Insertion and Substitution Chemistry at the Boron Fourth Position in Charge-Neutral Zwitterionic Tripodal Tris(methimazolyl)borate Ligands
Philip J. Bailey; Nicola L. Bell; Gary S. Nichol; Simon Parsons; Fraser White; Inorganic Chemistry 51 (2012) 3677–3689; doi:10.1021/ic202618p

data_4328661
_publ_contact_author_email       fraser.white@ed.ac.uk
_publ_contact_author_name        'Fraser J. White'
_publ_section_title
;
 Insertion and Substitution Chemistry at the Boron Fourth Position in
 Charge-Neutral Zwitterionic Tripodal Tris(methimazolyl)borate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3677
_journal_page_last               3689
_journal_paper_doi               10.1021/ic202618p
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        'Nicola L Bell'
_chemical_formula_moiety
'C23 H29 B N7 Ru S4, C24 H20 B, 2(Et2O), 2(MeOH)'
_chemical_formula_sum            'C56.5 H75 B2 N7 O3.5 Ru S4'
_chemical_formula_weight         1159.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.7680(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.1020(4)
_cell_length_b                   25.7120(7)
_cell_length_c                   27.9161(9)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.8495
_cell_measurement_theta_min      2.3135
_cell_volume                     11122.8(5)
_computing_cell_refinement       Saint
_computing_data_reduction        Saint
_computing_molecular_graphics    Shelxp
_computing_publication_material  'Platon, encifer'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'Shelxs Sheldrick'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex II CCD on D8'
_diffrn_measurement_method       'Phi and Omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            79158
_diffrn_reflns_theta_full        27.15
_diffrn_reflns_theta_max         27.15
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    0.484
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             4872
_exptl_crystal_recrystallization_method
'slow diffusion of Et2O into CDCl3 solution'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         12310
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0411P)^2^+0.9475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0959
_reflns_number_gt                9154
_reflns_number_total             12310
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202618p_si_002_2.cif
_cod_data_source_block           pb0011
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_original_formula_sum        'C56.50 H75 B2 N7 O3.50 Ru S4'
_cod_database_code               4328661