Mechanistic Studies on the Catalytic Synthesis of BN Heterocycles (1H-2,1-Benzazaboroles) at Ruthenium
Beguerie, Marion; Dinoi, Chiara; del Rosal, Iker; Faradji, Charly; Alcaraz, Gilles; Vendier, Laure; Sabo-Etienne, Sylviane; ACS Catalysis 8 (2018) 939–; doi:10.1021/acscatal.7b03461

data_4514344
_publ_section_title
;
 Mechanistic Studies on the Catalytic Synthesis of BN Heterocycles
 (1H-2,1-Benzazaboroles) at Ruthenium
;
_journal_issue                   2
_journal_name_full               'ACS Catalysis'
_journal_page_first              939
_journal_paper_doi               10.1021/acscatal.7b03461
_journal_volume                  8
_journal_year                    2018
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C31 H50 B N2 P Ru'
_chemical_formula_sum            'C31 H50 B N2 P Ru'
_chemical_formula_weight         593.58
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-09-26T16:30:40-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                103.406(2)
_cell_angle_beta                 99.818(2)
_cell_angle_gamma                90.008(2)
_cell_formula_units_Z            4
_cell_length_a                   9.9745(6)
_cell_length_b                   14.6282(9)
_cell_length_c                   21.2096(13)
_cell_measurement_reflns_used    9820
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.49
_cell_measurement_wavelength     0.71073
_cell_volume                     2963.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       \w-\f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         micro-source
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            63843
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.19
_diffrn_reflns_theta_min         1.002
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.33
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.65
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         14169
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+1.8880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0855
_reflns_Friedel_coverage         0
_reflns_number_gt                10987
_reflns_number_total             14169
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b03461_si_003.cif
_cod_data_source_block           MBO170316new
_cod_depositor_comments          'Adding full bibliography for 4514344.cif.'
_cod_database_code               4514344