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_7716959
_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 H58.05 Cl2 Dy N4 O9 Zn2, Cl O4, 4(H2 O)'
_chemical_formula_sum            'C48 H66.05 Cl3 Dy N4 O17 Zn2'
_chemical_formula_weight         1370.68
_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                 95.720(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5292(15)
_cell_length_b                   19.500(2)
_cell_length_c                   23.808(3)
_cell_measurement_reflns_used    546
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.99
_cell_volume                     5787.8(12)
_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 0.988
_diffrn_measured_fraction_theta_max 0.741
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.741
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            234637
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.741
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.226
_diffrn_reflns_theta_min         2.652
_exptl_absorpt_coefficient_mu    2.307
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       block
_exptl_crystal_F_000             2780
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.457
_refine_diff_density_min         -1.577
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         12766
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+41.1730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1227
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11783
_reflns_number_total             12766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01582g2.cif
_cod_data_source_block           apjg142
_cod_database_code               7716959
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.631
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H20 of C20, H22 of C22, H15 of C15, H27 of C27, H16 of
  C16, H46 of C46, H44 of C44, H40 of C40, H39 of C39, H33 of C33, H34 of C34,
  H29 of C29, H5 of C5, H10 of C10, H9 of C9, H3 of C3
 At 1.5 times of:
  All C(H,H,H) groups, H20A of C13, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O200-O300
 2.8 with sigma of 0.01
 C13-C12
 1.5 with sigma of 0.02
 C41-C40
 1.45 with sigma of 0.02
 C6-C9
 1.45 with sigma of 0.02
 H200-H20A
 1.4 with sigma of 0.02
 O9-H9B = O9-H9A
 0.87 with sigma of 0.02
 H9B-H9A
 1.38 with sigma of 0.04
 C11-C15 \\sim C11-N1 \\sim C15-N1
 with sigma of 0.02
 C10-C11 \\sim C10-C15
 with sigma of 0.01
 C10-H11A \\sim C10-H11B \\sim C10-C12
 with sigma of 0.02
 C15-C10 \\sim C15-N2
 with sigma of 0.01
 C14-C15 \\sim C14-C50
 with sigma of 0.01
 C14-C15 \\sim C14-C50 \\sim C14-C13
 with sigma of 0.01
 C12-C11 \\sim C12-C50
 with sigma of 0.01
 Dy1-H9B \\sim Dy1-H9A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C49) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C13) \\sim Ueq, Uanis(C50) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Others
 Fixed Sof: H14A(0.875) H14B(0.875) C23(0.8) H23A(0.8) H23B(0.8) H23C(0.8)
 O300(0.8) H30A(0.8) H30B(0.8) O400(0.6) H40A(0.6) H40B(0.6) O11(0.6) H11C(0.6)
 H11D(0.6) C49(0.2) H49A(0.2) H49B(0.2) H49C(0.2) C50(0.85) C13(0.15)
 H13A(0.15) H13B(0.15)
 Fixed U11: O400(0.087113) O11(0.095637)
 Fixed U22: O400(0.1013) O11(0.12055)
 Fixed U33: O400(0.10898) O11(0.08622)
 Fixed X: H20A(0.84994)
 Fixed Y: H20A(0.71151)
 Fixed Z: H20A(0.19972)
5.a Free rotating group:
 O100(H10A,H10B,O200,H200,O300,H30A,H30B,O400,H40A,H40B,O11,H11C,H11D)
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), C14(H14A,H14B), C35(H35A,H35B), C36(H36A,
 H36B), C37(H37A,H37B), C38(H38A,H38B), C50(H50A,H50B), C13(H13A,H13B)
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), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              68483
_shelx_hkl_checksum              17464
_olex2_submission_special_instructions 'No special instructions were received'