#------------------------------------------------------------------------------
#$Date: 2025-06-03 21:26:02 +0200 (Tue, 03 Jun 2025) $
#$Revision: 299929 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/34/2023483.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_2023483
loop_
_publ_author_name
'Baisch, Ulrich'
'Scicluna, Marie Christine'
'Vella-Zarb, Liana'
_publ_section_title
;
Rapid and facile one-step microwave synthesis of macrobicyclic cryptands.
;
_journal_coeditor_code NX2023
_journal_issue 'Pt 5'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 448
_journal_page_last 451
_journal_paper_doi 10.1107/S2056989025003044
_journal_volume 81
_journal_year 2025
_chemical_absolute_configuration ad
_chemical_formula_iupac 'C36 H42 N8, 6H2 O'
_chemical_formula_moiety 'C36 H42 N8, 6(H2 O)'
_chemical_formula_sum 'C36 H54 N8 O6'
_chemical_formula_weight 694.87
_chemical_name_systematic
'6,16,25(1,4)-Tribenzena-1,4,8,11,14,18,23,27-octaazabicyclo[9.9.9]nonacosaphane-4,7,14,17,23,26-hexaene hexahydrate'
_space_group_crystal_system trigonal
_space_group_IT_number 155
_space_group_name_Hall 'R 3 2"'
_space_group_name_H-M_alt 'R 3 2 :H'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 3
_cell_length_a 14.5942(2)
_cell_length_b 14.5942(2)
_cell_length_c 15.4565(2)
_cell_measurement_reflns_used 4384
_cell_measurement_temperature 120
_cell_measurement_theta_max 25.9610
_cell_measurement_theta_min 1.8680
_cell_volume 2851.03(7)
_computing_cell_refinement
;
CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)
;
_computing_data_collection
;
CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)
;
_computing_data_reduction
;
CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)
;
_computing_molecular_graphics
;
Olex2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
Olex2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
ShelXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 120
_diffrn_detector 'Pilatus 2M'
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device 'Kappa CCD diffractometer at BM01 ESRF'
_diffrn_measurement_device_type 'Kappa CCD diffractometer at BM01 ESRF'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator synchrotron
_diffrn_radiation_probe x-ray
_diffrn_radiation_type synchrotron
_diffrn_radiation_wavelength 0.64066
_diffrn_reflns_av_R_equivalents 0.0173
_diffrn_reflns_av_unetI/netI 0.0104
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 4982
_diffrn_reflns_theta_full 22.606
_diffrn_reflns_theta_max 25.954
_diffrn_reflns_theta_min 1.876
_diffrn_source synchrotron
_exptl_absorpt_coefficient_mu 0.068
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.74689
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2018)
;
_exptl_crystal_colour 'clear dark orange'
_exptl_crystal_density_diffrn 1.214
_exptl_crystal_description block
_exptl_crystal_F_000 1122
_exptl_crystal_size_max 0.12
_exptl_crystal_size_mid 0.11
_exptl_crystal_size_min 0.1
_refine_diff_density_max 0.262
_refine_diff_density_min -0.158
_refine_ls_abs_structure_details
;
Flack x determined using 691 quotients
[(I^+^)-(I^-^)]/[(I^+^)+(I^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack 0.2(3)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.058
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 83
_refine_ls_number_reflns 1565
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.058
_refine_ls_R_factor_all 0.0293
_refine_ls_R_factor_gt 0.0292
