Synthesis of an Extremely Crowded Naphthalene via a Stable Norbornadienone
Jiajia Zhang; Douglas M. Ho; Robert A. Pascal; Journal of the American Chemical Society 123 (2001) 10919–10926; doi:10.1021/ja011453m

data_4115760
_publ_section_title
;
 Synthesis of an Extremely Crowded Naphthalene via a Stable
 Norbornadienone
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10919
_journal_page_last               10926
_journal_paper_doi               10.1021/ja011453m
_journal_volume                  123
_journal_year                    2001
_chemical_compound_source        'chemical synthesis'
_chemical_formula_moiety         'C46 H46 Br2'
_chemical_formula_structural     'C46 H46 Br2'
_chemical_formula_sum            'C46 H46 Br2'
_chemical_formula_weight         758.65
_chemical_name_systematic
; 
 5,6,8-Tri(t-butyl)-2,3-bis(4-bromophenyl)-1,4-diphenylnaphthalene 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 104.0340(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7798(4)
_cell_length_b                   10.6379(3)
_cell_length_c                   27.2058(9)
_cell_measurement_reflns_used    35580
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.52
_cell_volume                     3869.0(2)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '1000 0.5-degree frames, 120 seconds/degree'
_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  0.046
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            35580
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.52
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.125
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.019
_refine_ls_goodness_of_fit_obs   1.075
_refine_ls_hydrogen_treatment    'XYZ riding, U(H) = 1.2U(C) or 1.5U(Cmethyl)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         8853
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_restrained_S_obs      1.075
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_obs          0.0490
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+5.1538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1132
_refine_ls_wR_factor_obs         0.1005
_reflns_number_observed          6379
_reflns_number_total             8853
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja011453m_4.cif
_cod_data_source_block           rap056
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+5.1538P] 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^+5.1538P] 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               4115760