Effect of co-crystallization of ethanol, pyridine and 2,2′-bipyridine on molecular aggregation in bis(1,2,3,4-tetrahydroquinolinedithiocarbamato-S,S′)mercury(ii) and synthesis of HgS nanoparticles
Srinivasan, Narayanaswamy; Thirumaran, Subbiah; Ciattini, Samuele; RSC Adv. 4 (2014) 22971–; doi:10.1039/C4RA01913J

data_7235576
_publ_section_title
;
 Effect of co-crystallization of ethanol, pyridine and
 2,2&#x2032;-bipyridine on molecular aggregation in
 bis(1,2,3,4-tetrahydroquinolinedithiocarbamato-S,S&#x2032;)mercury(ii)
 and synthesis of HgS nanoparticles
;
_journal_issue                   44
_journal_name_full               'RSC Adv.'
_journal_page_first              22971
_journal_paper_doi               10.1039/C4RA01913J
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety
'(c10 N1 S2 1-)3, (Hg1.5 2+), (c2.5 h2.5 n0.5)1'
_chemical_formula_sum            'C32.5 H32.5 Hg1.5 N3.5 S6'
_chemical_formula_weight         965.36
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                74.64(1)
_cell_angle_beta                 77.36(1)
_cell_angle_gamma                87.72(1)
_cell_formula_units_Z            2
_cell_length_a                   8.899(1)
_cell_length_b                   10.782(1)
_cell_length_c                   18.880(1)
_cell_measurement_reflns_used    6003
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.86
_cell_measurement_theta_min      3.78
_cell_volume                     1704.2(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.864
_diffrn_measurement_details
;
  1 omega    0.00   52.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.0487   45.0000  240.0000    0.0000    0.0000 52

  2 omega  -48.00    4.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.0487   45.0000  240.0000    0.0000    0.0000 52

  3 omega    6.00   46.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.0487 -139.0000  355.0000    0.0000    0.0000 40

  4 omega  -43.00   11.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.0487  -75.0000  120.0000    0.0000    0.0000 54

  5 omega    1.00   54.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.2987  -75.0000  240.0000    0.0000    0.0000 53

  6 omega   41.00   95.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.2987   75.0000    0.0000    0.0000    0.0000 54

  7 omega   -8.00   45.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.2987   75.0000  120.0000    0.0000    0.0000 53

  8 omega   43.00   95.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.2987   45.0000  120.0000    0.0000    0.0000 52

  9 omega   -1.00   45.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.2987   45.0000  120.0000    0.0000    0.0000 46

 10 omega   -2.00   50.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.2987  -45.0000  120.0000    0.0000    0.0000 52

 11 omega   -1.00   44.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.2987   75.0000    0.0000    0.0000    0.0000 45

 12 omega  -50.00    2.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.2987  -45.0000  120.0000    0.0000    0.0000 52

;
_diffrn_measurement_device_type  'Oxford diffraction Xcalibur3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.1102
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18412
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.86
_diffrn_reflns_theta_min         3.78
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_number         12
_exptl_absorpt_coefficient_mu    7.154
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.402
_refine_diff_density_min         -1.537
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         7726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0963
_reflns_number_gt                3608
_reflns_number_total             7726
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra01913j1.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C32.50 H32.50 Hg1.50 N3.50 S6'
_cod_database_code               7235576