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_7048541
_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 Gd12 N12 O72, 3(C3 H7 N O)'
_chemical_formula_sum            'C141 H165 Gd12 N15 O75'
_chemical_formula_weight         5156.88
_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                71.244(5)
_cell_angle_beta                 84.760(5)
_cell_angle_gamma                87.213(5)
_cell_formula_units_Z            1
_cell_length_a                   17.2373(12)
_cell_length_b                   17.2380(11)
_cell_length_c                   17.9087(9)
_cell_measurement_reflns_used    7809
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      30.4240
_cell_measurement_theta_min      1.6280
_cell_volume                     5016.6(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  89.00   1.00   30.00    --   26.19  77.00   0.00   90
  2  \w     -1.00  94.00   1.00   30.00    --   26.19  77.00  90.00   95
  3  \w    -25.00  10.00   1.00   30.00    --   26.19 -99.00-150.00   35
  4  \w     12.00  39.00   1.00   30.00    --   26.19 -99.00-150.00   27
  5  \w     22.00  65.00   1.00   30.00    --   26.19 -99.00 -90.00   43
  6  \w    -43.00  35.00   1.00   30.00    --   26.19 -38.00-150.00   78
  7  \w    -41.00   4.00   1.00   30.00    --   26.19 -77.00 -30.00   45
  8  \w    -72.00  -3.00   1.00   30.00    --  -23.85 -77.00 150.00   69
;
_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      0.0106825000
_diffrn_orient_matrix_UB_12      0.0054921000
_diffrn_orient_matrix_UB_13      -0.0405425000
_diffrn_orient_matrix_UB_21      -0.0334819000
_diffrn_orient_matrix_UB_22      0.0254513000
_diffrn_orient_matrix_UB_23      -0.0105007000
_diffrn_orient_matrix_UB_31      0.0217478000
_diffrn_orient_matrix_UB_32      0.0348023000
_diffrn_orient_matrix_UB_33      -0.0026300000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0883
_diffrn_reflns_av_unetI/netI     0.1274
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33305
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.62
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.988
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2484
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.561
_refine_diff_density_min         -2.556
_refine_diff_density_rms         0.284
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1084
_refine_ls_number_reflns         14368
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1185
_refine_ls_R_factor_gt           0.0805
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0810P)^2^+82.7804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1812
_refine_ls_wR_factor_ref         0.2111
_reflns_number_gt                9935
_reflns_number_total             14368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt04602f2.cif
_cod_data_source_block           shi_3524_didr
_cod_depositor_comments
'Adding full bibliography for 7048539--7048541.cif.'
_cod_original_cell_volume        5016.6(5)
_cod_database_code               7048541
_chemical_oxdiff_formula         'C30 H30 N4 O8 Dy2'
_chemical_oxdiff_usercomment     ???
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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
 C49X-C51X
 2.45 with sigma of 0.01
 C49X-C50X
 2.45 with sigma of 0.01
 C51-C50
 2.45 with sigma of 0.01
 C51X-C50X
 2.45 with sigma of 0.01
 C51-C49
 2.45 with sigma of 0.01
 C49-C50
 2.45 with sigma of 0.01
 O31-C49 = O31-C49X
 1.2 with sigma of 0.01
 N1-C49 = N1X-C49X
 1.4 with sigma of 0.01
 O34-C58X \\sim O34-C58
 with sigma of 0.01
 N4-C58 \\sim N4X-C58X
 with sigma of 0.01
