Selective arc-discharge synthesis of Dy2S-clusterfullerenes and their isomer-dependent single molecule magnetism
Chen, Chia-Hsiang; Krylov, Denis; Avdoshenko, Stanislav; Liu, Fupin; Spree, Lukas; Yadav, Ravi; Alvertis, Antonis; Hozoi, Liviu; Nenkov, Konstantin; Kostanyan, Aram; Greber, Thomas; Wolter, A.; Popov, Alexey A.; Chem. Sci.  (2017) –; doi:10.1039/C7SC02395B

data_1546438
_publ_section_title
;
 Selective arc-discharge synthesis of Dy2S-clusterfullerenes and their
 isomer-dependent single molecule magnetism
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC02395B
_journal_year                    2017
_chemical_formula_moiety         ;Dy2S@C3v(8)-C82/Ni(OEP)/2(C7H8);
_chemical_formula_sum            'C132 H60 Dy2 N4 Ni S'
_chemical_formula_weight         2117.61
_chemical_name_common            ;Dy2S@C3v(8)-C82/Ni(OEP)/2(C7H8);
_chemical_name_systematic        Dy2S@C3v(8)-C82/Ni(OEP)/2(C7H8)
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-05-21 deposited with the CCDC.
2017-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.74(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.250(5)
_cell_length_b                   14.860(3)
_cell_length_c                   20.460(4)
_cell_measurement_reflns_used    56365
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      1
_cell_volume                     7607(3)
_computing_cell_refinement       XDS
_computing_data_collection       XDS
_computing_data_reduction        XDS
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  MAR225CCD
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.89429
_diffrn_reflns_av_R_equivalents  0.2753
_diffrn_reflns_av_unetI/netI     0.2024
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            56365
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        32.451
_diffrn_reflns_theta_max         36.099
_diffrn_reflns_theta_min         2.258
_diffrn_source                   'BESSY BL MX-14.3'
_exptl_absorpt_coefficient_mu    4.092
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_description       block
_exptl_crystal_F_000             4224
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.760
_refine_diff_density_min         -1.397
_refine_diff_density_rms         0.164
_refine_ls_extinction_coef       0.0038(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1082
_refine_ls_number_reflns         8627
_refine_ls_number_restraints     956
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.2340
_refine_ls_R_factor_gt           0.1630
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1528P)^2^+233.2237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4063
_refine_ls_wR_factor_ref         0.4406
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4462
_reflns_number_total             8627
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc02395b2.cif
_cod_data_source_block           shelx
_cod_database_code               1546438
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              47038