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_4116374
_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
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 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            'C22 H18'
_chemical_formula_weight         282.36
_chemical_name_common            Phenylbicubane
_chemical_name_systematic        1-Phenyl-p-[2]cubyl
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 107.52(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.889(4)
_cell_length_b                   34.220(11)
_cell_length_c                   7.690(3)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      5.16
_cell_volume                     1477.8(13)
_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      293(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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0968
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2746
_diffrn_reflns_theta_max         45.00
_diffrn_reflns_theta_min         2.58
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_T_max  0.9893
_exptl_absorpt_correction_T_min  0.8901
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            clear_colorless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       v_thin_plate
_exptl_crystal_F_000             600
_exptl_crystal_size_max          .02
_exptl_crystal_size_mid          .36
_exptl_crystal_size_min          .26
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0031(10)
_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   1.049
_refine_ls_goodness_of_fit_obs   1.165
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         1188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_restrained_S_obs      1.165
_refine_ls_R_factor_all          0.1432
_refine_ls_R_factor_obs          0.0771
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1289P)^2^+1.1626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2674
_refine_ls_wR_factor_obs         0.1913
_reflns_number_observed          660
_reflns_number_total             1195
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja983441f_5.cif
_cod_data_source_block           eat37x3a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1289P)^2^+1.1626P] 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^)+(0.1289P)^2^+1.1626P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1477.7(13)
_cod_database_code               4116374