#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_mer
_database_code_depnum_ccdc_archive 'CCDC 1511902'
# publcif _publ_body_element loop end
loop_
_journal_name_full 'European Journal of Chemistry'
_journal_coden_ASTM EJCUA9
_journal_volume 8
_journal_issue 2
_journal_year 2017
_journal_page_first 137
_journal_page_last 143
_audit_update_record
;
2016-10-27 deposited with the CCDC.
2017-04-04 downloaded from the CCDC.
;
_publcif_datablock.id {f3966e52-0f67-49dc-8ba3-2fcc6d4d2dd2}
# publcif _publ_body_element loop start
loop_
_publ_body_element
_publ_body_title
_publ_body_contents
section
;
Chemical context
;
;
;
section
;
Structural commentary
;
;
;
section
;
Supramolecular features
;
;
;
section
;
Database survey
;
;
;
section
;
Synthesis and crystallization
;
;
In a ....
;
section
;
Refinement
;
;
Crystal data, data collection and structure refinement details are summarized
in Table 1. H atoms of the water molecules were located in the Fourier
difference maps and refined with O-H distance restraints of 0.85(2) \%A.Others
H atoms (=CH and CH~3~groups) were geometrically optimized and refined as
riding model by AFIX instructions with U~iso~(H) =
1.2U~eq~(C)(1.5 for CH~3~ groups).
;
_publ_section_related_literature
;
For related structure: see ...
;
_audit_creation_date 31-10-15
_publ_contact_author_name
;
'Mohamed Gaye'
;
_publ_contact_author_address
;
D\'epartement de Chimie
Facult\'e des Sciences et Techniques
Universit\'e Cheikh Anta Diop
Dakar S\'en\'egal
;
_publ_contact_author_phone 00221338247804
_publ_contact_author_fax 00221338246318
_publ_contact_author_email mlgayeastou@yahoo.fr
_publ_requested_journal 'Acta Cryst. E'
_publ_contact_letter
;
;
_publ_requested_category EO
_publ_section_title
;
Title (type here to add)
;
loop_
_publ_author_name
_publ_author_address
"Ndiaye, Mboss\'e"
;
D\'epartement de Chimie
Facult\'e des Sciences et Techniques
Universit\'e Cheikh Anta Diop
Dakar, S\'en\'egal
;
'Dieng, Moussa'
;
D\'epartement de Chimie
Facult\'e des Sciences et Techniques
Universit\'e Cheikh Anta Diop
Dakar, S\'en\'egal
;
'Thiam, Ibrahima Elhadj'
;
D\'epartement de Chimie
Facult\'e des Sciences et Techniques
Universit\'e Cheikh Anta Diop
Dakar, S\'en\'egal
;
'Barry, Aliou Hamady'
;
D\'epartement de Chimie
Facult\'e des Sciences
Universit\'e de Nouakchott
Nouakchott, Mauritanie
;
'Gaye, Mohamed'
;
D\'epartement de Chimie
Facult\'e des Sciences et Techniques
Universit\'e Cheikh Anta Diop
Dakar, S\'en\'egal
;
'Retailleau, Pascal'
;
Centre de Recherche de Gif,
Institut de Chimie des Substances Naturelles,
CNRS-UPR2301, 1 Avenue la Terrasse,
91198 Gif sur Yvette, France
;
_publ_section_abstract
;
(type here to add)
;
_publ_section_references
;
Bruker AXS BV (1997--2004). COLLECT. Bruker AXS BV, Delft, The
Netherlands.
Farrugia, J. L. (1999). J. Appl. Cryst. 32, 837--838.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, pp.
