#------------------------------------------------------------------------------
#$Date: 2024-08-31 05:04:27 +0300 (Sat, 31 Aug 2024) $
#$Revision: 294310 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/32/2023241.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_2023241
loop_
_publ_author_name
'Wackerle, Brandon G.'
'Werner, Eric J.'
'Staples, Richard J.'
'Biros, Shannon M.'
_publ_section_title
;
Crystal structure of a tris(2-aminoethyl)methane capped
carbamoylmethylphosphine oxide compound
;
_journal_coeditor_code VU2007
_journal_issue 9
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 993
_journal_page_last 996
_journal_paper_doi 10.1107/S2056989024008478
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C25 H52 N3 O12 P3'
_chemical_formula_moiety 'C25 H52 N3 O12 P3'
_chemical_formula_sum 'C25 H52 N3 O12 P3'
_chemical_formula_weight 679.60
_chemical_name_systematic
'Diethyl {[(5-[2-(diethoxyphosphoryl)acetamido]-3-{2-[2-(diethoxyphosphoryl)acetamido]ethyl}pentyl)carbamoyl]methyl}phosphonate'
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_atom_sites_solution_secondary difmap
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha 100.4792(11)
_cell_angle_beta 100.1240(10)
_cell_angle_gamma 111.1313(11)
_cell_formula_units_Z 2
_cell_length_a 10.02487(11)
_cell_length_b 11.92992(15)
_cell_length_c 16.6237(2)
_cell_measurement_reflns_used 13811
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 79.8460
_cell_measurement_theta_min 4.1040
_cell_volume 1759.25(4)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.69a (Oxford Diffraction, 2006)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.69a (Oxford Diffraction, 2006)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.69a (Oxford Diffraction, 2006)
;
_computing_molecular_graphics
;
CrystalMaker (Palmer, 2007)
;
_computing_publication_material
;
Olex2 (Dolomanov et al., 2009; Bourhis et al.,
2015)
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.00(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy-S, Dualflex, HyPix-6000HE'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0432
_diffrn_reflns_av_unetI/netI 0.0414
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 27502
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 80.209
_diffrn_reflns_theta_min 2.802
_exptl_absorpt_coefficient_mu 2.056
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.700
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Oxford Diffraction, 2006)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.283
_exptl_crystal_description irregular
_exptl_crystal_F_000 728
_exptl_crystal_size_max 0.163
_exptl_crystal_size_mid 0.087
_exptl_crystal_size_min 0.036
_refine_diff_density_max 0.612
_refine_diff_density_min -0.345
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.072
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 438
_refine_ls_number_reflns 7504
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.072
_refine_ls_R_factor_all 0.0435
_refine_ls_R_factor_gt 0.0371
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+0.5632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0952
_refine_ls_wR_factor_ref 0.0993
_reflns_number_gt 6481
_reflns_number_total 7504
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vu2007.cif
_cod_data_source_block I
_cod_database_code 2023241
_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_min 0.730
_shelx_estimated_absorpt_t_max 0.930
_shelx_hkl_file
;
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-11 5 6 163.430 132.296 15
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-11 5 6 72.9244 112.794 51
-11 5 5 7784.65 559.912 35
-11 5 5 9068.41 586.681 15
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-11 5 5 8717.34 601.774 64
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-11 5 4-104.322 108.409 47
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-11 5 2 55.4306 84.3160 52
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-11 5 1 240.289 131.551 35
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-11 4 10 735.601 109.095 53
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-11 4 9 1630.17 214.771 51
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-11 2 6 2781.62 260.913 14
-11 2 6 2818.77 279.839 35
-11 2 5 5065.47 375.870 53
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-11 2 5 5394.69 406.556 52
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-11 2 2 1229.73 187.170 35
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-11 1 6 1739.95 200.142 53
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-12 2 1 223.211 61.7652 46
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-12 1 9 436.635 61.0150 52
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-12 1 7 1735.83 141.616 52
-12 1 7 1670.50 128.837 46
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-12 1 6 2576.75 190.404 46
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-12 1 2 4161.20 243.413 46
0 0 0 0.00 0.00 0
TITL GVSU1122A in P-1
REM P-1 (#2 in standard setting)
CELL 1.54184 10.024875 11.929917 16.623708 100.4792 100.1240 111.1313
ZERR 6.00 0.000111 0.000152 0.000209 0.0011 0.0010 0.0011
LATT 1
SFAC C H N O
UNIT 72.00 72.00 12.00 18.00
REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0
TEMP -173
SIZE 0.04 0.09 0.16
TREF
HKLF 4
END
;
_shelx_hkl_checksum 37982
_shelx_res_file
