1(9)
O4 Cd1 O1 C39 5_666 . 85.1(4)
O4 Cd1 O2 C39 5_666 . -84.6(5)
O4 Cd1 O5 Cd1 5_666 2_656 -41.74(16)
O5 Cd1 O1 C39 . . 161.5(4)
O5 Cd1 O2 C39 . . -27.1(7)
O6 Cd1 O1 C39 . . -107.9(5)
O6 Cd1 O2 C39 . . 83.5(5)
O6 Cd1 O5 Cd1 . 2_656 145.28(19)
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_meas
_refln_F_squared_sigma
0 0 -4 34786800 142622
0 0 6 1078652 44517
0 0 8 16326090 188236
0 0 10 1251291 41278
0 0 12 908633 32305
0 0 12 770194 51786
0 0 14 1929979 53550
0 0 14 1694420 85394
0 0 16 2162036 44673
0 0 16 2379251 70987
0 0 16 2250060 69731
0 0 18 1509808 39931
0 0 20 327001 33745
0 0 22 732230 48960
0 0 24 574092 40852
0 0 26 152837 19704
0 0 28 711754 44157
0 0 30 534841 40922
0 0 30 567582 48503
0 0 32 408031 38570
0 0 32 349156 42818
0 0 34 499691 49701
0 0 34 508239 45177
0 0 36 212647 30642
0 0 38 281623 30728
0 0 40 378770 37184
0 0 42 155453 25395
0 0 44 228267 28311
0 0 46 182090 19002
0 -2 0 7631746 158917
0 -2 -1 550951 55431
0 -2 1 526453 60563
0 -2 -2 5837112 112670
0 -2 2 5643388 136046
0 -2 -3 85187 21491
0 -2 3 87985 27137
0 2 4 67684 7993
0 -2 -5 10621103 96279
0 2 5 10677075 85946
0 -2 -6 21130260 241081
0 2 6 19907636 129426
0 -2 -7 1487437 73056
0 2 7 1410472 38928
0 -2 7 1400910 42461
0 -2 8 1086884 43534
0 2 8 1180882 41554
0 -2 -9 217937 7879
0 -2 9 192003 4041
0 -2 9 206174 9249
0 -2 -10 9183207 161942
0 2 10 8365712 89589
0 -2 10 9319369 223159
0 -2 10 8297426 103930
0 -2 11 2370966 60370
0 -2 -11 2469583 95438
0 2 11 2370283 53525
0 -2 -12 1749178 83992
0 -2 12 1896435 123687
0 -2 -13 758159 48895
0 -2 13 648563 29441
0 2 13 713052 26116
0 -2 14 4494664 86972
0 2 14 4325028 78649
0 -2 15 3434731 70454
0 2 15 3608079 64539
0 -2 16 5617970 94978
0 2 16 5409252 88521
0 -2 17 594723 34461
0 2 17 592351 33137
0 -2 18 1308783 45232
0 2 18 1192590 41535
0 -2 19 1357146 52888
0 2 19 1446183 50072
0 2 20 386822 25071
0 -2 20 355600 26596
0 -2 21 436 3697
0 2 21 2142 3285
0 2 22 12716 6554
0 -2 22 7345 6340
0 -2 23 92062 16314
0 2 23 92574 15859
0 2 24 94318 13122
0 -2 24 76065 12489
0 2 25 71784 18141
0 -2 25 97754 17366
0 -2 26 12898 1758
0 2 26 10424 3047
0 2 27 192335 27106
0 -2 27 222260 27323
0 -2 28 36386 7213
0 -2 29 52566 12625
0 -2 29 69306 15237
0 -2 30 54412 19035
0 -2 30 53285 20458
0 -2 31 264704 33411
0 -2 31 273831 29958
0 -2 32 1981 2955
0 -2 32 4112 3905
0 -2 33 164643 21614
0 -2 33 130597 25434
0 -2 34 260424 36777
0 -2 35 7781 7480
0 -2 36 156882 29390
0 -2 37 8947 9371
0 -2 38 217148 30058
