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_7049547
_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
'C55.62 H69.24 F6 N10 O20 P2 Tb4, 2(Cl), 0.38(H2 O)'
_chemical_formula_sum            'C55.62 H70 Cl2 F6 N10 O20.38 P2 Tb4'
_chemical_formula_weight         2087.25
_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             2019-03-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-29 deposited with the CCDC.    2019-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                112.5610(10)
_cell_angle_beta                 99.3550(10)
_cell_angle_gamma                108.9880(10)
_cell_formula_units_Z            1
_cell_length_a                   12.2855(5)
_cell_length_b                   12.8600(5)
_cell_length_c                   14.6338(6)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      2.79
_cell_volume                     1906.44(14)
_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_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0353
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_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            29176
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.378
_diffrn_reflns_theta_min         2.734
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.862
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6034
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0681 before and 0.0450 after correction.
The Ratio of minimum to maximum transmission is 0.8092.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.818
_exptl_crystal_description       block
_exptl_crystal_F_000             1015
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.011
_refine_diff_density_max         1.294
_refine_diff_density_min         -1.136
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         9554
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0337P)^2^+2.4541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0747
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7817
_reflns_number_total             9554
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00592g2.cif
_cod_data_source_block           complex2_sq
_cod_depositor_comments
'Adding full bibliography for 7049546--7049548.cif.'
_cod_original_cell_volume        1906.43(13)
_cod_database_code               7049547
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.614
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(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
 O17-H17
 0.87 with sigma of 0.01
 O3-H3
 0.87 with sigma of 0.01
 C26-H17
 1.916347 with sigma of 0.02
 Tb2-H17
 3.015924 with sigma of 0.02
 C1AA-H3
 1.917636 with sigma of 0.02
 Tb1-H3
 2.869836 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3) = Uanis(O0AA)
4. Others
 Fixed Sof: O3(0.81) H3(0.81) C1AA(0.81) H1AA(0.81) H1AB(0.81) H1AC(0.81)
 O1AA(0.19) H1AD(0.19) H1AE(0.19) O0AA(0.19) H0AA(0.19) H0AB(0.19)
5.a Riding coordinates:
 O1AA(H1AD,H1AE)
5.b Rotating group:
 O0AA(H0AA,H0AB)
5.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C28(H28A,H28B), C29(H29A,H29B), C26(H26A,H26B), C27(H27A,H27B)
5.d Aromatic/amide H refined with riding coordinates:
 N2(H2), C7(H7), C5(H5), C15(H15), C10(H10), C14(H14), C13(H13), C6(H6),
 C24(H24), C23(H23)
5.e Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C1AA(H1AA,H1AB,
 H1AC)
;
_shelx_res_checksum              98168
_shelx_fab_checksum              4898
_olex2_submission_special_instructions 'No special instructions were received'