Mercuration of thiacalix[4]arenes in the cone and 1,3-alternate conformations.
Botha, F.; Böhm, S; Dvořáková, H; Eigner, V.; Lhoták, P; Organic & biomolecular chemistry 12 (2014) 5136–5143; doi:10.1039/c4ob00799a

data_7153832
_publ_section_title
;
 Mercuration of thiacalix[4]arenes in the cone and 1,3-alternate
 conformations.
;
_journal_issue                   28
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              5136
_journal_page_last               5143
_journal_paper_doi               10.1039/c4ob00799a
_journal_volume                  12
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C36 H39 Cl1 Hg1 O4 S4'
_chemical_formula_sum            'C36 H39 Cl Hg O4 S4'
_chemical_formula_weight         900.01
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 97.027(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6542(2)
_cell_length_b                   20.3405(4)
_cell_length_c                   16.8979(4)
_cell_measurement_reflns_used    8585
_cell_measurement_temperature    120
_cell_measurement_theta_max      67
_cell_measurement_theta_min      3
_cell_volume                     3634.47(13)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_pressure         101
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21312
_diffrn_reflns_theta_full        67.110
_diffrn_reflns_theta_max         67.110
_diffrn_reflns_theta_min         3.416
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.719
_exptl_absorpt_correction_T_max  0.46
_exptl_absorpt_correction_T_min  0.13
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.072
_refine_diff_density_max         2.43
_refine_diff_density_min         -1.09
_refine_ls_abs_structure_details 'Flack (1983), 5838 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.185(14)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9277
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     929
_refine_ls_number_reflns         12344
_refine_ls_number_restraints     175
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.0426880
_refine_ls_shift/su_mean         0.0066840
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.329E+04 0.534E+04 0.341E+04 0.153E+04 409. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1324
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1324
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              23
_reflns_limit_k_min              -24
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                10366
_reflns_number_total             12397
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.48
_oxford_diffrn_Wilson_scale      0.25
_oxford_refine_ls_r_factor_ref   0.0606
_oxford_refine_ls_scale          2.380(13)
_oxford_reflns_number_all        12345
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_cod_data_source_file            c4ob00799a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7153832--7153834.cif.'
_cod_original_cell_volume        3634.46(13)
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        'C36 H39 Cl1 Hg1 O4 S4'
_cod_database_code               7153832
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  30,X'S) H   ( 302,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 312,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 322,X'S) H   ( 323,X'S) H   ( 321,X'S) 
RIDE C   (  34,X'S) H   ( 342,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 362,X'S) H   ( 363,X'S) H   ( 361,X'S) 
RIDE C   (  38,X'S) H   ( 382,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 392,X'S) 
RIDE C   (  40,X'S) H   ( 403,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) H   ( 432,X'S) 
RIDE C   (  44,X'S) H   ( 443,X'S) H   ( 442,X'S) H   ( 441,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) 
RIDE C   ( 105,X'S) H   (1051,X'S) 
RIDE C   ( 106,X'S) H   (1061,X'S) 
RIDE C   ( 110,X'S) H   (1101,X'S) 
RIDE C   ( 111,X'S) H   (1111,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) 
RIDE C   ( 116,X'S) H   (1161,X'S) 
RIDE C   ( 117,X'S) H   (1171,X'S) 
