Solution and Solid-State Study of Heteroleptic Hg(II)-Thiolates: Crystal Structures of [Hg4I4(SCH2CH2NH2)4] and [Hg4I8(SCH2CH2NH3)2]n·nH2O
Bharara, Mohan S.; Parkin, Sean; Atwood, David A.; Inorganic Chemistry 45 (2006) 2112–2118; doi:10.1021/ic051993a

data_4331986
_publ_section_title
;
 Solution and Solid-State Study of Heteroleptic Hg(II)-Thiolates:&#x00A0;
 Crystal Structures of [Hg4I4(SCH2CH2NH2)4] and
 [Hg4I8(SCH2CH2NH3)2]n&#x00B7;nH2O
;
_journal_issue                   5
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2112
_journal_page_last               2118
_journal_paper_doi               10.1021/ic051993a
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C4 H12 Hg2 I2 N2 S2'
_chemical_formula_weight         807.26
_chemical_name_systematic
; 
 ? 
;
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.5020(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2107(2)
_cell_length_b                   8.1173(2)
_cell_length_c                   18.1332(4)
_cell_measurement_reflns_used    11386
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1333.04(5)
_computing_cell_refinement       'DENZO-SMN (Nonius, 1998)'
_computing_data_collection       'Collect (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN (Nonius, 1998)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 1994)'
_computing_publication_material
;
SHELX-97 (Sheldrick, 1997) and local procedures
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\w scans at fixed \c=55\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20973
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        <1%
_exptl_absorpt_coefficient_mu    27.911
_exptl_absorpt_correction_T_max  0.4015
_exptl_absorpt_correction_T_min  0.2331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.022
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.339
_refine_diff_density_min         -1.164
_refine_diff_density_rms         0.281
_refine_ls_extinction_coef       0.00040(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         3054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0149P)^2^+0.5665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0427
_refine_ls_wR_factor_ref         0.0455
_reflns_number_gt                2558
_reflns_number_total             3054
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic051993asup1.cif
_cod_data_source_block           k05101s
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4331986