Chemistry of 2,14-Dithiacalix[4]arene: Alkylation and Conformational Behavior of Peralkylated Products.
Kortus, Daniel; Mikšátko, Jiří; Kundrát, Ondřej; Babor, Martin; Eigner, Václav; Dvořáková, Hana; Lhoták, Pavel; The Journal of organic chemistry 84 (2019) 11572–11580; doi:10.1021/acs.joc.9b01493

data_4034510
_publ_section_title
;
 Chemistry of 2,14-Dithiacalix[4]arene: Alkylation and Conformational
 Behavior of Peralkylated Products.
;
_journal_issue                   18
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              11572
_journal_page_last               11580
_journal_paper_doi               10.1021/acs.joc.9b01493
_journal_volume                  84
_journal_year                    2019
_chemical_formula_moiety         'C50 H68 O4 S2'
_chemical_formula_sum            'C50 H68 O4 S2'
_chemical_formula_weight         797.22
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 107.3283(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1236(3)
_cell_length_b                   22.2391(7)
_cell_length_c                   10.7810(3)
_cell_measurement_reflns_used    119
_cell_measurement_temperature    180
_cell_measurement_theta_max      78
_cell_measurement_theta_min      9
_cell_volume                     2317.07(12)
_computing_cell_refinement       'Apex3 (Bruker AXS, 2015)'
_computing_data_collection       'Apex3 (Bruker AXS, 2015)'
_computing_data_reduction        'Apex3 (Bruker AXS, 2015)'
_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      180
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex3'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            34039
_diffrn_reflns_theta_full        68.291
_diffrn_reflns_theta_max         68.291
_diffrn_reflns_theta_min         4.734
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.355
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             864.000
_exptl_crystal_size_max          0.553
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.255
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.22
_refine_ls_extinction_coef       187(8)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9291
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         4237
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.0023697
_refine_ls_shift/su_mean         0.0000514
_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: 
 3.76 5.06 1.49 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0890
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0890
_reflns_limit_h_max              11
_reflns_limit_h_min              -12
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                4180
_reflns_number_total             4238
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.86
_oxford_diffrn_Wilson_scale      31.33
_oxford_refine_ls_r_factor_ref   0.0352
_oxford_refine_ls_scale          0.2596(3)
_oxford_reflns_number_all        4238
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            jo9b01493_si_005.cif
_cod_data_source_block           DK19_1
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Other' was changed to
'other' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               4034510
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
EQUIVALENCE PART(1001, OCC) 
EQUIVALENCE PART(1002, OCC) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) H   ( 173,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) H   ( 203,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) H   ( 223,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) H   ( 233,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) H   ( 243,X'S) 
RIDE C   ( 122,X'S) H   (1221,X'S) H   (1222,X'S) H   (1223,X'S) 
RIDE C   ( 123,X'S) H   (1231,X'S) H   (1232,X'S) H   (1233,X'S) 
RIDE C   ( 124,X'S) H   (1241,X'S) H   (1242,X'S) H   (1243,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) H   ( 263,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) H   ( 273,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) H   ( 283,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.540000 , 0.005000 = C(21) TO C(22) 
DISTANCE 1.540000 , 0.005000 = C(21) TO C(23) 
DISTANCE 1.540000 , 0.005000 = C(21) TO C(24) 
ANGLE 109.000000 , 1.000000 = C(22) TO C(21) TO C(23) 
ANGLE 109.000000 , 1.000000 = C(23) TO C(21) TO C(24) 
ANGLE 109.000000 , 1.000000 = C(24) TO C(21) TO C(22) 
DISTANCE 1.540000 , 0.005000 = C(121) TO C(122) 
DISTANCE 1.540000 , 0.005000 = C(121) TO C(123) 
DISTANCE 1.540000 , 0.005000 = C(121) TO C(124) 
ANGLE 109.000000 , 1.000000 = C(122) TO C(121) TO C(123) 
ANGLE 109.000000 , 1.000000 = C(123) TO C(121) TO C(124) 
ANGLE 109.000000 , 1.000000 = C(124) TO C(121) TO C(122) 
U(IJ)'S  0.0, 0.001000 = C(21) TO C(121) 
U(IJ)'S  0.0, 0.010000 = C(22) TO C(122) 
U(IJ)'S  0.0, 0.010000 = C(23) TO C(123) 
U(IJ)'S  0.0, 0.010000 = C(24) TO C(124) 
SUM 0.0001 PART(1001, OCC) PART(1002, OCC) 
END                                                                             
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