Zinc, Cadmium, and Mercury 1,2-Benzenedithiolates with Intramolecular NH...S Hydrogen Bonds
Koji Baba; Taka-aki Okamura; Hitoshi Yamamoto; Tetsuo Yamamoto; Norikazu Ueyama; Inorganic Chemistry 47 (2008) 2837–2848; doi:10.1021/ic702037k

data_4304539
_publ_contact_author_address
;
Department of Macromolecular Science, Graduate School of Science
Osaka University
Toyonaka, Osaka 560-0043, Japan
;
_publ_contact_author_email       tokamura@chem.sci.osaka-u.ac.jp
_publ_contact_author_fax         +81-6-6850-5474
_publ_contact_author_name        'Taka-aki Okamura'
_publ_contact_author_phone       +81-6-6850-5451
_publ_section_title
;
Zinc, Cadmium, and Mercury 1,2-Benzenedithiolates with Intramolecular
NH...S Hydrogen Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2837
_journal_page_last               2848
_journal_paper_doi               10.1021/ic702037k
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C29.50 H52.25 Hg N2.75 O S4 '
_chemical_formula_sum            'C29.5 H52.25 Hg N2.75 O S4'
_chemical_formula_weight         790.32
_chemical_name_systematic
; 
(NEt4)2[Hg(bdt)2]-3/4(CH3CN)-H2O 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'Mon Jul  3 09:16:11 2006'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.064(2)
_cell_angle_beta                 112.208(2)
_cell_angle_gamma                97.1440(10)
_cell_formula_units_Z            4
_cell_length_a                   17.0547(7)
_cell_length_b                   17.6005(6)
_cell_length_c                   14.0856(6)
_cell_measurement_reflns_used    19251
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.2
_cell_volume                     3802.5(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.1092
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21642
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    4.290
_exptl_absorpt_correction_T_max  0.525
_exptl_absorpt_correction_T_min  0.302
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1602
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.715
_refine_diff_density_min         -2.553
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         13226
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0816P)^2^+4.6368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1481
_refine_ls_wR_factor_ref         0.1629
_reflns_number_gt                8086
_reflns_number_total             13226
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic702037k-file003_4.cif
_cod_data_source_block           13-3/4(CH3CN)-H2O
_cod_original_formula_sum        'C29.50 H52.25 Hg N2.75 O S4'
_cod_database_code               4304539