Solubilizing the Most Easily Ionized Molecules and Generating Powerful Reducing Agents
Gina M. Chiarella; F. Albert Cotton; Jason C. Durivage; Dennis L. Lichtenberger; Carlos A. Murillo; Journal of the American Chemical Society 135 (2013) 17889–17896; doi:10.1021/ja408291k

data_4121201
_publ_contact_author_address
;
Departmentof Chemistry, Texas A&M University,P.O. Box 3255, College Station,
Texas 77843-3255, USA
;
_publ_contact_author_email       'murillo@tamu.edu '
_publ_contact_author_name        'Carlos A. Murillo'
_publ_contact_author_phone       979-845-1533
_publ_section_title
;
 Solubilizing the Most Easily Ionized Molecules and Generating Powerful
 Reducing Agents
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17889
_journal_page_last               17896
_journal_paper_doi               10.1021/ja408291k
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C60 H112 N12 W2, 2(Cl)'
_chemical_formula_sum            'C60 H112 Cl2 N12 W2'
_chemical_formula_weight         1440.22
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 97.635(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.894(4)
_cell_length_b                   16.778(4)
_cell_length_c                   22.935(6)
_cell_measurement_reflns_used    7938
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.22
_cell_measurement_theta_min      2.16
_cell_volume                     6443(3)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SMART (Bruker, 2001)'
_computing_molecular_graphics    'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART 1K CCD area-detector'
_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  0.0729
_diffrn_reflns_av_sigmaI/netI    0.1111
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            42958
_diffrn_reflns_theta_full        27.65
_diffrn_reflns_theta_max         27.65
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.697
_exptl_absorpt_correction_T_max  0.6070
_exptl_absorpt_correction_T_min  0.4835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrick, 2004'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       block
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.353
_refine_diff_density_min         -1.423
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         14770
_refine_ls_number_restraints     290
_refine_ls_restrained_S_all      0.901
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1077
_reflns_number_gt                7930
_reflns_number_total             14770
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja408291k_si_002_1.cif
_cod_data_source_block           W2Cl2(TEhpp)4
_cod_database_code               4121201