Aggregation of [Ln] clusters by the dianion of 3-formylsalicylic acid. Synthesis, crystal structures, magnetic and luminescence properties.
Dinca, Alina S.; Mindru, Alexei; Dragancea, Diana; Tiseanu, Carmen; Shova, Sergiu; Cornia, Samuele; Carrella, Luca M.; Rentschler, Eva; Affronte, Marco; Andruh, Marius; Dalton transactions (Cambridge, England : 2003) 48 (2019) 1700–1708; doi:10.1039/c8dt04602f

data_7048540
_publ_section_title
;
 Aggregation of [Ln] clusters by the dianion of 3-formylsalicylic acid.
 Synthesis, crystal structures, magnetic and luminescence properties.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1700
_journal_page_last               1708
_journal_paper_doi               10.1039/c8dt04602f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C132 H144 Dy12 N12 O72, 3.5(C3 H7 N O)'
_chemical_formula_sum            'C142.5 H168.5 Dy12 N15.5 O75.5'
_chemical_formula_weight         5256.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-02-24 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                71.221(3)
_cell_angle_beta                 84.773(3)
_cell_angle_gamma                87.821(3)
_cell_formula_units_Z            1
_cell_length_a                   17.0435(6)
_cell_length_b                   17.1107(5)
_cell_length_c                   17.8280(6)
_cell_measurement_reflns_used    8690
_cell_measurement_temperature    199.95(10)
_cell_measurement_theta_max      28.0070
_cell_measurement_theta_min      1.5270
_cell_volume                     4901.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      199.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1593
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      1.00  85.00   1.00   30.00    --   17.71  57.00  90.00   84
  2  \w     60.00  85.00   1.00   30.00    --   17.71  57.00 120.00   25
  3  \w     35.00  70.00   1.00   30.00    --   17.71 178.00 -30.00   35
  4  \w     36.00  61.00   1.00   30.00    --   17.71 178.00-120.00   25
  5  \w     11.00  38.00   1.00   30.00    --   17.71  57.00-150.00   27
  6  \w    -43.00  25.00   1.00   30.00    --   17.71 -77.00-150.00   68
  7  \w    -17.00  23.00   1.00   30.00    --  -15.44 -99.00-150.00   40
  8  \w     47.00  72.00   1.00   30.00    --   17.71-178.00-150.00   25
  9  \w     -6.00  21.00   1.00   30.00    --  -15.44 -99.00  90.00   27
 10  \w    -50.00  44.00   1.00   30.00    --   17.71 -77.00 -30.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0401017000
_diffrn_orient_matrix_UB_12      -0.0022838000
_diffrn_orient_matrix_UB_13      0.0151348000
_diffrn_orient_matrix_UB_21      0.0112903000
_diffrn_orient_matrix_UB_22      0.0032102000
_diffrn_orient_matrix_UB_23      0.0362122000
_diffrn_orient_matrix_UB_31      -0.0033181000
_diffrn_orient_matrix_UB_32      0.0436086000
_diffrn_orient_matrix_UB_33      -0.0154232000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_unetI/netI     0.0970
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41006
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.632
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.596
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.781
_exptl_crystal_description       prism
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.117
_refine_diff_density_min         -1.616
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1075
_refine_ls_number_reflns         17250
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0639P)^2^+0.5219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1473
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11809
_reflns_number_total             17250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04602f2.cif
_cod_data_source_block           shi_3062_dili
_cod_depositor_comments
'Adding full bibliography for 7048539--7048541.cif.'
