Building with Cubane-1,4-diyl. Synthesis of Aryl-Substituted Cubanes, p-[n]Cubyls, and Cubane-Separated Bis(arenes)1
Eaton, Philip E.; Pramod, Kakumanu; Emrick, Todd; Gilardi, Richard; Journal of the American Chemical Society 121 (1999) 4111–4123; doi:10.1021/ja983441f

data_4116371
_publ_contact_author
;
      Richard Gilardi
      Laboratory for the Structure of Matter
      The Naval Research Laboratory, Code 6030
      Washington, D. C. ; USA 20375-5341
;
_publ_contact_author_email       gilardi@nrl.navy.mil
_publ_contact_author_fax         '202 767 6874'
_publ_contact_author_phone       '202 404 2135'
_publ_section_title
;
 Building with Cubane-1,4-diyl. Synthesis of Aryl-Substituted Cubanes,
 p-[n]Cubyls, and Cubane-Separated Bis(arenes)1
;
_journal_coden_ASTM              JACSAT
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4111
_journal_page_last               4123
_journal_paper_doi               10.1021/ja983441f
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C16 H12 I2'
_chemical_formula_weight         458.06
_space_group_IT_number           166
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   8.9775(3)
_cell_length_b                   8.9775(3)
_cell_length_c                   15.3644(10)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      15.03
_cell_measurement_theta_min      7.04
_cell_volume                     1072.40(9)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            804
_diffrn_reflns_theta_max         28.97
_diffrn_reflns_theta_min         2.94
_diffrn_standards_decay_%        18.27
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.378
_exptl_absorpt_correction_T_max  0.4360
_exptl_absorpt_correction_T_min  0.2418
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    2.128
_exptl_crystal_description       almost-cubic_chunk
_exptl_crystal_F_000             642
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.239
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       0.0016(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.166
_refine_ls_goodness_of_fit_obs   1.215
_refine_ls_matrix_type           full
_refine_ls_number_parameters     27
_refine_ls_number_reflns         373
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.166
_refine_ls_restrained_S_obs      1.215
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_obs          0.0265
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0655
_refine_ls_wR_factor_obs         0.0631
_reflns_number_observed          323
_reflns_number_total             373
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja983441f_2.cif
_cod_data_source_block           eat32
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+0.0000P] 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^)+(0.0341P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               4116371