;
TITL gvsu1122a_a.res in P-1
gvsu1122a.res
created by SHELXL-2019/2 at 14:07:08 on 28-Jun-2024
REM Old TITL GVSU1122A in P-1 #2
REM SHELXT solution in P-1: R1 0.127, Rweak 0.007, Alpha 0.057
REM 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C25 N4 O11 P3
CELL 1.54184 10.024875 11.929917 16.623708 100.4792 100.124 111.1313
ZERR 2 0.000111 0.000152 0.000209 0.0011 0.001 0.0011
LATT 1
SFAC C H N O P
UNIT 50 104 6 24 6
EQIV $1 1-X,1-Y,-Z
EQIV $2 1-X,2-Y,1-Z
EQIV $3 -1+X,+Y,+Z
EQIV $4 2-X,2-Y,1-Z
L.S. 14
PLAN 11
SIZE 0.036 0.087 0.163
TEMP -173.15(10)
CONF
HTAB N1 O6
HTAB N2 O4
HTAB N3 O5
HTAB C11 O6
HTAB C11 O6_$1
HTAB C12 O2_$2
HTAB C12 O4
HTAB C13 O5
HTAB C14 O1
HTAB C17 O3_$3
HTAB C18 O2
HTAB C22 O1_$1
HTAB C23 O3
HTAB C24 O1_$1
HTAB C24 O8
HTAB C4A O2_$4
BOND
list 4
MORE -1
BOND $H
fmap 2
acta
REM
REM
REM
WGHT 0.044300 0.563200
FVAR 4.65146 0.67600
P1 5 0.358902 0.688475 0.125266 11.00000 0.01846 0.02538 =
0.01788 0.00221 0.00438 0.00752
P2 5 0.532816 0.380997 0.202272 11.00000 0.01955 0.02467 =
0.01902 0.00554 0.00611 0.00989
P3 5 0.472901 0.712662 0.459590 11.00000 0.02313 0.02747 =
0.01929 0.00510 0.00539 0.01144
O1 4 0.629527 0.824899 0.048501 11.00000 0.02751 0.03150 =
0.03132 0.01423 0.01089 0.01265
O2 4 0.695884 0.997795 0.497746 11.00000 0.03377 0.03277 =
0.02036 -0.00055 0.00353 0.01053
O3 4 0.863591 0.486628 0.296514 11.00000 0.02794 0.03822 =
0.03390 0.00229 0.00876 0.01571
O4 4 0.451432 0.758985 0.211643 11.00000 0.02633 0.04110 =
0.01876 0.00128 0.00521 0.00953
O5 4 0.587830 0.668669 0.443371 11.00000 0.03393 0.03443 =
0.03026 0.00945 0.01190 0.02013
O6 4 0.591140 0.463937 0.149554 11.00000 0.02782 0.02871 =
0.02360 0.00975 0.00828 0.01162
O7 4 0.284275 0.764602 0.079672 11.00000 0.02681 0.02218 =
0.02928 -0.00136 0.00011 0.00992
O8 4 0.222475 0.565665 0.117562 11.00000 0.02275 0.02918 =
0.03070 0.00561 0.01276 0.00881
O9 4 0.485620 0.756460 0.557287 11.00000 0.02123 0.04055 =
0.01913 0.00742 0.00507 0.01138
O10 4 0.308024 0.614493 0.423400 11.00000 0.02741 0.03061 =
0.02721 0.00922 0.00214 0.00836
O11 4 0.535762 0.248584 0.174238 11.00000 0.02482 0.02667 =
0.02654 0.00725 0.01064 0.01244
O12 4 0.365114 0.346041 0.201332 11.00000 0.02095 0.03336 =
0.02576 0.00460 0.00687 0.01218
N1 3 0.718519 0.704096 0.112704 11.00000 0.02080 0.03088 =
0.02184 0.00902 0.00668 0.01011
H1 2 0.693211 0.636090 0.127683 11.00000 0.02515
N2 3 0.667175 0.943350 0.356056 11.00000 0.02572 0.02638 =
0.01853 0.00257 0.00359 0.00892
H2 2 0.614046 0.895882 0.312356 11.00000 0.02973
N3 3 0.827630 0.641812 0.378296 11.00000 0.02230 0.02994 =
0.02052 0.00430 0.00558 0.00937
H3 2 0.765947 0.661414 0.396056 11.00000 0.02941
C1 1 0.892824 0.855609 0.296725 11.00000 0.02213 0.03630 =
0.02288 0.00824 0.00637 0.01199
H1A 2 0.790772 0.797266 0.286455 11.00000 0.02520
C5 1 0.872898 0.792472 0.135610 11.00000 0.01933 0.04407 =
0.02475 0.01020 0.00944 0.00982
PART 1
AFIX 23
H5AA 2 0.893030 0.827828 0.087376 21.00000 -1.20000
H5AB 2 0.937439 0.747536 0.145957 21.00000 -1.20000
AFIX 23
PART 2
H5BC 2 0.878553 0.876708 0.134409 -21.00000 -1.20000
H5BD 2 0.924175 0.767149 0.094618 -21.00000 -1.20000
AFIX 0
PART 0
C6 1 0.815213 1.029699 0.359239 11.00000 0.02870 0.02587 =
0.02529 0.00499 0.00536 0.00736
PART 1
AFIX 23
H6AA 2 0.846342 1.105489 0.406285 21.00000 -1.20000
H6AB 2 0.812996 1.055031 0.305686 21.00000 -1.20000
AFIX 23
PART 2
H6BC 2 0.882153 1.049504 0.416062 -21.00000 -1.20000
H6BD 2 0.811939 1.108309 0.349705 -21.00000 -1.20000
AFIX 0
PART 0
C7 1 0.978304 0.735671 0.395267 11.00000 0.02190 0.03269 =
0.02537 0.00631 -0.00016 0.00797
PART 1
AFIX 23
H7AA 2 1.049062 0.696112 0.404807 21.00000 -1.20000
H7AB 2 0.999863 0.800928 0.447785 21.00000 -1.20000
AFIX 23
PART 2
H7BC 2 1.030570 0.707191 0.356172 -21.00000 -1.20000
H7BD 2 1.034145 0.749897 0.454197 -21.00000 -1.20000
AFIX 0
PART 0
C8 1 0.608964 0.729640 0.072367 11.00000 0.02173 0.02943 =
0.01680 0.00585 0.00764 0.01065
C9 1 0.620783 0.933122 0.426022 11.00000 0.02836 0.02459 =
0.02145 0.00399 0.00567 0.01396
C10 1 0.782570 0.526570 0.328782 11.00000 0.02500 0.03069 =
0.01879 0.00680 0.00465 0.01156
C11 1 0.453761 0.630763 0.057929 11.00000 0.02078 0.02618 =
0.01976 0.00500 0.00555 0.00972
AFIX 23
H11A 2 0.459884 0.554470 0.070441 11.00000 -1.20000
H11B 2 0.398214 0.608946 -0.002128 11.00000 -1.20000
AFIX 0
C12 1 0.466076 0.834072 0.411822 11.00000 0.02730 0.02913 =
0.02024 0.00473 0.00659 0.01434
AFIX 23
H12A 2 0.419042 0.798180 0.350200 11.00000 -1.20000
H12B 2 0.404881 0.872627 0.436542 11.00000 -1.20000
AFIX 0
C13 1 0.619434 0.444868 0.313840 11.00000 0.02691 0.02925 =
0.01958 0.00584 0.00834 0.00898
AFIX 23
H13A 2 0.569838 0.494936 0.339364 11.00000 -1.20000
H13B 2 0.609095 0.376363 0.341386 11.00000 -1.20000
AFIX 0
C14 1 0.360171 0.899774 0.099179 11.00000 0.02978 0.02175 =
0.03688 0.00083 0.00914 0.00922
AFIX 23
H14A 2 0.447502 0.922709 0.075691 11.00000 -1.20000
H14B 2 0.394467 0.936564 0.161344 11.00000 -1.20000
AFIX 0
C15 1 0.252612 0.947423 0.060224 11.00000 0.03745 0.03348 =
0.06814 0.01906 0.01842 0.01886
AFIX 137
H15A 2 0.217905 0.909149 -0.001106 11.00000 -1.50000
H15B 2 0.301497 1.038212 0.071238 11.00000 -1.50000
H15C 2 0.167935 0.926141 0.085007 11.00000 -1.50000
AFIX 0
C16 1 0.117435 0.569528 0.167699 11.00000 0.03160 0.04304 =
0.03267 0.00777 0.01898 0.01097
AFIX 23
