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_4328663
_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 Bell'
_chemical_formula_moiety         '2(C31 H41 B N8 Ru S3), 3(C2 H3 N), 4(F6 P)'
_chemical_formula_sum            'C68 H91 B2 F24 N19 P4 Ru2 S6'
_chemical_formula_weight         2170.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.9930(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.0566(3)
_cell_length_b                   13.0618(2)
_cell_length_c                   19.9834(3)
_cell_measurement_reflns_used    9486
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.9675
_cell_measurement_theta_min      2.194
_cell_volume                     4449.41(12)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0736
_diffrn_reflns_av_sigmaI/netI    0.0849
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44375
_diffrn_reflns_theta_full        26.45
_diffrn_reflns_theta_max         26.45
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_description       block
_exptl_crystal_F_000             2204
_exptl_crystal_recrystallization_method
'vapour diffusion of EtO2 into MeCN solution'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.572
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         9083
_refine_ls_number_restraints     577
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0510P)^2^+4.6393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1256
_reflns_number_gt                5836
_reflns_number_total             9083
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202618p_si_002_4.cif
_cod_data_source_block           pb0005
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4328663