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+0.4923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0824
_refine_ls_wR_factor_ref 0.0824
_reflns_number_gt 1553
_reflns_number_total 1565
_reflns_threshold_expression 'I > 2\s(I)'
_iucr_refine_instructions_details
;
TITL 15mlvzmcs003_a.res in R32
15mlvzmcs003_sx.res
created by SHELXL-2017/1 at 13:05:23 on 08-Jan-2019
REM Old TITL 15MLVZMCS003 in R-3m
REM SHELXT solution in R32: R1 0.114, Rweak 0.033, Alpha 0.002
REM 0.000 for 0 systematic absences, Orientation as input
REM Flack x = 0.235 ( 0.265 ) from 566 Parsons' quotients
REM Formula found by SHELXT: C18 N4 O3
CELL 0.64066 14.5942 14.5942 15.4565 90 90 120
ZERR 3 0.0002 0.0002 0.0002 0 0 0
LATT -3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM +Y,+X,-Z
SYMM -Y+X,-Y,-Z
SYMM -X,-X+Y,-Z
SFAC C H N O
DISP C 0.0025 0.0013 9.345
DISP H -0 0 0.6198
DISP N 0.0049 0.0025 15.406
DISP O 0.009 0.0048 24.8551
UNIT 108 162 24 18
L.S. 10
PLAN 10
SIZE 0.1 0.11 0.12
TEMP -153.15
BOND $H
list 4
fmap 2
acta
OMIT 2 2 0
OMIT -2 4 0
OMIT 0 0 3
OMIT -2 3 1
OMIT -3 2 1
OMIT 0 12 6
OMIT 0 4 8
OMIT -4 8 3
OMIT 4 4 3
OMIT -2 11 5
OMIT 2 9 5
OMIT 3 7 2
OMIT -3 10 2
OMIT 3 7 5
OMIT -3 10 5
REM
REM
REM
WGHT 0.059200 0.492300
FVAR 0.61683
AFIX 6
O1 4 0.631581 0.608101 0.589503 11.00000 0.04414 0.03276 =
0.03086 0.00053 -0.00301 0.01156
H1C 2 0.662121 0.660324 0.625960 10.50000 -1.50000
H1D 2 0.636344 0.638318 0.539870 10.50000 -1.50000
AFIX 0
N1 3 0.666667 0.333333 0.494114 10.33333 0.02992 0.02992 =
0.01858 0.00000 0.00000 0.01496
N2 3 0.515721 0.382209 0.595077 11.00000 0.03119 0.03430 =
0.02509 -0.00172 0.00147 0.01733
C1 1 0.612498 0.388274 0.462818 11.00000 0.03476 0.03560 =
0.01971 0.00238 0.00148 0.01968
AFIX 23
H1A 2 0.602840 0.377965 0.399467 11.00000 -1.20000
H1B 2 0.658443 0.465002 0.473532 11.00000 -1.20000
AFIX 0
C6 1 0.535506 0.432787 0.870194 11.00000 0.03657 0.02752 =
0.02861 -0.00219 0.00287 0.01405
AFIX 43
H6 2 0.569410 0.501297 0.895476 11.00000 -1.20000
AFIX 0
C5 1 0.529760 0.422584 0.781132 11.00000 0.03781 0.02811 =
0.02755 0.00175 0.00496 0.01436
AFIX 43
H5 2 0.558765 0.483953 0.745679 11.00000 -1.20000
AFIX 0
C3 1 0.477812 0.307203 0.649411 11.00000 0.02919 0.03121 =
0.02686 -0.00332 -0.00134 0.01512
AFIX 43
H3 2 0.444964 0.236743 0.628129 11.00000 -1.20000
AFIX 0
C4 1 0.481772 0.323014 0.743366 11.00000 0.02773 0.03019 =
0.02592 -0.00093 -0.00019 0.01515
C2 1 0.505277 0.352252 0.504099 11.00000 0.03361 0.03998 =
0.02375 -0.00291 -0.00137 0.02051
AFIX 23
H2A 2 0.469113 0.384344 0.472734 11.00000 -1.20000
H2B 2 0.461084 0.274407 0.499024 11.00000 -1.20000
AFIX 0
H1E 2 0.594999 0.542181 0.597115 11.00000 0.04492
HKLF 4
REM 15mlvzmcs003_a.res in R32
REM R1 = 0.0292 for 1553 Fo > 4sig(Fo) and 0.0293 for all 1565 data
REM 83 parameters refined using 0 restraints
END
WGHT 0.0592 0.4922
REM Highest difference peak 0.262, deepest hole -0.158, 1-sigma level 0.031
Q1 1 0.4841 0.3205 0.6950 11.00000 0.05 0.26
Q2 1 0.5163 0.3697 0.7613 11.00000 0.05 0.21
Q3 1 0.4527 0.2829 0.7693 11.00000 0.05 0.18
Q4 1 0.5342 0.4249 0.8267 11.00000 0.05 0.17
Q5 1 0.6344 0.6248 0.6431 11.00000 0.05 0.16
Q6 1 0.6667 0.3333 0.5410 10.33333 0.05 0.16
Q7 1 0.7172 0.3587 0.4761 11.00000 0.05 0.16
Q8 1 0.5190 0.3709 0.5521 11.00000 0.05 0.16
Q9 1 0.5586 0.3626 0.4858 11.00000 0.05 0.15
Q10 1 0.5300 0.4366 0.6081 11.00000 0.05 0.15
REM The information below was added by Olex2.
