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_7049548
_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         'C28 H34 F3 Gd2 N5 O10 P, Cl, C H4 O'
_chemical_formula_sum            'C29 H38 Cl F3 Gd2 N5 O11 P'
_chemical_formula_weight         1070.56
_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
_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                112.258(5)
_cell_angle_beta                 99.430(5)
_cell_angle_gamma                108.876(5)
_cell_formula_units_Z            2
_cell_length_a                   12.294(5)
_cell_length_b                   12.897(5)
_cell_length_c                   14.668(5)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.39
_cell_volume                     1924.7(13)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_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            23430
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         4.120
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.601
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0623 before and 0.0480 after correction. The Ratio of minimum to maximum transmission is 0.8609. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_description       block
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.822
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.109
_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     484
_refine_ls_number_reflns         6780
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+2.7285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0695
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5670
_reflns_number_total             6780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00592g2.cif
_cod_data_source_block           complex3_sq
_cod_depositor_comments
'Adding full bibliography for 7049546--7049548.cif.'
_cod_database_code               7049548
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.738
_shelx_estimated_absorpt_t_min   0.672
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H13 of O13, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H19 of O19, H12 of O12, H26 of O26
2. Restrained distances
 O19-H19
 0.87 with sigma of 0.01
 C29-H19
 1.909152 with sigma of 0.02
 Gd1-H19
 2.930386 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C4(H4A,H4B)
3.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C9(H9), C20(H20), C11(H11), C14(H14), C17(H17), C10(H10), C21(H21),
 C16(H16)
3.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C24(H24A,H24B,H24C), C29(H29A,H29B,
 H29C), C31(H31A,H31B,H31C)
3.d Idealised tetrahedral OH refined as rotating group:
 O26(H26)
;
_shelx_res_checksum              621
_shelx_fab_checksum              6606
_olex2_submission_special_instructions 'No special instructions were received'