Arylation of thiacalix[4]arenes using organomercurial intermediates
Botha, F.; Eigner, V.; Dvořáková, H.; Lhoták, P.; New J. Chem. 40 (2016) 1104–; doi:10.1039/C5NJ02427G

data_7055160
_publ_section_title
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 Arylation of thiacalix[4]arenes using organomercurial intermediates
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_journal_issue                   2
_journal_name_full               'New J. Chem.'
_journal_page_first              1104
_journal_paper_doi               10.1039/C5NJ02427G
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C72 H78 O8 S8'
_chemical_formula_sum            'C72 H78 O8 S8'
_chemical_formula_weight         1327.93
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2015-11-03 deposited with the CCDC.
2015-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.901(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.3452(6)
_cell_length_b                   9.1412(3)
_cell_length_c                   19.3696(7)
_cell_measurement_reflns_used    8072
_cell_measurement_temperature    200
_cell_measurement_theta_max      76
_cell_measurement_theta_min      5
_cell_volume                     3407.1(2)
_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      200
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.951
_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  0.055
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21605
_diffrn_reflns_theta_full        68.953
_diffrn_reflns_theta_max         77.476
_diffrn_reflns_theta_min         4.590
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.860
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.27
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.90
_refine_diff_density_min         -0.51
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9939
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         6871
_refine_ls_number_restraints     86
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.0018180
_refine_ls_shift/su_mean         0.0000551
_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: 
 869. 0.142E+04 819. 309. 60.7 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1804
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1804
_reflns_limit_h_max              23
_reflns_limit_h_min              -23
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                5216
_reflns_number_total             6896
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.85
_oxford_diffrn_Wilson_scale      0.24
_oxford_refine_ls_r_factor_ref   0.0826
_oxford_refine_ls_scale          1.674(11)
_oxford_reflns_number_all        6871
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_cod_data_source_file            c5nj02427g2.cif
_cod_data_source_block           13
_cod_depositor_comments
'Adding full bibliography for 7055158--7055162.cif.'
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               7055160
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   4,X'S) H   (  41,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   ( 311,X'S) H   ( 312,X'S) 
RIDE C   (  32,X'S) H   ( 322,X'S) H   ( 321,X'S) H   ( 323,X'S) 
CONTINUE C   ( 132,X'S) H   (1321,X'S) H   (1323,X'S) H   (1322,X'S) 
RIDE C   ( 130,X'S) H   (1302,X'S) H   (1301,X'S) 
RIDE C   ( 131,X'S) H   (1312,X'S) H   (1311,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 352,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 363,X'S) H   ( 362,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) 
RIDE C   (  39,X'S) H   ( 392,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 403,X'S) H   ( 402,X'S) H   ( 401,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 432,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 443,X'S) H   ( 442,X'S) H   ( 441,X'S) 
CONTINUE C   ( 144,X'S) H   (1442,X'S) H   (1441,X'S) H   (1443,X'S) 
RIDE C   ( 142,X'S) H   (1422,X'S) H   (1421,X'S) 
RIDE C   ( 143,X'S) H   (1431,X'S) H   (1432,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(130) 
U(IJ)'S  0.0, 0.010000 = O(29) TO C(131) 
U(IJ)'S  0.0, 0.001000 = C(32) TO C(132) 
DISTANCE 1.441000 , 0.005000 = O(41) TO C(42) 
DISTANCE 1.525000 , 0.005000 = C(42) TO C(43) 
DISTANCE 1.539000 , 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 1.441000 , 0.005000 = O(41) TO C(142) 
DISTANCE 1.525000 , 0.005000 = C(142) TO C(143) 
DISTANCE 1.539000 , 0.005000 = C(143) TO C(144) 
ANGLE 109.000000 , 1.000000 = O(41) TO C(142) TO C(143) 
ANGLE 109.000000 , 1.000000 = C(142) TO C(143) TO C(144) 
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(142) 
U(IJ)'S  0.0, 0.010000 = O(41) TO C(143) 
U(IJ)'S  0.0, 0.001000 = C(42) TO C(142) 
U(IJ)'S  0.0, 0.001000 = C(44) TO C(144) 
END                                                                             
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