REM
REM R1 = 0.0292 for 1553 Fo > 4sig(Fo) and 0.0293 for all 5038 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.26, deepest hole -0.16
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0293
REM R1_gt = 0.0292
REM wR_ref = 0.0824
REM GOOF = 1.058
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 5038
REM Reflections_gt = 1553
REM Parameters = n/a
REM Hole = -0.16
REM Peak = 0.26
REM Flack = 0.2(3)
;
_cod_data_source_file nx2023.cif
_cod_data_source_block I
_cod_depositor_comments 'Adding full bibliography for 2023483.cif.'
_cod_original_cell_volume 2851.03(9)
_cod_original_sg_symbol_H-M 'R 3 2'
_cod_database_code 2023483
_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 0.992
_shelx_estimated_absorpt_t_max 0.993
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
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
O O1 0.63158(9) 0.60810(8) 0.58950(6) 0.0393(3) Uani d 1 . .
H H1C 0.662121 0.660324 0.625960 0.059 Uiso d 0.5 . .
H H1D 0.636344 0.638318 0.539870 0.059 Uiso d 0.5 . .
N N1 0.666667 0.333333 0.49411(11) 0.0261(3) Uani d 1 . .
N N2 0.51572(8) 0.38221(8) 0.59508(6) 0.0298(2) Uani d 1 . .
C C1 0.61250(11) 0.38827(10) 0.46282(7) 0.0291(3) Uani d 1 . .
H H1A 0.602840 0.377965 0.399467 0.035 Uiso calc 1 . .
H H1B 0.658443 0.465002 0.473532 0.035 Uiso calc 1 . .
C C6 0.53551(10) 0.43279(10) 0.87019(8) 0.0318(3) Uani d 1 . .
H H6 0.569410 0.501297 0.895476 0.038 Uiso calc 1 . .
C C5 0.52976(10) 0.42258(9) 0.78113(8) 0.0321(3) Uani d 1 . .
H H5 0.558765 0.483953 0.745679 0.039 Uiso calc 1 . .
C C3 0.47781(10) 0.30720(9) 0.64941(8) 0.0291(3) Uani d 1 . .
H H3 0.444964 0.236743 0.628129 0.035 Uiso calc 1 . .
C C4 0.48177(9) 0.32301(10) 0.74337(8) 0.0277(3) Uani d 1 . .
C C2 0.50528(10) 0.35225(11) 0.50410(8) 0.0315(3) Uani d 1 . .
H H2A 0.469113 0.384344 0.472734 0.038 Uiso calc 1 . .
H H2B 0.461084 0.274407 0.499024 0.038 Uiso calc 1 . .
H H1E 0.5950(16) 0.5422(18) 0.5971(12) 0.045(5) Uiso d 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
O1 0.0441(6) 0.0328(5) 0.0309(5) 0.0116(4) -0.0030(4) 0.0005(3)
N1 0.0299(5) 0.0299(5) 0.0186(7) 0.0150(3) 0.000 0.000
N2 0.0312(5) 0.0343(5) 0.0251(5) 0.0173(4) 0.0015(4) -0.0017(4)
C1 0.0348(6) 0.0356(6) 0.0197(5) 0.0197(5) 0.0015(4) 0.0024(4)
C6 0.0366(6) 0.0275(5) 0.0286(6) 0.0140(5) 0.0029(5) -0.0022(4)
C5 0.0378(6) 0.0281(5) 0.0275(6) 0.0144(5) 0.0050(5) 0.0018(4)
C3 0.0292(6) 0.0312(5) 0.0269(6) 0.0151(5) -0.0013(4) -0.0033(4)
C4 0.0277(5) 0.0302(5) 0.0259(5) 0.0151(4) -0.0002(4) -0.0009(4)
C2 0.0336(6) 0.0400(6) 0.0237(5) 0.0205(5) -0.0014(4) -0.0029(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0025 0.0013 '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 0.0049 0.0025 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0090 0.0048 '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
H1C O1 H1D . . 104.5 ?
H1C O1 H1E . . 131.6 ?
H1D O1 H1E . . 123.1 ?
C1 N1 C1 2_655 3_665 109.61(8) ?
C1 N1 C1 3_665 . 109.62(8) ?
C1 N1 C1 2_655 . 109.62(8) ?
C3 N2 C2 . . 116.45(11) ?
N1 C1 H1A . . 108.6 ?
N1 C1 H1B . . 108.6 ?
N1 C1 C2 . . 114.65(10) ?
H1A C1 H1B . . 107.6 ?
C2 C1 H1A . . 108.6 ?
C2 C1 H1B . . 108.6 ?
C5 C6 H6 . . 119.6 ?
C5 C6 C4 . 17_556 120.73(11) ?
C4 C6 H6 17_556 . 119.6 ?
C6 C5 H5 . . 119.9 ?
C6 C5 C4 . . 120.22(11) ?