307--326. New York: Academic Press.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
;
_iucr_refine_instructions_details
;
TITL mer_a.res in P-1
CELL 0.71073 7.913092 11.71884 12.486666 78.8319 73.6743 72.0123
ZERR 2 0.000136 0.000193 0.000181 0.0013 0.0014 0.0015
LATT 1
SFAC C H N O Er
UNIT 30 44 10 20 2
PLAN 20
BOND $H
HTAB
LIST 6
MORE -1
REM CONF
fmap 2
acta 50
OMIT 2 3 1
OMIT -2 -1 2
OMIT 6 7 4
HTAB
EQIV $1 x-1, y, z
EQIV $2 -x+1, -y+1, -z
EQIV $3 x-1, y, z
EQIV $4 -x+2, -y, -z
EQIV $5 -x, -y+1, -z+1
EQIV $6 -x, -y, -z
HTAB O5W O10_$1
HTAB O5W O2_$2
HTAB O6W O7W
HTAB O6W O8
HTAB O7W O10_$3
HTAB O7W O9_$4
HTAB N5 O3_$5
DFIX .90 .02 H5N N5
DFIX .82 .02 O5W H5WA O5W H5WB
DFIX 1.36 .02 H5WA H5WB
DFIX .82 .02 O6W H6WA O6W H6WB
DFIX 1.36 .02 H6WA H6WB
DFIX .82 .02 O7W H7WA O7W H7WB
DFIX 1.36 .02 H7WA H7WB
BIND ER1 ER1_$2
L.S. 4
WGHT 0.0214 1.4516
FVAR 0.49827
ER1 5 0.419485 0.379711 0.259115 11.00000 0.02505 0.02535 =
0.02067 -0.00326 -0.00369 -0.00717
O1 4 0.650064 0.453253 0.284224 11.00000 0.04498 0.05062 =
0.02892 0.00366 -0.01276 -0.02556
O2 4 0.611701 0.489614 0.113418 11.00000 0.03719 0.04519 =
0.02514 -0.00138 -0.00671 -0.02014
O3 4 0.112899 0.361870 0.344577 11.00000 0.03388 0.04311 =
0.05270 -0.00533 0.00149 -0.01008
O4 4 0.309283 0.202124 0.277584 11.00000 0.03902 0.03634 =
0.04240 -0.00513 -0.00610 -0.01408
O5W 4 0.325625 0.390012 0.096494 11.00000 0.05484 0.04462 =
0.02473 0.00062 -0.01405 -0.02834
H5WA 2 0.308443 0.326828 0.092573 11.00000 -1.50000
H5WB 2 0.342984 0.430765 0.035885 11.00000 -1.50000
O6W 4 0.669598 0.229828 0.182146 11.00000 0.03229 0.04096 =
0.04867 -0.01818 0.00093 -0.00639
H6WA 2 0.647645 0.182541 0.151853 11.00000 -1.50000
H6WB 2 0.773396 0.238038 0.155328 11.00000 -1.50000
O7W 4 0.623307 0.043919 0.111687 11.00000 0.06352 0.06573 =
0.09772 -0.04323 -0.01981 0.00061
H7WA 2 0.528364 0.080643 0.094052 11.00000 -1.50000
H7WB 2 0.707511 0.020153 0.059595 11.00000 -1.50000
O8 4 1.016309 0.264493 0.102720 11.00000 0.04913 0.03856 =
0.07192 -0.01719 0.00356 -0.00517
O9 4 1.093325 0.078198 0.075500 11.00000 0.07650 0.03826 =
0.09308 -0.00910 -0.01798 -0.02555
O10 4 1.295924 0.178151 0.030842 11.00000 0.03671 0.06506 =
0.07374 -0.01543 -0.00643 -0.01270
N1 3 0.293113 0.472545 0.439812 11.00000 0.07755 0.03675 =
0.02579 -0.00529 -0.01030 0.01323
N2 3 0.501386 0.248754 0.434811 11.00000 0.03526 0.03184 =
0.02959 0.00100 -0.00897 -0.00957
N3 3 0.234777 0.599683 0.246795 11.00000 0.03630 0.02885 =
0.02839 -0.00306 -0.00808 -0.00516
N4 3 1.134502 0.171800 0.070783 11.00000 0.04202 0.03798 =
0.04194 -0.00620 -0.01132 -0.01096
N5 3 0.172933 0.580297 0.442312 11.00000 0.19367 0.05720 =
0.02605 -0.00964 0.00129 0.04790
H5N 2 0.107065 0.608118 0.509204 11.00000 -1.20000
C1 1 0.446752 0.292989 0.532303 11.00000 0.06884 0.04517 =
0.03061 0.00119 -0.01755 -0.00259
C2 1 0.497298 0.226904 0.629613 11.00000 0.14629 0.06982 =
0.03668 -0.00298 -0.03944 0.01836
AFIX 43
H2 2 0.459855 0.262062 0.696066 11.00000 -1.20000
AFIX 0
C3 1 0.602077 0.110358 0.626053 11.00000 0.08444 0.05420 =
0.05327 0.02077 -0.03542 -0.00951
AFIX 43
H3 2 0.634977 0.064137 0.690204 11.00000 -1.20000
AFIX 0
C4 1 0.656519 0.063945 0.528300 11.00000 0.07761 0.04122 =
