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_7715904
_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 N5 O13 Tb, C17 H16 Cu N2 O3'
_chemical_formula_sum            'C33.998 H33.998 Cu2 N7 O16 Tb'
_chemical_formula_weight         1082.671
_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     dual
_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                 102.026(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2030(9)
_cell_length_b                   21.1661(17)
_cell_length_c                   18.4262(16)
_cell_measurement_reflns_used    6788
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.26
_cell_volume                     3891.9(6)
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.9928
_diffrn_measured_fraction_theta_max 0.9928
_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  0.0458
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_Laue_measured_fraction_full 0.9928
_diffrn_reflns_Laue_measured_fraction_max 0.9928
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19928
_diffrn_reflns_point_group_measured_fraction_full 0.9928
_diffrn_reflns_point_group_measured_fraction_max 0.9928
_diffrn_reflns_theta_full        24.9999
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    2.963
_exptl_absorpt_correction_T_max  0.685
_exptl_absorpt_correction_T_min  0.320
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_description       block
_exptl_crystal_F_000             2155.968
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.9269
_refine_diff_density_min         -1.7956
_refine_diff_density_rms         0.3302
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             9.0109
_refine_ls_goodness_of_fit_ref   1.0841
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    102
_refine_ls_number_parameters     692
_refine_ls_number_reflns         6788
_refine_ls_number_restraints     832
_refine_ls_restrained_S_all      1.0170
_refine_ls_R_factor_all          0.1537
_refine_ls_R_factor_gt           0.1207
_refine_ls_shift/su_max          -0.0015
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+193.7704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2666
_refine_ls_wR_factor_ref         0.2875
_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                4876
_reflns_number_total             6788
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt00304g2.cif
_cod_data_source_block           2Tb
_cod_depositor_comments
'Adding full bibliography for 7715903--7715905.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7715904
_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,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-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
 O331-C332 \\sim O3-C3
 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
 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
 C38-N39 \\sim C38A-N39A
 with sigma of 0.02
 C37-C35 \\sim C37A-C35A
 with sigma of 0.04
 N39-C40 \\sim N39A-C4
 with sigma of 0.02
 C37-N39 \\sim C37A-N39A
 with sigma of 0.04
 C40-C41 \\sim C4-C1
 with sigma of 0.02
 C32-C34 \\sim C32A-C34A
 with sigma of 0.04
 C41-N42 \\sim C1-N42A
 with sigma of 0.02
 C32-C36 \\sim C32A-C36A
 with sigma of 0.04
 N42-C43 \\sim N42A-C43A
 with sigma of 0.02
 C32-C38 \\sim C32A-C38A
 with sigma of 0.04
 C33A-C35 \\sim C33B-C35A
 with sigma of 0.04
 C43-C44 \\sim C43A-C44A
 with sigma of 0.02
 C34-C36 \\sim C34A-C36A
 with sigma of 0.04
 C44-C45 \\sim C44A-C45A
 with sigma of 0.02
 C44-C49 \\sim C44A-C49A
 with sigma of 0.02
 C36-C38 \\sim C36A-C38A
 with sigma of 0.04
 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
 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 0.05 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 0.05 and sigma for terminal
atoms of 0.01
Uanis(O331) \\sim Ueq, Uanis(C332) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.01
Uanis(C35) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C33A) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
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
Uanis(C48B) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.01
Uanis(Tb1b) = Uanis(Tb1a)
4. Rigid body (RIGU) restrains
 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
 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
 O11, C12, C13, C17, C14, C16, C18, C15, N19, 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
5. Others
 Sof(Tb1b)=Sof(H1Wc)=Sof(H1Wd)=1-FVAR(1)
 Sof(H1Wa)=Sof(H1Wb)=Sof(Tb1a)=FVAR(1)
 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:
 O1W(H1Wc,H1Wd), O1W(H1Wa,H1Wb), C4(H4a,H4b), C1(H1a,H1b), C2(H2a,H2b), C5(H5a,
 H5b)
6.b Secondary CH2 refined with riding coordinates:
 C20(H20a,H20b), C21(H21a,H21b), C40(H40a,H40b), C41(H41a,H41b)
6.c 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.d 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.e 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'