Carbonyl Derivatives of Boradiazaindacene via Catalytic CO Insertion
Gilles Ulrich; Alexandre Haefele; Pascal Retailleau; Raymond Ziessel; Journal of Organic Chemistry 77 (2012) 5036–5048; doi:10.1021/jo300477p

data_4027222
_publ_contact_author_address
;Laboratoire de Chimie Organique et Spectroscopies Avanc\'ees (LCOSA)
CNRS, Universit\'e Louis Pasteur, Ecole de Chimie, Polym\`eres, 
Mat\'eriaux de Strasbourg (ECPM)
25 rue Becquerel
67087 Strasbourg Cedex 02
France
;
_publ_contact_author_email       'gulrich@unistra.fr; ziessel@unistra.fr'
_publ_contact_author_fax         0390242635
_publ_contact_author_name
;
Gilles Ulrich
Raymond Ziessel
;
_publ_contact_author_phone       0390242689
_publ_section_title
;
 Carbonyl Derivatives of Boradiazaindacene via Catalytic CO Insertion
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              5036
_journal_page_last               5048
_journal_paper_doi               10.1021/jo300477p
_journal_volume                  77
_journal_year                    2012
_chemical_formula_moiety         'C33 H35 B F2 N2 O4'
_chemical_formula_sum            'C33 H35 B F2 N2 O4'
_chemical_formula_weight         572.44
_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                106.330(8)
_cell_angle_beta                 96.692(5)
_cell_angle_gamma                92.331(5)
_cell_formula_units_Z            2
_cell_length_a                   7.702(2)
_cell_length_b                   11.706(3)
_cell_length_c                   17.463(5)
_cell_measurement_reflns_used    6572
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.49
_cell_measurement_theta_min      1
_cell_volume                     1496.2(7)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) COLLECT (Hooft, 1998)'
_computing_data_collection
'DENZO (Otwinowski & Minor, 1997) COLLECT (Hooft, 1998)'
_computing_data_reduction        'HKL package (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 1980-2004)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .990
_diffrn_measured_fraction_theta_max .990
_diffrn_measurement_device_type  'Nonius kappa-CCD diffractometer'
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0776
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8167
_diffrn_reflns_theta_full        21.39
_diffrn_reflns_theta_max         21.39
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepack (Minor & Otwinovski, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       plate
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         .327
_refine_diff_density_min         -.218
_refine_diff_density_rms         .052
_refine_ls_extinction_coef       0.048(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   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         3336
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.1309
_refine_ls_R_factor_gt           0.0947
_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^)+(0.0526P)^2^+4.9885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2305
_refine_ls_wR_factor_ref         0.2481
_reflns_number_gt                2285
_reflns_number_total             3336
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo300477p_si_001_2.cif
_cod_data_source_block           compound_1f
_cod_database_code               4027222