H16A 2 0.136218 0.657160 0.193669 11.00000 -1.20000
H16B 2 0.129442 0.528868 0.213731 11.00000 -1.20000
AFIX 0
C17 1 -0.035851 0.503048 0.110890 11.00000 0.02731 0.06094 =
0.05094 -0.00797 0.02110 0.00223
AFIX 137
H17A 2 -0.046762 0.543631 0.065403 11.00000 -1.50000
H17B 2 -0.107391 0.505756 0.143687 11.00000 -1.50000
H17C 2 -0.054202 0.416041 0.086221 11.00000 -1.50000
AFIX 0
C18 1 0.629434 0.814829 0.619507 11.00000 0.02126 0.04047 =
0.02113 0.00823 0.00195 0.01071
AFIX 23
H18A 2 0.708701 0.850973 0.591946 11.00000 -1.20000
H18B 2 0.650082 0.752204 0.645208 11.00000 -1.20000
AFIX 0
C19 1 0.624835 0.915487 0.686474 11.00000 0.03443 0.03340 =
0.02775 0.00515 0.00511 0.00851
AFIX 137
H19A 2 0.612075 0.980235 0.661174 11.00000 -1.50000
H19B 2 0.717792 0.952208 0.731421 11.00000 -1.50000
H19C 2 0.541637 0.879707 0.710529 11.00000 -1.50000
AFIX 0
C20 1 0.254753 0.502569 0.451835 11.00000 0.03842 0.04179 =
0.04911 0.02294 -0.00019 0.00785
AFIX 23
H20A 2 0.209606 0.517026 0.498961 11.00000 -1.20000
H20B 2 0.338692 0.481182 0.472970 11.00000 -1.20000
AFIX 0
C21 1 0.144679 0.399537 0.381580 11.00000 0.04621 0.03692 =
0.07287 0.01393 -0.01489 0.00883
AFIX 137
H21A 2 0.191132 0.382672 0.336272 11.00000 -1.50000
H21B 2 0.063215 0.422058 0.359740 11.00000 -1.50000
H21C 2 0.105937 0.324849 0.401657 11.00000 -1.50000
AFIX 0
C22 1 0.642053 0.225771 0.131941 11.00000 0.03012 0.03628 =
0.02919 0.00860 0.01365 0.02013
AFIX 23
H22A 2 0.708598 0.304258 0.122922 11.00000 -1.20000
H22B 2 0.589477 0.164576 0.075948 11.00000 -1.20000
AFIX 0
C23 1 0.730889 0.176098 0.186274 11.00000 0.02765 0.03670 =
0.04683 0.01009 0.00561 0.01755
AFIX 137
H23A 2 0.797129 0.153545 0.156173 11.00000 -1.50000
H23B 2 0.663732 0.102142 0.198646 11.00000 -1.50000
H23C 2 0.789814 0.240173 0.239481 11.00000 -1.50000
AFIX 0
C24 1 0.251788 0.287571 0.121035 11.00000 0.02395 0.03456 =
0.02931 0.00465 0.00174 0.01426
AFIX 23
H24A 2 0.282073 0.234942 0.081284 11.00000 -1.20000
H24B 2 0.237004 0.352005 0.095038 11.00000 -1.20000
AFIX 0
C25 1 0.112046 0.209671 0.138883 11.00000 0.02326 0.09431 =
0.04997 -0.00444 0.00859 -0.00115
AFIX 137
H25A 2 0.032790 0.170273 0.085977 11.00000 -1.50000
H25B 2 0.084140 0.262460 0.179047 11.00000 -1.50000
H25C 2 0.127335 0.145065 0.163357 11.00000 -1.50000
AFIX 0
PART 1
C2 1 0.913795 0.902404 0.216867 21.00000 0.02125 0.03209 =
0.02704 0.01128 0.00733 0.00699
AFIX 23
H2A 2 1.018299 0.961080 0.227461 21.00000 -1.20000
H2B 2 0.850660 0.948454 0.206276 21.00000 -1.20000
AFIX 0
C3 1 0.925942 0.973192 0.371863 21.00000 0.02225 0.03325 =
0.02352 0.00379 0.00192 0.00722
AFIX 23
H3A 2 0.927444 0.947845 0.425396 21.00000 -1.20000
H3B 2 1.025648 1.037297 0.377840 21.00000 -1.20000
AFIX 0
C4 1 1.001803 0.797205 0.321755 21.00000 0.01830 0.03553 =
0.02730 0.00909 0.00560 0.00890
AFIX 23
H4A 2 1.103868 0.862754 0.338242 21.00000 -1.20000
H4B 2 0.993196 0.733465 0.271490 21.00000 -1.20000
AFIX 0
PART 2
C2A 1 0.947665 0.794363 0.225412 -21.00000 0.01901 0.02993 =
0.02736 0.00208 0.00543 0.00785
AFIX 23
H2AA 2 1.056167 0.840578 0.236832 -21.00000 -1.20000
H2AB 2 0.928389 0.707658 0.227536 -21.00000 -1.20000
AFIX 0
C3A 1 0.878947 0.969618 0.287726 -21.00000 0.02548 0.02494 =
0.02532 0.00524 0.00719 0.00729
AFIX 23
H3AA 2 0.812478 0.952468 0.231216 -21.00000 -1.20000
H3AB 2 0.977608 1.031831 0.289758 -21.00000 -1.20000
AFIX 0
C4A 1 0.968200 0.853069 0.382520 -21.00000 0.02624 0.02867 =
0.02401 0.00172 0.00093 0.00672
AFIX 23
H4AA 2 1.070549 0.918112 0.398768 -21.00000 -1.20000
H4AB 2 0.916861 0.878735 0.423347 -21.00000 -1.20000
AFIX 0
HKLF 4
REM gvsu1122a_a.res in P-1
REM wR2 = 0.0993, GooF = S = 1.072, Restrained GooF = 1.072 for all data
REM R1 = 0.0371 for 6481 Fo > 4sig(Fo) and 0.0435 for all 7504 data
REM 438 parameters refined using 0 restraints
END
WGHT 0.0442 0.5629
REM Highest difference peak 0.612, deepest hole -0.345, 1-sigma level 0.051
Q1 1 0.1121 0.4419 0.4331 11.00000 0.05 0.61
Q2 1 0.2908 0.4801 0.4127 11.00000 0.05 0.54
Q3 1 0.5929 0.4215 0.2645 11.00000 0.05 0.38
Q4 1 0.4241 0.7357 0.1768 11.00000 0.05 0.30
Q5 1 0.4693 0.7822 0.4343 11.00000 0.05 0.28
Q6 1 0.6944 0.4842 0.3212 11.00000 0.05 0.27
Q7 1 0.4833 0.7225 0.5284 11.00000 0.05 0.27
Q8 1 0.5408 0.8810 0.4247 11.00000 0.05 0.27
Q9 1 0.4079 0.6554 0.0803 11.00000 0.05 0.27
Q10 1 0.5118 0.6678 0.0665 11.00000 0.05 0.24
Q11 1 0.4334 0.3560 0.2051 11.00000 0.05 0.21
;
_shelx_res_checksum 30977
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P P1 0.35890(4) 0.68848(4) 0.12527(2) 0.02154(10) Uani d 1 . .
P P2 0.53282(4) 0.38100(4) 0.20227(2) 0.02071(9) Uani d 1 . .
P P3 0.47290(4) 0.71266(4) 0.45959(2) 0.02314(10) Uani d 1 . .
O O1 0.62953(12) 0.82490(11) 0.04850(8) 0.0286(2) Uani d 1 . .
O O2 0.69588(13) 0.99779(11) 0.49775(7) 0.0314(3) Uani d 1 . .
O O3 0.86359(13) 0.48663(12) 0.29651(8) 0.0336(3) Uani d 1 . .
O O4 0.45143(13) 0.75898(12) 0.21164(7) 0.0310(3) Uani d 1 . .
O O5 0.58783(13) 0.66867(11) 0.44337(8) 0.0304(3) Uani d 1 . .
O O6 0.59114(12) 0.46394(10) 0.14955(7) 0.0261(2) Uani d 1 . .
O O7 0.28427(12) 0.76460(10) 0.07967(8) 0.0283(2) Uani d 1 . .
O O8 0.22248(12) 0.56567(11) 0.11756(8) 0.0276(2) Uani d 1 . .
O O9 0.48562(12) 0.75646(11) 0.55729(7) 0.0274(2) Uani d 1 . .
O O10 0.30802(13) 0.61449(11) 0.42340(8) 0.0299(3) Uani d 1 . .
O O11 0.53576(12) 0.24858(10) 0.17424(7) 0.0249(2) Uani d 1 . .