0.06351 0.01107 -0.02285 0.00361
AFIX 43
H4 2 0.729611 -0.014920 0.523093 11.00000 -1.20000
AFIX 0
C5 1 0.602535 0.134978 0.434808 11.00000 0.08715 0.03630 =
0.04712 -0.00136 -0.01849 0.00262
AFIX 43
H5 2 0.639571 0.100696 0.367902 11.00000 -1.20000
AFIX 0
C6 1 0.334805 0.413067 0.533594 11.00000 0.15483 0.04047 =
0.01899 -0.00685 -0.01852 0.02012
AFIX 43
H6 2 0.291434 0.449327 0.599634 11.00000 -1.20000
AFIX 0
C7 1 0.143721 0.649101 0.340918 11.00000 0.07896 0.04093 =
0.03391 -0.00400 -0.00826 0.01860
C8 1 0.020779 0.763937 0.340521 11.00000 0.14682 0.05868 =
0.04243 -0.00777 -0.00283 0.04951
AFIX 43
H8 2 -0.047597 0.793814 0.407928 11.00000 -1.20000
AFIX 0
C9 1 0.001547 0.832009 0.240764 11.00000 0.09305 0.04396 =
0.06410 -0.00014 -0.02086 0.02296
AFIX 43
H9 2 -0.077683 0.909405 0.239210 11.00000 -1.20000
AFIX 0
C10 1 0.100297 0.784775 0.143435 11.00000 0.06326 0.03749 =
0.05064 0.00902 -0.02461 -0.01028
AFIX 43
H10 2 0.092386 0.829851 0.074125 11.00000 -1.20000
AFIX 0
C11 1 0.212188 0.668629 0.150100 11.00000 0.05236 0.03547 =
0.03231 0.00114 -0.01417 -0.01447
AFIX 43
H11 2 0.276103 0.635972 0.083302 11.00000 -1.20000
AFIX 0
C12 1 0.695434 0.496977 0.183069 11.00000 0.03136 0.03205 =
0.02969 -0.00084 -0.00724 -0.01133
C13 1 0.848145 0.556495 0.147979 11.00000 0.04323 0.05588 =
0.04623 0.00128 -0.01070 -0.02692
AFIX 137
H13A 2 0.807894 0.632668 0.177640 11.00000 -1.50000
H13B 2 0.883713 0.569483 0.067448 11.00000 -1.50000
H13C 2 0.950709 0.505484 0.176359 11.00000 -1.50000
AFIX 0
C14 1 0.149204 0.252496 0.327677 11.00000 0.03103 0.03816 =
0.02478 0.00243 -0.00874 -0.01365
C15 1 0.017524 0.192872 0.363707 11.00000 0.05740 0.05029 =
0.04542 0.00633 -0.00317 -0.02876
AFIX 137
H15A 2 -0.004310 0.173029 0.443796 11.00000 -1.50000
H15B 2 0.056962 0.120034 0.328605 11.00000 -1.50000
H15C 2 -0.093255 0.243364 0.344214 11.00000 -1.50000
HKLF 4
REM mer_a.res in P-1
REM R1 = 0.0280 for 5100 Fo > 4sig(Fo) and 0.0316 for all 5545 data
REM 303 parameters refined using 10 restraints
END
WGHT 0.0214 1.4516
REM Highest difference peak 0.683, deepest hole -1.004, 1-sigma level 0.119
Q1 1 0.4068 0.4073 0.5179 11.00000 0.05 0.68
Q2 1 0.1235 0.5624 0.4513 11.00000 0.05 0.66
Q3 1 0.2669 0.4069 0.5353 11.00000 0.05 0.62
Q4 1 0.2362 0.5951 0.4345 11.00000 0.05 0.62
Q5 1 0.3297 0.3978 0.3572 11.00000 0.05 0.58
Q6 1 0.5082 0.3127 0.2444 11.00000 0.05 0.58
Q7 1 0.3034 0.4582 0.2315 11.00000 0.05 0.57
Q8 1 0.3577 0.4364 0.5497 11.00000 0.05 0.56
Q9 1 0.0847 0.1654 0.3912 11.00000 0.05 0.54
Q10 1 0.3432 0.4543 0.2739 11.00000 0.05 0.54
Q11 1 0.5007 0.3864 0.1568 11.00000 0.05 0.52
Q12 1 0.5749 0.2538 0.1970 11.00000 0.05 0.51
Q13 1 0.0926 0.6182 0.3693 11.00000 0.05 0.49
Q14 1 0.3675 0.4800 0.4044 11.00000 0.05 0.49
Q15 1 0.3959 0.3413 0.1694 11.00000 0.05 0.49
Q16 1 0.4659 0.4786 0.2315 11.00000 0.05 0.49
Q17 1 0.2493 0.4668 0.4218 11.00000 0.05 0.48
Q18 1 0.5329 0.2510 0.5774 11.00000 0.05 0.47
Q19 1 0.3954 0.3177 0.3096 11.00000 0.05 0.45
Q20 1 0.3725 0.2789 0.2719 11.00000 0.05 0.44
;
_publ_section_figure_captions
;
Fig. 1. An ORTEP view of the title compound, showing the atom-numbering
scheme. Displacement ellipsoids are plotted at the 50% probability level.
