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_4115305
_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
; 
CoC41H31 (CH2Cl2) 
;
_chemical_formula_sum            'C42 H33 Cl2 Co'
_chemical_formula_weight         667.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.265(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4538(7)
_cell_length_b                   22.1839(16)
_cell_length_c                   16.7388(12)
_cell_measurement_reflns_used    2042
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.043
_cell_measurement_theta_min      2.204
_cell_volume                     3504.8(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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_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  0.1112
_diffrn_reflns_av_sigmaI/netI    0.1887
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17709
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       bar
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.1507
_refine_ls_R_factor_gt           0.0573
_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 
 [0.00000+1.00000exp(3.50(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0302P)^2^+0.0000sin\q/\l] 
 where P = 0.33333Fo^2^ + 0.66667Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1315
_reflns_number_gt                1868
_reflns_number_total             5043
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja026809o_s3_3.cif
_cod_data_source_block           10e
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4115305