O O12 0.36511(12) 0.34604(11) 0.20133(7) 0.0267(2) Uani d 1 . .
N N1 0.71852(14) 0.70410(14) 0.11270(9) 0.0242(3) Uani d 1 . .
H H1 0.693(2) 0.636(2) 0.1277(13) 0.025(5) Uiso d 1 . .
N N2 0.66717(15) 0.94335(13) 0.35606(9) 0.0248(3) Uani d 1 . .
H H2 0.614(2) 0.896(2) 0.3124(15) 0.030(5) Uiso d 1 . .
N N3 0.82763(15) 0.64181(13) 0.37830(9) 0.0250(3) Uani d 1 . .
H H3 0.766(2) 0.661(2) 0.3961(14) 0.029(5) Uiso d 1 . .
C C1 0.89282(17) 0.85561(16) 0.29672(10) 0.0270(3) Uani d 1 . .
H H1A 0.791(2) 0.7973(18) 0.2865(13) 0.025(5) Uiso d 1 . .
C C5 0.87290(17) 0.79247(17) 0.13561(11) 0.0296(3) Uani d 1 . .
H H5AA 0.893030 0.827828 0.087376 0.036 Uiso calc 0.676(3) A 1
H H5AB 0.937439 0.747536 0.145957 0.036 Uiso calc 0.676(3) A 1
H H5BC 0.878553 0.876708 0.134409 0.036 Uiso calc 0.324(3) A 2
H H5BD 0.924175 0.767149 0.094618 0.036 Uiso calc 0.324(3) A 2
C C6 0.81521(18) 1.02970(15) 0.35924(11) 0.0282(3) Uani d 1 . .
H H6AA 0.846342 1.105489 0.406285 0.034 Uiso calc 0.676(3) A 1
H H6AB 0.812996 1.055031 0.305686 0.034 Uiso calc 0.676(3) A 1
H H6BC 0.882153 1.049504 0.416062 0.034 Uiso calc 0.324(3) A 2
H H6BD 0.811939 1.108309 0.349705 0.034 Uiso calc 0.324(3) A 2
C C7 0.97830(17) 0.73567(16) 0.39527(11) 0.0287(3) Uani d 1 . .
H H7AA 1.049062 0.696112 0.404807 0.034 Uiso calc 0.676(3) A 1
H H7AB 0.999863 0.800928 0.447785 0.034 Uiso calc 0.676(3) A 1
H H7BC 1.030570 0.707191 0.356172 0.034 Uiso calc 0.324(3) A 2
H H7BD 1.034145 0.749897 0.454197 0.034 Uiso calc 0.324(3) A 2
C C8 0.60896(16) 0.72964(15) 0.07237(9) 0.0223(3) Uani d 1 . .
C C9 0.62078(18) 0.93312(14) 0.42602(10) 0.0243(3) Uani d 1 . .
C C10 0.78257(17) 0.52657(15) 0.32878(10) 0.0249(3) Uani d 1 . .
C C11 0.45376(16) 0.63076(14) 0.05793(10) 0.0223(3) Uani d 1 . .
H H11A 0.459884 0.554470 0.070441 0.027 Uiso calc 1 . .
H H11B 0.398214 0.608946 -0.002128 0.027 Uiso calc 1 . .
C C12 0.46608(17) 0.83407(15) 0.41182(10) 0.0249(3) Uani d 1 . .
H H12A 0.419042 0.798180 0.350200 0.030 Uiso calc 1 . .
H H12B 0.404881 0.872627 0.436542 0.030 Uiso calc 1 . .
C C13 0.61943(17) 0.44487(15) 0.31384(10) 0.0258(3) Uani d 1 . .
H H13A 0.569838 0.494936 0.339364 0.031 Uiso calc 1 . .
H H13B 0.609095 0.376363 0.341386 0.031 Uiso calc 1 . .
C C14 0.36017(19) 0.89977(15) 0.09918(12) 0.0308(4) Uani d 1 . .
H H14A 0.447502 0.922709 0.075691 0.037 Uiso calc 1 . .
H H14B 0.394467 0.936564 0.161344 0.037 Uiso calc 1 . .
C C15 0.2526(2) 0.94742(19) 0.06022(16) 0.0436(5) Uani d 1 . .
H H15A 0.217905 0.909149 -0.001106 0.065 Uiso calc 1 . .
H H15B 0.301497 1.038212 0.071238 0.065 Uiso calc 1 . .
H H15C 0.167935 0.926141 0.085007 0.065 Uiso calc 1 . .
C C16 0.1174(2) 0.56953(19) 0.16770(12) 0.0359(4) Uani d 1 . .
H H16A 0.136218 0.657160 0.193669 0.043 Uiso calc 1 . .
H H16B 0.129442 0.528868 0.213731 0.043 Uiso calc 1 . .
C C17 -0.0359(2) 0.5030(2) 0.11089(15) 0.0528(6) Uani d 1 . .
H H17A -0.046762 0.543631 0.065403 0.079 Uiso calc 1 . .
H H17B -0.107391 0.505756 0.143687 0.079 Uiso calc 1 . .
H H17C -0.054202 0.416041 0.086221 0.079 Uiso calc 1 . .
C C18 0.62943(17) 0.81483(17) 0.61951(10) 0.0287(3) Uani d 1 . .
H H18A 0.708701 0.850973 0.591946 0.034 Uiso calc 1 . .
H H18B 0.650082 0.752204 0.645208 0.034 Uiso calc 1 . .
C C19 0.6248(2) 0.91549(17) 0.68647(12) 0.0343(4) Uani d 1 . .
H H19A 0.612075 0.980235 0.661174 0.051 Uiso calc 1 . .
H H19B 0.717792 0.952208 0.731421 0.051 Uiso calc 1 . .
H H19C 0.541637 0.879707 0.710529 0.051 Uiso calc 1 . .
C C20 0.2548(2) 0.5026(2) 0.45184(15) 0.0457(5) Uani d 1 . .
H H20A 0.209606 0.517026 0.498961 0.055 Uiso calc 1 . .
H H20B 0.338692 0.481182 0.472970 0.055 Uiso calc 1 . .
C C21 0.1447(3) 0.3995(2) 0.38158(18) 0.0587(7) Uani d 1 . .
H H21A 0.191132 0.382672 0.336272 0.088 Uiso calc 1 . .
H H21B 0.063215 0.422058 0.359740 0.088 Uiso calc 1 . .
H H21C 0.105937 0.324849 0.401657 0.088 Uiso calc 1 . .
C C22 0.64205(19) 0.22577(17) 0.13194(11) 0.0291(3) Uani d 1 . .
H H22A 0.708598 0.304258 0.122922 0.035 Uiso calc 1 . .
H H22B 0.589477 0.164576 0.075948 0.035 Uiso calc 1 . .
C C23 0.7309(2) 0.17610(18) 0.18627(13) 0.0364(4) Uani d 1 . .
H H23A 0.797129 0.153545 0.156173 0.055 Uiso calc 1 . .
H H23B 0.663732 0.102142 0.198646 0.055 Uiso calc 1 . .
H H23C 0.789814 0.240173 0.239481 0.055 Uiso calc 1 . .
C C24 0.25179(18) 0.28757(16) 0.12104(11) 0.0298(3) Uani d 1 . .
