Cationic Terminal Borylenes by Halide Abstraction: Synthesis and Spectroscopic and Structural Characterization of an FeB Double Bond
Deborah L. Coombs; Simon Aldridge; Cameron Jones; David J. Willock; Journal of the American Chemical Society 125 (2003) 6356–6357; doi:10.1021/ja0346936

data_4113765
_publ_section_title
;
 Cationic Terminal Borylenes by Halide Abstraction: Synthesis and
 Spectroscopic and Structural Characterization of an FeB Double Bond
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6356
_journal_page_last               6357
_journal_paper_doi               10.1021/ja0346936
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C53.5 H39 B2 Cl F24 Fe O2'
_chemical_formula_weight         1282.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 93.81(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   36.301(7)
_cell_length_b                   25.675(5)
_cell_length_c                   23.956(5)
_cell_measurement_temperature    150(2)
_cell_volume                     22278(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Nonius Kappa CCD '
_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  0.0553
_diffrn_reflns_av_sigmaI/netI    0.0956
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            34393
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    0.440
_exptl_absorpt_correction_T_max  0.9370
_exptl_absorpt_correction_T_min  0.8613
_exptl_absorpt_correction_type   'Sortav (Blessing 1995) '
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       prism
_exptl_crystal_F_000             10320
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.00007(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1560
_refine_ls_number_reflns         19345
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.1679
_refine_ls_R_factor_gt           0.0888
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0829P)^2^+124.1025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1974
_refine_ls_wR_factor_ref         0.2356
_reflns_number_gt                10780
_reflns_number_total             19345
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0346936si20030217_061423.cif
_cod_data_source_block           compoundX
_cod_original_formula_sum        'C53.50 H39 B2 Cl F24 Fe O2'
_cod_database_code               4113765