Synthesis, Structure, and Reactivity of Naphthalyne-Co2(CO)6 Complexes
Nobuharu Iwasawa; Maiko Otsuka; Satomi Yamashita; Masao Aoki; Jun Takaya; Journal of the American Chemical Society 130 (2008) 6328–6329; doi:10.1021/ja801569q

data_4107802
_publ_section_title
;
 Synthesis, Structure, and Reactivity of Naphthalyne-Co2(CO)6 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6328
_journal_page_last               6329
_journal_paper_doi               10.1021/ja801569q
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C18 H7 Br Co2 O6'
_chemical_formula_sum            'C18 H7 Br Co2 O6'
_chemical_formula_weight         517.01
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.193(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.931(5)
_cell_length_b                   7.498(3)
_cell_length_c                   16.677(6)
_cell_measurement_reflns_used    17486
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.01
_cell_volume                     1869.6(12)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998) '
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku, 1998) '
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'R-AXIS RAPID IP area detector'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17486
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.01
_diffrn_source                   'rotating anode x-ray tube'
_exptl_absorpt_coefficient_mu    3.942
_exptl_absorpt_correction_T_max  0.5966
_exptl_absorpt_correction_T_min  0.3487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'absorption was corrected by ABSCOR'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+1.7826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0733
_reflns_number_gt                3666
_reflns_number_total             4241
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja801569q-file003.cif
_cod_data_source_block           ohtsuka1
_cod_original_cell_volume        1869.7(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4107802