Intramolecular carboboration of carbonyl ligands to form boroxycarbenes
Celedonio M. Alvarez; Romen Carrillo; Raul Garcia-Rodriguez; Daniel Miguel; Chem.Commun. 48 (2012) 7705–; doi:10.1039/c2cc33443g

data_7108081
_publ_section_title
;
 Intramolecular carboboration of carbonyl ligands to form boroxycarbenes
;
_journal_name_full               Chem.Commun.
_journal_page_first              7705
_journal_paper_doi               10.1039/c2cc33443g
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C13 H15 Br N O5 Re'
_chemical_formula_weight         531.37
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.642(5)
_cell_angle_beta                 66.993(5)
_cell_angle_gamma                74.222(5)
_cell_formula_units_Z            2
_cell_length_a                   9.083(3)
_cell_length_b                   9.093(3)
_cell_length_c                   11.271(4)
_cell_measurement_reflns_used    886
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      2.858
_cell_volume                     813.9(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6731
_diffrn_reflns_theta_full        25.73
_diffrn_reflns_theta_max         25.73
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    9.938
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.441382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    2.168
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.032
_refine_diff_density_min         -1.266
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       0.0037(5)
_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   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         3080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0419P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0717
_reflns_number_gt                2640
_reflns_number_total             3080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc33443g.txt
_cod_data_source_block           Compound_((Re)_rg741cm
_cod_original_cell_volume        813.9(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7108081