_cod_original_formula_sum        'C142.50 H168.50 Dy12 N15.50 O75.50'
_cod_database_code               7048540
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C35 H40 N4 O8 Dy1'
_chemical_oxdiff_usercomment     'DD18-65B = DD18-78'
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C57X-C56X
 2.5 with sigma of 0.01
 O33-C55 = O33-C55X
 1.2 with sigma of 0.01
 N3-C55 = N3X-C55X
 1.4 with sigma of 0.01
 N3-C57 = N3X-C57X = N3-C56 = N3X-C56X
 1.48 with sigma of 0.01
 C62X-C61X \\sim C61X-C63X
 with sigma of 0.01
 O35-C61 \\sim O35-C61
 with sigma of 0.01
 C63-C61 \\sim C61-C62
 with sigma of 0.01
 O35-C61X \\sim O35-C61
 with sigma of 0.01
 N5X-C61 \\sim N5X-C61
 with sigma of 0.01
 N5X-C61X \\sim N5-C61
 with sigma of 0.01
 N5X-C63X \\sim N5-C63 \\sim N5X-C62X \\sim N5-C62
 with sigma of 0.01
 C56-C55 \\sim C55-C57
 with sigma of 0.01
 C56X-C55X \\sim C55X-C57X
 with sigma of 0.01
3. Restrained planarity
 N3X, C55X, C56X, C57X
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uiso(C61) = Uiso(C61X)
Uiso(C61X) = Uiso(C61) = Uiso(C63X) = Uiso(C63) = Uiso(C62X) = Uiso(C62)
Uiso(N3) = Uiso(N3X)
Uiso(N5) = Uiso(N5X)
Uanis(C70) = Uanis(C72) = Uanis(C71)
Uiso(C55X) = Uiso(C55) = Uiso(C57X) = Uiso(C56X) = Uiso(C56) = Uiso(C57)
Uiso(C70X) = Uiso(C72X) = Uiso(C71X)
5. Others
 Sof(C70X)=Sof(H70X)=Sof(C71X)=Sof(H71D)=Sof(H71E)=Sof(H71F)=Sof(C72X)=
 Sof(H72D)=Sof(H72E)=Sof(H72F)=1-FVAR(1)
 Sof(C70)=Sof(H70)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=Sof(C72)=Sof(H72A)=
 Sof(H72B)=Sof(H72C)=FVAR(1)
 Sof(N5X)=Sof(C61X)=Sof(H61X)=Sof(C62X)=Sof(H62D)=Sof(H62E)=Sof(H62F)=
 Sof(C63X)=Sof(H63D)=Sof(H63E)=Sof(H63F)=1-FVAR(2)
 Sof(N5)=Sof(C61)=Sof(H61)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=Sof(C63)=
 Sof(H63A)=Sof(H63B)=Sof(H63C)=FVAR(2)
 Sof(N3X)=Sof(C55X)=Sof(H55X)=Sof(C56X)=Sof(H56D)=Sof(H56E)=Sof(H56F)=
 Sof(C57X)=Sof(H57D)=Sof(H57E)=Sof(H57F)=1-FVAR(3)
 Sof(N3)=Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(C57)=
 Sof(H57A)=Sof(H57B)=Sof(H57C)=FVAR(3)
 Fixed Sof: O37(0.75) N7(0.75) C67(0.75) H67(0.75) C68(0.75) H68A(0.75)
 H68B(0.75) H68C(0.75) C69(0.75) H69A(0.75) H69B(0.75) H69C(0.75)
6.a Riding coordinates:
 O1(H1), O2(H2), O3(H3), O4(H4), O5(H5), O6(H6), C50(H50A,H50B,H50C), C51(H51A,
 H51B,H51C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C),
 C56X(H56D,H56E,H56F), C57(H57A,H57B,H57C), C57X(H57D,H57E,H57F), C59(H59A,H59B,
 H59C), C62(H62A,H62B,H62C), C62X(H62D,H62E,H62F), C63(H63A,H63B,H63C),
 C63X(H63D,H63E,H63F), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C71X(H71D,H71E,
 H71F), C72(H72A,H72B,H72C), C72X(H72D,H72E,H72F), C68(H68A,H68B,H68C),
 C69(H69A,H69B,H69C)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5A), C6(H6A), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13), C16(H16),
 C19(H19), C20(H20), C21(H21), C24(H24), C27(H27), C28(H28), C29(H29), C32(H32),
  C35(H35), C36(H36), C37(H37), C40(H40), C43(H43), C44(H44), C45(H45),
 C48(H48), C49(H49), C52(H52), C55(H55), C55X(H55X), C58(H58), C61(H61),
 C61X(H61X), C64(H64), C70(H70), C70X(H70X), C67(H67)
6.c Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C71(H71A,H71B,H71C)
;
_olex2_date_sample_data_collection 2016-01-11
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.749
_oxdiff_exptl_absorpt_empirical_full_min 0.762