0 -2 39 56533 14215
0 -2 40 270169 32916
0 -2 41 21374 7406
0 -2 42 223081 26361
0 -2 43 1129 4573
0 -2 44 142560 21526
0 -2 45 22068 9947
0 -2 46 101864 16098
0 4 0 3465243 62310
0 4 1 423506 20019
0 4 -1 353078 19778
0 4 -2 478228 23893
0 4 2 469604 22403
0 4 3 968724 28362
0 4 -3 1015323 32700
0 4 4 323808 24978
0 4 -4 339100 27542
0 4 5 1203084 38194
0 4 -5 1270767 44356
0 4 -6 3650195 84826
0 4 6 3328319 71882
0 4 7 212373 15846
0 4 -7 276048 20279
0 4 -8 3112890 74837
0 4 8 3032662 64837
0 -4 9 547693 23743
0 4 -9 598230 29634
0 4 9 534274 24605
0 4 -10 778476 36851
0 4 10 710330 30327
0 -4 10 744072 29016
0 -4 11 4780923 88325
0 4 -11 4868439 109135
0 4 11 4855258 89976
0 -4 12 1928285 49266
0 -4 13 1132772 50026
0 -4 14 1051856 39689
0 -4 15 14257 2008
0 -4 16 1236798 51851
0 -4 17 7432 3000
0 -4 18 93920 15926
0 -4 19 135600 19174
0 -4 20 73249 15626
0 -4 21 62681 8802
0 -4 22 123966 20137
0 -4 23 532 5586
0 -4 24 82054 17980
0 -4 25 9592 5126
0 -4 26 433582 37677
0 -4 26 349142 32469
0 -4 27 65 6258
0 -4 27 65 5606
0 -4 28 65036 15079
0 -4 28 61629 18023
0 -4 29 2512 3576
0 -4 29 1457 5380
0 -4 30 50254 18936
0 -4 30 52481 15301
0 -4 31 16537 8378
0 -4 32 11932 7830
0 -4 33 213743 26101
0 -4 34 45618 14549
0 -4 35 38721 11047
0 -4 36 113 5479
0 4 -36 282 4432
0 4 -37 94162 19008
0 -4 37 77749 17160
0 -4 38 9413 5021
0 4 -38 4350 2965
0 4 -39 20103 7632
0 -4 39 15680 6661
0 4 -40 111040 16433
0 -4 40 108259 17847
0 4 -41 50990 11498
0 -4 41 35439 11021
0 -4 41 31394 8367
0 4 -42 11878 4172
0 -4 42 16665 4520
0 -4 43 19876 8400
0 6 0 1085196 48264
0 6 1 392952 25975
0 6 -1 377871 26267
0 6 -2 178235 20229
0 6 2 157601 19209
0 6 3 983581 46700
0 6 -3 1178333 53403
0 6 -4 668917 41556
0 6 4 682042 39221
0 6 -5 558511 39487
0 6 5 496268 34294
0 6 -6 230685 26405
0 6 6 285722 24894
0 6 -7 479564 33264
0 6 7 518239 30083
0 6 8 71507 13161
0 6 -8 69087 14924
0 6 9 289618 22144
0 6 -9 281667 26286
0 6 -10 615024 45035
0 6 10 655254 38853
0 6 -11 759066 51162
0 6 11 783228 43241
0 6 -12 46595 15846
0 6 -13 448635 35821
0 6 -14 123806 24346
0 6 -15 4073 6911
0 6 -16 105837 26779
0 6 -16 108531 21517
0 6 -17 124995 21133
0 6 17 119941 18769
0 6 -17 105175 23239
0 6 -17 95224 19886
0 6 -18 45565 13494
0 6 18 39936 9285
0 6 -18 64354 15442
0 6 -18 71066 14822
0 6 -19 337679 38446
0 6 -19 466748 45219
0 6 19 262609 29850
0 6 -19 508474 43335
0 6 -20 914540 60987
0 6 -20 566525 52478
0 6 -20 779584 62372
0 6 20 353670 38360
0 6 -21 2046 7227
