Synthesis of a Dy@C82 Derivative Bearing a Single Phosphorus Substituent via a Zwitterion Approach
Xiaofang Li; Louzhen Fan; Dongfang Liu; Herman H. Y. Sung; Ian D. Williams; Shihe Yang; Kai Tan; Xin Lu; Journal of the American Chemical Society 129 (2007) 10636–10637; doi:10.1021/ja074321n

data_4109875
_publ_section_title
;
 Synthesis of a Dy@C82 Derivative Bearing a Single Phosphorus Substituent
 via a Zwitterion Approach
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10636
_journal_page_last               10637
_journal_paper_doi               10.1021/ja074321n
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C106 H21 Dy O4 P'
_chemical_formula_weight         1551.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 110.742(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.7121(6)
_cell_length_b                   18.3146(6)
_cell_length_c                   22.2350(7)
_cell_measurement_reflns_used    8083
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.22
_cell_volume                     6364.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_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  0.0783
_diffrn_reflns_av_sigmaI/netI    0.0920
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37603
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    1.268
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.42
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       plate
_exptl_crystal_F_000             3080
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
;
_refine_diff_density_max         5.368
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1009
_refine_ls_number_reflns         10583
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0754
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1360P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1854
_refine_ls_wR_factor_ref         0.2022
_reflns_number_gt                7147
_reflns_number_total             10583
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja074321nsi20070614_054913.cif
_cod_data_source_block           fang1
_cod_database_code               4109875