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#$Date: 2024-09-04 18:51:38 +0300 (Wed, 04 Sep 2024) $
#$Revision: 294367 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/69/7716960.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_7716960
loop_
_publ_author_name
'Nandy, Rakhi'
'Jagličić, Zvonko'
'Jana, Narayan Ch'
'Brandão, Paula'
'Bustamante, Fabián'
'Aravena, Daniel'
'Panja, Anangamohan'
_publ_section_title
;
 The effect of co-ligands on the performance of single-molecule magnet
 behaviours in a family of linear trinuclear Zn-Dy-Zn complexes with a
 compartmental Schiff base.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13968
_journal_page_last               13981
_journal_paper_doi               10.1039/d4dt01582g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_sum            'C24 H30 N2 O4'
_chemical_formula_weight         410.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-07-09 deposited with the CCDC.	2024-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.8442(10)
_cell_length_b                   25.538(2)
_cell_length_c                   8.7128(5)
_cell_measurement_reflns_used    560
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.99
_cell_volume                     4638.0(5)
_computing_cell_refinement       'Bruker APEX-II'
_computing_data_collection       'Bruker Smart APEX-II CCD Diffractometer'
_computing_data_reduction        'Bruker SAINT plus'
_computing_molecular_graphics
'Olex2 1.5-alpha (Dolomanov et al., 2009)and mercury'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'photon 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_unetI/netI     0.0097
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            25447
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.121
_diffrn_reflns_theta_min         2.523
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_description       Block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.152
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Flack x determined using 1144 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.09(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2548
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0304
_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/[σ²(Fo²)+(0.0557P)²+2.8072P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0875
_reflns_Friedel_coverage         0.875
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                2489
_reflns_number_total             2548
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01582g2.cif
_cod_data_source_block           f
_cod_original_cell_volume        4637.9(5)
_cod_database_code               7716960
_shelx_shelxl_version_number     2018/3
_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   0.983
_shelx_estimated_absorpt_t_max   0.997
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'
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
O1 O 0.62886(6) 0.32622(5) 0.61759(15) 0.0303(3) Uani 1 1 d . . . . .
H1 H 0.6493(11) 0.3112(9) 0.544(3) 0.036(6) Uiso 1 1 d . . . . .
O2 O 0.55686(6) 0.34909(5) 0.85606(15) 0.0334(3) Uani 1 1 d . . . . .
N1 N 0.68066(6) 0.25468(6) 0.44158(16) 0.0260(3) Uani 1 1 d . . . . .
C1 C 0.60424(7) 0.28576(6) 0.69850(19) 0.0237(3) Uani 1 1 d . . . . .
C2 C 0.56573(7) 0.29684(7) 0.82720(19) 0.0266(4) Uani 1 1 d . . . . .
C3 C 0.54038(8) 0.25669(7) 0.9146(2) 0.0292(4) Uani 1 1 d . . . . .
H3 H 0.514284 0.264737 1.000857 0.035 Uiso 1 1 calc R U . . .
C4 C 0.55278(8) 0.20402(7) 0.8774(2) 0.0321(4) Uani 1 1 d . . . . .
C5 C 0.58962(8) 0.19312(7) 0.7499(2) 0.0278(4) Uani 1 1 d . . . . .
H5 H 0.597630 0.157685 0.722745 0.033 Uiso 1 1 calc R U . . .
C6 C 0.61549(7) 0.23341(6) 0.65948(19) 0.0242(3) Uani 1 1 d . . . . .
C7 C 0.51518(10) 0.36221(8) 0.9804(3) 0.0409(5) Uani 1 1 d . . . . .
H7A H 0.472715 0.346959 0.962235 0.061 Uiso 1 1 calc R U . . .
H7B H 0.511392 0.400373 0.988015 0.061 Uiso 1 1 calc R U . . .
H7C H 0.532848 0.348299 1.076365 0.061 Uiso 1 1 calc R U . . .
C8 C 0.52687(12) 0.16073(8) 0.9777(3) 0.0517(6) Uani 1 1 d . . . . .
