The First Structurally Characterized Homofullerene (Fulleroid)
Andrew F. Kiely; Robert C. Haddon; Mark S. Meier; John P. Selegue; Carolyn Pratt Brock; Brian O. Patrick; Guan-Wu Wang; Yongsheng Chen; Journal of the American Chemical Society 121 (1999) 7971–7972; doi:10.1021/ja991692y

data_4116505
_publ_contact_author
;
                                  Prof. Carolyn P. Brock
                                  Department of Chemistry
                                  University of Kentucky
                                  Lexington, KY  40506-0055
                                  USA
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_publ_contact_author_email       cpbrock@ukcc.uky.edu
_publ_contact_author_fax         '606 323 1069'
_publ_contact_author_phone       '606 257 1959'
_publ_section_title
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 The First Structurally Characterized Homofullerene (Fulleroid)
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7971
_journal_page_last               7972
_journal_paper_doi               10.1021/ja991692y
_journal_volume                  121
_journal_year                    1999
_chemical_compound_source
;
Synthesized in the laboratory of Mark S. Meier
;
_chemical_formula_moiety         '(C71 Cl2), 0.445(C5 H12), 0.055(C7 H8)'
_chemical_formula_sum            'C73.61 H5.78 Cl2'
_chemical_formula_weight         960.86
_chemical_name_systematic
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7,8-dichloromethanohomo70-fullerene
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_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             99-04-27
_audit_creation_method           'created by SHELXL-93 and C P Brock'
_cell_angle_alpha                90.
_cell_angle_beta                 96.75(1)
_cell_angle_gamma                90.
_cell_formula_units_Z            8
_cell_length_a                   17.876(1)
_cell_length_b                   10.730(1)
_cell_length_c                   37.935(2)
_cell_measurement_reflns_used    53613
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.67
_cell_volume                     7225.9(9)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT software (Nonius, 1998)'
_computing_data_reduction        'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL PC (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(1)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 25.0
_diffrn_measurement_device       'Nonius Kappa-CCD diffractometer'
_diffrn_measurement_method       '\w scans with 1\% steps'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.143
_diffrn_reflns_av_sigmaI/netI    0.189
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            23001
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        <2
_exptl_absorpt_coefficient_mu    0.25
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_description
;
Laths.
;
_exptl_crystal_F_000             3851.5
_exptl_crystal_preparation
;
Crystals were grown by slow evaporation of n-pentane/toluene solutions.
;
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.42
_refine_diff_density_rms         0.07
_refine_ls_extinction_coef       0.00072(13)
_refine_ls_extinction_expression Fc^*^=kFc+0.001xFc^2^\l^3^/sin(2\q)|^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.10
_refine_ls_goodness_of_fit_obs   1.25
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1369
_refine_ls_number_reflns         12647
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.10
_refine_ls_restrained_S_obs      1.26
_refine_ls_R_factor_all          0.175
_refine_ls_R_factor_obs          0.089
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.00
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/\s^2^(Fo^2^)+(0.0343P)^2^+10.5000P| where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.144
_refine_ls_wR_factor_obs         0.126
_reflns_number_observed          8032
_reflns_number_total             12658
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja991692y.cif
_cod_data_source_block           C71-110
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/\s^2^(Fo^2^)+(0.0343P)^2^+10.5000P| where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/\s^2^(Fo^2^)+(0.0343P)^2^+10.5000P| where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4116505