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_7048539
_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 Eu12 N12 O72, 4(C3 H7 N O)'
_chemical_formula_sum            'C144 H172 Eu12 N16 O76'
_chemical_formula_weight         5166.50
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-02-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-24 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                70.087(4)
_cell_angle_beta                 87.863(3)
_cell_angle_gamma                86.218(3)
_cell_formula_units_Z            1
_cell_length_a                   17.1451(6)
_cell_length_b                   17.1531(7)
_cell_length_c                   17.7334(7)
_cell_measurement_reflns_used    12741
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      28.7560
_cell_measurement_theta_min      1.7090
_cell_volume                     4892.1(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  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1593
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -12.00  72.00   1.00   20.00    --   17.71  19.00  30.00   84
  2  \w      2.00  80.00   1.00   20.00    --   17.71  57.00 -90.00   78
  3  \w    -18.00  16.00   1.00   20.00    --   17.71 -57.00-150.00   34
  4  \w      3.00  43.00   1.00   20.00    --   17.71 -77.00 -60.00   40
  5  \w     -1.00  44.00   1.00   20.00    --   17.71 -77.00   0.00   45
  6  \w     -8.00  24.00   1.00   20.00    --  -15.44 -99.00 120.00   32
  7  \w      2.00  79.00   1.00   20.00    --   17.71  57.00 120.00   77
  8  \w    -20.00   5.00   1.00   20.00    --  -15.44 -99.00  30.00   25
  9  \w    -50.00  26.00   1.00   20.00    --   17.71 -57.00-180.00   76
;
_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      0.0241673000
_diffrn_orient_matrix_UB_12      0.0278904000
_diffrn_orient_matrix_UB_13      -0.0286105000
_diffrn_orient_matrix_UB_21      0.0329740000
_diffrn_orient_matrix_UB_22      -0.0174176000
_diffrn_orient_matrix_UB_23      0.0243281000
_diffrn_orient_matrix_UB_31      0.0069335000
_diffrn_orient_matrix_UB_32      -0.0293136000
_diffrn_orient_matrix_UB_33      -0.0199953000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41593
_diffrn_reflns_theta_full        24.41
_diffrn_reflns_theta_max         24.41
_diffrn_reflns_theta_min         1.69
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.870
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41518
_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 dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.753
_refine_diff_density_min         -1.485
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         16003
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+47.8946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1452
_reflns_number_gt                11930
_reflns_number_total             16003
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt04602f2.cif
_cod_data_source_block           shi_3042_maan_1
_cod_depositor_comments
'Adding full bibliography for 7048539--7048541.cif.'
_cod_database_code               7048539
_chemical_oxdiff_formula         'C30 H30 N2 O6 Eu1'
_chemical_oxdiff_usercomment     R_99
_reflns_odcompleteness_completeness 99.94
_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
 O32-C70 = O32X-C70X
 1.2 with sigma of 0.01
 O32X-C70X \\sim O32-C70
 with sigma of 0.01
 N8-C70 \\sim N8-C70X
 with sigma of 0.01
 Eu5-O29 \\sim Eu5-O29X
 with sigma of 0.01
 O29X-C61X \\sim O29-C61
 with sigma of 0.01
 N5-C61 \\sim N5X-C61X
 with sigma of 0.01
 N5X-C62X \\sim N5-C63 \\sim N5X-C63X \\sim N5-C62
 with sigma of 0.01
 Eu5-O28X \\sim Eu5-O28
 with sigma of 0.01
