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_7153833
_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_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           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   39.4696(5)
_cell_length_b                   39.4696(5)
_cell_length_c                   21.8104(4)
_cell_measurement_reflns_used    21544
_cell_measurement_temperature    120
_cell_measurement_theta_max      56
_cell_measurement_theta_min      4
_cell_volume                     33977.3(9)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_pressure         101
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.108
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49332
_diffrn_reflns_theta_full        54.630
_diffrn_reflns_theta_max         56.319
_diffrn_reflns_theta_min         3.221
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.173
_exptl_absorpt_correction_T_max  0.13
_exptl_absorpt_correction_T_min  0.02
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             14336
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.220
_refine_diff_density_max         1.44
_refine_diff_density_min         -1.83
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1045
_refine_ls_number_reflns         10981
_refine_ls_number_restraints     392
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0786
_refine_ls_shift/su_max          0.0308935
_refine_ls_shift/su_mean         0.0016979
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.17P)^2^ +*****P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2476
_refine_ls_wR_factor_gt          0.2225
_refine_ls_wR_factor_ref         0.2475
_reflns_limit_h_max              29
_reflns_limit_h_min              -29
_reflns_limit_k_max              42
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                8463
_reflns_number_total             11046
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   6.81
_oxford_diffrn_Wilson_scale      7.82
_oxford_refine_ls_r_factor_ref   0.0947
_oxford_refine_ls_scale          0.3865(8)
_oxford_reflns_number_all        10982
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_cod_data_source_file            c4ob00799a2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7153832--7153834.cif.
;
_cod_original_sg_symbol_H-M      'I 41/a '
_cod_original_formula_sum        'C36 H39 Cl1 Hg1 O4 S4'
_cod_database_code               7153833
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
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   ( 301,X'S) H   ( 302,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) H   ( 323,X'S) 
RIDE C   ( 230,X'S) H   (2301,X'S) H   (2302,X'S) 
RIDE C   ( 231,X'S) H   (2311,X'S) H   (2312,X'S) 
RIDE C   ( 232,X'S) H   (2321,X'S) H   (2322,X'S) H   (2323,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) H   ( 363,X'S) 
RIDE C   ( 234,X'S) H   (2341,X'S) H   (2342,X'S) 
RIDE C   ( 235,X'S) H   (2351,X'S) H   (2352,X'S) 
RIDE C   ( 236,X'S) H   (2361,X'S) H   (2362,X'S) H   (2363,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 392,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 402,X'S) H   ( 403,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   (2401,X'S) H   (2402,X'S) H   (2403,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   ( 441,X'S) H   ( 442,X'S) H   ( 443,X'S) 
RIDE C   ( 242,X'S) H   (2421,X'S) H   (2422,X'S) 
RIDE C   ( 243,X'S) H   (2431,X'S) H   (2432,X'S) 
RIDE C   ( 244,X'S) H   (2441,X'S) H   (2442,X'S) H   (2443,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   (1311,X'S) H   (1312,X'S) 
