Fullerenes without symmetry: crystallographic characterization of C1(30)‒C~90~ and C1(32)‒C~90~
Wang, Hua; Mercado, Brandon Q.; Jin, Hongxiao; Wang, Zhimin; Jiang, An; Li, Ziyang; Beavers, Christine M.; Olmstead, Marilyn M.; Balch, Alan L.; Chemical Communications (Cambridge, United Kingdom) 47 (2011) 2068–2070; doi:10.1039/c0cc03017a

data_7105962
_publ_section_title
;
 Fullerenes without symmetry: crystallographic characterization of
 C1(30)--C~90~ and C1(32)--C~90~
;
_journal_coden_ASTM              CHCOFS
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2068
_journal_page_last               2070
_journal_paper_doi               10.1039/c0cc03017a
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety
'C90, C36 H44 N4 Ni, C7 H8, 0.6(C7 H8), 0.4(C7 H8)'
_chemical_formula_sum            'C140 H60 N4 Ni'
_chemical_formula_weight         1856.63
_chemical_name_common            C1(30)-C90.NiOEP.2toluene
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/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                 95.4680(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.5124(6)
_cell_length_b                   15.2234(4)
_cell_length_c                   20.7457(5)
_cell_measurement_reflns_used    9403
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.8
_cell_measurement_theta_min      2.6
_cell_volume                     8020.7(3)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'Apex2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL, XP (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker SMART Apex II'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  silicon(111)
_diffrn_radiation_source         'Advanced Light Source, beamline 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            147412
_diffrn_reflns_theta_full        40.11
_diffrn_reflns_theta_max         40.11
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.390
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             3824
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.016
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1225
_refine_ls_number_reflns         19543
_refine_ls_number_restraints     1415
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0812
_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^)+(0.1982P)^2^+3.2354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2595
_refine_ls_wR_factor_ref         0.2835
_reflns_number_gt                15855
_reflns_number_total             19543
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            C0CC03017A.TXT
_cod_data_source_block           bqm58
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7105962