H H24A 0.282073 0.234942 0.081284 0.036 Uiso calc 1 . .
H H24B 0.237004 0.352005 0.095038 0.036 Uiso calc 1 . .
C C25 0.1120(2) 0.2097(3) 0.13888(17) 0.0668(8) Uani d 1 . .
H H25A 0.032790 0.170273 0.085977 0.100 Uiso calc 1 . .
H H25B 0.084140 0.262460 0.179047 0.100 Uiso calc 1 . .
H H25C 0.127335 0.145065 0.163357 0.100 Uiso calc 1 . .
C C2 0.9138(3) 0.9024(2) 0.21687(16) 0.0273(5) Uani d 0.676(3) A 1
H H2A 1.018299 0.961080 0.227461 0.033 Uiso calc 0.676(3) A 1
H H2B 0.850660 0.948454 0.206276 0.033 Uiso calc 0.676(3) A 1
C C3 0.9259(3) 0.9732(2) 0.37186(16) 0.0286(6) Uani d 0.676(3) A 1
H H3A 0.927444 0.947845 0.425396 0.034 Uiso calc 0.676(3) A 1
H H3B 1.025648 1.037297 0.377840 0.034 Uiso calc 0.676(3) A 1
C C4 1.0018(2) 0.7972(2) 0.32176(16) 0.0276(6) Uani d 0.676(3) A 1
H H4A 1.103868 0.862754 0.338242 0.033 Uiso calc 0.676(3) A 1
H H4B 0.993196 0.733465 0.271490 0.033 Uiso calc 0.676(3) A 1
C C2A 0.9477(5) 0.7944(5) 0.2254(3) 0.0269(11) Uani d 0.324(3) A 2
H H2AA 1.056167 0.840578 0.236832 0.032 Uiso calc 0.324(3) A 2
H H2AB 0.928389 0.707658 0.227536 0.032 Uiso calc 0.324(3) A 2
C C3A 0.8789(5) 0.9696(5) 0.2877(3) 0.0263(11) Uani d 0.324(3) A 2
H H3AA 0.812478 0.952468 0.231216 0.032 Uiso calc 0.324(3) A 2
H H3AB 0.977608 1.031831 0.289758 0.032 Uiso calc 0.324(3) A 2
C C4A 0.9682(6) 0.8531(5) 0.3825(3) 0.0292(12) Uani d 0.324(3) A 2
H H4AA 1.070549 0.918112 0.398768 0.035 Uiso calc 0.324(3) A 2
H H4AB 0.916861 0.878735 0.423347 0.035 Uiso calc 0.324(3) A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
P1 0.01846(17) 0.02538(19) 0.01788(19) 0.00752(15) 0.00438(14) 0.00221(14)
P2 0.01955(18) 0.02467(19) 0.01902(18) 0.00989(14) 0.00611(13) 0.00554(14)
P3 0.02313(19) 0.02747(19) 0.01929(19) 0.01144(15) 0.00539(14) 0.00510(14)
O1 0.0275(6) 0.0315(6) 0.0313(6) 0.0127(5) 0.0109(5) 0.0142(5)
O2 0.0338(6) 0.0328(6) 0.0204(6) 0.0105(5) 0.0035(5) -0.0005(5)
O3 0.0279(6) 0.0382(7) 0.0339(7) 0.0157(5) 0.0088(5) 0.0023(5)
O4 0.0263(5) 0.0411(7) 0.0188(6) 0.0095(5) 0.0052(4) 0.0013(5)
O5 0.0339(6) 0.0344(6) 0.0303(6) 0.0201(5) 0.0119(5) 0.0095(5)
O6 0.0278(5) 0.0287(6) 0.0236(6) 0.0116(4) 0.0083(4) 0.0098(4)
O7 0.0268(5) 0.0222(5) 0.0293(6) 0.0099(4) 0.0001(4) -0.0014(4)
O8 0.0227(5) 0.0292(6) 0.0307(6) 0.0088(4) 0.0128(5) 0.0056(5)
O9 0.0212(5) 0.0406(6) 0.0191(5) 0.0114(5) 0.0051(4) 0.0074(5)
O10 0.0274(6) 0.0306(6) 0.0272(6) 0.0084(5) 0.0021(5) 0.0092(5)
O11 0.0248(5) 0.0267(5) 0.0265(6) 0.0124(4) 0.0106(4) 0.0072(4)
O12 0.0210(5) 0.0334(6) 0.0258(6) 0.0122(4) 0.0069(4) 0.0046(5)
N1 0.0208(6) 0.0309(7) 0.0218(6) 0.0101(5) 0.0067(5) 0.0090(5)
N2 0.0257(6) 0.0264(7) 0.0185(6) 0.0089(5) 0.0036(5) 0.0026(5)
N3 0.0223(6) 0.0299(7) 0.0205(6) 0.0094(5) 0.0056(5) 0.0043(5)
C1 0.0221(7) 0.0363(9) 0.0229(8) 0.0120(7) 0.0064(6) 0.0082(6)
C5 0.0193(7) 0.0441(9) 0.0247(8) 0.0098(7) 0.0094(6) 0.0102(7)
C6 0.0287(8) 0.0259(8) 0.0253(8) 0.0074(6) 0.0054(6) 0.0050(6)
C7 0.0219(7) 0.0327(8) 0.0254(8) 0.0080(6) -0.0002(6) 0.0063(6)
C8 0.0217(7) 0.0294(7) 0.0168(7) 0.0107(6) 0.0076(5) 0.0058(6)
C9 0.0284(7) 0.0246(7) 0.0214(7) 0.0140(6) 0.0057(6) 0.0040(6)
C10 0.0250(7) 0.0307(8) 0.0188(7) 0.0116(6) 0.0046(6) 0.0068(6)
C11 0.0208(7) 0.0262(7) 0.0198(7) 0.0097(6) 0.0056(5) 0.0050(6)
C12 0.0273(7) 0.0291(8) 0.0202(7) 0.0143(6) 0.0066(6) 0.0047(6)
C13 0.0269(7) 0.0293(8) 0.0196(7) 0.0090(6) 0.0083(6) 0.0058(6)
C14 0.0298(8) 0.0217(7) 0.0369(9) 0.0092(6) 0.0091(7) 0.0008(6)
C15 0.0374(10) 0.0335(9) 0.0681(14) 0.0189(8) 0.0184(9) 0.0191(9)
C16 0.0316(9) 0.0430(10) 0.0327(9) 0.0110(8) 0.0190(7) 0.0078(8)
C17 0.0273(9) 0.0609(13) 0.0509(13) 0.0022(9) 0.0211(9) -0.0080(10)
C18 0.0213(7) 0.0405(9) 0.0211(8) 0.0107(7) 0.0019(6) 0.0082(7)
C19 0.0344(9) 0.0334(9) 0.0278(9) 0.0085(7) 0.0051(7) 0.0051(7)
C20 0.0384(10) 0.0418(11) 0.0491(12) 0.0078(8) -0.0002(9) 0.0229(9)
C21 0.0462(12) 0.0369(11) 0.0729(17) 0.0088(9) -0.0149(11) 0.0139(11)
C22 0.0301(8) 0.0363(9) 0.0292(8) 0.0201(7) 0.0137(7) 0.0086(7)
C23 0.0276(8) 0.0367(9) 0.0468(11) 0.0175(7) 0.0056(7) 0.0101(8)
C24 0.0239(7) 0.0346(8) 0.0293(8) 0.0143(7) 0.0017(6) 0.0047(7)
C25 0.0233(9) 0.094(2) 0.0500(14) -0.0012(11) 0.0086(9) -0.0044(13)
C2 0.0212(11) 0.0321(12) 0.0270(12) 0.0070(9) 0.0073(9) 0.0113(10)
C3 0.0223(11) 0.0332(12) 0.0235(12) 0.0072(9) 0.0019(9) 0.0038(10)
C4 0.0183(10) 0.0355(13) 0.0273(12) 0.0089(9) 0.0056(9) 0.0091(10)
C2A 0.019(2) 0.030(2) 0.027(3) 0.0078(19) 0.0054(18) 0.0021(19)
C3A 0.025(2) 0.025(2) 0.025(2) 0.0073(19) 0.0072(19) 0.0052(19)
C4A 0.026(2) 0.029(2) 0.024(3) 0.007(2) 0.0009(19) 0.0017(19)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 0 -3 0.0756
2 -5 9 0.0319
5 -2 6 0.0375
-1 5 -9 0.0495
4 -5 -6 0.0229
-4 6 5 0.0122
-1 -1 1 0.0724
3 4 -5 0.0829
-4 5 6 0.0095
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
O4 P1 O7 . . 112.90(7) ?
