Efficient cage-opening cascade process for the preparation of water-encapsulated [60]fullerene derivatives.
Zhang, Qianyan; Jia, Zhenshan; Liu, Shuming; Zhang, Gang; Xiao, Zuo; Yang, Dazhi; Gan, Liangbing; Wang, Zheming; Li, Yuliang; Organic letters 11 (2009) 2772–2774; doi:10.1021/ol9009305

data_1503975
_publ_section_title
;
 Efficient cage-opening cascade process for the preparation of
 water-encapsulated [60]fullerene derivatives.
;
_journal_issue                   13
_journal_name_full               'Organic letters'
_journal_page_first              2772
_journal_page_last               2774
_journal_paper_doi               10.1021/ol9009305
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C73.8 H12.9 N2 O6.3 S2.4'
_chemical_formula_weight         1105.11
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.8266(5)
_cell_angle_beta                 104.6941(5)
_cell_angle_gamma                94.1097(8)
_cell_formula_units_Z            4
_cell_length_a                   14.0617(2)
_cell_length_b                   17.0906(2)
_cell_length_c                   19.3399(3)
_cell_measurement_reflns_used    46533
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     4481.69(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_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  0.0586
_diffrn_reflns_av_sigmaI/netI    0.0813
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            76597
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.44
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995, 1997)
;
_exptl_crystal_colour            'black red'
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'long plate'
_exptl_crystal_F_000             2234
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1549
_refine_ls_number_reflns         20300
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1349
_refine_ls_R_factor_gt           0.0648
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1180P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1726
_refine_ls_wR_factor_ref         0.2011
_reflns_number_gt                10782
_reflns_number_total             20300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol9009305_si_002.cif
_cod_data_source_block           09jan20a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constr.' was replaced with the
value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_formula_sum        'C73.80 H12.90 N2 O6.30 S2.40'
_cod_database_code               1503975