RIDE C   ( 132,X'S) H   (1321,X'S) H   (1322,X'S) H   (1323,X'S) 
RIDE C   ( 330,X'S) H   (3301,X'S) H   (3302,X'S) 
RIDE C   ( 331,X'S) H   (3311,X'S) H   (3312,X'S) 
RIDE C   ( 332,X'S) H   (3321,X'S) H   (3322,X'S) H   (3323,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   (1361,X'S) H   (1362,X'S) H   (1363,X'S) 
RIDE C   ( 334,X'S) H   (3341,X'S) H   (3342,X'S) 
RIDE C   ( 335,X'S) H   (3351,X'S) H   (3352,X'S) 
RIDE C   ( 336,X'S) H   (3361,X'S) H   (3362,X'S) H   (3363,X'S) 
RIDE C   ( 138,X'S) H   (1381,X'S) H   (1382,X'S) 
RIDE C   ( 139,X'S) H   (1391,X'S) H   (1392,X'S) 
RIDE C   ( 140,X'S) H   (1401,X'S) H   (1402,X'S) H   (1403,X'S) 
RIDE C   ( 338,X'S) H   (3381,X'S) H   (3382,X'S) 
RIDE C   ( 339,X'S) H   (3391,X'S) H   (3392,X'S) 
RIDE C   ( 340,X'S) H   (3401,X'S) H   (3402,X'S) H   (3403,X'S) 
RIDE C   ( 142,X'S) H   (1421,X'S) H   (1422,X'S) 
RIDE C   ( 143,X'S) H   (1431,X'S) H   (1432,X'S) 
RIDE C   ( 144,X'S) H   (1441,X'S) H   (1442,X'S) H   (1443,X'S) 
RIDE C   ( 342,X'S) H   (3421,X'S) H   (3422,X'S) 
RIDE C   ( 343,X'S) H   (3431,X'S) H   (3432,X'S) 
RIDE C   ( 344,X'S) H   (3441,X'S) H   (3442,X'S) H   (3443,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 1.460000 , 0.005000 = O(29) TO C(30) 
DISTANCE 1.505000 , 0.005000 = C(30) TO C(31) 
DISTANCE 1.540000 , 0.005000 = 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) 
DISTANCE 1.460000 , 0.005000 = O(29) TO C(230) 
DISTANCE 1.505000 , 0.005000 = C(230) TO C(231) 
DISTANCE 1.540000 , 0.005000 = 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 = O(29) TO C(30) 
U(IJ)'S  0.0, 0.010000 = O(29) TO C(31) 
U(IJ)'S  0.0, 0.010000 = O(29) TO C(32) 
U(IJ)'S  0.0, 0.010000 = O(29) TO C(230) 
U(IJ)'S  0.0, 0.010000 = O(29) TO C(231) 
U(IJ)'S  0.0, 0.010000 = O(29) TO C(232) 
DISTANCE 1.460000 , 0.005000 = O(33) TO C(34) 
DISTANCE 1.505000 , 0.005000 = C(34) TO C(35) 
DISTANCE 1.540000 , 0.005000 = C(35) TO C(36) 
ANGLE 109.000000 , 1.000000 = O(33) TO C(34) TO C(35) 
ANGLE 109.000000 , 1.000000 = C(34) TO C(35) TO C(36) 
DISTANCE 1.460000 , 0.005000 = O(33) TO C(234) 
DISTANCE 1.505000 , 0.005000 = C(234) TO C(235) 
DISTANCE 1.540000 , 0.005000 = C(235) TO C(236) 
ANGLE 109.000000 , 1.000000 = O(33) TO C(234) TO C(235) 
ANGLE 109.000000 , 1.000000 = C(234) TO C(235) TO C(236) 
U(IJ)'S  0.0, 0.010000 = O(33) TO C(34) 
U(IJ)'S  0.0, 0.010000 = O(33) TO C(35) 
U(IJ)'S  0.0, 0.010000 = O(33) TO C(36) 
U(IJ)'S  0.0, 0.010000 = O(33) TO C(234) 
U(IJ)'S  0.0, 0.010000 = O(33) TO C(235) 
U(IJ)'S  0.0, 0.010000 = O(33) TO C(236) 
DISTANCE 1.460000 , 0.005000 = O(37) TO C(38) 
DISTANCE 1.505000 , 0.005000 = C(38) TO C(39) 
DISTANCE 1.540000 , 0.005000 = 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) 
DISTANCE 1.460000 , 0.005000 = O(37) TO C(238) 
DISTANCE 1.505000 , 0.005000 = C(238) TO C(239) 
DISTANCE 1.540000 , 0.005000 = 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 = O(37) TO C(38) 
U(IJ)'S  0.0, 0.010000 = O(37) TO C(39) 
U(IJ)'S  0.0, 0.010000 = O(37) TO C(40) 
U(IJ)'S  0.0, 0.010000 = O(37) TO C(238) 
U(IJ)'S  0.0, 0.010000 = O(37) TO C(239) 
U(IJ)'S  0.0, 0.010000 = O(37) TO C(240) 
DISTANCE 1.460000 , 0.005000 = O(41) TO C(42) 
DISTANCE 1.505000 , 0.005000 = C(42) TO C(43) 
DISTANCE 1.544000 , 0.005000 = C(43) TO C(44) 
ANGLE 109.000000 , 1.000000 = O(41) TO C(42) TO C(43) 
ANGLE 109.000000 , 1.000000 = C(42) TO C(43) TO C(44) 
DISTANCE 1.460000 , 0.005000 = O(41) TO C(242) 
DISTANCE 1.505000 , 0.005000 = C(242) TO C(243) 
DISTANCE 1.544000 , 0.005000 = C(243) TO C(244) 
ANGLE 109.000000 , 1.000000 = O(41) TO C(242) TO C(243) 