 N4-C60 \\sim N4-C59 \\sim N4X-C60X \\sim N4X-C59X
 with sigma of 0.01
 C59X-C58X \\sim C58X-C60X
 with sigma of 0.01
 C59-C58 \\sim C58-C60
 with sigma of 0.01
 N1-C50 \\sim N1-C51 \\sim N1X-C51X \\sim N1X-C50X
 with sigma of 0.01
 C51X-C49X \\sim C49X-C50X
 with sigma of 0.01
 C70-O37 \\sim C70X-O37X
 with sigma of 0.01
 C70-N8 \\sim C70X-N8X
 with sigma of 0.01
 C72X-C70X \\sim C70X-C71X
 with sigma of 0.01
 O31-C49X \\sim O31-C49
 with sigma of 0.01
 N1-C49 \\sim N1X-C49X
 with sigma of 0.01
 C51-C49 \\sim C49-C50
 with sigma of 0.01
 N8X-C72X \\sim N8-C72 \\sim N8-C71 \\sim N8X-C71X
 with sigma of 0.01
 C72-C70 \\sim C70-C71
 with sigma of 0.01
 O33-C55X \\sim O33-C55
 with sigma of 0.01
 N3X-C55X \\sim N3-C55
 with sigma of 0.01
 N3X-C57X \\sim N3-C56 \\sim N3X-C56X \\sim N3-C57
 with sigma of 0.01
 C56-C55 \\sim C55-C57
 with sigma of 0.01
 C57X-C55X \\sim C55X-C56X
 with sigma of 0.01
3. Restrained planarity
 N4X, C58X, C59X, C60X
 with sigma of 0.1
 N4, C58, C59, C60
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(O35)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C34) \\sim Ueq,
Uanis(O36) \\sim Ueq, Uanis(C48) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(C58X) = Uiso(C58) = Uiso(N4) = Uiso(C60) = Uiso(C60X) = Uiso(C59) =
Uiso(N4X) = Uiso(C59X)
Uiso(C49) = Uiso(C49X) = Uiso(N1X) = Uiso(C51X) = Uiso(C51) = Uiso(C50X) =
Uiso(C50)
Uiso(C70X) = Uiso(C70) = Uiso(O37) = Uiso(O37X) = Uiso(N8X) = Uiso(C71X) =
Uiso(C72X) = Uiso(N8) = Uiso(C71) = Uiso(C72)
Uanis(C57X) = Uanis(C56) = Uanis(N3X) = Uanis(N3) = Uanis(C56X) = Uanis(C57) =
Uanis(C55) = Uanis(C55X)
5. Others
 Fixed Sof: N1(0.5) N3X(0.5) N4(0.5) C49(0.5) H49(0.5) C50(0.5) H50A(0.5)
 H50B(0.5) H50C(0.5) C51(0.5) H51A(0.5) H51B(0.5) H51C(0.5) C55X(0.5) H55X(0.5)
 C56X(0.5) H56A(0.5) H56B(0.5) H56C(0.5) C57X(0.5) H57A(0.5) H57B(0.5)
 H57C(0.5) C58(0.5) H58(0.5) C59(0.5) H59A(0.5) H59B(0.5) H59C(0.5) C60(0.5)
 H60A(0.5) H60B(0.5) H60C(0.5) N1X(0.5) N3(0.5) N4X(0.5) C49X(0.5) H49X(0.5)
 C50X(0.5) H50D(0.5) H50E(0.5) H50F(0.5) C51X(0.5) H51D(0.5) H51E(0.5)
 H51F(0.5) C55(0.5) H55(0.5) C56(0.5) H56D(0.5) H56E(0.5) H56F(0.5) C57(0.5)
 H57D(0.5) H57E(0.5) H57F(0.5) C58X(0.5) H58X(0.5) C59X(0.5) H59D(0.5)
 H59E(0.5) H59F(0.5) C60X(0.5) H60D(0.5) H60E(0.5) H60F(0.5) O37X(0.25)
 N8X(0.25) C70X(0.25) H70X(0.25) C71X(0.25) H71A(0.25) H71B(0.25) H71C(0.25)
 C72X(0.25) H72A(0.25) H72B(0.25) H72C(0.25) O37(0.25) N8(0.25) C70(0.25)
 H70(0.25) C71(0.25) H71D(0.25) H71E(0.25) H71F(0.25) C72(0.25) H72D(0.25)
 H72E(0.25) H72F(0.25)
6.a Riding coordinates:
 C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C), C51(H51A,H51B,
 H51C), C56X(H56A,H56B,H56C), C57X(H57A,H57B,H57C), C59(H59A,H59B,H59C),
 C50X(H50D,H50E,H50F), C51X(H51D,H51E,H51F), C56(H56D,H56E,H56F), C57(H57D,H57E,
 H57F), C59X(H59D,H59E,H59F), C72X(H72A,H72B,H72C), C69(H69A,H69B,H69C),
 C71(H71D,H71E,H71F), C72(H72D,H72E,H72F)
6.b Ternary CH refined with riding coordinates:
 O1(H1), O2(H2), O3(H3), O4(H4), O5(H5), O6(H6)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4A), C5(H5A), 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), C52(H52), C61(H61), C64(H64), C49(H49), C55X(H55X), C58(H58),
 C49X(H49X), C55(H55), C58X(H58X), C70X(H70X), C67(H67), C70(H70)
6.d Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C66(H66A,H66B,H66C), C50(H50A,H50B,
 H50C), C60(H60A,H60B,H60C), C60X(H60D,H60E,H60F), C71X(H71A,H71B,H71C),
 C68(H68A,H68B,H68C)
;
_olex2_date_sample_data_collection 2017-04-05
_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 2.000
_oxdiff_exptl_absorpt_empirical_full_min 0.744