Stepwise Bromination of Two Acetylene Molecules on a Butterfly-Type Tetrairon Core and Reactivity of the Resulting Bromoacetylene Fragment toward Nucleophiles
Masato Takano; Masaaki Okazaki; Hiromi Tobita; Journal of the American Chemical Society 126 (2004) 9190–9191; doi:10.1021/ja047569a

data_4112797
_publ_contact_author_address
;Department of Chemistry, Graduate School of Science
Tohoku University
Sendai 980-8578, JAPAN.
;
_publ_contact_author_email       mokazaki@mail.tains.tohoku.ac.jp
_publ_contact_author_fax         +81-22-217-6543
_publ_contact_author_name        'Masaaki Okazaki'
_publ_contact_author_phone       +81-22-217-6541
_publ_section_title
;
 Stepwise Bromination of Two Acetylene Molecules on a Butterfly-Type
 Tetrairon Core and Reactivity of the Resulting Bromoacetylene Fragment
 toward Nucleophiles
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9190
_journal_page_last               9191
_journal_paper_doi               10.1021/ja047569a
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         C33H36Fe4N1''P1F6''P1F6''C1H1.5N0.5
_chemical_formula_sum            'C34 H37.5 F12 Fe4 N1.5 P2'
_chemical_formula_weight         980.50
_chemical_name_common            cluster[7](PF6)2
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 92.868(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1054(6)
_cell_length_b                   14.1386(7)
_cell_length_c                   21.0710(11)
_cell_measurement_reflns_used    30772
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.90
_cell_volume                     3601.9(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0869
_diffrn_reflns_av_sigmaI/netI    0.0698
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28029
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         0.97
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    1.759
_exptl_absorpt_correction_T_max  0.8437
_exptl_absorpt_correction_T_min  0.8437
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   NUM2
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.942
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.201
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         14608
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0704P)^2^+16.4362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1730
_reflns_number_gt                12983
_reflns_number_total             14608
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja047569asi20040611_121610.cif
_cod_data_source_block           py
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C34 H37.50 F12 Fe4 N1.50 P2'
_cod_database_code               4112797