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_7109466
_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
'0.5(C H2 Cl1.47), 0.26(Cl1), 0.5(C0.53 H1.11 Cl0.55), 0.5(C0.48 H0.81 Cl1.45), C32 H32 O8 S8'
_chemical_formula_sum            'C33 H33.96 Cl2 O8 S8'
_chemical_formula_weight         885.99
_chemical_name_systematic
;
?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-04-10
_audit_creation_method
;
Olex2 1.1
(compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                74.053(3)
_cell_angle_beta                 77.801(3)
_cell_angle_gamma                86.239(3)
_cell_formula_units_Z            4
_cell_length_a                   12.2168(4)
_cell_length_b                   14.4704(5)
_cell_length_c                   23.0473(9)
_cell_measurement_reflns_used    14527
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.1513
_cell_measurement_theta_min      2.7986
_cell_volume                     3829.0(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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      100.00(10)
_diffrn_detector_area_resol_mean 15.9631
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.838
_diffrn_measurement_details
;
1 omega -47.00 12.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- -17.1513 77.0000 60.0000 59

2 omega -19.00 23.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- -17.1513 -99.0000 90.0000 42

3 omega -86.00 1.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- -17.1513 -57.0000 -180.0000 87

4 omega 24.00 52.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- -17.1513 57.0000 -30.0000 28

5 omega -42.00 87.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 18.8701 0.0000 -180.0000 129

6 omega 2.00 57.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 18.8701 -99.0000 -30.0000 55
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0141124000
_diffrn_orient_matrix_UB_12      -0.0223590000
_diffrn_orient_matrix_UB_13      -0.0212064000
_diffrn_orient_matrix_UB_21      -0.0458871000
_diffrn_orient_matrix_UB_22      0.0322305000
_diffrn_orient_matrix_UB_23      -0.0036994000
_diffrn_orient_matrix_UB_31      0.0349839000
_diffrn_orient_matrix_UB_32      0.0325625000
_diffrn_orient_matrix_UB_33      -0.0245853000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            31867
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.22
_diffrn_reflns_theta_min         2.80
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     998
_refine_ls_number_reflns         17402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+1.3747P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0843
_reflns_number_gt                14749
_reflns_number_total             17402
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc42984a.txt
_cod_data_source_block           wdh1011
_cod_database_code               7109466
_chemical_oxdiff_formula         'C32 H32 O8 S8'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32