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_7235575
_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 N S2 1-)2, Hg 2+, (c2 H6 o1)0.25'
_chemical_formula_sum            'C20.5 H21.5 Hg N2 O0.25 S4'
_chemical_formula_weight         628.73
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.898(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.7060(10)
_cell_length_b                   7.3860(10)
_cell_length_c                   19.9140(10)
_cell_measurement_reflns_used    4845
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.610
_cell_measurement_theta_min      3.9863
_cell_volume                     2439.4(4)
_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 0.969
_diffrn_measured_fraction_theta_max 0.836
_diffrn_measurement_details
;
  1 omega  -71.00  -26.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.2830  110.0000  172.0000    0.0000    0.0000 45

  2 omega  -48.00    4.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.2830   45.0000  120.0000    0.0000    0.0000 52

  3 omega   -2.00   43.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.6112 -127.0000  314.0000    0.0000    0.0000 45

  4 omega  -49.00    5.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.6112  -75.0000  240.0000    0.0000    0.0000 54

  5 omega  -28.00   15.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.6112  110.0000   -7.0000    0.0000    0.0000 43

  6 omega  -50.00    1.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.6112  -45.0000  120.0000    0.0000    0.0000 51

  7 omega   40.00   74.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.6112 -127.0000  314.0000    0.0000    0.0000 34

  8 phi    -26.00    2.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   22.6112    0.0000     -        0.0000    0.0000 28
;
_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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0761
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            12983
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.65
_diffrn_reflns_theta_min         4.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_number         8
_exptl_absorpt_coefficient_mu    6.661
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23178
_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    1.712
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1218
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.861
_refine_diff_density_min         -1.498
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         5247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0975P)^2^+12.8659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1700
_refine_ls_wR_factor_ref         0.2082
_reflns_number_gt                3001
_reflns_number_total             5247
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra01913j1.cif
_cod_data_source_block           nts6
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C20.50 H21.50 Hg N2 O0.25 S4'
_cod_database_code               7235575