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_7235574
_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 H10 S2 N 1-)2, hg 2+, (c5 h4 N)1'
_chemical_formula_sum            'C25 H24 Hg N3 S4'
_chemical_formula_weight         695.30
_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                84.01(1)
_cell_angle_beta                 87.05(1)
_cell_angle_gamma                70.49(1)
_cell_formula_units_Z            2
_cell_length_a                   8.696(1)
_cell_length_b                   10.994(1)
_cell_length_c                   14.457(1)
_cell_measurement_reflns_used    4860
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7615
_cell_measurement_theta_min      3.7948
_cell_volume                     1295.5(2)
_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 0.991
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_details
;
  1 omega   21.00   58.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.1268 -161.0000  240.0000    0.0000    0.0000 37

  2 omega   -2.00   51.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.1268   75.0000    0.0000    0.0000    0.0000 53

  3 omega  -92.00  -40.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.1268  -75.0000  120.0000    0.0000    0.0000 52

  4 omega  -42.00   11.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.1268  -75.0000  120.0000    0.0000    0.0000 53

  5 omega    1.00   53.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.2987  -75.0000    0.0000    0.0000    0.0000 52

  6 omega   -4.00   46.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.2987   45.0000    0.0000    0.0000    0.0000 50

  7 omega   44.00   94.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.2987   45.0000    0.0000    0.0000    0.0000 50

  8 omega   42.00   85.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.2987 -130.0000  322.0000    0.0000    0.0000 43

  9 omega   41.00   95.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.2987   75.0000  240.0000    0.0000    0.0000 54

 10 omega   -4.00   40.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.2987   45.0000  120.0000    0.0000    0.0000 44

 11 omega   -5.00   44.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.2987   75.0000  240.0000    0.0000    0.0000 49
;
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0788
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12189
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.80
_diffrn_reflns_theta_min         3.80
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_number         11
_exptl_absorpt_coefficient_mu    6.282
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27839
_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            'pale yellow'
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             678
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.095
_refine_diff_density_min         -1.269
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5769
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0880
_reflns_number_gt                3423
_reflns_number_total             5769
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra01913j1.cif
_cod_data_source_block           NST5
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7235574