0 6 -21 894 2972
0 6 21 221 3265
0 6 22 1169 1828
0 6 -22 495 2646
0 6 -22 425 3548
0 6 -23 3131 7959
0 6 -23 767 4899
0 6 -24 31323 13562
0 6 -25 216 6380
0 6 -26 62842 21487
0 6 -27 22988 13368
0 6 -28 9927 7413
0 6 -29 31947 14847
0 6 -30 600 2729
0 6 -31 1013 6554
0 6 -32 197 3149
0 6 -33 8100 3776
0 6 -34 342 5077
0 6 -35 833 3251
0 6 -36 479 4302
0 6 -37 5863 2798
0 6 -38 29 2350
0 -6 38 5825 3183
0 -6 39 28793 5665
0 8 0 33039 10531
0 8 0 120029 25428
0 8 -1 110549 21096
0 8 1 3703 8285
0 8 1 101315 20321
0 8 -1 7439 10818
0 8 -2 19207 6198
0 8 2 15204 4656
0 8 -3 291641 43035
0 8 -3 336418 39688
0 8 3 355207 41275
0 8 -4 216493 36471
0 8 -4 194098 43569
0 8 4 245760 34145
0 8 -5 60223 27909
0 8 5 68476 19410
0 8 5 71360 26072
0 8 6 71490 20859
0 8 6 57966 14617
0 8 -6 54373 19879
0 8 -6 41107 15471
0 8 -7 52613 15509
0 8 7 71564 14636
0 8 7 52447 20276
0 8 -8 22622 9582
0 8 8 17818 9451
0 8 8 9160 4423
0 8 9 85225 19793
0 8 -9 103063 21306
0 8 10 43374 13226
0 8 10 13815 14527
0 8 -10 51828 16551
0 8 -11 91197 22129
0 8 11 112716 25083
0 8 11 73716 20057
0 8 12 28995 11862
0 8 -12 30728 11843
0 8 12 11872 7376
0 8 -13 29262 11616
0 8 13 30677 11394
0 8 -14 53138 16655
0 8 14 49848 13361
0 8 -15 166776 28544
0 8 15 135861 24132
0 8 -16 3555 4122
0 8 16 4611 4495
0 8 -17 17920 10099
0 8 17 16925 9827
0 8 -18 180 5202
0 8 18 1883 2311
0 8 19 17339 7869
0 8 -19 17368 9407
0 8 20 114755 20104
0 8 -20 106150 23833
0 8 -21 12732 8939
0 8 21 13892 8005
0 8 -22 4564 4460
0 8 22 594 2399
0 8 -23 5978 3937
0 8 23 3931 3146
0 8 24 22402 8946
0 8 -24 35743 13095
0 8 25 2910 3547
0 8 -25 694 2945
0 8 -26 7957 5965
0 8 -27 3999 5786
0 8 -28 3652 3907
0 8 -29 5473 4556
0 8 -30 689 2705
0 8 -31 463 2471
0 10 0 5683 6249
0 10 1 24713 10690
0 10 -1 27282 10347
0 10 2 45 2585
0 10 3 8619 7973
0 10 4 6482 3892
0 10 5 19272 10058
0 10 6 13969 8236
0 10 7 4510 6687
0 10 8 8292 4828
0 10 9 8464 7893
0 10 10 6946 6070
0 10 11 17839 8439
0 10 12 5226 3925
0 10 13 9766 6275
0 10 14 7572 4688
0 10 15 9490 5733
0 10 16 39 2206
0 10 17 1997 3361
0 10 18 18 1561
0 10 19 8409 4898
-1 -1 47 24385 7961
-1 -1 46 194667 22144
-1 1 45 29 1527
-1 -1 45 3232 3712
-1 -1 44 365976 34796
-1 1 44 335871 31452
-1 -1 43 3126 3223
-1 1 43 588 2814
-1 1 42 518028 43919
-1 -1 42 622891 47272
-1 -1 41 293 5248
-1 1 41 266 3304
-1 1 40 501019 40441
-1 -1 40 491502 45463
-1 1 39 489 3541
-1 -1 39 1581 3509
-1 -1 38 385768 43551
-1 1 38 424765 39432
-1 1 37 110624 20962
-1 -1 37 75230 24296
