Enneanuclear [Ni6Ln3] Cages: [Ln(III)3] Triangles Capping [Ni(II)6] Trigonal Prisms Including a [Ni6Dy3] Single-Molecule Magnet.
Canaj, Angelos B.; Tzimopoulos, Demetrios I.; Siczek, Milosz; Lis, Tadeusz; Inglis, Ross; Milios, Constantinos J.; Inorganic chemistry 54 (2015) 7089–7095; doi:10.1021/acs.inorgchem.5b01149

data_4346274
_publ_section_title
;
 Enneanuclear [Ni6Ln3] Cages: [Ln(III)3] Triangles Capping [Ni(II)6]
 Trigonal Prisms Including a [Ni6Dy3] Single-Molecule Magnet.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7089
_journal_page_last               7095
_journal_paper_doi               10.1021/acs.inorgchem.5b01149
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety
'C90 H96 Dy3 N9 Ni6 O33, 2.7(C4 H10 O), 2(C2 H3 N), 2.4(H2 O)'
_chemical_formula_sum            'C104.8 H133.8 Dy3 N11 Ni6 O38.1'
_chemical_formula_weight         2996.98
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                93.70(2)
_cell_angle_beta                 91.76(2)
_cell_angle_gamma                94.76(2)
_cell_formula_units_Z            2
_cell_length_a                   15.021(4)
_cell_length_b                   15.270(5)
_cell_length_c                   26.430(8)
_cell_measurement_temperature    80(2)
_cell_volume                     6025(3)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.839
_diffrn_measurement_device_type
;
Xcalibur R kappa-geometry diffractometer with a Ruby CCD detector
;
_diffrn_measurement_method       w/
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_unetI/netI     0.2039
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.839
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            48423
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.432
_diffrn_reflns_theta_min         2.683
_exptl_absorpt_coefficient_mu    2.834
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_correction_T_min  0.760
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5
Analytical numeric absorption correction using a
multifaceted crystal model based on expressions
derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_description       plate
_exptl_crystal_F_000             3021
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.361
_refine_diff_density_min         -1.106
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1479
_refine_ls_number_reflns         27973
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1862
_refine_ls_R_factor_gt           0.0872
_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^)+(0.0313P)^2^+1.8720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1477
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14353
_reflns_number_total             27973
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01149_si_002.cif
_cod_data_source_block           at2520a
_cod_original_formula_sum        'C104.80 H133.80 Dy3 N11 Ni6 O38.10'
_cod_database_code               4346274
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.727
_shelx_estimated_absorpt_t_max   0.895
_shelx_res_checksum              41512
_shelx_hkl_checksum              46872