Fig. 2. Molecular representation of the compound showing hydrogen bonds.
;
_publ_section_acknowledgements
;
(type here to add acknowledgements)
;
_audit_creation_method SHELXL-97
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C15 H20 Er N4 O6, N O3, H2 O'
_chemical_formula_sum 'C15 H22 Er N5 O10'
_chemical_formula_weight 599.64
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'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 7.91309(14)
_cell_length_b 11.71884(19)
_cell_length_c 12.48666(18)
_cell_angle_alpha 78.8319(13)
_cell_angle_beta 73.6743(14)
_cell_angle_gamma 72.0123(15)
_cell_volume 1049.64(3)
_cell_formula_units_Z 2
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 25
_cell_measurement_theta_min 11
_cell_measurement_theta_max 15
_exptl_crystal_description prismatic
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.08
_exptl_crystal_size_mid 0.07
_exptl_crystal_size_min 0.05
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.897
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 590
_exptl_absorpt_coefficient_mu 4.060
_exptl_absorpt_correction_type none
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_process_details ?
_exptl_special_details ?
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator 'horizonally mounted graphite crystal'
_diffrn_measurement_device_type KappaCCD
_diffrn_measurement_device '95mm CCD camera on \k-goniostat'
_diffrn_measurement_method CCD
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time none
_diffrn_standards_decay_% 0
_diffrn_reflns_number 25647
_diffrn_reflns_av_R_equivalents 0.0523
_diffrn_reflns_av_sigmaI/netI 0.0391
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_theta_min 3.42
_diffrn_reflns_theta_max 30.30
_reflns_number_total 5545
_reflns_number_gt 5100
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick,2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'ORTEP3 for Windows (Farrugia,1997)'
_computing_publication_material 'SHELXL-97 (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+1.4516P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 5545
_refine_ls_number_parameters 303
_refine_ls_number_restraints 10
_refine_ls_R_factor_all 0.0316
_refine_ls_R_factor_gt 0.0280
_refine_ls_wR_factor_ref 0.0616
_refine_ls_wR_factor_gt 0.0604
_refine_ls_goodness_of_fit_ref 1.038
_refine_ls_restrained_S_all 1.037
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.419485(17) 0.379711(11) 0.259115(10) 0.02389(5) Uani 1 1 d . . .
O1 O 0.6501(3) 0.4533(2) 0.2842(2) 0.0389(6) Uani 1 1 d . . .
O2 O 0.6117(3) 0.4896(2) 0.11342(19) 0.0343(5) Uani 1 1 d . . .
O3 O 0.1129(3) 0.3619(2) 0.3446(2) 0.0458(6) Uani 1 1 d . . .
O4 O 0.3093(3) 0.2021(2) 0.2776(2) 0.0390(5) Uani 1 1 d . . .
O5W O 0.3256(4) 0.3900(2) 0.0965(2) 0.0376(6) Uani 1 1 d D . .
H5WA H 0.308(6) 0.327(2) 0.093(4) 0.056 Uiso 1 1 d D . .
H5WB H 0.343(6) 0.431(3) 0.036(2) 0.056 Uiso 1 1 d D . .
O6W O 0.6696(3) 0.2298(2) 0.1821(2) 0.0419(6) Uani 1 1 d D . .
H6WA H 0.648(6) 0.183(4) 0.152(4) 0.063 Uiso 1 1 d D . .
H6WB H 0.773(4) 0.238(4) 0.155(4) 0.063 Uiso 1 1 d D . .
O7W O 0.6233(5) 0.0439(3) 0.1117(4) 0.0749(11) Uani 1 1 d D . .
H7WA H 0.528(5) 0.081(6) 0.094(5) 0.112 Uiso 1 1 d D . .
H7WB H 0.708(6) 0.020(6) 0.060(4) 0.112 Uiso 1 1 d D . .
