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_4328666
_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_formula_moiety         '2 C23 H27 N7 Ru S3 +, 2 P F6 -, C2 H3 N'
_chemical_formula_sum            'C48 H61 B2 F12 N15 P2 Ru2 S6'
_chemical_formula_weight         1554.18
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.3560(10)
_cell_angle_beta                 85.9250(10)
_cell_angle_gamma                75.8420(10)
_cell_formula_units_Z            2
_cell_length_a                   10.0598(3)
_cell_length_b                   16.6932(4)
_cell_length_c                   19.9429(5)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.28
_cell_volume                     3155.33(15)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    OLEX2
_computing_publication_material  OLEX2
_computing_structure_refinement  OLEX2
_computing_structure_solution    'SIR92 (Altomare et al., 1992)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34132
_diffrn_reflns_theta_full        26.45
_diffrn_reflns_theta_max         26.45
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.812
_exptl_absorpt_correction_T_max  0.9232
_exptl_absorpt_correction_T_min  0.8106
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrick, 2008'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.439
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         12924
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0437P)^2^+2.2733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.1012
_reflns_number_gt                10189
_reflns_number_total             12924
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic202618p_si_002_7.cif
_cod_data_source_block           pb1014
_cod_original_cell_volume        3155.34(14)
_cod_database_code               4328666