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_7129476
_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         'C30 H26 B2 N6 Ru, 3(C6 H6)'
_chemical_formula_sum            'C48 H44 B2 N6 Ru'
_chemical_formula_weight         827.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_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                 94.508(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.0601(6)
_cell_length_b                   9.7294(2)
_cell_length_c                   18.0199(5)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.96
_cell_measurement_theta_min      3.85
_cell_volume                     4030.45(17)
_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 0.964
_diffrn_measured_fraction_theta_max 0.947
_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  0.0308
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18211
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.956
_diffrn_reflns_theta_min         3.846
_exptl_absorpt_coefficient_mu    3.470
_exptl_absorpt_correction_T_max  0.784
_exptl_absorpt_correction_T_min  0.656
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       paralellepiped
_exptl_crystal_F_000             1712
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene and n-octane'
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.000048(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3542
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+6.9493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3160
_reflns_number_total             3542
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06181j2.cif
_cod_data_source_block           180326RAL_JG_95R_100K_0m_a
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7129476
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.590
_shelx_estimated_absorpt_t_max   0.714
_shelx_res_checksum              79717