Deviation from the Planaritya Large Dy3N Cluster Encapsulated in an Ih-C80 Cage: An X-ray Crystallographic and Vibrational Spectroscopic Study
Shangfeng Yang; Sergey I. Troyanov; Alexey A. Popov; Matthias Krause; Lothar Dunsch; Journal of the American Chemical Society 128 (2006) 16733–16739; doi:10.1021/ja066814i

data_4111303
_publ_section_title
;
 Deviation from the Planaritya Large Dy3N Cluster Encapsulated in an
 Ih-C80 Cage: An X-ray Crystallographic and Vibrational Spectroscopic
 Study
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16733
_journal_page_last               16739
_journal_paper_doi               10.1021/ja066814i
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'Dy3N C80 Ni(C36H42N4) 2(C6H6)'
_chemical_formula_sum            'C128 H56 Dy3 N5 Ni'
_chemical_formula_weight         2209.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 95.1949(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.3119(2)
_cell_length_b                   15.0979(1)
_cell_length_c                   39.4098(3)
_cell_measurement_reflns_used    25437
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35
_cell_measurement_theta_min      5
_cell_volume                     14998.85(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.776
_diffrn_measured_fraction_theta_max 0.776
_diffrn_measurement_device_type  MAR345
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.91000
_diffrn_reflns_av_R_equivalents  0.1765
_diffrn_reflns_av_sigmaI/netI    0.0912
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            53218
_diffrn_reflns_theta_full        36.20
_diffrn_reflns_theta_max         36.20
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    3.274
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.957
_exptl_crystal_description       prism
_exptl_crystal_F_000             8680
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.869
_refine_diff_density_min         -1.952
_refine_diff_density_rms         0.201
_refine_ls_extinction_coef       0.00037(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    restraint
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1288
_refine_ls_number_reflns         13337
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0864
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1210P)^2^+160.0352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2259
_refine_ls_wR_factor_ref         0.2383
_reflns_number_gt                11051
_reflns_number_total             13337
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja066814isi20061101_012751.cif
_cod_data_source_block           dy3nb
_cod_original_cell_volume        14998.9(2)
_cod_database_code               4111303