New Tetraazaannulene Hosts for Fullerenes
Jimmy U. Franco; Justin C. Hammons; Daniel Rios; Marilyn M. Olmstead; Inorganic Chemistry 49 (2010) 5120–5125; doi:10.1021/ic1002513

data_4315616
_publ_contact_author_email       mmolmstead@ucdavis.edu
_publ_contact_author_fax         5307528995
_publ_contact_author_name        'Marilyn M. Olmstead'
_publ_section_title
;
 New Tetraazaannulene Hosts for Fullerenes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5120
_journal_page_last               5125
_journal_paper_doi               10.1021/ic1002513
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C60, C22 H18 Cl4 N4 Ni, 2(C S2)'
_chemical_formula_sum            'C84 H18 Cl4 N4 Ni S4'
_chemical_formula_weight         1411.77
_chemical_name_common            Ni(Cl4TMTAA).C60.2CS2
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 106.583(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.6523(15)
_cell_length_b                   13.1967(9)
_cell_length_c                   19.5618(13)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.9
_cell_measurement_theta_min      3.2
_cell_volume                     5357.1(6)
_computing_cell_refinement       'SAINT 7.46A (Bruker, 2008)'
_computing_data_collection       'Apex2 (Bruker, 2008)'
_computing_data_reduction        'SAINT 7.46A (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL, XP (sheldrick, 1994)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART ApexII'
_diffrn_measurement_method       \w
_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  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29158
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/4 (Sheldrick, 2007)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.86
_exptl_crystal_size_mid          0.82
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.986
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         6136
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0521P)^2^+11.2223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0961
_reflns_number_gt                5456
_reflns_number_total             6136
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic1002513_si_002_1.cif
_cod_data_source_block           juf45
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4315616