Triangular Monometallic Cyanide Cluster Entrapped in Carbon Cage with Geometry-Dependent Molecular Magnetism.
Liu, Fupin; Gao, Cong-Li; Deng, Qingming; Zhu, Xianjun; Kostanyan, Aram; Westerström, Rasmus; Wang, Song; Tan, Yuan-Zhi; Tao, Jun; Xie, Su-Yuan; Popov, Alexey A.; Greber, Thomas; Yang, Shangfeng; Journal of the American Chemical Society 138 (2016) 14764–14771; doi:10.1021/jacs.6b09329

data_4131115
_publ_section_title
;
 Triangular Monometallic Cyanide Cluster Entrapped in Carbon Cage with
 Geometry-Dependent Molecular Magnetism.
;
_journal_issue                   44
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14764
_journal_page_last               14771
_journal_paper_doi               10.1021/jacs.6b09329
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety
;
Tb CN C82, Ni N4 C36 H44, 2 (C6 H6)
;
_chemical_formula_sum            'C131 H56 N5 Ni Tb'
_chemical_formula_weight         1917.43
_chemical_name_common            ;TbNC@C2v(9)-C82/Ni(OEP)/2benzene;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 94.727(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.3790(12)
_cell_length_b                   15.1280(7)
_cell_length_c                   19.8700(10)
_cell_measurement_reflns_used    4222
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      62.1440
_cell_measurement_theta_min      5.4290
_cell_volume                     7602.8(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3415
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0717
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12641
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        62.336
_diffrn_reflns_theta_max         62.336
_diffrn_reflns_theta_min         3.404
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.374
_exptl_absorpt_correction_T_max  0.9482
_exptl_absorpt_correction_T_min  0.9001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3880
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.441
_refine_diff_density_min         -1.228
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.575
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     957
_refine_ls_number_reflns         6119
_refine_ls_number_restraints     1451
_refine_ls_restrained_S_all      1.812
_refine_ls_R_factor_all          0.1928
_refine_ls_R_factor_gt           0.1386
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3759
_refine_ls_wR_factor_ref         0.4197
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3802
_reflns_number_total             6119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b09329_si_003.cif
_cod_data_source_block           tbc83niii
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4131115
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.900
_shelx_estimated_absorpt_t_max   0.948
_shelx_res_checksum              96689
_shelx_hkl_checksum              53336