Electrophilic and Nucleophilic Displacement Reactions at the Bridgehead Borons of Tris(pyridyl)borate Scorpionate Complexes
Goura, Joydeb; McQuade, James; Shimoyama, Daisuke; Lalancette, Roger A.; Sheridan, John B.; Jaekle, Frieder; Chemical Communications  (2022) –; doi:10.1039/D1CC06181J

data_7129475
_publ_section_title
;
 Electrophilic and Nucleophilic Displacement Reactions at the Bridgehead
 Borons of Tris(pyridyl)borate Scorpionate Complexes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06181J
_journal_year                    2022
_chemical_formula_moiety         'C50 H50 B2 N6 Ru'
_chemical_formula_sum            'C50 H50 B2 N6 Ru'
_chemical_formula_weight         857.65
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_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-10-25 deposited with the CCDC.	2021-12-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   35.5240(4)
_cell_length_b                   35.5240(4)
_cell_length_c                   9.91390(10)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.91
_cell_measurement_theta_min      2.49
_cell_volume                     10834.7(2)
_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    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.885
_diffrn_measured_fraction_theta_max 0.880
_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  0.0430
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_Laue_measured_fraction_full 0.885
_diffrn_reflns_Laue_measured_fraction_max 0.880
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            20068
_diffrn_reflns_point_group_measured_fraction_full 0.885
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.096
_diffrn_reflns_theta_min         2.487
_exptl_absorpt_coefficient_mu    2.920
_exptl_absorpt_correction_T_max  0.668
_exptl_absorpt_correction_T_min  0.330
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       prism
_exptl_crystal_F_000             4014
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene and n-decane'
_exptl_crystal_size_max          0.419
_exptl_crystal_size_mid          0.265
_exptl_crystal_size_min          0.129
_platon_squeeze_details
;
Disordered solvent n-decane molecules were not determined, but 
SQUEEZE found that there were approximately five such disordered 
solvent molecules per cell.
;
_refine_diff_density_max         0.901
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         3864
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0430P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3198
_reflns_number_total             3864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06181j2.cif
_cod_data_source_block           2nd_a_sq
_cod_original_cell_volume        10834.7(3)
_cod_database_code               7129475
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              26259
_shelx_fab_checksum              1601