#------------------------------------------------------------------------------
#$Date: 2026-04-28 00:55:15 +0200 (Tue, 28 Apr 2026) $
#$Revision: 305635 $
#$URL: svn://saulius.grazulis.lt/cod-secondary/cif/7/72/09/7720926.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7720926
loop_
_publ_author_name
'Gu, Ziyi'
'Li, Jun'
'Zhang, Xuan'
'Li, Yangjuan'
'Gong, Yu'
_publ_section_title
;
 Synthesis of hydroxo-bridged Dy(III) dimers supported by crown ethers
 through C-H activation and oxygen-atom transfer of Me3NO
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D6DT00818F
_journal_year                    2026
_chemical_formula_moiety         'C14 H26 Dy I N2 O5, 2(I)'
_chemical_formula_sum            'C14 H26 Dy I3 N2 O5'
_chemical_formula_weight         845.57
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2026-01-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.17 svn.r577a77a9 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2026-01-05 deposited with the CCDC.	2026-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8869(4)
_cell_length_b                   11.4727(3)
_cell_length_c                   12.0691(4)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      34.2910
_cell_measurement_theta_min      2.0540
_cell_volume                     2338.25(11)
_computing_cell_refinement       'CrysAlisPro 1.171.43.124a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.124a 64-bit (release 23-05-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.124a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -31.00  45.00   0.50    1.40    --  -16.23  55.00  12.00  152
  2  ω    -45.00 -13.00   0.50    1.40    --  -16.23 111.00  92.00   64
  3  ω    -76.00 -42.00   0.50    1.40    --  -16.23-178.00  90.00   68
  4  ω    -76.00 -42.00   0.50    1.40    --  -16.23-178.00   0.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0145753000
_diffrn_orient_matrix_UB_12      0.0428544000
_diffrn_orient_matrix_UB_13      -0.0371838000
_diffrn_orient_matrix_UB_21      0.0238371000
_diffrn_orient_matrix_UB_22      0.0427541000
_diffrn_orient_matrix_UB_23      0.0261422000
_diffrn_orient_matrix_UB_31      0.0314048000
_diffrn_orient_matrix_UB_32      -0.0125755000
_diffrn_orient_matrix_UB_33      -0.0371807000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10420
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.074
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.180
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.124a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.402
_exptl_crystal_description       block
_exptl_crystal_F_000             1556
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.308
_refine_diff_density_min         -1.739
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         2495
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0231P)²+10.4611P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0587
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2257
_reflns_number_total             2495
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d6dt00818f2.cif
_cod_data_source_block           gzy-75-3_auto
_cod_database_code               7720926
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Dy1C1N1O1I1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.358
_shelx_estimated_absorpt_t_min   0.328
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1_$1-C1
 1.495 with sigma of 0.001
 C3_$1-C2_$1
 1.495 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C3(H3A,H3B), C4(H4A,H4B), C2(H2A,H2B), C1(H1A,H1B)
4.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.150
_oxdiff_exptl_absorpt_empirical_full_min 0.901
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.26798(2) 0.750000 0.49786(2) 0.01729(8) Uani 1 2 d S T P . .
I3 I 0.36053(2) 0.750000 0.28606(4) 0.02647(11) Uani 1 2 d S T P . .
I2 I 0.45724(2) 0.750000 0.89178(4) 0.02808(11) Uani 1 2 d S T P . .
I1 I 0.11820(2) 0.750000 1.04908(4) 0.02807(11) Uani 1 2 d S T P . .
O3 O 0.1462(2) 0.750000 0.3970(4) 0.0254(9) Uani 1 2 d S T P . .
O2 O 0.22256(18) 0.5570(3) 0.4456(3) 0.0308(7) Uani 1 1 d . . . . .
N1 N 0.3748(2) 0.8747(4) 0.5660(3) 0.0308(9) Uani 1 1 d . . . . .
O1 O 0.2152(3) 0.6386(3) 0.6492(3) 0.0563(12) Uani 1 1 d . U . . .
C5 C 0.1055(3) 0.6439(4) 0.3649(4) 0.0278(10) Uani 1 1 d . . . . .
H5A H 0.076153 0.655418 0.294725 0.033 Uiso 1 1 calc R U . . .
H5B H 0.067782 0.619308 0.423117 0.033 Uiso 1 1 calc R U . . .
C6 C 0.4300(3) 0.9169(4) 0.6015(4) 0.0251(9) Uani 1 1 d . . . . .
C7 C 0.5009(2) 0.9705(4) 0.6461(4) 0.0278(10) Uani 1 1 d . . . . .
H7A H 0.547536 0.938801 0.608306 0.042 Uiso 1 1 calc R U . . .
H7B H 0.504552 0.953844 0.725611 0.042 Uiso 1 1 calc R U . . .
H7C H 0.498544 1.054946 0.634644 0.042 Uiso 1 1 calc R U . . .
C3 C 0.2026(3) 0.4774(4) 0.5348(4) 0.0421(14) Uani 1 1 d . . . . .
H3A H 0.251115 0.438122 0.561758 0.050 Uiso 1 1 calc R U . . .
H3B H 0.165717 0.416888 0.507187 0.050 Uiso 1 1 calc R U . . .
C4 C 0.1696(3) 0.5552(4) 0.3505(4) 0.0332(11) Uani 1 1 d . . . . .
H4A H 0.145884 0.476684 0.342814 0.040 Uiso 1 1 calc R U . . .
H4B H 0.199982 0.572225 0.282205 0.040 Uiso 1 1 calc R U . . .
C2 C 0.1647(3) 0.5433(5) 0.6276(5) 0.0532(17) Uani 1 1 d . . . . .
H2A H 0.111394 0.570764 0.605810 0.064 Uiso 1 1 calc R U . . .
