Protolytic Cleavage of Hg-C Bonds Induced by 1-Methyl-1,3-dihydro-2H-benzimidazole-2-selone: Synthesis and Structural Characterization of Mercury Complexes.
Palmer, Joshua H.; Parkin, Gerard; Journal of the American Chemical Society 137 (2015) 4503–4516; doi:10.1021/jacs.5b00840

data_4123774
_publ_section_title
;
 Protolytic Cleavage of Hg-C Bonds Induced by
 1-Methyl-1,3-dihydro-2H-benzimidazole-2-selone: Synthesis and Structural
 Characterization of Mercury Complexes.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4503
_journal_page_last               4516
_journal_paper_doi               10.1021/jacs.5b00840
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C32 H32 Cl2 Hg N8 Se4'
_chemical_formula_weight         1115.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 94.939(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8918(14)
_cell_length_b                   14.5673(15)
_cell_length_c                   19.000(2)
_cell_measurement_reflns_used    9232
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      2.31
_cell_volume                     3554.9(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0743
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            42569
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.612
_diffrn_reflns_theta_min         1.764
_exptl_absorpt_coefficient_mu    8.612
_exptl_absorpt_correction_T_max  0.480
_exptl_absorpt_correction_T_min  0.138
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.085
_exptl_crystal_description       block
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.317
_refine_diff_density_min         -1.089
_refine_diff_density_rms         0.184
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.531(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     888
_refine_ls_number_reflns         21344
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0196P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0688
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                16326
_reflns_number_total             21344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b00840_si_006.cif
_cod_data_source_block           se4hgcl2
_cod_database_code               4123774
_shelx_estimated_absorpt_t_min   0.138
_shelx_estimated_absorpt_t_max   0.480
_shelxl_version_number           2013-4
_shelx_res_checksum              71132
_shelx_hkl_checksum              50844