Phosphonate-assisted tetranuclear lanthanide assemblies: observation of the toroidic ground state in the Tb<sup>III</sup> analogue.
Biswas, Sourav; Kumar, Pawan; Swain, Abinash; Gupta, Tulika; Kalita, Pankaj; Kundu, Subrata; Rajaraman, Gopalan; Chandrasekhar, Vadapalli; Dalton transactions (Cambridge, England : 2003) 48 (2019) 6421–6434; doi:10.1039/c9dt00592g

data_7049546
_publ_section_title
;
 Phosphonate-assisted tetranuclear lanthanide assemblies: observation of
 the toroidic ground state in the Tb<sup>III</sup> analogue.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6421
_journal_page_last               6434
_journal_paper_doi               10.1039/c9dt00592g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'C55.7 H67.4 Dy4 F6 N10 O20 P2, 2(Cl), 2(C H4 O), 0.3(H2 O)'
_chemical_formula_sum            'C57.7 H76 Cl2 Dy4 F6 N10 O22.3 P2'
_chemical_formula_weight         2163.32
_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     iterative
_audit_creation_date             2019-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-22 deposited with the CCDC.    2019-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                112.8160(10)
_cell_angle_beta                 98.8770(10)
_cell_angle_gamma                108.9790(10)
_cell_formula_units_Z            1
_cell_length_a                   12.2754(8)
_cell_length_b                   12.9357(8)
_cell_length_c                   14.5715(9)
_cell_measurement_reflns_used    6923
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      2.38
_cell_volume                     1909.6(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12451
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.063
_diffrn_reflns_theta_max         25.063
_diffrn_reflns_theta_min         2.383
_exptl_absorpt_coefficient_mu    4.070
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6528
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0738 before and 0.0353 after correction.
The Ratio of minimum to maximum transmission is 0.8760.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_description       block
_exptl_crystal_F_000             1053
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         6718
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0193P)^2^+1.9331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0542
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5542
_reflns_number_total             6718
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00592g2.cif
_cod_data_source_block           complex1
_cod_depositor_comments
'Adding full bibliography for 7049546--7049548.cif.'
_cod_original_formula_sum        'C57.70 H76 Cl2 Dy4 F6 N10 O22.30 P2'
_cod_database_code               7049546
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.737
_shelx_estimated_absorpt_t_min   0.663
_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) groups, All O(H,H) groups
2. Restrained distances
 O5-H5
 0.85 with sigma of 0.01
 O4-H4
 0.85 with sigma of 0.01
 O3-H3
 0.87 with sigma of 0.01
 O12-H12A = O12-H12B
 0.87 with sigma of 0.02
 C21-H5
 1.915796 with sigma of 0.02
 Dy1-H5
 2.969387 with sigma of 0.02
 C19-H4
 1.909474 with sigma of 0.02
 Dy1-H4
 2.976831 with sigma of 0.02
 Dy2-H3
 2.9126 with sigma of 0.02
 H12A-H12B
 1.38 with sigma of 0.04
 C22-H3
 1.914506 with sigma of 0.02
 Dy2-H12A \\sim Dy2-H12B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3) = Uanis(O12)
4. Others
 Fixed Sof: O3(0.85) H3(0.85) C22(0.85) H22A(0.85) H22B(0.85) H22C(0.85)
 O30(0.15) H30A(0.15) H30B(0.15) O12(0.15) H12A(0.15) H12B(0.15)
5.a Riding coordinates:
 O30(H30A,H30B), O12(H12A,H12B)
5.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C21(H21A,H21B), C18(H18A,H18B), C20(H20A,H20B), C19(H19A,H19B)
5.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C3(H3A), C9(H9), C2(H2), C15(H15), C14(H14), C4(H4A), C10(H10),
 C8(H8)
5.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C26(H26A,H26B,H26C), C22(H22A,H22B,
 H22C), C29(H29A,H29B,H29C)
5.e Idealised tetrahedral OH refined as rotating group:
 O11(H11)
;
_shelx_res_checksum              18281
_shelx_fab_checksum              83818
_olex2_submission_special_instructions 'No special instructions were received'