Structural and Thermodynamic Analysis of a Three-Component Assembly Forming ortho-Iminophenylboronate Esters.
Chapin, Brette M.; Metola, Pedro; Lynch, Vincent M.; Stanton, John F.; James, Tony D.; Anslyn, Eric V.; The Journal of organic chemistry 81 (2016) 8319–8330; doi:10.1021/acs.joc.6b01495

data_4037103
_publ_section_title
;
 Structural and Thermodynamic Analysis of a Three-Component Assembly
 Forming ortho-Iminophenylboronate Esters.
;
_journal_issue                   18
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              8319
_journal_page_last               8330
_journal_paper_doi               10.1021/acs.joc.6b01495
_journal_volume                  81
_journal_year                    2016
_chemical_formula_sum            'C20 H16 B N O2'
_chemical_formula_weight         313.15
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        '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                99.202(12)
_cell_angle_beta                 96.890(12)
_cell_angle_gamma                90.327(11)
_cell_formula_units_Z            4
_cell_length_a                   9.2797(18)
_cell_length_b                   10.762(2)
_cell_length_c                   16.496(4)
_cell_measurement_temperature    153(2)
_cell_volume                     1614.0(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1315
_diffrn_reflns_av_sigmaI/netI    0.2294
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28985
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.082
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             656
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         11089
_refine_ls_number_restraints     579
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.2080
_refine_ls_R_factor_gt           0.1035
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1411P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2246
_refine_ls_wR_factor_ref         0.2813
_reflns_number_gt                5530
_reflns_number_total             11089
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo6b01495_si_002.cif
_cod_data_source_block           shelxl
_cod_database_code               4037103