Novel rearrangement of conformationally restrained [3.3]orthocyclophanes
Isobe, Shin-ichiro; Taniguchi, Masahiko; Sawada, Tsuyoshi; Thiemann, Thies; Yonemitsu, Tadashi; Mataka, Shuntaro; Journal of the Chemical Society, Perkin Transactions 1  (1999) 2101–; doi:10.1039/a903156a

data_7213086
_publ_section_title
;
 Novel rearrangement of conformationally restrained [3.3]orthocyclophanes
;
_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              2101
_journal_paper_doi               10.1039/a903156a
_journal_year                    1999
_chemical_formula_sum            'C35 H30'
_chemical_formula_weight         450.59
_chemical_melting_point          518.15
_chemical_name_common            11b
_chemical_name_systematic
; 
 1-(1'-Naphthyl)-4,5:9,10-dibenzobicyclo[5,4,0,02,11]undeca-4,9-diene 
;
_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                 94.688(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.260(4)
_cell_length_b                   19.770(9)
_cell_length_c                   10.336(2)
_cell_measurement_reflns_used    19
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      42
_cell_measurement_theta_min      22
_cell_volume                     2496.9(15)
_computing_cell_refinement       'CAD4 Enraf-Nonius software'
_computing_data_collection       'CAD4 Enraf-Nonius software'
_computing_data_reduction        'MolEN  Enraf-Nonius software'
_computing_molecular_graphics    'Xtal_GX (Hall & Boulay, 1995)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution
;SIR92 (Altomare, Burla, Camalli, Cascarano, Giacovazzo,
Guagliardi & Polidori, 1994) 
;
_diffrn_ambient_temperature      296(2)
_diffrn_measurement_device       Enraf_Nonius_CAD4
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuKa
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0768
_diffrn_reflns_av_sigmaI/netI    0.0619
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4817
_diffrn_reflns_theta_max         68.00
_diffrn_reflns_theta_min         3.62
_diffrn_standards_decay_%        -1.71
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         .202
_refine_diff_density_min         -.211
_refine_diff_density_rms         .055
_refine_ls_extinction_coef       0.0015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.108
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4548
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_restrained_S_obs      1.087
_refine_ls_R_factor_all          0.1323
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0732P)^2^+0.7478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1869
_reflns_number_gt                2481
_reflns_number_total             4549
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903156asup1.cif
_cod_data_source_block           11b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '245c' was changed to '518.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0732P)^2^+0.7478P] 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^)+( 0.0732P)^2^+0.7478P] 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      'p 1 21/c 1'
_cod_database_code               7213086