"Third-Generation"-Type Functional Tris(2-pyridyl)borate Ligands and Their Transition-Metal Complexes.
Jeong, So Yi; Lalancette, Roger A.; Lin, Huina; Lupinska, Patrycja; Shipman, Patrick O.; John, Alexandra; Sheridan, John B.; Jäkle, Frieder; Inorganic chemistry 55 (2016) 3605–3615; doi:10.1021/acs.inorgchem.6b00124

data_4347404
_publ_section_title
;
 &quot;Third-Generation&quot;-Type Functional Tris(2-pyridyl)borate
 Ligands and Their Transition-Metal Complexes.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3605
_journal_page_last               3615
_journal_paper_doi               10.1021/acs.inorgchem.6b00124
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C24 H26 B N3 Si'
_chemical_formula_sum            'C24 H26 B N3 Si'
_chemical_formula_weight         395.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90.00
_cell_angle_beta                 109.493(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.2456(2)
_cell_length_b                   7.2679(1)
_cell_length_c                   14.5517(3)
_cell_measurement_reflns_used    7293
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.5
_cell_measurement_theta_min      3.22
_cell_volume                     1121.17(3)
_computing_cell_refinement       'APEX 2'
_computing_data_collection       'APEX 2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008b)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Bruker SMART CCD Apex-II area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10329
_diffrn_reflns_point_group_measured_fraction_full 0.908
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.497
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.018
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3704
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+0.1639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0834
_reflns_Friedel_coverage         0.734
_reflns_Friedel_fraction_full    0.845
_reflns_Friedel_fraction_max     0.812
_reflns_number_gt                3411
_reflns_number_total             3704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00124_si_002.cif
_cod_data_source_block           TpybSi
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4347404
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              78975
_shelx_hkl_checksum              33008