Synthesis and structural exploration of disulfide bridged [2n] pillararene-like molecules
Mahendra P. Sonawane; Jeroen Jacobs; Joice Thomas; Luc Van Meervelt; Wim Dehaen; Chem.Commun. 49 (2013) 6310–; doi:10.1039/c3cc42984a

data_7109467
_publ_section_title
;
 Synthesis and structural exploration of disulfide bridged [2n]
 pillararene-like molecules
;
_journal_name_full               Chem.Commun.
_journal_page_first              6310
_journal_paper_doi               10.1039/c3cc42984a
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C36 H40 O8 S4, 0.5(C4 H6 N2)'
_chemical_formula_sum            'C38 H43 N O8 S4'
_chemical_formula_weight         769.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-04-11
_audit_creation_method
;
Olex2 1.1
(compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.785(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.8050(10)
_cell_length_b                   16.8099(6)
_cell_length_c                   11.1767(5)
_cell_measurement_reflns_used    5116
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1450
_cell_measurement_theta_min      3.2230
_cell_volume                     3628.7(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb 1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb 1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb 1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9631
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
1 omega -4.00 52.00 1.0000 95.0000
omega____ theta____ kappa____ phi______ frames
- -17.1513 57.0000 -180.0000 56

2 omega -11.00 21.00 1.0000 95.0000
omega____ theta____ kappa____ phi______ frames
- -17.1513 -99.0000 -60.0000 32

3 omega -39.00 52.00 1.0000 95.0000
omega____ theta____ kappa____ phi______ frames
- -17.1513 57.0000 -60.0000 91

4 omega -3.00 22.00 1.0000 95.0000
omega____ theta____ kappa____ phi______ frames
- -17.1513 -99.0000 -180.0000 25

5 omega -74.00 -36.00 1.0000 95.0000
omega____ theta____ kappa____ phi______ frames
- -17.1513 -178.0000 150.0000 38

6 omega -59.00 -34.00 1.0000 95.0000
omega____ theta____ kappa____ phi______ frames
- -17.1513 178.0000 -120.0000 25

7 omega -94.00 -49.00 1.0000 95.0000
omega____ theta____ kappa____ phi______ frames
- -17.1513 178.0000 60.0000 45

8 omega 19.00 52.00 1.0000 95.0000
omega____ theta____ kappa____ phi______ frames
- -17.1513 57.0000 -30.0000 33

9 omega -86.00 0.00 1.0000 95.0000
omega____ theta____ kappa____ phi______ frames
- -17.1513 -57.0000 30.0000 86
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0039346000
_diffrn_orient_matrix_UB_12      0.0181080000
_diffrn_orient_matrix_UB_13      -0.0553616000
_diffrn_orient_matrix_UB_21      0.0365003000
_diffrn_orient_matrix_UB_22      -0.0032142000
_diffrn_orient_matrix_UB_23      0.0195644000
_diffrn_orient_matrix_UB_31      -0.0012225000
_diffrn_orient_matrix_UB_32      -0.0379586000
_diffrn_orient_matrix_UB_33      -0.0281125000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4231
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.06
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb 1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         4231
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+8.4547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1199
_reflns_number_gt                3679
_reflns_number_total             4231
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc42984a.txt
_cod_data_source_block           wdh1020b_twin1_hklf4
_cod_database_code               7109467
_chemical_oxdiff_formula         'C15 H20 O5 N4 S4'