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.
Nandy, Rakhi; Jagličić, Zvonko; Jana, Narayan Ch; Brandão, Paula; Bustamante, Fabián; Aravena, Daniel; Panja, Anangamohan; Dalton transactions (Cambridge, England : 2003) 53 (2024) 13968–13981; doi:10.1039/d4dt01582g

data_7716962
_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_moiety
'C48 H58 Br2 Dy N4 O9 Zn2, Cl O4, 2(O1), H2 O, 1[H2O]'
_chemical_formula_sum            'C48 H62 Br2 Cl Dy N4 O17 Zn2'
_chemical_formula_weight         1455.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-07-08
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-09 deposited with the CCDC.	2024-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.405(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5327(7)
_cell_length_b                   19.9571(11)
_cell_length_c                   23.5431(12)
_cell_measurement_reflns_used    612
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.16
_cell_measurement_theta_min      2.90
_cell_volume                     5839.4(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      150.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0382
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            295248
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.564
_diffrn_reflns_theta_min         2.456
_exptl_absorpt_coefficient_mu    3.563
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_description       block
_exptl_crystal_F_000             2908
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.376
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         17826
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.182
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0474
_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/[\s^2^(Fo^2^)+(0.0382P)^2^+27.1529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15478
_reflns_number_total             17826
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01582g2.cif
_cod_data_source_block           apjg334_sq
_cod_database_code               7716962
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.815
_shelx_estimated_absorpt_t_min   0.536
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O11) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O15)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O27) \\sim Ueq, Uanis(O102) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O103)
\\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O104) \\sim Ueq, Uanis(O101) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 O27, O103, O18, O104, O17, O102, O101, Cl1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: Br2(0.8) Br2A(0.2) O102(0.8) O103(0.8) O104(0.8) O10(0.7) O15(0.3)
 O17(0.2) O18(0.2) O27(0.2) O12(0.65) H12C(0.65) O13(0.35) H13C(0.35)
 H13D(0.35) O11(0.5) O14(0.5) H12D(0.65)
 Fixed X: H12D(0.163931)
 Fixed Y: H12D(0.732589)
 Fixed Z: H12D(0.234839)
5.a Free rotating group:
 O9(H9A,H9B), O12(H12C,O13,H13C,H13D)
5.b Ternary CH refined with riding coordinates:
 C10(H10), C15(H15), C34(H34), C39(H39)
5.c Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C35(H35A,
 H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C16(H16), C20(H20), C22(H22), C27(H27), C29(H29),
 C33(H33), C40(H40), C44(H44), C46(H46)
5.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C47(H47A,H47B,H47C), C48(H48A,H48B,
 H48C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              58664
_shelx_hkl_checksum              84528
_shelx_fab_checksum              951
_olex2_submission_special_instructions 'No special instructions were received'