Novel Ruthenium Complex-Catalyzed Dimerization of 2,5-Norbornadiene to Pentacyclo[6.6.0.0^2,6^.0^3,13^.0^10,14^]tetradeca-4,11-diene Involving Carbon-Carbon Bond Cleavage
Take-aki Mitsudo; Toshiaki Suzuki; Shi-Wei Zhang; Daisuke Imai; Ken-ichi Fujita; Takao Manabe; Masashi Shiotsuki; Yoshihisa Watanabe; Kenji Wada; Teruyuki Kondo; Journal of the American Chemical Society 121 (1999) 1839–1850; doi:10.1021/ja9835741

data_4116338
_publ_contact_author_address
;
Department of Energy and Hydrocarbon Chemistry, Graduate School of
Engineering, Kyoto University, Sakyo-ku, Kyoto 606-8501, Japan
;
_publ_contact_author_email       mitsudo@ep3000.scl.kyoto-u.ac.jp
_publ_contact_author_fax         +81-75-753-4976
_publ_contact_author_name        'Take-aki Mitsudo'
_publ_contact_author_phone       +81-75-753-5685
_publ_section_title
;
Novel Ruthenium Complex-Catalyzed Dimerization of 2,5-Norbornadiene to 
Pentacyclo[6.6.0.0^2,6^.0^3,13^.0^10,14^]tetradeca-4,11-diene Involving 
Carbon-Carbon Bond Cleavage
;
_journal_issue                   9
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1839
_journal_page_last               1850
_journal_paper_doi               10.1021/ja9835741
_journal_volume                  121
_journal_year                    1999
_chemical_compound_source        'prepared by T. Mitsudo'
_chemical_formula_analytical     'C14 H16 Br4'
_chemical_formula_moiety         'C14 H16 Br4'
_chemical_formula_structural     'C14 H16 Br4'
_chemical_formula_sum            'C14 H16 Br4'
_chemical_formula_weight         503.90
_chemical_melting_point          506(1)
_chemical_name_common            tetrabromopentacyclotetradecane
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_audit_creation_date             'Sat Oct 17 12:49:52 1998'
_audit_creation_method           'from TEXRAY.INF file'
_audit_update_record             'Mon Oct 20 1998'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.183(4)
_cell_length_b                   16.477(4)
_cell_length_c                   6.387(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    291.2
_cell_measurement_theta_max      13.3
_cell_measurement_theta_min      10.5
_cell_volume                     1492.6(11)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_molecular_graphics    'ORTEP (Johnson 1976)'
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      291.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.00681
_diffrn_orient_matrix_UB_12      -0.04577
_diffrn_orient_matrix_UB_13      -0.10170
_diffrn_orient_matrix_UB_21      -0.00506
_diffrn_orient_matrix_UB_22      -0.03918
_diffrn_orient_matrix_UB_23      0.11904
_diffrn_orient_matrix_UB_31      -0.06999
_diffrn_orient_matrix_UB_32      0.00728
_diffrn_orient_matrix_UB_33      0.00128
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_sigmaI/netI    0.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2310
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         0.00
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        9.65
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    10.664
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.715
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.242
_exptl_crystal_description       plate
_exptl_crystal_F_000             960.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.77
_refine_diff_density_min         -0.88
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     'Zachariasen(1967) type 2 gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.880
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     116
_refine_ls_number_reflns         729
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0000
_refine_ls_R_factor_gt           0.0000
_refine_ls_shift/su_max          0.1320
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00003|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0000
_refine_ls_wR_factor_ref         0.0340
_reflns_number_gt                0
_reflns_number_total             2310
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ja9835741_1.cif
_cod_data_source_block           C14H16Br4
_cod_depositor_comments
;
Moving '_atom_site_refinement_flags' tag values which correspond to atom 
names to '_atom_site_calc_attached_atom' tag. Removed values were 
replaced with a '?'.

Antanas Vaitkus,
2015-03-29
;
_cod_original_cell_volume        1492(1)
_cod_database_code               4116338