New Selective Synthesis of Dithiaboroles as a Viable Pathway to Functionalized Benzenedithiolenes and Their Complexes.
Schlindwein, Simon H.; Bader, Katharina; Sibold, Carlo; Frey, Wolfgang; Neugebauer, Petr; Orlita, Milan; Slageren, Joris van; Gudat, Dietrich; Inorganic chemistry 55 (2016) 6186–6194; doi:10.1021/acs.inorgchem.6b00821

data_4347976
_publ_section_title
;
 New Selective Synthesis of Dithiaboroles as a Viable Pathway to
 Functionalized Benzenedithiolenes and Their Complexes.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6186
_journal_page_last               6194
_journal_paper_doi               10.1021/acs.inorgchem.6b00821
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C44 H46 N2 O2 P2 Pd S4'
_chemical_formula_weight         931.41
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2yn'
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_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 106.460(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.2038(10)
_cell_length_b                   8.1279(5)
_cell_length_c                   19.2114(13)
_cell_measurement_reflns_used    2751
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.277
_cell_measurement_theta_min      3.445
_cell_volume                     2127.0(3)
_computing_cell_refinement       'Bruker ApexII Software Suite, 2008'
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_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 0.960
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_diffrn_reflns_limit_h_min       -14
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_diffrn_reflns_point_group_measured_fraction_full 0.960
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_diffrn_reflns_theta_full        66.277
_diffrn_reflns_theta_max         66.277
_diffrn_reflns_theta_min         3.445
_exptl_absorpt_coefficient_mu    6.373
_exptl_absorpt_correction_T_max  0.8787
_exptl_absorpt_correction_T_min  0.3440
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'BLESSING 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       plate
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.026
_refine_diff_density_max         1.777
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_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         3584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0767P)^2^+1.4589P] where P=(Fo^2^+2Fc^2^)/3'
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_reflns_number_total             3584
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_original_sg_symbol_H-M      'P 21/n'
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_shelx_estimated_absorpt_t_min   0.310
_shelx_estimated_absorpt_t_max   0.852
_shelx_res_checksum              93199
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