H2B H 0.159659 0.493281 0.694076 0.064 Uiso 1 1 calc R U . . .
C1 C 0.1968(7) 0.68489(4) 0.7525(7) 0.117(3) Uani 1 1 d D U . . .
H1A H 0.235870 0.656653 0.807449 0.140 Uiso 1 1 calc R U . . .
H1B H 0.143908 0.656653 0.775450 0.140 Uiso 1 1 calc R U . . .
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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Dy1 I3 90.82(11) . . ?
O3 Dy1 O2 66.15(7) . 7_575 ?
O3 Dy1 O2 66.15(7) . . ?
O3 Dy1 N1 143.75(10) . 7_575 ?
O3 Dy1 N1 143.75(10) . . ?
O3 Dy1 O1 93.89(16) . 7_575 ?
O3 Dy1 O1 93.89(16) . . ?
O2 Dy1 I3 86.74(9) 7_575 . ?
O2 Dy1 I3 86.74(9) . . ?
O2 Dy1 O2 131.69(15) 7_575 . ?
O2 Dy1 N1 77.70(12) . 7_575 ?
O2 Dy1 N1 148.71(12) 7_575 7_575 ?
O2 Dy1 N1 148.71(12) . . ?
O2 Dy1 N1 77.70(12) 7_575 . ?
N1 Dy1 I3 84.39(10) 7_575 . ?
N1 Dy1 I3 84.39(10) . . ?
N1 Dy1 N1 71.61(19) . 7_575 ?
O1 Dy1 I3 147.43(9) . . ?
O1 Dy1 I3 147.43(9) 7_575 . ?
O1 Dy1 O2 66.08(13) 7_575 7_575 ?
O1 Dy1 O2 124.47(13) . 7_575 ?
O1 Dy1 O2 66.08(13) . . ?
O1 Dy1 O2 124.47(13) 7_575 . ?
O1 Dy1 N1 109.23(15) 7_575 7_575 ?
O1 Dy1 N1 109.23(16) . . ?
O1 Dy1 N1 72.94(15) 7_575 . ?
O1 Dy1 N1 72.94(15) . 7_575 ?
O1 Dy1 O1 64.32(18) 7_575 . ?
C5 O3 Dy1 122.9(2) 7_575 . ?
C5 O3 Dy1 122.9(2) . . ?
C5 O3 C5 114.1(5) 7_575 . ?
C3 O2 Dy1 117.1(3) . . ?
C3 O2 C4 115.7(4) . . ?
C4 O2 Dy1 114.4(3) . . ?
C6 N1 Dy1 169.5(4) . . ?
C2 O1 Dy1 119.7(3) . . ?
C1 O1 Dy1 124.2(3) . . ?
C1 O1 C2 109.1(5) . . ?
O3 C5 H5A 110.7 . . ?
O3 C5 H5B 110.7 . . ?
O3 C5 C4 105.0(3) . . ?
H5A C5 H5B 108.8 . . ?
C4 C5 H5A 110.7 . . ?
C4 C5 H5B 110.7 . . ?
N1 C6 C7 179.6(6) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O2 C3 H3A 109.7 . . ?
O2 C3 H3B 109.7 . . ?
O2 C3 C2 109.7(4) . . ?
H3A C3 H3B 108.2 . . ?
C2 C3 H3A 109.7 . . ?
C2 C3 H3B 109.7 . . ?
O2 C4 C5 110.1(4) . . ?
O2 C4 H4A 109.7 . . ?
O2 C4 H4B 109.7 . . ?
C5 C4 H4A 109.7 . . ?
C5 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
O1 C2 C3 105.8(4) . . ?
O1 C2 H2A 110.6 . . ?
O1 C2 H2B 110.6 . . ?
C3 C2 H2A 110.6 . . ?
C3 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
O1 C1 C1 112.5(2) . 7_575 ?
O1 C1 H1A 109.1 . . ?
O1 C1 H1B 109.1 . . ?
C1 C1 H1A 109.1 7_575 . ?
C1 C1 H1B 109.1 7_575 . ?
H1A C1 H1B 107.8 . . ?
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
Dy1 I3 2.9962(5) . ?
Dy1 O3 2.389(4) . ?
Dy1 O2 2.426(3) 7_575 ?
Dy1 O2 2.426(3) . ?
Dy1 N1 2.445(4) . ?
Dy1 N1 2.445(4) 7_575 ?
Dy1 O1 2.401(4) 7_575 ?
Dy1 O1 2.401(4) . ?
O3 C5 1.451(5) . ?
O3 C5 1.451(5) 7_575 ?
O2 C3 1.452(6) . ?
O2 C4 1.455(6) . ?
N1 C6 1.135(6) . ?
O1 C2 1.410(7) . ?
O1 C1 1.390(8) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C4 1.497(7) . ?
C6 C7 1.449(6) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C2 1.4947(10) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C1 C1 1.4939(10) 7_575 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O3 C5 C4 -29.6(5) . . . . ?
Dy1 O2 C3 C2 36.5(5) . . . . ?
Dy1 O2 C4 C5 -48.8(4) . . . . ?
Dy1 O1 C2 C3 44.6(5) . . . . ?
Dy1 O1 C1 C1 12.3(7) . . . 7_575 ?
O3 C5 C4 O2 48.3(5) . . . . ?
O2 C3 C2 O1 -50.0(6) . . . . ?
C5 O3 C5 C4 151.8(3) 7_575 . . . ?
C3 O2 C4 C5 91.8(5) . . . . ?
C4 O2 C3 C2 -103.0(5) . . . . ?
C2 O1 C1 C1 -138.1(3) . . . 7_575 ?
C1 O1 C2 C3 -163.4(6) . . . . ?
