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_4304537
_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         'C81 H85.50 Cd N4.50 O4 P2 S4 '
_chemical_formula_sum            'C81 H85.5 Cd N4.5 O4 P2 S4'
_chemical_formula_weight         1488.62
_chemical_name_systematic
; 
(PPh4)2[Cd{S2-3,6-(t-BuCONH)2C6H2}2]-1/2(CH3CN) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'Tue Jun 27 19:51:13 2006'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.1140(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1271(7)
_cell_length_b                   19.6683(7)
_cell_length_c                   22.4298(10)
_cell_measurement_reflns_used    27844
_cell_measurement_temperature    223
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.3
_cell_volume                     7536.3(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0634
_diffrn_reflns_av_sigmaI/netI    0.2722
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            31779
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3108
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     896
_refine_ls_number_reflns         17089
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1633
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0426
_refine_ls_wR_factor_ref         0.0487
_reflns_number_gt                6577
_reflns_number_total             17089
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic702037k-file003_2.cif
_cod_data_source_block           5-1/2(CH3CN)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C81 H85.50 Cd N4.50 O4 P2 S4'
_cod_database_code               4304537