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_7108080
_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            'C9 H7 Br Mn N O4'
_chemical_formula_weight         328.01
_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                 114.688(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.534(6)
_cell_length_b                   11.294(4)
_cell_length_c                   13.542(5)
_cell_measurement_reflns_used    736
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.205
_cell_measurement_theta_min      2.440
_cell_volume                     2297.6(14)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0872
_diffrn_reflns_av_sigmaI/netI    0.0931
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8735
_diffrn_reflns_theta_full        25.41
_diffrn_reflns_theta_max         25.41
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    4.623
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.585207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.896
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.841
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.841
_refine_ls_R_factor_all          0.1443
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0342P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.1019
_reflns_number_gt                948
_reflns_number_total             2117
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc33443g.txt
_cod_data_source_block           C_8_rg740cm
_cod_original_cell_volume        2297.7(13)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7108080