X-ray crystal structure and spectral characterization of pseudo five-coordinate Hg(II) polymeric and four-coordinate binuclear complexes of an ambidentate sulfonium ylide
Sabounchei, Seyyed Javad; Bagherjeri, Fateme Akhlaghi; Hosseinzadeh, Marjan; Boskovic, Colette; Gable, Robert W.; Comptes Rendus Chimie 17 (2014) 1257–1263; doi:10.1016/j.crci.2014.03.016

data_1566119
_publ_contact_author_name
;
;
_publ_section_title
;
 X-ray crystal structure and spectral characterization of pseudo
 five-coordinate Hg(II) polymeric and four-coordinate binuclear complexes
 of an ambidentate sulfonium ylide
;
_journal_issue                   12
_journal_name_full               'Comptes Rendus Chimie'
_journal_page_first              1257
_journal_page_last               1263
_journal_paper_doi               10.1016/j.crci.2014.03.016
_journal_volume                  17
_journal_year                    2014
_chemical_formula_moiety         'C22 H28 Cl4 Hg2 O4 S2, 2(C2 H6 O S)'
_chemical_formula_sum            'C26 H40 Cl4 Hg2 O6 S4'
_chemical_formula_weight         1119.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-07-11
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_cell_angle_alpha                110.370(4)
_cell_angle_beta                 96.693(3)
_cell_angle_gamma                90.526(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1329(3)
_cell_length_b                   12.4857(4)
_cell_length_c                   15.3870(7)
_cell_measurement_reflns_used    8301
_cell_measurement_temperature    130.00(10)
_cell_measurement_theta_max      30.0138
_cell_measurement_theta_min      2.7372
_cell_volume                     1809.94(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      130.00(10)
_diffrn_detector_area_resol_mean 10.2273
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_details
;
  1 omega  -60.00   41.00   1.0000    8.0500
omega____ theta____ kappa____ phi______ frames
    -       13.6163  -57.0000  -30.0000 101

  2 omega   43.00  102.00   1.0000    8.0500
omega____ theta____ kappa____ phi______ frames
    -       13.6163 -178.0000  -30.0000 59

  3 omega   35.00   98.00   1.0000    8.0500
omega____ theta____ kappa____ phi______ frames
    -       13.6163 -178.0000 -120.0000 63

  4 omega    0.00   90.00   1.0000    8.0500
omega____ theta____ kappa____ phi______ frames
    -       13.6163   37.0000  120.0000 90

  5 omega  -19.00   28.00   1.0000    8.0500
omega____ theta____ kappa____ phi______ frames
    -      -13.6945  -99.0000 -120.0000 47
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0675678000
_diffrn_orient_matrix_UB_12      -0.0091603000
_diffrn_orient_matrix_UB_13      -0.0069154000
_diffrn_orient_matrix_UB_21      -0.0174478000
_diffrn_orient_matrix_UB_22      -0.0131107000
_diffrn_orient_matrix_UB_23      -0.0487163000
_diffrn_orient_matrix_UB_31      0.0105753000
_diffrn_orient_matrix_UB_32      0.0585395000
_diffrn_orient_matrix_UB_33      0.0060760000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17790
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.08
_diffrn_reflns_theta_min         2.74
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.034
_exptl_absorpt_correction_T_max  0.637
_exptl_absorpt_correction_T_min  0.208
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.2703
_exptl_crystal_size_mid          0.0866
_exptl_crystal_size_min          0.0600
_refine_diff_density_max         5.862
_refine_diff_density_min         -1.664
_refine_diff_density_rms         0.264
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         9370
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0560P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1137
_reflns_number_gt                7543
_reflns_number_total             9370
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            CRC-2014-17-1257.cif
_cod_data_source_block           fa-lsogau
_cod_original_cell_volume        1809.94(11)
_cod_database_code               1566119
_chemical_oxdiff_formula         'Hg2 S4 O6 Cl4 C26 H40'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50