Where Does the Metal Cation Stay in Gd@C2v(9)-C82? A Single-Crystal X-ray Diffraction Study
Mitsuaki Suzuki; Xing Lu; Satoru Sato; Hidefumi Nikawa; Naomi Mizorogi; Zdenek Slanina; Takahiro Tsuchiya; Shigeru Nagase; Takeshi Akasaka; Inorganic Chemistry 51 (2012) 5270–5273; doi:10.1021/ic300186y

data_4329104
_publ_section_title
;
 Where Does the Metal Cation Stay in Gd@C2v(9)-C82? A Single-Crystal X-ray
 Diffraction Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5270
_journal_page_last               5273
_journal_paper_doi               10.1021/ic300186y
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
'Gd C82, Ni N4 C36 H44, 1.4(C6 H6), 0.6(C H Cl3)'
_chemical_formula_sum            'C127 H53 Cl1.8 Gd N4 Ni'
_chemical_formula_weight         1914.50
_chemical_name_common            Gd@C82/NiOEP/1.4benzene/0.6chloroform
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.998(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.3645(9)
_cell_length_b                   15.1820(6)
_cell_length_c                   19.7167(7)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    90
_cell_measurement_theta_max      27.20
_cell_measurement_theta_min      2.51
_cell_volume                     7563.7(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita, et al., 2009)'
_computing_publication_material  'Yadokari-XG 2009 (Wakita, et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33392
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.04
_exptl_absorpt_coefficient_mu    1.251
_exptl_absorpt_correction_T_max  0.9065
_exptl_absorpt_correction_T_min  0.6829
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_description       plate
_exptl_crystal_F_000             3862
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.091
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1025
_refine_ls_number_reflns         8660
_refine_ls_number_restraints     946
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0931P)^2^+38.2145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1745
_refine_ls_wR_factor_ref         0.1858
_reflns_number_gt                7175
_reflns_number_total             8660
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300186y_si_002.cif
_cod_data_source_block           k1
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_original_formula_sum        'C127 H53 Cl1.80 Gd N4 Ni'
_cod_database_code               4329104