New examples of triangular terbium(iii) and holmium(iii) and hexagonal dysprosium(iii) single molecule toroics.
Langley, Stuart K.; Vignesh, Kuduva R.; Gupta, Tulika; Gartshore, Christopher J.; Rajaraman, Gopalan; Forsyth, Craig M.; Murray, Keith S.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15657–15667; doi:10.1039/c9dt02419k

data_7700949
_publ_section_title
;
 New examples of triangular terbium(iii) and holmium(iii) and hexagonal
 dysprosium(iii) single molecule toroics.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15657
_journal_page_last               15667
_journal_paper_doi               10.1039/c9dt02419k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C45 H74 Cl2 Dy3 N9 O18'
_chemical_formula_weight         1587.53
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-08-22 deposited with the CCDC.    2019-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   17.5986(3)
_cell_length_b                   17.5986(3)
_cell_length_c                   13.1888(5)
_cell_measurement_reflns_used    9753
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      31.12
_cell_measurement_theta_min      2.15
_cell_volume                     3537.47(16)
_computing_cell_refinement       'Bruker Apex2 V2.0'
_computing_data_collection       'Bruker Apex2 V2.0'
_computing_data_reduction        'Bruker Apex2 V2.0'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'APEX X8'
_diffrn_measurement_method       'scans in phi and omega'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            37039
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         2.315
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.272
_exptl_absorpt_correction_T_max  0.720
_exptl_absorpt_correction_T_min  0.460
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       block
_exptl_crystal_F_000             1566
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
 After refinement of the main molecule, residual electron density was tentatively 
 assigned as partially occupied acetonitrile and water molecules. In the final model, 
 these were accounted for using PLATON/SQUEEZE (Spek, 2015). The calculated electron 
 count of 230.5 electrons per formula unit corresponds approximately to 8 x CH3CN and 
 6 x H2O molecules (calc 224 e-).
;
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         5411
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0233
_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^)+(0.0346P)^2^+5.7229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0693
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5125
_reflns_number_total             5411
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02419k2.cif
_cod_data_source_block           dy3_new_sq
_cod_depositor_comments
'Adding full bibliography for 7700946--7700949.cif.'
_cod_original_cell_volume        3537.46(18)
_cod_database_code               7700949
_shelx_shelxl_version_number     2018/3
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              31358
_shelx_fab_checksum              7246