C4 C5 H5 . . 119.9 ?
N2 C3 H3 . . 118.2 ?
N2 C3 C4 . . 123.69(11) ?
C4 C3 H3 . . 118.2 ?
C6 C4 C3 17_556 . 118.24(11) ?
C5 C4 C6 . 17_556 119.02(11) ?
C5 C4 C3 . . 122.73(11) ?
N2 C2 C1 . . 111.47(10) ?
N2 C2 H2A . . 109.3 ?
N2 C2 H2B . . 109.3 ?
C1 C2 H2A . . 109.3 ?
C1 C2 H2B . . 109.3 ?
H2A C2 H2B . . 108.0 ?
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
O1 H1C . 0.8703 ?
O1 H1D . 0.8701 ?
O1 H1E . 0.84(2) ?
N1 C1 3_665 1.4614(13) ?
N1 C1 . 1.4614(13) ?
N1 C1 2_655 1.4614(13) ?
N2 C3 . 1.2665(16) ?
N2 C2 . 1.4578(15) ?
C1 H1A . 0.9900 ?
C1 H1B . 0.9900 ?
C1 C2 . 1.5197(18) ?
C6 H6 . 0.9500 ?
C6 C5 . 1.3826(17) ?
C6 C4 17_556 1.3940(17) ?
C5 H5 . 0.9500 ?
C5 C4 . 1.3875(17) ?
C3 H3 . 0.9500 ?
C3 C4 . 1.4670(16) ?
C2 H2A . 0.9900 ?
C2 H2B . 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
O1 H1C O1 11_566 0.87 2.00 2.8075(13) 154
O1 H1D O1 4_556 0.87 2.03 2.8297(13) 152
O1 H1E N2 . 0.84(2) 2.02(2) 2.8566(14) 170.3(18)
C6 H6 O1 9_565 0.95 2.60 3.5173(17) 163
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_meas
_refln_F_squared_sigma
0 0 -3 3963.63 11.19
0 0 3 4293.6 10.75
0 0 -6 3795.25 10.8
0 0 6 3878.9 10.96
0 0 9 527.84 3.11
0 0 -9 540.15 3
0 0 12 1097.2 5.32
0 0 -12 1117.77 5.23
0 0 15 949.85 5.43
0 0 -15 1014.26 5.39
-1 1 -14 340.55 2.72
0 -1 -14 352.19 2.86
-1 0 14 342.9 3.04
0 1 14 343.91 2.92
1 -1 14 348.23 2.91
1 0 -11 11.88 0.49
-1 1 -11 11.88 0.45
0 -1 -11 12.75 0.5
-1 0 11 11.89 0.52
0 1 11 12.61 0.51
1 -1 11 11.35 0.47
-1 0 8 162.61 1.59
1 0 -8 157.81 1.5
0 -1 -8 170.27 1.54
-1 1 -8 156.45 1.35
0 1 8 164.11 1.55
1 -1 8 164.07 1.46
0 1 5 1076.02 3.91
0 -1 -5 1079.18 3.94
1 0 -5 1085.19 4.03
-1 0 2 2611.77 6.46
0 -1 -2 2600.94 6.36
1 -1 -1 596.04 1.93
0 -1 1 591.69 1.96
1 0 4 1018.23 3.27
-1 1 4 1019.42 3.68
1 -1 -4 1007.89 3.65
-1 0 -4 1002.75 3.29
0 -1 7 8068.04 18.56
-1 1 7 7351.6 18.41
1 -1 -7 8074.74 18.7
1 0 7 6653.71 18.25
1 -1 -10 1702.82 6.66
0 -1 10 1680.15 6.67
1 0 10 1694.29 6.46
0 1 -10 1715.6 6.47
-1 0 -10 1673.61 6.27
-1 1 10 1674.02 6.84
1 -1 -13 47.2 1.02
-1 0 -13 48.83 0.99
1 0 13 47.38 1.02
-1 1 13 45.25 1.04
1 -1 -16 88.84 1.51
-1 1 16 83.82 1.57
-2 1 0 1996.04 4.86
1 -2 0 2001.29 5.12
-1 -1 0 1990.44 5.16
1 1 3 2807.38 7.66
-1 -1 3 2803.52 8.14
1 -2 -3 2879.8 8.08
-1 2 3 2872.09 7.96
-2 1 3 2785.18 8.11
-1 -1 -3 2826.34 7.89
-1 2 -3 2708.05 7.52
2 -1 -3 2833.53 8.03
1 -2 3 2870.64 7.67
1 1 -3 2798.09 7.94
1 1 6 3986.37 11.33
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