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_7108076
_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 H11 F3 Mn N O8 S'
_chemical_formula_weight         453.23
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 105.772(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.030(4)
_cell_length_b                   8.432(3)
_cell_length_c                   16.566(5)
_cell_measurement_reflns_used    933
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.035
_cell_measurement_theta_min      2.320
_cell_volume                     1751.6(10)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11433
_diffrn_reflns_theta_full        23.32
_diffrn_reflns_theta_max         23.32
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.946
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.799375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         2542
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0451P)^2^+0.3602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                1716
_reflns_number_total             2542
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc33443g.txt
_cod_data_source_block           Compound_3OTf_rg524cm
_cod_original_cell_volume        1751.4(10)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7108076