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_4315617
_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         'C30 H26 N4 Ni, 2(C6 H6)'
_chemical_formula_sum            'C42 H38 N4 Ni'
_chemical_formula_weight         657.47
_chemical_name_common            Ni(NapTMTAA).2benzene
_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                 95.371(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   26.1470(16)
_cell_length_b                   21.2466(16)
_cell_length_c                   23.8863(15)
_cell_measurement_reflns_used    5558
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      2.9
_cell_volume                     13211.4(15)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'Apex2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL 5.1, 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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0731
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            78603
_diffrn_reflns_theta_full        28.49
_diffrn_reflns_theta_max         28.49
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  0.835
_exptl_absorpt_correction_T_min  0.754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5536
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     886
_refine_ls_number_reflns         16677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0675P)^2^+15.0222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1185
_refine_ls_wR_factor_ref         0.1416
_reflns_number_gt                10830
_reflns_number_total             16677
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic1002513_si_002_2.cif
_cod_data_source_block           juf72
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4315617