Use of solvent to regulate the degree of polymerisation in weakly associated supramolecular oligomers
Steffen Bahring; Dong Sub Kim; Troels Duedal; Vincent M. Lynch; Kent A. Nielsen; Jan O. Jeppesen; Jonathan L. Sessler; Chem.Commun. 50 (2014) 5497–; doi:10.1039/C4CC01514B

data_7113312
_publ_section_title
;
 Use of solvent to regulate the degree of polymerisation in weakly
 associated supramolecular oligomers
;
_journal_name_full               Chem.Commun.
_journal_page_first              5497
_journal_paper_doi               10.1039/C4CC01514B
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C68 H84 N4 S24, C17 H12 N4 O12, 4 C H2 Cl2'
_chemical_formula_sum            'C89 H104 Cl8 N8 O12 S24'
_chemical_formula_weight         2530.84
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                85.987(2)
_cell_angle_beta                 68.623(2)
_cell_angle_gamma                81.231(3)
_cell_formula_units_Z            2
_cell_length_a                   16.645(6)
_cell_length_b                   18.555(7)
_cell_length_c                   20.012(6)
_cell_measurement_reflns_used    20868
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.5
_cell_volume                     5687(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1734
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            26041
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2620
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
What appeared to be two molecules of DCM were badly disordered.  These 
molecules could not be adequately modeled.  Their contributions to the 
scattering were removed by the use of the utility Squeeze as 
incorporated into Platon98 (Spek, 1998).
;
_refine_diff_density_max         1.650
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.227
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1229
_refine_ls_number_reflns         26041
_refine_ls_number_restraints     850
_refine_ls_restrained_S_all      1.347
_refine_ls_R_factor_all          0.2256
_refine_ls_R_factor_gt           0.1385
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3197
_refine_ls_wR_factor_ref         0.3599
_reflns_number_gt                11574
_reflns_number_total             26041
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc01514b2.cif
_cod_data_source_block           shelxl_a
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7113312