 O28-C58 \\sim O28X-C58X
 with sigma of 0.01
 N4-C58 \\sim N4X-C58X
 with sigma of 0.01
 N4X-C59X \\sim N4-C59 \\sim N4-C60 \\sim N4X-C60X
 with sigma of 0.01
 Eu3-O27X \\sim Eu3-O27
 with sigma of 0.01
 O27X-C55X \\sim O27-C55
 with sigma of 0.01
 N3X-C55X \\sim N3-C55
 with sigma of 0.01
 N3-C56 \\sim N3X-C57X \\sim N3-C57 \\sim N3X-C56X
 with sigma of 0.01
 N8-C72X \\sim N8-C72 \\sim N8-C71X \\sim N8-C71
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C67X) = Uanis(C67) = Uanis(C69X) = Uanis(C68) = Uanis(C68X) = Uanis(C69)
Uiso(C51) = Uiso(C49X) = Uiso(C49) = Uiso(C50X) = Uiso(C50) = Uiso(C51X)
Uiso(C58) = Uiso(C58X) = Uiso(C59) = Uiso(C59X) = Uiso(N4) = Uiso(N4X) =
Uiso(C60) = Uiso(C60X)
Uiso(O28) = Uiso(O28X)
Uiso(O27) = Uiso(O27X)
Uiso(C55X) = Uiso(C55) = Uiso(N3X) = Uiso(N3) = Uiso(C56) = Uiso(C57X) =
Uiso(C57) = Uiso(C56X)
Uiso(O32) = Uiso(O32X) = Uiso(C70) = Uiso(C70X) = Uiso(C71) = Uiso(C71X) =
Uiso(C72) = Uiso(C72X)
4. Others
 Sof(O29)=Sof(N5)=Sof(C61)=Sof(H61)=Sof(C62)=Sof(H62D)=Sof(H62E)=Sof(H62F)=
 Sof(C63)=Sof(H63D)=Sof(H63E)=Sof(H63F)=1-FVAR(1)
 Sof(O29X)=Sof(N5X)=Sof(C61X)=Sof(H61X)=Sof(C62X)=Sof(H62A)=Sof(H62B)=
 Sof(H62C)=Sof(C63X)=Sof(H63A)=Sof(H63B)=Sof(H63C)=FVAR(1)
 Sof(O28X)=Sof(N4X)=Sof(C58X)=Sof(H58X)=Sof(C59X)=Sof(H59D)=Sof(H59E)=
 Sof(H59F)=Sof(C60X)=Sof(H60D)=Sof(H60E)=Sof(H60F)=1-FVAR(2)
 Sof(O28)=Sof(N4)=Sof(C58)=Sof(H58)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=
 Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=FVAR(2)
 Sof(O27)=Sof(N3)=Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56D)=Sof(H56E)=Sof(H56F)=
 Sof(C57)=Sof(H57D)=Sof(H57E)=Sof(H57F)=1-FVAR(3)
 Sof(O27X)=Sof(N3X)=Sof(C55X)=Sof(H55X)=Sof(C56X)=Sof(H56A)=Sof(H56B)=
 Sof(H56C)=Sof(C57X)=Sof(H57A)=Sof(H57B)=Sof(H57C)=FVAR(3)
 Fixed Sof: C49X(0.5) H49X(0.5) C50X(0.5) H50A(0.5) H50B(0.5) H50C(0.5)
 C51X(0.5) H51A(0.5) H51B(0.5) H51C(0.5) C67(0.5) H67(0.5) C68(0.5) H68A(0.5)
 H68B(0.5) H68C(0.5) C69(0.5) H69A(0.5) H69B(0.5) H69C(0.5) C49(0.5) H49(0.5)
 C50(0.5) H50D(0.5) H50E(0.5) H50F(0.5) C51(0.5) H51D(0.5) H51E(0.5) H51F(0.5)
 C67X(0.5) H67X(0.5) C68X(0.5) H68D(0.5) H68E(0.5) H68F(0.5) C69X(0.5)
 H69D(0.5) H69E(0.5) H69F(0.5) O32(0.5) C70(0.5) H70(0.5) C71(0.5) H71A(0.5)
 H71B(0.5) H71C(0.5) C72(0.5) H72A(0.5) H72B(0.5) H72C(0.5) O32X(0.5) C70X(0.5)
 H70X(0.5) C71X(0.5) H71D(0.5) H71E(0.5) H71F(0.5) C72X(0.5) H72D(0.5)
 H72E(0.5) H72F(0.5)
5.a Riding coordinates:
 C54(H54A,H54B,H54C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C50X(H50A,H50B,
 H50C), C51X(H51A,H51B,H51C), C56X(H56A,H56B,H56C), C57X(H57A,H57B,H57C),
 C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62X(H62A,H62B,H62C), C63X(H63A,H63B,
 H63C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C50(H50D,H50E,H50F), C51(H51D,
 H51E,H51F), C56(H56D,H56E,H56F), C57(H57D,H57E,H57F), C59X(H59D,H59E,H59F),
 C60X(H60D,H60E,H60F), C62(H62D,H62E,H62F), C63(H63D,H63E,H63F), C68X(H68D,H68E,
 H68F), C69X(H69D,H69E,H69F), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C),
 C71X(H71D,H71E,H71F), C72X(H72D,H72E,H72F)
5.b Ternary CH refined with riding coordinates:
 O33(H33), O34(H34), O35(H35), O36(H36), O37(H37), O38(H38)
5.c Me refined as rotating group:
 C53(H53A,H53B,H53C)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), 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(H35A), C36(H36A), C37(H37A), C40(H40), C43(H43), C44(H44), C45(H45),
 C48(H48), C52(H52), C64(H64), C49X(H49X), C55X(H55X), C58(H58), C61X(H61X),
 C67(H67), C49(H49), C55(H55), C58X(H58X), C61(H61), C67X(H67X), C70(H70),
 C70X(H70X)
;
_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 1.488
_oxdiff_exptl_absorpt_empirical_full_min 0.695