Synthesis, Structure, and multi-NMR studies of (Me~4~N)[A{M(SC{O}Ph)~3~] (A = Na, M = Hg; A = K, M = Cd or Hg)
Theivanayagam C. Deivaraj; Philip A.W. Dean; Jagadese Jayapurandara Vittal; Inorganic Chemistry 39 (2000) 3071–3074; doi:10.1021/ic0000810

data_4321115
_publ_contact_author_address
; Department of Chemistry
  National University of Singapore
  Kent Ridge
  Singapore 119 260
;
_publ_contact_author_email       chmjjv@nus.edu.sg
_publ_contact_author_fax         '(65) 874 2975'
_publ_contact_author_name        'Jagadese J. Vittal'
_publ_contact_author_phone       '(65) 779 1691'
_publ_section_title
;
 Synthesis, Structure, and multi-NMR studies of (Me~4~N)[A{M(SC{O}Ph)~3~]
 (A = Na, M = Hg; A = K, M = Cd or Hg)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3071
_journal_page_last               3074
_journal_paper_doi               10.1021/ic0000810
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source        'see text'
_chemical_formula_sum            'C46 H42 Cd2 K N O6 S6'
_chemical_formula_weight         1161.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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
_cell_angle_alpha                71.782(1)
_cell_angle_beta                 85.208(1)
_cell_angle_gamma                69.418(1)
_cell_formula_units_Z            1
_cell_length_a                   10.6670(2)
_cell_length_b                   11.1522(2)
_cell_length_c                   11.9294(2)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.25
_cell_measurement_theta_min      1.80
_cell_volume                     1261.40(4)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1996)'
_computing_publication_material  'SHELXTL (Siemens, 1996)'
_computing_structure_refinement  'SHELXTL (Siemens, 1996)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens SMART CCD System'
_diffrn_measurement_method       'frames \w scans'
_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  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8026
_diffrn_reflns_theta_max         29.25
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    1.219
_exptl_absorpt_correction_T_max  0.8934
_exptl_absorpt_correction_T_min  0.6744
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'creamy yellow'
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'long thin plates, cut'
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.088
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       0.0002(8)
_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_all   1.050
_refine_ls_goodness_of_fit_obs   1.097
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         5692
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.064
_refine_ls_restrained_S_obs      1.114
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_obs          0.0599
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+2.5239P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1464
_refine_ls_wR_factor_obs         0.1304
_reflns_number_observed          4192
_reflns_number_total             5692
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0000810_2.cif
_cod_data_source_block           tcd3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+2.5239P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+2.5239P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321115