Cu(II)-Ln(III) (Ln = Gd, Tb and Dy) complexes of an unsymmetrical N<sub>2</sub>O<sub>3</sub> donor ligand: field induced SMM behaviour of Cu(II)-Tb(III) complexes.
Bhunia, Pradip; Maity, Souvik; Ghosh, Tanmoy Kumar; Mondal, Arpan; Mayans, Júlia; Ghosh, Ashutosh; Dalton transactions (Cambridge, England : 2003) 53 (2024) 9171–9182; doi:10.1039/d4dt00304g

data_7715905
_publ_section_title
;
 Cu(II)-Ln(III) (Ln = Gd, Tb and Dy) complexes of an unsymmetrical
 N<sub>2</sub>O<sub>3</sub> donor ligand: field induced SMM behaviour of
 Cu(II)-Tb(III) complexes.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9171
_journal_page_last               9182
_journal_paper_doi               10.1039/d4dt00304g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C16.998 H17.998 Cu Dy N5 O13, C17 H16 Cu N2 O3'
_chemical_formula_sum            'C33.998 H33.998 Cu2 Dy N7 O16'
_chemical_formula_weight         1086.242
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-01-14
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6380)
;
_audit_update_record
;
2024-04-19 deposited with the CCDC.	2024-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.830(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2493(10)
_cell_length_b                   21.151(2)
_cell_length_c                   18.4526(18)
_cell_measurement_reflns_used    6855
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.26
_cell_volume                     3915.2(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.9958
_diffrn_measured_fraction_theta_max 0.9958
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_unetI/netI     0.0732
_diffrn_reflns_Laue_measured_fraction_full 0.9958
_diffrn_reflns_Laue_measured_fraction_max 0.9958
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28624
_diffrn_reflns_point_group_measured_fraction_full 0.9958
_diffrn_reflns_point_group_measured_fraction_max 0.9958
_diffrn_reflns_theta_full        24.9988
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    3.047
_exptl_absorpt_correction_T_max  0.615
_exptl_absorpt_correction_T_min  0.330
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_description       block
_exptl_crystal_F_000             2159.955
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.16
_refine_diff_density_max         3.0056
_refine_diff_density_min         -4.0679
_refine_diff_density_rms         0.2629
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             9.0303
_refine_ls_goodness_of_fit_ref   1.0843
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    97
_refine_ls_number_parameters     689
_refine_ls_number_reflns         6856
_refine_ls_number_restraints     658
_refine_ls_restrained_S_all      1.0308
_refine_ls_R_factor_all          0.1367
_refine_ls_R_factor_gt           0.0982
_refine_ls_shift/su_max          0.0014
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+83.1994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2133
_refine_ls_wR_factor_ref         0.2372
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -12
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              -8
_reflns_number_gt                4725
_reflns_number_total             6856
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt00304g2.cif
_cod_data_source_block           3Dy
_cod_depositor_comments
'Adding full bibliography for 7715903--7715905.cif.'
_cod_original_cell_volume        3915.3(7)
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7715905
_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,H) groups
2. Restrained distances
 C33A-O331
 1.35 with sigma of 0.02
 O331-C332
 1.4 with sigma of 0.02
 C41-C40
 1.457 with sigma of 0.01
 C1-C4
 1.457 with sigma of 0.01
 C2-C1
 1.457 with sigma of 0.01
 O31-C32 \\sim O31A-C32A
 with sigma of 0.02
 O331-C332 \\sim O3-C3
 with sigma of 0.02
 O331-C33A \\sim O3-C33B
 with sigma of 0.02
 C37-C32 \\sim C37A-C32A
 with sigma of 0.02
 C37-C36 \\sim C37A-C36A
 with sigma of 0.02
 C37-C38 \\sim C37A-C38A
 with sigma of 0.02
 C32-C33A \\sim C32A-C33B
 with sigma of 0.02
 C33A-C34 \\sim C33B-C34A
 with sigma of 0.02
 C34-C35 \\sim C34A-C35A
 with sigma of 0.02
 C35-C36 \\sim C35A-C36A
 with sigma of 0.02
 C38-N39 \\sim C38A-N39A
 with sigma of 0.02
 N39-C40 \\sim N39A-C4
 with sigma of 0.02
 C40-C41 \\sim C4-C1
 with sigma of 0.02
 C41-N42 \\sim C1-N42A
 with sigma of 0.02
 N42-C43 \\sim N42A-C43A
 with sigma of 0.02
 C43-C44 \\sim C43A-C44A
 with sigma of 0.02
 C44-C45 \\sim C44A-C45A
 with sigma of 0.02
 C44-C49 \\sim C44A-C49A
 with sigma of 0.02
