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_4347975
_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_moiety         'C19 H15 Cl2 O P'
_chemical_formula_sum            'C19 H15 Cl2 O P'
_chemical_formula_weight         361.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.447(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.4262(5)
_cell_length_b                   9.5083(9)
_cell_length_c                   32.704(4)
_cell_measurement_reflns_used    2341
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.365
_cell_measurement_theta_min      2.231
_cell_volume                     1687.3(3)
_computing_cell_refinement       'Bruker ApexII Software Suite, 2008'
_computing_data_collection       'Bruker ApexII Software Suite, 2008'
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_computing_molecular_graphics    'SHELXS plus XP (Sheldrick, 1991)'
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_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
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_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -40
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_diffrn_reflns_point_group_measured_fraction_full 1.000
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_diffrn_reflns_theta_max         26.365
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_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  0.7444
_exptl_absorpt_correction_T_min  0.6973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BLESSING 1995'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       block
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_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.376
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_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3448
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+0.2500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
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_reflns_number_total             3448
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           gud171
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4347975
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.891
_shelx_estimated_absorpt_t_max   0.962
_shelx_res_checksum              74741
_shelx_hkl_checksum              3552