Mononuclear lanthanide(III)-oxamate complexes as new photoluminescent field-induced single-molecule magnets: solid-state photophysical and magnetic properties.
Vaz, Raphael C. A.; Esteves, Isabela O.; Oliveira, Willian X. C.; Honorato, João; Martins, Felipe T.; Marques, Lippy F.; Dos Santos, Guilherme L.; Freire, Ricardo O.; Jesus, Larissa T.; Pedroso, Emerson F.; Nunes, Wallace C.; Julve, Miguel; Pereira, Cynthia L. M.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 16106–16124; doi:10.1039/d0dt02497j

data_7704948
_publ_section_title
;
 Mononuclear lanthanide(III)-oxamate complexes as new photoluminescent
 field-induced single-molecule magnets: solid-state photophysical and
 magnetic properties.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16106
_journal_page_last               16124
_journal_paper_doi               10.1039/d0dt02497j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C34 H26 Dy F4 N4 O13 S, 2(H2 O), C16 H36 N'
_chemical_formula_sum            'C50 H66 Dy F4 N5 O15 S'
_chemical_formula_weight         1247.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-04-30
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.04.02 svn.r1fbe7b6f for OlexSys, GUI svn.r6076)
;
_audit_update_record
;
2020-05-07 deposited with the CCDC.	2020-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                74.941(3)
_cell_angle_beta                 89.817(3)
_cell_angle_gamma                61.784(4)
_cell_formula_units_Z            2
_cell_length_a                   14.2143(5)
_cell_length_b                   14.5314(6)
_cell_length_c                   16.1788(5)
_cell_measurement_reflns_used    43700
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.682
_cell_measurement_theta_min      2.634
_cell_volume                     2815.3(2)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX2 CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43987
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.750
_diffrn_reflns_theta_min         2.634
_exptl_absorpt_coefficient_mu    1.445
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_correction_T_min  0.773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Multi-scan (SADABS; Krause et al., 2015)'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       plate
_exptl_crystal_F_000             1278
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.941
_refine_diff_density_min         -1.332
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         10769
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.203
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0436P)^2^+7.5024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1231
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9351
_reflns_number_total             10769
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02497j2.cif
_cod_data_source_block           3_F
_cod_depositor_comments
'Adding full bibliography for 7704941--7704948.cif.'
_cod_database_code               7704948
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.473
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C9T-C10T = C11T-C10T = C6-C4 = C12T-C11T = C2T-C1T = C2T'-C1T' = C2T'-C3T' =