O8 O 1.0163(4) 0.2645(2) 0.1027(3) 0.0571(8) Uani 1 1 d . . .
O9 O 1.0933(5) 0.0782(3) 0.0755(3) 0.0672(9) Uani 1 1 d . . .
O10 O 1.2959(4) 0.1782(3) 0.0308(3) 0.0591(8) Uani 1 1 d . . .
N1 N 0.2931(5) 0.4725(3) 0.4398(3) 0.0536(10) Uani 1 1 d . . .
N2 N 0.5014(4) 0.2488(2) 0.4348(2) 0.0325(6) Uani 1 1 d . . .
N3 N 0.2348(4) 0.5997(2) 0.2468(2) 0.0320(6) Uani 1 1 d . . .
N4 N 1.1345(4) 0.1718(3) 0.0708(3) 0.0401(7) Uani 1 1 d . . .
N5 N 0.1729(10) 0.5803(4) 0.4423(3) 0.117(3) Uani 1 1 d D . .
H5N H 0.107(10) 0.608(7) 0.509(4) 0.140 Uiso 1 1 d D . .
C1 C 0.4468(6) 0.2930(4) 0.5323(3) 0.0508(10) Uani 1 1 d . . .
C2 C 0.4973(10) 0.2269(5) 0.6296(4) 0.092(2) Uani 1 1 d . . .
H2 H 0.4599 0.2621 0.6961 0.111 Uiso 1 1 calc R . .
C3 C 0.6021(7) 0.1104(4) 0.6261(4) 0.0660(14) Uani 1 1 d . . .
H3 H 0.6350 0.0641 0.6902 0.079 Uiso 1 1 calc R . .
C4 C 0.6565(7) 0.0639(4) 0.5283(5) 0.0666(14) Uani 1 1 d . . .
H4 H 0.7296 -0.0149 0.5231 0.080 Uiso 1 1 calc R . .
C5 C 0.6025(7) 0.1350(4) 0.4348(4) 0.0614(13) Uani 1 1 d . . .
H5 H 0.6396 0.1007 0.3679 0.074 Uiso 1 1 calc R . .
C6 C 0.3348(9) 0.4131(4) 0.5336(3) 0.082(2) Uani 1 1 d . . .
H6 H 0.2914 0.4493 0.5996 0.099 Uiso 1 1 calc R . .
C7 C 0.1437(7) 0.6491(4) 0.3409(4) 0.0606(13) Uani 1 1 d . . .
C8 C 0.0208(10) 0.7639(5) 0.3405(4) 0.105(3) Uani 1 1 d . . .
H8 H -0.0476 0.7938 0.4079 0.126 Uiso 1 1 calc R . .
C9 C 0.0015(8) 0.8320(4) 0.2408(5) 0.0772(17) Uani 1 1 d . . .
H9 H -0.0777 0.9094 0.2392 0.093 Uiso 1 1 calc R . .
C10 C 0.1003(6) 0.7848(4) 0.1434(4) 0.0509(10) Uani 1 1 d . . .
H10 H 0.0924 0.8299 0.0741 0.061 Uiso 1 1 calc R . .
C11 C 0.2122(5) 0.6686(3) 0.1501(3) 0.0393(8) Uani 1 1 d . . .
H11 H 0.2761 0.6360 0.0833 0.047 Uiso 1 1 calc R . .
C12 C 0.6954(4) 0.4970(3) 0.1831(3) 0.0308(7) Uani 1 1 d . . .
C13 C 0.8481(5) 0.5565(4) 0.1480(4) 0.0463(9) Uani 1 1 d . . .
H13A H 0.8079 0.6327 0.1776 0.069 Uiso 1 1 calc R . .
H13B H 0.8837 0.5695 0.0674 0.069 Uiso 1 1 calc R . .
H13C H 0.9507 0.5055 0.1764 0.069 Uiso 1 1 calc R . .
C14 C 0.1492(4) 0.2525(3) 0.3277(3) 0.0307(7) Uani 1 1 d . . .
C15 C 0.0175(6) 0.1929(4) 0.3637(4) 0.0513(10) Uani 1 1 d . . .
H15A H -0.0043 0.1730 0.4438 0.077 Uiso 1 1 calc R . .
H15B H 0.0570 0.1200 0.3286 0.077 Uiso 1 1 calc R . .
H15C H -0.0933 0.2434 0.3442 0.077 Uiso 1 1 calc R . .
