Synthesis, structure and palladium coordination of ambiphilic, pyridine- and phosphine-tethered N-boryl imine ligands.
Lorenzini, Fabio; Lagueux-Tremblay, Pierre-Louis; Kayser, Laure V.; Anderson, Ethan; Arndtsen, Bruce A.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 5766–5772; doi:10.1039/c8dt05100c

data_7049384
_publ_section_title
;
 Synthesis, structure and palladium coordination of ambiphilic, pyridine-
 and phosphine-tethered N-boryl imine ligands.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5766
_journal_page_last               5772
_journal_paper_doi               10.1039/c8dt05100c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C24 H20 B N2, C F3 O3 S'
_chemical_formula_sum            'C25 H20 B F3 N2 O3 S'
_chemical_formula_weight         496.30
_chemical_name_systematic
'[N-(diphenylboryl)-2-benzoylpyridinketimine]H+OTf-'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-03-16 deposited with the CCDC.    2019-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.7270(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.2146(6)
_cell_length_b                   18.4610(10)
_cell_length_c                   22.6386(12)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      55.512
_cell_measurement_theta_min      4.298
_cell_volume                     4571.8(4)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'bruker APEX2'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'ShelXle (J. Appl. Cryst. 2011, 44, 1281-1284)'
_computing_publication_material  'ShelXle (J. Appl. Cryst. 2011, 44, 1281-1284)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            51660
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.413
_diffrn_reflns_theta_min         1.438
_exptl_absorpt_coefficient_mu    0.198
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       losange
_exptl_crystal_F_000             2048
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         10701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+3.7925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1159
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8262
_reflns_number_total             10701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05100c2.cif
_cod_data_source_block           Compound1aHOTf
_cod_depositor_comments
'Adding full bibliography for 7049383--7049388.cif.'
_cod_database_code               7049384
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.925
_shelx_estimated_absorpt_t_max   0.986
_shelx_res_checksum              78258