Crystallographic characterization of Kr@C60 in (0.09Kr@C60/0.91C60)·{NiII(OEP)}·2C6H6
Lee, Hon Man; Olmstead, Marilyn M.; Suetsuna, Tomohiro; Shimotani, Hidekazu; Dragoe, Nita; Cross, R. James; Kitazawa, Koichi; Balch, Alan L.; Chemical Communications  (2002) 1352–; doi:10.1039/b202925c

data_7114008
_publ_section_title
;
 Crystallographic characterization of Kr@C60 in
 (0.09Kr@C60/0.91C60)&#x00B7;{NiII(OEP)}&#x00B7;2C6H6
;
_journal_issue                   13
_journal_name_full               'Chemical Communications'
_journal_page_first              1352
_journal_paper_doi               10.1039/b202925c
_journal_year                    2002
_chemical_formula_sum            'C108 H56 N4 Ni'
_chemical_formula_weight         1468.28
_chemical_name_common            C60.Ni(OEP).2benzene
_chemical_name_systematic
;  
?  
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.583(4)
_cell_angle_beta                 75.762(4)
_cell_angle_gamma                75.615(5)
_cell_formula_units_Z            2
_cell_length_a                   14.1318(8)
_cell_length_b                   14.3851(9)
_cell_length_c                   17.2064(12)
_cell_measurement_reflns_used    6521
_cell_measurement_temperature    92(2)
_cell_measurement_theta_max      31.4
_cell_measurement_theta_min      2.2
_cell_volume                     3283.4(4)
_computing_cell_refinement       'Bruker SAINT/SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 5, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      92(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.906
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.022
_diffrn_reflns_av_sigmaI/netI    0.028
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44245
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         31.50
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.361
_exptl_absorpt_correction_T_max  0.9313
_exptl_absorpt_correction_T_min  0.8871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1026
_refine_ls_number_reflns         19789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+1.1345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1072
_reflns_number_gt                16575
_reflns_number_total             19789
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b202925c.txt
_cod_data_source_block           mn1209
_cod_database_code               7114008