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_4315619
_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         'C22 H18 Cl4 N4 Ni, C H2 Cl2'
_chemical_formula_sum            'C23 H20 Cl6 N4 Ni'
_chemical_formula_weight         623.82
_chemical_name_common            Ni(Cl4TMTAA).CH2Cl2
_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                73.985(3)
_cell_angle_beta                 80.445(3)
_cell_angle_gamma                76.468(3)
_cell_formula_units_Z            8
_cell_length_a                   14.017(3)
_cell_length_b                   16.479(3)
_cell_length_c                   22.848(4)
_cell_measurement_reflns_used    4421
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      23.9
_cell_measurement_theta_min      2.8
_cell_volume                     4902.8(16)
_computing_cell_refinement       'Apex2 (Bruker, 2007)'
_computing_data_collection       'Apex2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART Apex II'
_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  0.117
_diffrn_reflns_av_sigmaI/netI    0.094
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            54423
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    1.467
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2007)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.253
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1277
_refine_ls_number_reflns         18677
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0413P)^2^+0.4275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1173
_reflns_number_gt                12695
_reflns_number_total             18677
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic1002513_si_002_4.cif
_cod_data_source_block           dr88tw
_cod_database_code               4315619