-1 -1 36 723310 63152
-1 1 36 821450 59063
-1 1 35 2889 4038
-1 -1 35 6032 9246
-1 -1 34 992300 60644
-1 -1 34 1043771 70929
-1 1 34 954479 61771
-1 1 33 377 7112
-1 -1 33 313 3786
-1 -1 33 664 2609
-1 1 33 532 6493
-1 -1 32 339053 32779
-1 1 32 341051 39825
-1 1 32 358164 32948
-1 -1 32 413509 40223
-1 -1 31 407665 38749
-1 -1 31 395303 35042
-1 1 31 375138 31244
-1 1 31 319707 33746
-1 1 30 428313 32459
-1 -1 30 359970 35223
-1 -1 29 5887 2598
-1 1 29 7143 4072
-1 -1 28 5307 5225
-1 1 28 10821 6860
-1 -1 27 36602 7652
-1 1 27 37609 7598
-1 -1 26 319509 31113
-1 1 26 245840 29855
-1 1 25 15219 2607
-1 -1 25 22469 4002
-1 -1 24 80513 14069
-1 1 24 93112 13516
-1 1 23 27580 5371
-1 -1 23 38263 4662
-1 -1 22 103312 17129
-1 1 22 113305 16743
-1 -1 21 1480 5346
-1 1 21 5669 1939
-1 -1 20 92937 8963
-1 1 20 93738 9521
-1 -1 19 49461 10788
-1 1 19 55295 11248
-1 1 18 458505 24199
-1 -1 18 429128 23122
-1 1 17 838699 37897
-1 -1 17 783177 71405
-1 -1 17 733817 36182
-1 1 16 1340495 47448
-1 -1 16 1362315 100468
-1 -1 16 1284796 47895
-1 1 15 372212 28279
-1 -1 15 384805 29176
-1 -1 15 391438 55608
-1 1 14 1602183 43850
-1 -1 14 1748507 88111
-1 -1 14 1645728 45676
-1 1 14 1703792 53190
-1 1 13 552997 50089
-1 -1 13 651302 29817
-1 1 13 620945 27345
-1 -1 13 619769 53439
-1 1 13 623135 32704
-1 1 12 803863 18129
-1 -1 12 784177 19725
-1 -1 12 826155 37433
-1 1 12 746979 33714
-1 1 11 79699 5596
-1 -1 11 77841 5462
-1 1 11 80726 3015
-1 -1 10 1703941 75597
-1 1 10 1848070 37746
-1 1 10 1639617 70456
1 -1 -9 689795 33731
-1 -1 9 564524 34185
-1 1 9 583268 32818
-1 1 8 3061315 45038
-1 1 8 2952141 94045
-1 1 7 848447 43533
1 -1 -7 915748 41251
1 -1 -6 8803722 74761
1 -1 -5 195785 3890
1 -1 -3 2556471 50155
-1 1 2 2812434 77202
1 -1 -2 2701266 71037
-1 1 1 1216307 16369
1 -1 -1 1312738 16016
-1 1 0 32396166 154770
-1 1 -1 16260420 105197
-1 1 -2 61660540 185353
-1 1 -3 3160 21396
-1 1 -4 2950412 54359
-1 -1 -4 3179729 41260
-1 1 -5 1347468 33048
-1 -1 -5 1347387 14828
1 1 6 23471944 215193
-1 1 -6 23569970 269478
1 1 7 685043 11959
-1 -1 -7 727564 13334
-1 -1 -7 670610 6972
-1 1 -7 699757 15440
1 1 8 281363 14640
-1 1 -8 302063 19346
-1 -1 -8 275586 9718
1 1 9 522413 31570
1 1 9 511267 44397
-1 1 -9 707202 61653
1 -1 9 675220 30126
1 1 9 665617 30545
-1 1 -10 2766239 100609
1 1 10 2423776 54139
1 -1 10 2671596 48372
1 1 10 2305782 48935
1 1 10 2281411 77669
1 1 11 22625 7704
1 1 11 15651 7538
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