Metallogrid Single-Molecule Magnet: Solvent-Induced Nuclearity Transformation and Magnetic Hysteresis at 16 K.
Huang, Wei; Shen, Fu-Xing; Wu, Shu-Qi; Liu, Li; Wu, Dayu; Zheng, Zhe; Xu, Jun; Zhang, Ming; Huang, Xing-Cai; Jiang, Jun; Pan, Feifei; Li, Yao; Zhu, Kun; Sato, Osamu; Inorganic chemistry 55 (2016) 5476–5484; doi:10.1021/acs.inorgchem.6b00500

data_4347706
_publ_section_title
;
 Metallogrid Single-Molecule Magnet: Solvent-Induced Nuclearity
 Transformation and Magnetic Hysteresis at 16 K.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5476
_journal_page_last               5484
_journal_paper_doi               10.1021/acs.inorgchem.6b00500
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C88 H72 Dy4 N28 O24, C2 O4, 4(C O), 4(O)'
_chemical_formula_sum            'C94 H116 Dy4 N28 O36'
_chemical_formula_weight         2864.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.112(7)
_cell_length_b                   36.81(2)
_cell_length_c                   61.22(4)
_cell_measurement_reflns_used    6408
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.725
_cell_measurement_theta_min      2.415
_cell_volume                     25041(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Diamond
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2023
_diffrn_reflns_av_unetI/netI     0.1440
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       72
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            20763
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.943
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.443
_exptl_absorpt_correction_T_max  0.613
_exptl_absorpt_correction_T_min  0.562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       block
_exptl_crystal_F_000             11424
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.516
_refine_diff_density_min         -1.853
_refine_diff_density_rms         0.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         5471
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.934
_refine_ls_R_factor_all          0.1613
_refine_ls_R_factor_gt           0.0973
_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^)+(0.1714P)^2^+332.4812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2635
_refine_ls_wR_factor_ref         0.3083
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3063
_reflns_number_total             5471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00500_si_002.cif
_cod_data_source_block           2
_cod_original_cell_volume        25041(26)
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               4347706
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.528
_shelx_estimated_absorpt_t_max   0.641
_shelx_res_checksum              89050
_shelx_hkl_checksum              95299