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_4346273
_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 Er3 N9 Ni6 O33, 5.75(C2 H3 N), 2(C4 H10 O), 1.5(H2 O)'
_chemical_formula_sum            'C109.5 H136.25 Er3 N14.75 Ni6 O36.5'
_chemical_formula_weight         3097.11
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                93.92(2)
_cell_angle_beta                 92.63(2)
_cell_angle_gamma                94.73(2)
_cell_formula_units_Z            2
_cell_length_a                   15.069(4)
_cell_length_b                   15.260(4)
_cell_length_c                   26.385(6)
_cell_measurement_reflns_used    18021
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      31
_cell_measurement_theta_min      2
_cell_volume                     6024(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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_device_type
;
Xcalibur R kappa-geometry diffractometer with a Ruby CCD detector
;
_diffrn_measurement_method       w/
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0835
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            62860
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         30.788
_diffrn_reflns_theta_min         2.686
_exptl_absorpt_coefficient_mu    3.066
_exptl_absorpt_correction_T_max  0.744
_exptl_absorpt_correction_T_min  0.494
_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            GREEN
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_description       PARALLEPIPED
_exptl_crystal_F_000             3121
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.110
_refine_diff_density_max         2.13
_refine_diff_density_min         -1.24
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1526
_refine_ls_number_reflns         33798
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+16.0281P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1441
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24958
_reflns_number_total             33798
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01149_si_004.cif
_cod_data_source_block           AT1932BA
_cod_original_formula_sum        'C109.50 H136.25 Er3 N14.75 Ni6 O36.50'
_cod_database_code               4346273
_shelx_estimated_absorpt_t_min   0.374
_shelx_estimated_absorpt_t_max   0.729
_shelxl_version_number           2013-2
_shelx_hkl_checksum              94863