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_7153834
_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           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 115.888(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1361(9)
_cell_length_b                   11.0596(5)
_cell_length_c                   20.1127(9)
_cell_measurement_reflns_used    3486
_cell_measurement_temperature    180
_cell_measurement_theta_max      76
_cell_measurement_theta_min      4
_cell_volume                     3629.3(3)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_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      180
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.084
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14943
_diffrn_reflns_theta_full        68.385
_diffrn_reflns_theta_max         75.984
_diffrn_reflns_theta_min         4.686
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.735
_exptl_absorpt_correction_T_max  0.14
_exptl_absorpt_correction_T_min  0.06
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1792.000
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.180
_refine_diff_density_max         2.47
_refine_diff_density_min         -2.48
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9890
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         7279
_refine_ls_number_restraints     64
_refine_ls_R_factor_all          0.1200
_refine_ls_R_factor_gt           0.1076
_refine_ls_shift/su_max          0.0094938
_refine_ls_shift/su_mean         0.0005521
_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: 
 0.375E+04 0.614E+04 0.382E+04 0.167E+04 421. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3006
_refine_ls_wR_factor_gt          0.2934
_refine_ls_wR_factor_ref         0.3006
_reflns_limit_h_max              20
_reflns_limit_h_min              -22
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                5978
_reflns_number_total             7289
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.71
_oxford_diffrn_Wilson_scale      0.83
_oxford_refine_ls_r_factor_ref   0.1200
_oxford_refine_ls_scale          1.439(15)
_oxford_reflns_number_all        7279
_oxford_reflns_threshold_expression_ref I>-3.0\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_sg_symbol_H-M      'P 1 21/a 1 '
_cod_original_formula_sum        'C36 H39 Cl1 Hg1 O4 S4'
_cod_database_code               7153834
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
SUMFIX ELEMENT SCALES 
RIDE C   (   4,X'S) H   ( 371,X'S) 
RIDE C   (   5,X'S) H   (  41,X'S) 
RIDE C   (   6,X'S) H   (  51,X'S) 
RIDE C   (  10,X'S) H   ( 471,X'S) 
RIDE C   (  11,X'S) H   ( 461,X'S) 
RIDE C   (  12,X'S) H   ( 451,X'S) 
RIDE C   (  16,X'S) H   ( 441,X'S) 
RIDE C   (  17,X'S) H   ( 431,X'S) 
RIDE C   (  18,X'S) H   ( 421,X'S) 
RIDE C   (  22,X'S) H   ( 411,X'S) 
RIDE C   (  23,X'S) H   ( 401,X'S) 
RIDE C   (  24,X'S) H   ( 391,X'S) 
RIDE C   (  30,X'S) H   (1011,X'S) H   (1012,X'S) 
RIDE C   (  31,X'S) H   (1021,X'S) H   (1022,X'S) 
RIDE C   (  32,X'S) H   (1031,X'S) H   (1032,X'S) H   (1033,X'S) 
RIDE C   (  34,X'S) H   ( 121,X'S) H   ( 122,X'S) 
RIDE C   (  35,X'S) H   ( 131,X'S) H   ( 132,X'S) 
RIDE C   (  36,X'S) H   ( 141,X'S) H   ( 142,X'S) H   ( 143,X'S) 
RIDE C   (  38,X'S) H   ( 201,X'S) H   ( 202,X'S) 
RIDE C   (  39,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE C   (  40,X'S) H   ( 221,X'S) H   ( 222,X'S) H   ( 223,X'S) 
RIDE C   (  42,X'S) H   ( 281,X'S) H   ( 282,X'S) 
RIDE C   (  43,X'S) H   ( 291,X'S) H   ( 292,X'S) 
RIDE C   (  44,X'S) H   ( 301,X'S) H   ( 302,X'S) H   ( 303,X'S) 
RIDE C   ( 130,X'S) H   (2011,X'S) H   (2012,X'S) 
RIDE C   ( 131,X'S) H   (2021,X'S) H   (2022,X'S) 
RIDE C   ( 132,X'S) H   (2031,X'S) H   (2032,X'S) H   (2033,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 1.441000 , 0.005000 = O(29) TO C(30) 
DISTANCE 1.525000 , 0.005000 = C(30) TO C(31) 
DISTANCE 1.539000 , 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 1.441000 , 0.005000 = O(29) TO C(130) 
DISTANCE 1.525000 , 0.005000 = C(130) TO C(131) 
DISTANCE 1.539000 , 0.005000 = C(131) TO C(132) 
ANGLE 109.000000 , 1.000000 = O(29) TO C(130) TO C(131) 
ANGLE 109.000000 , 1.000000 = C(130) TO C(131) TO C(132) 
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(130) 
U(IJ)'S  0.0, 0.010000 = O(29) TO C(131) 
U(IJ)'S  0.0, 0.010000 = O(29) TO C(132) 
U(IJ)'S  0.0, 0.010000 = CL(46) TO CL(48) 
U(IJ)'S  0.0, 0.010000 = C(38) TO C(39) 
U(IJ)'S  0.0, 0.010000 = C(39) TO C(40) 
END                                                                             
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