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
Er1 0.02505(8) 0.02535(7) 0.02067(7) -0.00326(5) -0.00369(5) -0.00717(5)
O1 0.0450(14) 0.0506(14) 0.0289(12) 0.0037(11) -0.0128(11) -0.0256(12)
O2 0.0372(13) 0.0452(13) 0.0251(11) -0.0014(10) -0.0067(10) -0.0201(10)
O3 0.0339(13) 0.0431(14) 0.0527(17) -0.0053(12) 0.0015(12) -0.0101(11)
O4 0.0390(14) 0.0363(12) 0.0424(14) -0.0051(10) -0.0061(11) -0.0141(10)
O5W 0.0548(15) 0.0446(14) 0.0247(12) 0.0006(10) -0.0140(11) -0.0283(12)
O6W 0.0323(13) 0.0410(14) 0.0487(16) -0.0182(12) 0.0009(11) -0.0064(11)
O7W 0.064(2) 0.066(2) 0.098(3) -0.043(2) -0.020(2) 0.0006(18)
O8 0.0491(17) 0.0386(14) 0.072(2) -0.0172(14) 0.0036(15) -0.0052(12)
O9 0.077(2) 0.0383(15) 0.093(3) -0.0091(16) -0.018(2) -0.0255(15)
O10 0.0367(15) 0.0651(19) 0.074(2) -0.0154(16) -0.0064(15) -0.0127(13)
N1 0.078(2) 0.0367(16) 0.0258(15) -0.0053(12) -0.0103(16) 0.0132(16)
N2 0.0353(15) 0.0318(14) 0.0296(14) 0.0010(11) -0.0090(12) -0.0096(11)
N3 0.0363(15) 0.0289(13) 0.0284(14) -0.0031(11) -0.0081(12) -0.0052(11)
N4 0.0420(17) 0.0380(16) 0.0419(17) -0.0062(13) -0.0113(14) -0.0110(13)
N5 0.194(6) 0.057(3) 0.0261(19) -0.0096(18) 0.001(3) 0.048(3)
C1 0.069(3) 0.045(2) 0.0306(19) 0.0012(16) -0.0175(19) -0.0026(19)
C2 0.146(6) 0.070(3) 0.037(3) -0.003(2) -0.039(3) 0.018(3)
C3 0.084(3) 0.054(3) 0.053(3) 0.021(2) -0.035(3) -0.010(2)
C4 0.078(3) 0.041(2) 0.064(3) 0.011(2) -0.023(3) 0.004(2)
C5 0.087(3) 0.036(2) 0.047(2) -0.0014(18) -0.018(2) 0.003(2)
C6 0.155(6) 0.040(2) 0.0190(18) -0.0069(16) -0.019(3) 0.020(3)
C7 0.079(3) 0.041(2) 0.034(2) -0.0040(16) -0.008(2) 0.019(2)
C8 0.147(6) 0.059(3) 0.042(3) -0.008(2) -0.003(3) 0.050(3)
C9 0.093(4) 0.044(2) 0.064(3) 0.000(2) -0.021(3) 0.023(2)
C10 0.063(3) 0.0375(19) 0.051(2) 0.0090(17) -0.025(2) -0.0103(18)
C11 0.052(2) 0.0355(17) 0.0323(18) 0.0011(14) -0.0142(16) -0.0145(16)
C12 0.0314(16) 0.0321(16) 0.0297(16) -0.0008(13) -0.0072(13) -0.0113(13)
C13 0.043(2) 0.056(2) 0.046(2) 0.0013(18) -0.0107(18) -0.0269(18)
C14 0.0310(17) 0.0382(17) 0.0248(15) 0.0024(13) -0.0087(13) -0.0136(13)
C15 0.057(3) 0.050(2) 0.045(2) 0.0063(18) -0.0032(19) -0.029(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O6W 2.316(2) . ?
Er1 O5W 2.321(2) . ?
Er1 O1 2.360(2) . ?
Er1 O3 2.417(3) . ?
Er1 O4 2.443(2) . ?
Er1 O2 2.455(2) . ?
Er1 N1 2.507(3) . ?
Er1 N3 2.540(3) . ?
Er1 N2 2.543(3) . ?
Er1 C12 2.782(3) . ?
Er1 C14 2.824(3) . ?
Er1 Er1 6.4778(3) 2_665 ?
O1 C12 1.263(4) . ?
O2 C12 1.261(4) . ?
O3 C14 1.270(4) . ?
O4 C14 1.257(4) . ?
O5W H5WA 0.806(18) . ?
O5W H5WB 0.813(18) . ?
O6W H6WA 0.811(18) . ?