H8A H 0.480078 0.159252 0.967805 0.078 Uiso 1 1 calc R U . . .
H8B H 0.538323 0.167628 1.084928 0.078 Uiso 1 1 calc R U . . .
H8C H 0.545404 0.127214 0.945580 0.078 Uiso 1 1 calc R U . . .
C9 C 0.65402(8) 0.21974(7) 0.52506(19) 0.0245(3) Uani 1 1 d . . . . .
H9 H 0.659402 0.183884 0.499061 0.029 Uiso 1 1 calc R U . . .
C10 C 0.71697(8) 0.23679(7) 0.30787(18) 0.0265(3) Uani 1 1 d . . . . .
H10 H 0.7250(9) 0.1989(8) 0.306(2) 0.019(4) Uiso 1 1 d . . . . .
C11 C 0.67959(9) 0.25029(8) 0.1625(2) 0.0350(4) Uani 1 1 d . . . . .
H11A H 0.638494 0.230857 0.162141 0.042 Uiso 1 1 calc R U . . .
H11B H 0.669615 0.288191 0.162096 0.042 Uiso 1 1 calc R U . . .
C12 C 0.71736(10) 0.23662(9) 0.0186(2) 0.0413(5) Uani 1 1 d . . . . .
H12A H 0.692854 0.247718 -0.073166 0.050 Uiso 1 1 calc R U . . .
H12B H 0.723334 0.198204 0.013049 0.050 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'
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
C1 O1 H1 103.7(15) . . ?
C2 O2 C7 116.71(14) . . ?
C9 N1 C10 117.39(14) . . ?
O1 C1 C6 122.67(15) . . ?
O1 C1 C2 118.57(14) . . ?
C6 C1 C2 118.76(15) . . ?
O2 C2 C3 124.72(15) . . ?
O2 C2 C1 114.76(14) . . ?
C3 C2 C1 120.52(15) . . ?
C2 C3 C4 120.77(16) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 118.75(16) . . ?
C5 C4 C8 121.19(17) . . ?
C3 C4 C8 120.05(18) . . ?
C4 C5 C6 121.20(15) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C1 C6 C5 119.98(15) . . ?
C1 C6 C9 120.97(15) . . ?
C5 C6 C9 119.05(15) . . ?
O2 C7 H7A 109.5 . . ?
O2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 C6 121.86(15) . . ?
N1 C9 H9 119.1 . . ?
C6 C9 H9 119.1 . . ?
N1 C10 C11 109.05(13) . . ?
N1 C10 C10 109.10(12) . 14_655 ?
C11 C10 C10 111.03(12) . 14_655 ?
N1 C10 H10 114.0(12) . . ?
C11 C10 H10 107.3(12) . . ?
C10 C10 H10 106.3(11) 14_655 . ?
C12 C11 C10 111.59(14) . . ?
C12 C11 H11A 109.3 . . ?
C10 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C11 C12 C12 111.07(15) . 14_655 ?
C11 C12 H12A 109.4 . . ?
C12 C12 H12A 109.4 14_655 . ?
C11 C12 H12B 109.4 . . ?
C12 C12 H12B 109.4 14_655 . ?
H12A C12 H12B 108.0 . . ?
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
O1 C1 1.3519(19) . ?
O1 H1 0.86(3) . ?
O2 C2 1.370(2) . ?
O2 C7 1.429(2) . ?
N1 C9 1.278(2) . ?
N1 C10 1.462(2) . ?
C1 C6 1.399(2) . ?
C1 C2 1.408(2) . ?
C2 C3 1.382(2) . ?
C3 C4 1.407(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.379(2) . ?
C4 C8 1.509(3) . ?
C5 C6 1.404(2) . ?
C5 H5 0.9500 . ?
C6 C9 1.462(2) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9 0.9500 . ?
C10 C11 1.527(2) . ?
C10 C10 1.534(3) 14_655 ?
C10 H10 0.983(19) . ?
C11 C12 1.521(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C12 1.523(4) 14_655 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
