Importance of Open Structure of Nonmetal Based Catalyst in Hydrogen Bond Promoted Methanolysis of Activated Amide: Structure Dynamics between Monomer and Dimer Enabling Recombinant Covalent, Dative, and Hydrogen Bonds
Oishi, Shunsuke; Yoshimoto, Junichi; Saito, Susumu; Journal of the American Chemical Society 131 (2009) 8748–8749; doi:10.1021/ja9029494

data_4119128
_publ_section_title
;
 Importance of Open Structure of Nonmetal Based Catalyst in Hydrogen Bond
 Promoted Methanolysis of Activated Amide: Structure Dynamics between
 Monomer and Dimer Enabling Recombinant Covalent, Dative, and Hydrogen
 Bonds
;
_journal_coden_ASTM              JACSAT
_journal_issue                   25
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8748
_journal_page_last               8749
_journal_paper_doi               10.1021/ja9029494
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C16 H20 B Cl N2'
_chemical_formula_weight         286.60
_chemical_name_common            closed-1b
_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                91.120(6)
_cell_angle_beta                 96.552(6)
_cell_angle_gamma                112.679(7)
_cell_formula_units_Z            4
_cell_length_a                   10.165(5)
_cell_length_b                   10.657(5)
_cell_length_c                   15.576(7)
_cell_measurement_reflns_used    1794
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.1979
_cell_volume                     1543.0(13)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_molecular_graphics    'ORTEP 3 for windows'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type
;
Saturn70 CCD (4x4 bin mode) with MicroMax-007
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0862
_diffrn_reflns_av_sigmaI/netI    0.1707
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10865
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.20
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_T_max  0.9538
_exptl_absorpt_correction_T_min  0.9538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         5609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1832
_refine_ls_R_factor_gt           0.0916
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1889
_refine_ls_wR_factor_ref         0.2461
_reflns_number_gt                2772
_reflns_number_total             5609
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4104628
_cod_data_source_file            ja9029494sup1.cif
_cod_data_source_block           closed-1b
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4119128