RIDE C   ( 118,X'S) H   (1181,X'S) 
RIDE C   ( 122,X'S) H   (1221,X'S) 
RIDE C   ( 123,X'S) H   (1231,X'S) 
RIDE C   ( 124,X'S) H   (1241,X'S) 
RIDE C   ( 130,X'S) H   (1301,X'S) H   (1302,X'S) 
RIDE C   ( 131,X'S) H   (1312,X'S) H   (1311,X'S) 
RIDE C   ( 132,X'S) H   (1321,X'S) H   (1322,X'S) H   (1323,X'S) 
RIDE C   ( 134,X'S) H   (1341,X'S) H   (1342,X'S) 
RIDE C   ( 135,X'S) H   (1351,X'S) H   (1352,X'S) 
RIDE C   ( 136,X'S) H   (1363,X'S) H   (1362,X'S) H   (1361,X'S) 
RIDE C   ( 138,X'S) H   (1382,X'S) H   (1381,X'S) 
RIDE C   ( 139,X'S) H   (1392,X'S) H   (1391,X'S) 
RIDE C   ( 140,X'S) H   (1402,X'S) H   (1401,X'S) H   (1403,X'S) 
RIDE C   ( 142,X'S) H   (1421,X'S) H   (1422,X'S) 
RIDE C   ( 143,X'S) H   (1432,X'S) H   (1431,X'S) 
RIDE C   ( 144,X'S) H   (1443,X'S) H   (1441,X'S) H   (1442,X'S) 
RIDE C   ( 230,X'S) H   (2302,X'S) H   (2301,X'S) 
RIDE C   ( 231,X'S) H   (2311,X'S) H   (2312,X'S) 
RIDE C   ( 232,X'S) H   (2323,X'S) H   (2321,X'S) H   (2322,X'S) 
RIDE C   ( 238,X'S) H   (2381,X'S) H   (2382,X'S) 
RIDE C   ( 239,X'S) H   (2391,X'S) H   (2392,X'S) 
RIDE C   ( 240,X'S) H   (2403,X'S) H   (2402,X'S) H   (2401,X'S) 
RIDE C   ( 338,X'S) H   (3381,X'S) H   (3382,X'S) 
RIDE C   ( 339,X'S) H   (3392,X'S) H   (3391,X'S) 
RIDE C   ( 340,X'S) H   (3403,X'S) H   (3402,X'S) H   (3401,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.420000 , 0.050000 = O(29) TO C(30) 
DISTANCE 1.540000 , 0.050000 = C(30) TO C(31) 
DISTANCE 1.540000 , 0.050000 = C(31) TO C(32) 
ANGLE 109.000000 , 1.000000 = O(29) TO C(30) TO C(31) 
ANGLE 109.000000 , 1.000000 = C(30) TO C(31) TO C(32) 
U(IJ)'S  0.0, 0.010000 = C(30) TO O(29) 
U(IJ)'S  0.0, 0.010000 = C(31) TO O(29) 
U(IJ)'S  0.0, 0.010000 = C(32) TO O(29) 
DISTANCE 1.420000 , 0.050000 = O(29) TO C(230) 
DISTANCE 1.540000 , 0.050000 = C(230) TO C(231) 
DISTANCE 1.540000 , 0.050000 = C(231) TO C(232) 
ANGLE 109.000000 , 1.000000 = O(29) TO C(230) TO C(231) 
ANGLE 109.000000 , 1.000000 = C(230) TO C(231) TO C(232) 
U(IJ)'S  0.0, 0.010000 = C(230) TO O(29) 
U(IJ)'S  0.0, 0.010000 = C(231) TO O(29) 
U(IJ)'S  0.0, 0.010000 = C(232) TO O(29) 
DISTANCE 1.420000 , 0.050000 = O(37) TO C(38) 
DISTANCE 1.540000 , 0.050000 = C(38) TO C(39) 
DISTANCE 1.540000 , 0.050000 = C(39) TO C(40) 
ANGLE 109.000000 , 1.000000 = O(37) TO C(38) TO C(39) 
ANGLE 109.000000 , 1.000000 = C(38) TO C(39) TO C(40) 
U(IJ)'S  0.0, 0.010000 = C(38) TO O(37) 
U(IJ)'S  0.0, 0.010000 = C(39) TO O(37) 
U(IJ)'S  0.0, 0.010000 = C(40) TO O(37) 
DISTANCE 1.420000 , 0.050000 = O(37) TO C(238) 
DISTANCE 1.540000 , 0.050000 = C(238) TO C(239) 
DISTANCE 1.540000 , 0.050000 = C(239) TO C(240) 
ANGLE 109.000000 , 1.000000 = O(37) TO C(238) TO C(239) 
ANGLE 109.000000 , 1.000000 = C(238) TO C(239) TO C(240) 
U(IJ)'S  0.0, 0.010000 = C(238) TO O(37) 
U(IJ)'S  0.0, 0.010000 = C(239) TO O(37) 
U(IJ)'S  0.0, 0.010000 = C(240) TO O(37) 
DISTANCE 1.420000 , 0.050000 = O(137) TO C(138) 
DISTANCE 1.540000 , 0.050000 = C(138) TO C(139) 
DISTANCE 1.540000 , 0.050000 = C(139) TO C(140) 
ANGLE 109.000000 , 1.000000 = O(137) TO C(138) TO C(139) 
ANGLE 109.000000 , 1.000000 = C(138) TO C(139) TO C(140) 
U(IJ)'S  0.0, 0.010000 = C(138) TO O(137) 
U(IJ)'S  0.0, 0.010000 = C(139) TO O(137) 
U(IJ)'S  0.0, 0.010000 = C(140) TO O(137) 
DISTANCE 1.420000 , 0.050000 = O(337) TO C(338) 
DISTANCE 1.540000 , 0.050000 = C(338) TO C(339) 
DISTANCE 1.540000 , 0.050000 = C(339) TO C(340) 
ANGLE 109.000000 , 1.000000 = O(337) TO C(338) TO C(339) 
ANGLE 109.000000 , 1.000000 = C(338) TO C(339) TO C(340) 
U(IJ)'S  0.0, 0.010000 = C(338) TO O(337) 
U(IJ)'S  0.0, 0.010000 = C(339) TO O(337) 
U(IJ)'S  0.0, 0.010000 = C(340) TO O(337) 
U(IJ)'S  0.0, 0.001000 = O(137) TO O(337) 
U(IJ)'S  0.0, 0.005000 = C(7) TO S(8) 
U(IJ)'S  0.0, 0.010000 = O(129) TO C(132) 
U(IJ)'S  0.0, 0.010000 = C(101) TO C(124) 
U(IJ)'S  0.0, 0.010000 = C(105) TO C(106) 
U(IJ)'S  0.0, 0.010000 = O(33) TO C(34) 
END                                                                             
;