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_4328660
_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         'C21 H24 B N7 S3'
_chemical_formula_sum            'C21 H24 B N7 S3'
_chemical_formula_weight         481.46
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8256(2)
_cell_length_b                   13.4721(3)
_cell_length_c                   16.4802(3)
_cell_measurement_reflns_used    8151
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.4671
_cell_measurement_theta_min      3.2777
_cell_volume                     2403.53(8)
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2011)'
_computing_data_collection       'CrysAlisPro (Agilent Technologies, 2011)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2011)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008) and local programs'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.3147
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19221
_diffrn_reflns_theta_full        74.63
_diffrn_reflns_theta_max         74.63
_diffrn_reflns_theta_min         4.24
_exptl_absorpt_coefficient_mu    3.007
_exptl_absorpt_correction_T_max  0.8995
_exptl_absorpt_correction_T_min  0.6870
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Analytical numeric absorption correction using a multifaceted crystal
   model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       rod
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881; 2086 Friedel pairs'
_refine_ls_abs_structure_Flack   0.000(16)
_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     295
_refine_ls_number_reflns         4854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0590P)^2^+0.0395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1019
_reflns_number_gt                4422
_reflns_number_total             4854
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic202618p_si_002_1.cif
_cod_data_source_block           pb2001
_cod_database_code               4328660