O6W H6WB 0.823(18) . ?
O7W H7WA 0.809(19) . ?
O7W H7WB 0.810(19) . ?
O8 N4 1.243(4) . ?
O9 N4 1.224(4) . ?
O10 N4 1.254(4) . ?
N1 C6 1.313(5) . ?
N1 N5 1.325(5) . ?
N2 C1 1.322(5) . ?
N2 C5 1.326(5) . ?
N3 C7 1.329(5) . ?
N3 C11 1.340(4) . ?
N5 C7 1.400(6) . ?
N5 H5N 0.91(2) . ?
C1 C2 1.398(6) . ?
C1 C6 1.413(6) . ?
C2 C3 1.363(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.337(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.387(6) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.396(6) . ?
C8 C9 1.363(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.361(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.377(5) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.498(5) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.357(5) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6W Er1 O5W 84.82(10) . . ?
O6W Er1 O1 82.14(10) . . ?
O5W Er1 O1 129.13(8) . . ?
O6W Er1 O3 126.73(9) . . ?
O5W Er1 O3 81.42(10) . . ?
O1 Er1 O3 142.71(10) . . ?
O6W Er1 O4 73.76(9) . . ?
O5W Er1 O4 73.12(9) . . ?
O1 Er1 O4 145.74(9) . . ?
O3 Er1 O4 52.98(9) . . ?
O6W Er1 O2 75.59(9) . . ?
O5W Er1 O2 75.32(8) . . ?
O1 Er1 O2 53.81(8) . . ?
O3 Er1 O2 146.14(9) . . ?
O4 Er1 O2 137.41(8) . . ?
O6W Er1 N1 137.72(11) . . ?
O5W Er1 N1 137.21(11) . . ?
O1 Er1 N1 73.51(12) . . ?
O3 Er1 N1 69.21(12) . . ?
O4 Er1 N1 109.07(11) . . ?
O2 Er1 N1 113.51(11) . . ?
O6W Er1 N3 148.64(10) . . ?
O5W Er1 N3 81.10(9) . . ?
O1 Er1 N3 85.28(9) . . ?
O3 Er1 N3 78.62(9) . . ?
O4 Er1 N3 127.31(9) . . ?
O2 Er1 N3 73.79(9) . . ?
N1 Er1 N3 63.49(9) . . ?
O6W Er1 N2 78.59(10) . . ?
O5W Er1 N2 146.42(9) . . ?
O1 Er1 N2 77.38(9) . . ?
O3 Er1 N2 85.43(9) . . ?
O4 Er1 N2 74.29(9) . . ?
O2 Er1 N2 126.91(8) . . ?
N1 Er1 N2 62.85(9) . . ?
N3 Er1 N2 126.26(9) . . ?
O6W Er1 C12 77.22(10) . . ?
O5W Er1 C12 102.27(9) . . ?
O1 Er1 C12 26.86(9) . . ?
O3 Er1 C12 156.04(10) . . ?
O4 Er1 C12 150.90(9) . . ?
O2 Er1 C12 26.96(9) . . ?
N1 Er1 C12 93.86(12) . . ?
N3 Er1 C12 78.61(9) . . ?
N2 Er1 C12 102.21(9) . . ?
O6W Er1 C14 100.11(10) . . ?
O5W Er1 C14 76.04(9) . . ?
O1 Er1 C14 154.71(9) . . ?
O3 Er1 C14 26.62(9) . . ?
O4 Er1 C14 26.36(9) . . ?
O2 Er1 C14 151.31(8) . . ?
N1 Er1 C14 89.01(12) . . ?
N3 Er1 C14 103.43(9) . . ?
N2 Er1 C14 78.40(9) . . ?
C12 Er1 C14 177.02(10) . . ?
O6W Er1 Er1 80.20(7) . 2_665 ?
O5W Er1 Er1 41.28(6) . 2_665 ?
O1 Er1 Er1 87.98(6) . 2_665 ?
O3 Er1 Er1 117.14(7) . 2_665 ?
O4 Er1 Er1 110.90(6) . 2_665 ?
O2 Er1 Er1 34.25(5) . 2_665 ?
N1 Er1 Er1 131.47(7) . 2_665 ?
N3 Er1 Er1 70.72(6) . 2_665 ?
N2 Er1 Er1 155.64(6) . 2_665 ?
C12 Er1 Er1 61.17(7) . 2_665 ?
C14 Er1 Er1 117.28(6) . 2_665 ?
C12 O1 Er1 95.6(2) . . ?