 C4T-C3T = C4T'-C3T' = C3T-C2T = C15T-C14T = C2-C1 = C2-C5 = C3-C1 = C14T-C13T =
  C5T'-C6T' = C6T-C5T = C7T'-C6T' = C7T'-C8T' = C8T-C7T = C7T-C6T
 1.54 with sigma of 0.01
 S2S-C1S = S1-C1S = S2S-C2S = S1-C2S
 1.77 with sigma of 0.02
 S2S-O1S = S1-O1S
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C9T) = Uanis(C9T') = Uanis(C1T') = Uanis(C1T) = Uanis(C5T) = Uanis(C5T')
= Uanis(C13T) = Uanis(C3)
Uanis(C2T) = Uanis(C2T') = Uanis(C14T) = Uanis(C1) = Uanis(C10T) = Uanis(C6T) =
Uanis(C6T')
Uanis(C4T) = Uanis(C4T') = Uanis(C12T) = Uanis(C6) = Uanis(C5) = Uanis(C16T) =
Uanis(C8T) = Uanis(C8T')
Uanis(C11T) = Uanis(C4) = Uanis(C2) = Uanis(C15T) = Uanis(C3T) = Uanis(C3T') =
Uanis(C7T) = Uanis(C7T')
4. Others
 Sof(C4T)=Sof(H4TA)=Sof(H4TB)=Sof(H4TC)=1-FVAR(1)
 Sof(C4T')=Sof(H4TD)=Sof(H4TE)=Sof(H4TF)=FVAR(1)
 Fixed Sof: S1(0.88) S2S(0.12) H1SA(0.8) H1SB(0.8) H1SC(0.8) H1SD(0.2)
 H1SE(0.2) H1SF(0.2) H2SA(0.8) H2SB(0.8) H2SC(0.8) H2SD(0.2) H2SE(0.2)
 H2SF(0.2) C1(0.5) H1A(0.5) H1B(0.5) C1T(0.5) H1TA(0.5) H1TB(0.5) C1T'(0.5)
 H1TC(0.5) H1TD(0.5) C2(0.5) H2A(0.5) H2B(0.5) C2T(0.5) H2TA(0.5) H2TB(0.5)
 C2T'(0.5) H2TC(0.5) H2TD(0.5) C3(0.5) H3A(0.5) H3B(0.5) C3T(0.5) H3TA(0.5)
 H3TB(0.5) C3T'(0.5) H3TC(0.5) H3TD(0.5) C4(0.5) H4A(0.5) H4B(0.5) C5(0.5)
 H5A(0.5) H5B(0.5) H5C(0.5) C5T(0.5) H5TA(0.5) H5TB(0.5) C5T'(0.5) H5TC(0.5)
 H5TD(0.5) C6(0.5) H6A(0.5) H6B(0.5) H6C(0.5) C6T(0.5) H6TA(0.5) H6TB(0.5)
 C6T'(0.5) H6TC(0.5) H6TD(0.5) C7T(0.5) H7TA(0.5) H7TB(0.5) C7T'(0.5) H7TC(0.5)
 H7TD(0.5) C8T(0.5) H8TA(0.5) H8TB(0.5) H8TC(0.5) C8T'(0.5) H8TD(0.5) H8TE(0.5)
 H8TF(0.5) C9T(0.5) H9TA(0.5) H9TB(0.5) C9T'(0.5) H9TC(0.5) H9TD(0.5) H10A(0.5)
 H10B(0.5) H10C(0.5) H10D(0.5) C11T(0.5) H11A(0.5) H11B(0.5) C12T(0.5)
 H12A(0.5) H12B(0.5) H12C(0.5) C13T(0.5) H13A(0.5) H13B(0.5) C14T(0.5)
 H14A(0.5) H14B(0.5) C15T(0.5) H15A(0.5) H15B(0.5) C16T(0.5) H16A(0.5)
 H16B(0.5) H16C(0.5)
5.a Free rotating group:
 O1X(H1XA,H1XB), O2W(H2WA,H2WB)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C1T(H1TA,H1TB), C1T'(H1TC,H1TD), C2(H2A,H2B), C2T(H2TA,H2TB),
 C2T'(H2TC,H2TD), C3(H3A,H3B), C3T(H3TA,H3TB), C3T'(H3TC,H3TD), C4(H4A,H4B),
 C5T(H5TA,H5TB), C5T'(H5TC,H5TD), C6T(H6TA,H6TB), C6T'(H6TC,H6TD), C7T(H7TA,
 H7TB), C7T'(H7TC,H7TD), C9T(H9TA,H9TB), C9T'(H9TC,H9TD), C10T(H10A,H10B),
 C10T(H10C,H10D), C11T(H11A,H11B), C13T(H13A,H13B), C14T(H14A,H14B), C15T(H15A,
 H15B)
5.c Aromatic/amide H refined with riding coordinates:
 N1A(H1AA), N1B(H1BA), N1C(H1C), N1D(H1D), C4C(H4C), C5C(H5CA), C7C(H7C),
 C8C(H8C), C8D(H8D), C7D(H7D), C5D(H5D), C4D(H4D), C4B(H4BA), C5B(H5BA),
 C7B(H7B), C8B(H8B), C8A(H8A), C4A(H4AA), C5A(H5AA), C7A(H7A)
5.d Fitted hexagon refined as free rotating group:
 C3C(C4C,C5C,C6C,C7C,C8C), C3D(C8D,C7D,C6D,C5D,C4D), C4B(C5B,C6B,C7B,C8B,C3B),
 C8A(C3A,C4A,C5A,C6A,C7A)
5.e Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC), C1S(H1SD,H1SE,H1SF), C2S(H2SA,H2SB,H2SC), C2S(H2SD,H2SE,
 H2SF), C4T(H4TA,H4TB,H4TC), C4T'(H4TD,H4TE,H4TF), C5(H5A,H5B,H5C), C6(H6A,H6B,
 H6C), C8T(H8TA,H8TB,H8TC), C8T'(H8TD,H8TE,H8TF), C12T(H12A,H12B,H12C),
 C16T(H16A,H16B,H16C)
;
_shelx_res_checksum              19176
_olex2_submission_special_instructions 'No special instructions were received'