O4 P1 O8 . . 116.05(7) ?
O4 P1 C11 . . 114.00(7) ?
O7 P1 C11 . . 108.90(7) ?
O8 P1 O7 . . 102.52(6) ?
O8 P1 C11 . . 101.26(7) ?
O6 P2 O11 . . 113.64(6) ?
O6 P2 O12 . . 115.95(7) ?
O6 P2 C13 . . 114.70(7) ?
O11 P2 C13 . . 108.50(7) ?
O12 P2 O11 . . 101.94(6) ?
O12 P2 C13 . . 100.62(7) ?
O5 P3 O9 . . 112.76(7) ?
O5 P3 O10 . . 116.32(7) ?
O5 P3 C12 . . 114.34(7) ?
O9 P3 C12 . . 108.77(7) ?
O10 P3 O9 . . 102.72(6) ?
O10 P3 C12 . . 100.66(7) ?
C14 O7 P1 . . 119.89(10) ?
C16 O8 P1 . . 119.61(11) ?
C18 O9 P3 . . 120.98(10) ?
C20 O10 P3 . . 121.18(11) ?
C22 O11 P2 . . 123.56(10) ?
C24 O12 P2 . . 119.46(10) ?
C5 N1 H1 . . 121.2(14) ?
C8 N1 H1 . . 117.1(14) ?
C8 N1 C5 . . 121.51(15) ?
C6 N2 H2 . . 119.9(16) ?
C9 N2 H2 . . 117.7(16) ?
C9 N2 C6 . . 122.08(14) ?
C7 N3 H3 . . 119.5(15) ?
C10 N3 H3 . . 117.9(15) ?
C10 N3 C7 . . 122.40(15) ?
C2 C1 H1A . . 109.5(12) ?
C2 C1 C3 . . 107.39(17) ?
C3 C1 H1A . . 108.6(12) ?
C4 C1 H1A . . 111.6(12) ?
C4 C1 C2 . . 110.97(17) ?
C4 C1 C3 . . 108.61(16) ?
C2A C1 H1A . . 103.4(12) ?
C3A C1 H1A . . 103.2(12) ?
C3A C1 C2A . . 114.5(3) ?
C3A C1 C4A . . 118.3(3) ?
C4A C1 H1A . . 104.2(12) ?
C4A C1 C2A . . 111.1(3) ?
N1 C5 H5AA . . 109.0 ?
N1 C5 H5AB . . 109.0 ?
N1 C5 H5BC . . 110.0 ?
N1 C5 H5BD . . 110.0 ?
N1 C5 C2 . . 113.05(14) ?
N1 C5 C2A . . 108.5(2) ?
H5AA C5 H5AB . . 107.8 ?
H5BC C5 H5BD . . 108.4 ?
C2 C5 H5AA . . 109.0 ?
C2 C5 H5AB . . 109.0 ?
C2A C5 H5BC . . 110.0 ?
C2A C5 H5BD . . 110.0 ?
N2 C6 H6AA . . 109.2 ?
N2 C6 H6AB . . 109.2 ?
N2 C6 H6BC . . 109.5 ?
N2 C6 H6BD . . 109.5 ?
N2 C6 C3 . . 111.97(16) ?
N2 C6 C3A . . 110.5(2) ?
H6AA C6 H6AB . . 107.9 ?
H6BC C6 H6BD . . 108.1 ?
C3 C6 H6AA . . 109.2 ?
C3 C6 H6AB . . 109.2 ?
C3A C6 H6BC . . 109.5 ?
C3A C6 H6BD . . 109.5 ?
N3 C7 H7AA . . 109.1 ?
N3 C7 H7AB . . 109.1 ?
N3 C7 H7BC . . 110.1 ?
N3 C7 H7BD . . 110.1 ?
N3 C7 C4 . . 112.46(15) ?
N3 C7 C4A . . 107.8(2) ?
H7AA C7 H7AB . . 107.8 ?
H7BC C7 H7BD . . 108.5 ?
C4 C7 H7AA . . 109.1 ?
C4 C7 H7AB . . 109.1 ?
C4A C7 H7BC . . 110.1 ?
C4A C7 H7BD . . 110.1 ?
O1 C8 N1 . . 123.86(14) ?
O1 C8 C11 . . 121.44(14) ?
N1 C8 C11 . . 114.70(14) ?
O2 C9 N2 . . 123.68(15) ?
O2 C9 C12 . . 121.02(15) ?
N2 C9 C12 . . 115.30(14) ?
O3 C10 N3 . . 124.25(15) ?
O3 C10 C13 . . 120.97(15) ?
N3 C10 C13 . . 114.78(14) ?
P1 C11 H11A . . 109.7 ?
P1 C11 H11B . . 109.7 ?
C8 C11 P1 . . 109.70(10) ?
C8 C11 H11A . . 109.7 ?
C8 C11 H11B . . 109.7 ?
H11A C11 H11B . . 108.2 ?
P3 C12 H12A . . 109.5 ?
P3 C12 H12B . . 109.5 ?
C9 C12 P3 . . 110.80(11) ?
C9 C12 H12A . . 109.5 ?
C9 C12 H12B . . 109.5 ?
H12A C12 H12B . . 108.1 ?
P2 C13 H13A . . 109.6 ?
P2 C13 H13B . . 109.6 ?
C10 C13 P2 . . 110.07(11) ?
C10 C13 H13A . . 109.6 ?
C10 C13 H13B . . 109.6 ?
H13A C13 H13B . . 108.2 ?
O7 C14 H14A . . 110.2 ?
O7 C14 H14B . . 110.2 ?
O7 C14 C15 . . 107.68(14) ?
H14A C14 H14B . . 108.5 ?
C15 C14 H14A . . 110.2 ?
C15 C14 H14B . . 110.2 ?
C14 C15 H15A . . 109.5 ?
C14 C15 H15B . . 109.5 ?
C14 C15 H15C . . 109.5 ?
