Synthesis and X-ray or NMR/DFT Structure Elucidation of Twenty-One New Trifluoromethyl Derivatives of Soluble Cage Isomers of C76, C78, C84, and C90
Ivan E. Kareev; Alexey A. Popov; Igor V. Kuvychko; Natalia B. Shustova; Sergey F. Lebedkin; Vyachevslav P. Bubnov; Oren P. Anderson; Konrad Seppelt; Steven H. Strauss; Olga V. Boltalina; Journal of the American Chemical Society 130 (2008) 13471–13489; doi:10.1021/ja8041614

data_4108430
_publ_section_title
;
 Synthesis and X-ray or NMR/DFT Structure Elucidation of Twenty-One New
 Trifluoromethyl Derivatives of Soluble Cage Isomers of C76, C78, C84, and
 C90
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13471
_journal_page_last               13489
_journal_paper_doi               10.1021/ja8041614
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C88F30, C7H8'
_chemical_formula_sum            'C95 H8 F30'
_chemical_formula_weight         1719.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 110.048(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.444(2)
_cell_length_b                   18.791(4)
_cell_length_c                   14.883(3)
_cell_measurement_reflns_used    9583
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      30.47
_cell_measurement_theta_min      2.61
_cell_volume                     3006.6(10)
_computing_cell_refinement       'APEX2, v. 2.0-2, Bruker AXS, 2006'
_computing_data_collection       'APEX2, v. 2.0-2, Bruker AXS, 2006'
_computing_data_reduction        'APEX2, v. 2.0-2, Bruker AXS, 2006'
_computing_molecular_graphics    'SHELXTL, v. 6.14, Bruker AXS'
_computing_publication_material  'SHELXTL, v. 6.14, Bruker AXS'
_computing_structure_refinement  'SHELXTL, v. 6.14, Bruker AXS'
_computing_structure_solution    'SHELXTL, v. 6.14, Bruker AXS'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEX II diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0680
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            57502
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.176
_exptl_absorpt_correction_T_max  0.9825
_exptl_absorpt_correction_T_min  0.9019
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, v. 2.10, Bruker AXS, Madison, WI'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_description       plate
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         7684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1028P)^2^+1.2350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1550
_refine_ls_wR_factor_ref         0.1695
_reflns_number_gt                5721
_reflns_number_total             7684
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8041614_si_003.cif
_cod_data_source_block           ss220r1_0m
_cod_original_cell_volume        3006.5(10)
_cod_database_code               4108430