Synthesis and Explosive Decomposition of Organometallic Dehydro[18]annulenes: An Access to Carbon Nanostructures
Matthew Laskoski; Winfried Steffen; Jason G. M. Morton; Mark D. Smith; Uwe H. F. Bunz; Journal of the American Chemical Society 124 (2002) 13814–13818; doi:10.1021/ja026809o

data_4115306
_publ_contact_author             'Professor Uwe H. F. Bunz'
_publ_contact_author_address
;
University of South Carolina
Department of Chemistry and Biochemistry
GSRC
Columbia, South Carolina 29208
USA
;
_publ_contact_author_email       bunz@mail.chem.sc.edu
_publ_contact_author_fax         '803 777 9521'
_publ_contact_author_phone       '803 777 8436'
_publ_section_title
;
 Synthesis and Explosive Decomposition of Organometallic
 Dehydro[18]annulenes: An Access to Carbon Nanostructures
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13814
_journal_page_last               13818
_journal_paper_doi               10.1021/ja026809o
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety
; 
[FeC34H16]2 (CH2Cl2)1.5 
;
_chemical_formula_sum            'C35 H18 Cl1.5 Fe'
_chemical_formula_weight         547.52
_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                69.471(2)
_cell_angle_beta                 79.704(2)
_cell_angle_gamma                89.862(2)
_cell_formula_units_Z            4
_cell_length_a                   11.9820(10)
_cell_length_b                   13.2987(11)
_cell_length_c                   18.2560(16)
_cell_measurement_reflns_used    2314
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.013
_cell_measurement_theta_min      2.296
_cell_volume                     2674.7(4)
_computing_cell_refinement       'SAINT+ NT V6.02a (Bruker, 1998)'
_computing_data_collection       'SMART NT V5.619 (Bruker, 2000)'
_computing_data_reduction        'SAINT+ NT V6.02a'
_computing_molecular_graphics    'SHELXTL V5.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_sigmaI/netI    0.1202
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15028
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.21
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.736
_exptl_absorpt_correction_T_max  0.9670
_exptl_absorpt_correction_T_min  0.8409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1118
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         7681
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.1586
_refine_ls_R_factor_gt           0.0744
_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^)+(0.0975P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1703
_refine_ls_wR_factor_ref         0.2096
_reflns_number_gt                3682
_reflns_number_total             7681
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja026809o_s3_4.cif
_cod_data_source_block           13a
_cod_original_formula_sum        'C35 H18 Cl1.50 Fe'
_cod_database_code               4115306