H15A C15 H15B . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
O8 C16 H16A . . 110.0 ?
O8 C16 H16B . . 110.0 ?
O8 C16 C17 . . 108.68(15) ?
H16A C16 H16B . . 108.3 ?
C17 C16 H16A . . 110.0 ?
C17 C16 H16B . . 110.0 ?
C16 C17 H17A . . 109.5 ?
C16 C17 H17B . . 109.5 ?
C16 C17 H17C . . 109.5 ?
H17A C17 H17B . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 109.5 ?
O9 C18 H18A . . 110.2 ?
O9 C18 H18B . . 110.2 ?
O9 C18 C19 . . 107.77(14) ?
H18A C18 H18B . . 108.5 ?
C19 C18 H18A . . 110.2 ?
C19 C18 H18B . . 110.2 ?
C18 C19 H19A . . 109.5 ?
C18 C19 H19B . . 109.5 ?
C18 C19 H19C . . 109.5 ?
H19A C19 H19B . . 109.5 ?
H19A C19 H19C . . 109.5 ?
H19B C19 H19C . . 109.5 ?
O10 C20 H20A . . 109.7 ?
O10 C20 H20B . . 109.7 ?
O10 C20 C21 . . 109.73(18) ?
H20A C20 H20B . . 108.2 ?
C21 C20 H20A . . 109.7 ?
C21 C20 H20B . . 109.7 ?
C20 C21 H21A . . 109.5 ?
C20 C21 H21B . . 109.5 ?
C20 C21 H21C . . 109.5 ?
H21A C21 H21B . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
O11 C22 H22A . . 109.9 ?
O11 C22 H22B . . 109.9 ?
O11 C22 C23 . . 108.74(14) ?
H22A C22 H22B . . 108.3 ?
C23 C22 H22A . . 109.9 ?
C23 C22 H22B . . 109.9 ?
C22 C23 H23A . . 109.5 ?
C22 C23 H23B . . 109.5 ?
C22 C23 H23C . . 109.5 ?
H23A C23 H23B . . 109.5 ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?
O12 C24 H24A . . 110.2 ?
O12 C24 H24B . . 110.2 ?
O12 C24 C25 . . 107.54(16) ?
H24A C24 H24B . . 108.5 ?
C25 C24 H24A . . 110.2 ?
C25 C24 H24B . . 110.2 ?
C24 C25 H25A . . 109.5 ?
C24 C25 H25B . . 109.5 ?
C24 C25 H25C . . 109.5 ?
H25A C25 H25B . . 109.5 ?
H25A C25 H25C . . 109.5 ?
H25B C25 H25C . . 109.5 ?
C1 C2 C5 . . 112.41(18) ?
C1 C2 H2A . . 109.1 ?
C1 C2 H2B . . 109.1 ?
C5 C2 H2A . . 109.1 ?
C5 C2 H2B . . 109.1 ?
H2A C2 H2B . . 107.9 ?
C1 C3 H3A . . 108.8 ?
C1 C3 H3B . . 108.8 ?
C6 C3 C1 . . 113.63(17) ?
C6 C3 H3A . . 108.8 ?
C6 C3 H3B . . 108.8 ?
H3A C3 H3B . . 107.7 ?
C1 C4 C7 . . 114.59(17) ?
C1 C4 H4A . . 108.6 ?
C1 C4 H4B . . 108.6 ?
C7 C4 H4A . . 108.6 ?
C7 C4 H4B . . 108.6 ?
H4A C4 H4B . . 107.6 ?
C1 C2A H2AA . . 108.8 ?
C1 C2A H2AB . . 108.8 ?
C5 C2A C1 . . 113.6(3) ?
C5 C2A H2AA . . 108.8 ?
C5 C2A H2AB . . 108.8 ?
H2AA C2A H2AB . . 107.7 ?
C1 C3A C6 . . 114.5(3) ?
C1 C3A H3AA . . 108.6 ?
C1 C3A H3AB . . 108.6 ?
C6 C3A H3AA . . 108.6 ?
C6 C3A H3AB . . 108.6 ?
H3AA C3A H3AB . . 107.6 ?
C1 C4A H4AA . . 107.4 ?
C1 C4A H4AB . . 107.4 ?
C7 C4A C1 . . 119.9(3) ?
C7 C4A H4AA . . 107.4 ?
C7 C4A H4AB . . 107.4 ?
H4AA C4A H4AB . . 106.9 ?
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
P1 O4 . 1.4696(12) ?
P1 O7 . 1.5811(12) ?
P1 O8 . 1.5681(11) ?
P1 C11 . 1.7881(16) ?
P2 O6 . 1.4722(12) ?
P2 O11 . 1.5761(12) ?
P2 O12 . 1.5759(11) ?
P2 C13 . 1.7936(16) ?
P3 O5 . 1.4729(12) ?
P3 O9 . 1.5803(12) ?
P3 O10 . 1.5697(12) ?
P3 C12 . 1.7899(17) ?
O1 C8 . 1.231(2) ?
O2 C9 . 1.231(2) ?
O3 C10 . 1.230(2) ?
O7 C14 . 1.457(2) ?
O8 C16 . 1.4612(19) ?
O9 C18 . 1.4571(18) ?
O10 C20 . 1.448(2) ?
O11 C22 . 1.4515(19) ?
O12 C24 . 1.455(2) ?
N1 H1 . 0.86(2) ?
N1 C5 . 1.457(2) ?
N1 C8 . 1.344(2) ?
N2 H2 . 0.79(2) ?
N2 C6 . 1.455(2) ?
N2 C9 . 1.336(2) ?
N3 H3 . 0.82(2) ?
N3 C7 . 1.460(2) ?
N3 C10 . 1.335(2) ?
C1 H1A . 0.97(2) ?
C1 C2 . 1.550(3) ?
C1 C3 . 1.587(3) ?
C1 C4 . 1.532(3) ?
C1 C2A . 1.564(5) ?
C1 C3A . 1.447(5) ?
C1 C4A . 1.503(5) ?
C5 H5AA . 0.9900 ?
C5 H5AB . 0.9900 ?
C5 H5BC . 0.9900 ?
C5 H5BD . 0.9900 ?
C5 C2 . 1.577(3) ?
C5 C2A . 1.540(5) ?
C6 H6AA . 0.9900 ?
C6 H6AB . 0.9900 ?
C6 H6BC . 0.9900 ?
C6 H6BD . 0.9900 ?
C6 C3 . 1.497(3) ?
C6 C3A . 1.619(5) ?
C7 H7AA . 0.9900 ?
C7 H7AB . 0.9900 ?
C7 H7BC . 0.9900 ?
C7 H7BD . 0.9900 ?
C7 C4 . 1.546(3) ?
C7 C4A . 1.490(6) ?
C8 C11 . 1.521(2) ?
C9 C12 . 1.519(2) ?
C10 C13 . 1.519(2) ?
C11 H11A . 0.9900 ?
C11 H11B . 0.9900 ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C14 H14A . 0.9900 ?
C14 H14B . 0.9900 ?
C14 C15 . 1.495(3) ?
C15 H15A . 0.9800 ?
C15 H15B . 0.9800 ?
C15 H15C . 0.9800 ?
C16 H16A . 0.9900 ?
C16 H16B . 0.9900 ?
