Regioselective synthesis and molecular structure of the first derivative of praseodymium-containing metallofullerenes
Qin Zhou; Hui Li; Yongfu Lian; Mitsuaki Suzuki; Lipiao Bao; Wenting Cai,c; Weiwei Wang; Shigeru Nagase; Xing Lu; Takeshi Akasaka; Chem.Commun. 50 (2014) 9876–; doi:10.1039/C4cc02949F

data_7115496
_publ_section_title
;
 Regioselective synthesis and molecular structure of the first derivative
 of praseodymium-containing metallofullerenes
;
_journal_name_full               Chem.Commun.
_journal_page_first              9876
_journal_paper_doi               10.1039/C4cc02949F
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C94.5 H14 Pr S5'
_chemical_formula_weight         1450.27
_chemical_name_common            Pr@C82-Ad
_chemical_name_systematic
; 
 PrC82Ad
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.373(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.325(2)
_cell_length_b                   21.950(4)
_cell_length_c                   20.931(4)
_cell_measurement_temperature    90(2)
_cell_volume                     5100.9(16)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.937
_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  0.0873
_diffrn_reflns_av_sigmaI/netI    0.0812
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            49841
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.21
_diffrn_reflns_theta_min         3.91
_exptl_absorpt_coefficient_mu    1.228
_exptl_absorpt_correction_T_max  0.8587
_exptl_absorpt_correction_T_min  0.4925
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.889
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.67
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         3.004
_refine_diff_density_min         -1.851
_refine_diff_density_rms         0.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2692
_refine_ls_number_reflns         12977
_refine_ls_number_restraints     4125
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1398
_refine_ls_R_factor_gt           0.1087
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0895P)^2^+97.7974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2518
_refine_ls_wR_factor_ref         0.2700
_reflns_number_gt                9575
_reflns_number_total             12977
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc02949f2.cif
_cod_data_source_block           prc82ada
_cod_original_cell_volume        5100.8(16)
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C94.50 H14 Pr S5'
_cod_database_code               7115496