C12 O2 Er1 91.12(19) . . ?
C14 O3 Er1 94.9(2) . . ?
C14 O4 Er1 94.0(2) . . ?
Er1 O5W H5WA 110(3) . . ?
Er1 O5W H5WB 132(3) . . ?
H5WA O5W H5WB 113(3) . . ?
Er1 O6W H6WA 116(3) . . ?
Er1 O6W H6WB 124(3) . . ?
H6WA O6W H6WB 113(3) . . ?
H7WA O7W H7WB 114(4) . . ?
C6 N1 N5 119.3(4) . . ?
C6 N1 Er1 121.1(3) . . ?
N5 N1 Er1 119.4(3) . . ?
C1 N2 C5 116.1(3) . . ?
C1 N2 Er1 120.7(2) . . ?
C5 N2 Er1 123.2(3) . . ?
C7 N3 C11 116.7(3) . . ?
C7 N3 Er1 119.2(2) . . ?
C11 N3 Er1 123.9(2) . . ?
O9 N4 O8 120.9(3) . . ?
O9 N4 O10 121.1(3) . . ?
O8 N4 O10 118.0(3) . . ?
N1 N5 C7 119.1(4) . . ?
N1 N5 H5N 120(5) . . ?
C7 N5 H5N 120(5) . . ?
N2 C1 C2 122.8(4) . . ?
N2 C1 C6 116.4(3) . . ?
C2 C1 C6 120.8(4) . . ?
C3 C2 C1 119.3(5) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C4 C3 C2 118.5(4) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C3 C4 C5 119.1(4) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
N2 C5 C4 124.1(5) . . ?
N2 C5 H5 117.9 . . ?
C4 C5 H5 117.9 . . ?
N1 C6 C1 118.8(4) . . ?
N1 C6 H6 120.6 . . ?
C1 C6 H6 120.6 . . ?
N3 C7 C8 122.1(4) . . ?
N3 C7 N5 117.3(3) . . ?
C8 C7 N5 120.6(4) . . ?
C9 C8 C7 119.6(5) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C10 C9 C8 118.9(4) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
C9 C10 C11 118.4(4) . . ?
C9 C10 H10 120.8 . . ?
C11 C10 H10 120.8 . . ?
N3 C11 C10 124.1(4) . . ?
N3 C11 H11 117.9 . . ?
C10 C11 H11 117.9 . . ?
O2 C12 O1 119.5(3) . . ?
O2 C12 C13 121.2(3) . . ?
O1 C12 C13 119.3(3) . . ?
O2 C12 Er1 61.93(16) . . ?
O1 C12 Er1 57.58(16) . . ?
C13 C12 Er1 176.7(2) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O4 C14 O3 118.1(3) . . ?
O4 C14 C15 121.7(4) . . ?
O3 C14 C15 120.2(3) . . ?
O4 C14 Er1 59.64(17) . . ?
O3 C14 Er1 58.49(17) . . ?
C15 C14 Er1 178.2(3) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5W H5WA O10 0.806(18) 2.08(2) 2.855(4) 162(4) 1_455
O5W H5WB O2 0.813(18) 1.91(2) 2.716(3) 174(4) 2_665
O6W H6WA O7W 0.811(18) 1.87(2) 2.659(5) 165(5) .
O6W H6WB O8 0.823(18) 1.950(18) 2.771(4) 175(4) .
O7W H7WA O10 0.809(19) 2.12(2) 2.923(5) 174(6) 1_455
O7W H7WB O9 0.810(19) 2.19(3) 2.984(5) 167(7) 2_755
N5 H5N O3 0.91(2) 2.14(4) 3.004(5) 158(7) 2_566
_diffrn_measured_fraction_theta_max 0.880
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max 0.683
_refine_diff_density_min -1.004
_refine_diff_density_rms 0.119
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
loop_
_publcif_info_datablock.id
_publcif_info_datablock.publ_exptl
_publcif_info_datablock.publ_geom
_publcif_info_datablock.structure
{f3966e52-0f67-49dc-8ba3-2fcc6d4d2dd2} y y y
loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max
loop_
_publcif_info_exptl_table_header_item
?
loop_
_publcif_info_tables.block_id
_publcif_info_tables.reference_item
{f3966e52-0f67-49dc-8ba3-2fcc6d4d2dd2} '_publcif_info_datablock.publ_exptl'
{f3966e52-0f67-49dc-8ba3-2fcc6d4d2dd2} '_geom_hbond_atom_site_label_D'
loop_
_publcif_info_cif.paper_type
EE