Enhancing the Photochemical Stability of N,C-Chelate Boryl Compounds: C-C Bond Formation versus C=C Bond cis,trans-Isomerization
Chul Baik; Zachary M. Hudson; Hazem Amarne; Suning Wang; Journal of the American Chemical Society 131 (2009) 14549–14559; doi:10.1021/ja906430s

data_4105130
_publ_section_title
;
 Enhancing the Photochemical Stability of N,C-Chelate Boryl Compounds: C-C
 Bond Formation versus C=C Bond cis,trans-Isomerization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14549
_journal_page_last               14559
_journal_paper_doi               10.1021/ja906430s
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C99 H96 B3 N3'
_chemical_formula_weight         1360.22
_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                79.126(4)
_cell_angle_beta                 65.471(3)
_cell_angle_gamma                64.616(3)
_cell_formula_units_Z            2
_cell_length_a                   16.582(4)
_cell_length_b                   17.149(4)
_cell_length_c                   19.939(6)
_cell_measurement_reflns_used    2147
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      18.17
_cell_measurement_theta_min      2.22
_cell_volume                     4660(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      180(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.1126
_diffrn_reflns_av_sigmaI/netI    0.2219
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            50862
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    0.055
_exptl_absorpt_correction_T_max  0.9945
_exptl_absorpt_correction_T_min  0.9891
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    0.969
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Disordered solvent molecules CH2Cl2 and hexane are removed
;
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.180
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.786
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     964
_refine_ls_number_reflns         19197
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.786
_refine_ls_R_factor_all          0.1993
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.069
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1619
_reflns_number_gt                5614
_reflns_number_total             19197
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906430s_si_004.cif
_cod_data_source_block           baik1
_cod_database_code               4105130