Addition of diprotic nucleophiles to a C60‒tetrazine monoadduct: structural reassignment and correction of a novel rearrangement
Miller, Glen P.; Tetreau, Mark C.; Olmstead, Marilyn M.; Lord, Pamela A.; Balch, Alan L.; Chemical Communications  (2001) 1758–; doi:10.1039/b104151g

data_7114686
_publ_section_title
;
 Addition of diprotic nucleophiles to a C60--tetrazine monoadduct:
 structural reassignment and correction of a novel rearrangement
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              1758
_journal_paper_doi               10.1039/b104151g
_journal_year                    2001
_chemical_formula_sum            'C82 H19 N5 S4'
_chemical_formula_weight         1202.26
_chemical_name_common            'RC60H~2~.2CS~2~, compound 3'
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0656(9)
_cell_length_b                   14.3786(9)
_cell_length_c                   25.8201(17)
_cell_measurement_reflns_used    6913
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      2.2
_cell_volume                     4850.7(6)
_computing_cell_refinement       'Bruker SAINT'
_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      91(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker SMART 1000'
_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  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0384
_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       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            64323
_diffrn_reflns_theta_full        31.51
_diffrn_reflns_theta_max         31.51
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_time  'beginning and end of data collection'
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_T_max  0.9255
_exptl_absorpt_correction_T_min  0.8627
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS 2.0 (Sheldrick, 2000)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.986
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         15217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0872
_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^)+(0.1117P)^2^+8.5293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2125
_refine_ls_wR_factor_ref         0.2314
_reflns_number_gt                12123
_reflns_number_total             15217
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104151g.txt
_cod_data_source_block           mn1179
_cod_original_sg_symbol_H-M      'P 2~1~ 2~1~ 2~1~'
_cod_database_code               7114686