C16 C17 . 1.490(3) ?
C17 H17A . 0.9800 ?
C17 H17B . 0.9800 ?
C17 H17C . 0.9800 ?
C18 H18A . 0.9900 ?
C18 H18B . 0.9900 ?
C18 C19 . 1.502(3) ?
C19 H19A . 0.9800 ?
C19 H19B . 0.9800 ?
C19 H19C . 0.9800 ?
C20 H20A . 0.9900 ?
C20 H20B . 0.9900 ?
C20 C21 . 1.463(3) ?
C21 H21A . 0.9800 ?
C21 H21B . 0.9800 ?
C21 H21C . 0.9800 ?
C22 H22A . 0.9900 ?
C22 H22B . 0.9900 ?
C22 C23 . 1.501(2) ?
C23 H23A . 0.9800 ?
C23 H23B . 0.9800 ?
C23 H23C . 0.9800 ?
C24 H24A . 0.9900 ?
C24 H24B . 0.9900 ?
C24 C25 . 1.491(3) ?
C25 H25A . 0.9800 ?
C25 H25B . 0.9800 ?
C25 H25C . 0.9800 ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C2A H2AA . 0.9900 ?
C2A H2AB . 0.9900 ?
C3A H3AA . 0.9900 ?
C3A H3AB . 0.9900 ?
C4A H4AA . 0.9900 ?
C4A H4AB . 0.9900 ?
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
_geom_hbond_publ_flag
N1 H1 O6 . 0.86(2) 2.07(2) 2.9138(18) 168.8(19) yes
N2 H2 O4 . 0.79(2) 2.06(2) 2.8465(18) 170(2) yes
N3 H3 O5 . 0.82(2) 2.10(2) 2.8975(19) 167(2) yes
C11 H11A O6 . 0.99 2.36 3.2433(19) 148.4 yes
C11 H11B O6 2_665 0.99 2.48 3.3235(19) 142.7 yes
C12 H12A O4 . 0.99 2.37 3.2476(19) 147.5 yes
C12 H12B O2 2_676 0.99 2.35 3.321(2) 168.1 yes
C13 H13A O5 . 0.99 2.37 3.259(2) 148.5 yes
C14 H14A O1 . 0.99 2.56 3.326(2) 134.6 yes
C17 H17B O3 1_455 0.98 2.65 3.427(3) 136.6 yes
C18 H18A O2 . 0.99 2.57 3.215(2) 122.4 yes
C22 H22B O1 2_665 0.99 2.80 3.472(2) 126.2 yes
C23 H23C O3 . 0.98 2.69 3.460(2) 135.2 yes
C24 H24A O1 2_665 0.99 2.55 3.480(2) 155.9 yes
C24 H24B O8 . 0.99 2.57 3.444(2) 147.4 yes
C4A H4AA O2 2_776 0.99 2.39 3.241(5) 143.7 yes
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
P1 O7 C14 C15 . . . . -169.31(13) ?
P1 O8 C16 C17 . . . . 131.70(16) ?
P2 O11 C22 C23 . . . . 119.26(14) ?
P2 O12 C24 C25 . . . . 151.86(17) ?
P3 O9 C18 C19 . . . . 142.53(12) ?
P3 O10 C20 C21 . . . . -145.69(17) ?
O1 C8 C11 P1 . . . . -70.88(17) ?
O2 C9 C12 P3 . . . . -65.17(18) ?
O3 C10 C13 P2 . . . . -53.21(19) ?
O4 P1 O7 C14 . . . . 31.54(14) ?
O4 P1 O8 C16 . . . . 52.59(15) ?
O4 P1 C11 C8 . . . . -41.31(13) ?
O5 P3 O9 C18 . . . . 33.23(14) ?
O5 P3 O10 C20 . . . . 62.32(17) ?
O5 P3 C12 C9 . . . . -45.33(13) ?
O6 P2 O11 C22 . . . . 27.99(14) ?
O6 P2 O12 C24 . . . . 56.73(14) ?
O6 P2 C13 C10 . . . . -34.53(14) ?
O7 P1 O8 C16 . . . . -70.93(14) ?
O7 P1 C11 C8 . . . . 85.75(12) ?
O8 P1 O7 C14 . . . . 157.15(12) ?
O8 P1 C11 C8 . . . . -166.67(11) ?
O9 P3 O10 C20 . . . . -61.33(16) ?
O9 P3 C12 C9 . . . . 81.70(12) ?
O10 P3 O9 C18 . . . . 159.22(12) ?
O10 P3 C12 C9 . . . . -170.81(11) ?
O11 P2 O12 C24 . . . . -67.24(13) ?
O11 P2 C13 C10 . . . . 93.74(12) ?
O12 P2 O11 C22 . . . . 153.50(12) ?
O12 P2 C13 C10 . . . . -159.72(12) ?
N1 C5 C2 C1 . . . . 61.5(2) ?
N1 C5 C2A C1 . . . . -69.9(3) ?
N1 C8 C11 P1 . . . . 108.97(13) ?
N2 C6 C3 C1 . . . . 62.7(2) ?
N2 C6 C3A C1 . . . . -60.9(4) ?
N2 C9 C12 P3 . . . . 114.58(14) ?
N3 C7 C4 C1 . . . . 55.4(2) ?
N3 C7 C4A C1 . . . . -62.0(4) ?
N3 C10 C13 P2 . . . . 126.59(13) ?
C5 N1 C8 O1 . . . . 3.3(2) ?
C5 N1 C8 C11 . . . . -176.51(13) ?
C6 N2 C9 O2 . . . . 2.7(3) ?
C6 N2 C9 C12 . . . . -177.08(14) ?
C7 N3 C10 O3 . . . . 3.7(3) ?
C7 N3 C10 C13 . . . . -176.07(14) ?
C8 N1 C5 C2 . . . . 78.0(2) ?
C8 N1 C5 C2A . . . . 138.4(2) ?
C9 N2 C6 C3 . . . . 87.1(2) ?
C9 N2 C6 C3A . . . . 143.7(2) ?
C10 N3 C7 C4 . . . . 79.6(2) ?
C10 N3 C7 C4A . . . . 132.3(3) ?
C11 P1 O7 C14 . . . . -96.14(13) ?
C11 P1 O8 C16 . . . . 176.58(13) ?
C12 P3 O9 C18 . . . . -94.69(13) ?
C12 P3 O10 C20 . . . . -173.55(16) ?
C13 P2 O11 C22 . . . . -100.87(13) ?
C13 P2 O12 C24 . . . . -178.94(12) ?
C2 C1 C3 C6 . . . . 66.6(2) ?
C2 C1 C4 C7 . . . . -174.01(17) ?
C3 C1 C2 C5 . . . . -175.92(16) ?
C3 C1 C4 C7 . . . . 68.2(2) ?
C4 C1 C2 C5 . . . . 65.5(2) ?
C4 C1 C3 C6 . . . . -173.29(18) ?
C2A C1 C3A C6 . . . . 177.4(3) ?
C2A C1 C4A C7 . . . . -47.4(5) ?
C3A C1 C2A C5 . . . . -43.5(4) ?
C3A C1 C4A C7 . . . . 177.1(3) ?
C4A C1 C2A C5 . . . . 179.2(3) ?
C4A C1 C3A C6 . . . . -48.6(5) ?