ANGLE 109.000000 , 1.000000 = C(242) TO C(243) TO C(244) 
U(IJ)'S  0.0, 0.010000 = O(41) TO C(42) 
U(IJ)'S  0.0, 0.010000 = O(41) TO C(43) 
U(IJ)'S  0.0, 0.010000 = O(41) TO C(44) 
U(IJ)'S  0.0, 0.010000 = O(41) TO C(242) 
U(IJ)'S  0.0, 0.010000 = O(41) TO C(243) 
U(IJ)'S  0.0, 0.010000 = O(41) TO C(244) 
DISTANCE 1.460000 , 0.005000 = O(129) TO C(130) 
DISTANCE 1.505000 , 0.005000 = C(130) TO C(131) 
DISTANCE 1.540000 , 0.005000 = C(131) TO C(132) 
ANGLE 109.000000 , 1.000000 = O(129) TO C(130) TO C(131) 
ANGLE 109.000000 , 1.000000 = C(130) TO C(131) TO C(132) 
DISTANCE 1.460000 , 0.005000 = O(129) TO C(330) 
DISTANCE 1.505000 , 0.005000 = C(330) TO C(331) 
DISTANCE 1.540000 , 0.005000 = C(331) TO C(332) 
ANGLE 109.000000 , 1.000000 = O(129) TO C(330) TO C(331) 
ANGLE 109.000000 , 1.000000 = C(330) TO C(331) TO C(332) 
U(IJ)'S  0.0, 0.010000 = O(129) TO C(130) 
U(IJ)'S  0.0, 0.010000 = O(129) TO C(131) 
U(IJ)'S  0.0, 0.010000 = O(129) TO C(132) 
U(IJ)'S  0.0, 0.010000 = O(129) TO C(330) 
U(IJ)'S  0.0, 0.010000 = O(129) TO C(331) 
U(IJ)'S  0.0, 0.010000 = O(129) TO C(332) 
DISTANCE 1.460000 , 0.005000 = O(133) TO C(134) 
DISTANCE 1.505000 , 0.005000 = C(134) TO C(135) 
DISTANCE 1.540000 , 0.005000 = C(135) TO C(136) 
ANGLE 109.000000 , 1.000000 = O(133) TO C(134) TO C(135) 
ANGLE 109.000000 , 1.000000 = C(134) TO C(135) TO C(136) 
DISTANCE 1.460000 , 0.005000 = O(133) TO C(334) 
DISTANCE 1.505000 , 0.005000 = C(334) TO C(335) 
DISTANCE 1.540000 , 0.005000 = C(335) TO C(336) 
ANGLE 109.000000 , 1.000000 = O(133) TO C(334) TO C(335) 
ANGLE 109.000000 , 1.000000 = C(334) TO C(335) TO C(336) 
U(IJ)'S  0.0, 0.010000 = O(133) TO C(134) 
U(IJ)'S  0.0, 0.010000 = O(133) TO C(135) 
U(IJ)'S  0.0, 0.010000 = O(133) TO C(136) 
U(IJ)'S  0.0, 0.010000 = O(133) TO C(334) 
U(IJ)'S  0.0, 0.010000 = O(133) TO C(335) 
U(IJ)'S  0.0, 0.010000 = O(133) TO C(336) 
DISTANCE 1.460000 , 0.005000 = O(137) TO C(138) 
DISTANCE 1.505000 , 0.005000 = C(138) TO C(139) 
DISTANCE 1.540000 , 0.005000 = 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) 
DISTANCE 1.460000 , 0.005000 = O(137) TO C(338) 
DISTANCE 1.505000 , 0.005000 = C(338) TO C(339) 
DISTANCE 1.540000 , 0.005000 = C(339) TO C(340) 
ANGLE 109.000000 , 1.000000 = O(137) 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 = O(137) TO C(138) 
U(IJ)'S  0.0, 0.010000 = O(137) TO C(139) 
U(IJ)'S  0.0, 0.010000 = O(137) TO C(140) 
U(IJ)'S  0.0, 0.010000 = O(137) TO C(338) 
U(IJ)'S  0.0, 0.010000 = O(137) TO C(339) 
U(IJ)'S  0.0, 0.010000 = O(137) TO C(340) 
DISTANCE 1.460000 , 0.005000 = O(141) TO C(142) 
DISTANCE 1.505000 , 0.005000 = C(142) TO C(143) 
DISTANCE 1.544000 , 0.005000 = C(143) TO C(144) 
ANGLE 109.000000 , 1.000000 = O(141) TO C(142) TO C(143) 
ANGLE 109.000000 , 1.000000 = C(142) TO C(143) TO C(144) 
DISTANCE 1.460000 , 0.005000 = O(141) TO C(342) 
DISTANCE 1.505000 , 0.005000 = C(342) TO C(343) 
DISTANCE 1.544000 , 0.005000 = C(343) TO C(344) 
ANGLE 109.000000 , 1.000000 = O(141) TO C(342) TO C(343) 
ANGLE 109.000000 , 1.000000 = C(342) TO C(343) TO C(344) 
U(IJ)'S  0.0, 0.010000 = O(141) TO C(142) 
U(IJ)'S  0.0, 0.010000 = O(141) TO C(143) 
U(IJ)'S  0.0, 0.010000 = O(141) TO C(144) 
U(IJ)'S  0.0, 0.010000 = O(141) TO C(342) 
U(IJ)'S  0.0, 0.010000 = O(141) TO C(343) 
U(IJ)'S  0.0, 0.010000 = O(141) TO C(344) 
U(IJ)'S  0.0, 0.010000 = C(11) TO C(13) 
U(IJ)'S  0.0, 0.010000 = C(10) TO C(26) 
U(IJ)'S  0.0, 0.010000 = C(7) TO C(9) 
U(IJ)'S  0.0, 0.010000 = C(7) TO C(13) 
END                                                                             
;