 C45-C46 \\sim C45A-C46A
 with sigma of 0.02
 C46-C47 \\sim C46A-C47A
 with sigma of 0.02
 C47-C48B \\sim C47A-C48C
 with sigma of 0.02
 C48B-C49 \\sim C48C-C49A
 with sigma of 0.02
 C49-O50 \\sim C49A-O50A
 with sigma of 0.02
 O31-C37 \\sim O31A-C37A
 with sigma of 0.04
 O31-C33A \\sim O31A-C33B
 with sigma of 0.04
 O331-C32 \\sim O3-C32A
 with sigma of 0.04
 O331-C34 \\sim O3-C34A
 with sigma of 0.04
 C332-C33A \\sim C3-C33B
 with sigma of 0.04
 C37-C33A \\sim C37A-C33B
 with sigma of 0.04
 C37-C35 \\sim C37A-C35A
 with sigma of 0.04
 C37-N39 \\sim C37A-N39A
 with sigma of 0.04
 C32-C34 \\sim C32A-C34A
 with sigma of 0.04
 C32-C36 \\sim C32A-C36A
 with sigma of 0.04
 C32-C38 \\sim C32A-C38A
 with sigma of 0.04
 C33A-C35 \\sim C33B-C35A
 with sigma of 0.04
 C34-C36 \\sim C34A-C36A
 with sigma of 0.04
 C36-C38 \\sim C36A-C38A
 with sigma of 0.04
 C38-C40 \\sim C38A-C4
 with sigma of 0.04
 N39-C41 \\sim N39A-C1
 with sigma of 0.04
 C40-N42 \\sim C4-N42A
 with sigma of 0.04
 C41-C43 \\sim C1-C43A
 with sigma of 0.04
 N42-C44 \\sim N42A-C44A
 with sigma of 0.04
 C43-C45 \\sim C43A-C45A
 with sigma of 0.04
 C43-C49 \\sim C43A-C49A
 with sigma of 0.04
 C44-C46 \\sim C44A-C46A
 with sigma of 0.04
 C44-C48B \\sim C44A-C48C
 with sigma of 0.04
 C44-O50 \\sim C44A-O50A
 with sigma of 0.04
 C45-C47 \\sim C45A-C47A
 with sigma of 0.04
 C45-C49 \\sim C45A-C49A
 with sigma of 0.04
 C46-C48B \\sim C46A-C48C
 with sigma of 0.04
 C47-C49 \\sim C47A-C49A
 with sigma of 0.04
 C48B-O50 \\sim C48C-O50A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq, Uanis(C38) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C33A) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C40) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46)
\\sim Ueq, Uanis(C47) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(O331) \\sim Ueq, Uanis(C332) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O50A) \\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(O31A) \\sim Ueq, Uanis(O50)
\\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
4. Rigid body (RIGU) restrains
 N19, O11, C12, C13, C17, C14, C16, C18, C15, C20, C21, N22, C23, C24, C25,
 C29, C26, C28, O30, C27, O281, C282
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, O31A, C32A, C37A, C33B, C36A, C38A, C34A, O3, C35A, N39A, C4, C1, N42A,
 C43A, C44A, C45A, C49A, C46A, C48C, O50A, C47A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C47, O31, C32, C37, C33A, C36, C38, O331, C34, C35, N39, C332, C40, C41, N42,
 C43, C44, C45, C49, C46, C48B, O50
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O31(0.3333) O331(0.3333) C332(0.3333) H33a(0.3333) H33b(0.3333)
 H33c(0.3333) C37(0.3333) C32(0.3333) C33A(0.3333) C34(0.3333) H34(0.3333)
 C35(0.3333) H35(0.3333) C36(0.3333) H36(0.3333) C38(0.3333) H38(0.3333)
 N39(0.3333) C40(0.3333) H40a(0.3333) H40b(0.3333) C41(0.3333) H41a(0.3333)
 H41b(0.3333) N42(0.3333) C43(0.3333) H43(0.3333) C44(0.3333) C45(0.3333)
 H45(0.3333) C46(0.3333) H46(0.3333) C47(0.3333) H47(0.3333) C48B(0.3333)
 H48B(0.3333) C49(0.3333) O50(0.3333) O31A(0.6666) C37A(0.6666) C32A(0.6666)
 C33B(0.6666) C34A(0.6666) H34A(0.6666) C35A(0.6666) H35A(0.6666) C36A(0.6666)
 H36A(0.6666) C38A(0.6666) H38A(0.6666) O3(0.6666) N39A(0.6666) C3(0.6666)
 H3a(0.6666) H3b(0.6666) H3c(0.6666) C4(0.3333) H4a(0.3333) H4b(0.3333)
 C1(0.3333) H1a(0.3333) H1b(0.3333) N42A(0.6666) C43A(0.6666) H43A(0.6666)
 C44A(0.6666) C45A(0.6666) H45A(0.6666) C46A(0.6666) H46A(0.6666) C47A(0.6666)
 H47A(0.6666) C48C(0.6666) H48C(0.6666) C49A(0.6666) O50A(0.6666) C2(0.3333)
 H2a(0.3333) H2b(0.3333) C5(0.3333) H5a(0.3333) H5b(0.3333)
 Fixed Uiso: C4(0.08) C1(0.08) C2(0.08) C5(0.08)
6.a Riding coordinates:
 C4(H4a,H4b), C1(H1a,H1b), C2(H2a,H2b), C5(H5a,H5b)
6.b Rotating group:
 O1W(H1Wa,H1Wb)
6.c Secondary CH2 refined with riding coordinates:
 C20(H20a,H20b), C21(H21a,H21b), C40(H40a,H40b), C41(H41a,H41b)
6.d Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C23(H23), C25(H25),
 C26(H26), C27(H27), C34(H34), C35(H35), C36(H36), C38(H38), C43(H43), C45(H45),
  C46(H46), C47(H47), C48B(H48B), C34A(H34A), C35A(H35A), C36A(H36A),
 C38A(H38A), C43A(H43A), C45A(H45A), C46A(H46A), C47A(H47A), C48C(H48C)
6.e Fitted hexagon refined as free rotating group:
 C37(C32,C33A,C34,C35,C36), C44(C45,C46,C47,C48B,C49), C37A(C32A,C33B,C34A,
 C35A,C36A), C44A(C45A,C46A,C47A,C48C,C49A)
6.f Idealised Me refined as rotating group:
 C282(H28a,H28b,H28c), C332(H33a,H33b,H33c), C3(H3a,H3b,H3c)
;
_olex2_submission_special_instructions 'No special instructions were received'