A General Method for Synthesis of Unclosed Cryptands via H-Bond Templated Macrocyclization and Subsequent Mild Postfunctionalization.
Dabrowa, Kajetan; Niedbala, Patryk; Majdecki, Maciej; Duszewski, Piotr; Jurczak, Janusz; Organic letters 17 (2015) 4774–4777; doi:10.1021/acs.orglett.5b02324

data_1555300
_publ_section_title
;
 A General Method for Synthesis of Unclosed Cryptands via H-Bond Templated
 Macrocyclization and Subsequent Mild Postfunctionalization.
;
_journal_issue                   19
_journal_name_full               'Organic letters'
_journal_page_first              4774
_journal_page_last               4777
_journal_paper_doi               10.1021/acs.orglett.5b02324
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C33 H38 N6 O8 * (CH3)2SO'
_chemical_formula_sum            'C35 H44 N6 O9 S'
_chemical_formula_weight         724.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           'APEX2 v2014.11-0'
_cell_angle_alpha                94.6150(10)
_cell_angle_beta                 91.322(2)
_cell_angle_gamma                103.134(2)
_cell_formula_units_Z            2
_cell_length_a                   8.5759(5)
_cell_length_b                   13.6900(8)
_cell_length_c                   15.1168(9)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      25.4254
_cell_measurement_theta_min      2.4410
_cell_volume                     1721.18(18)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 V2014 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_publication_material  'APEX2 V2014 (Bruker AXS Inc., 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  TRIUMPH
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23866
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.44
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.254
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         6079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.6607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0942
_reflns_number_gt                4979
_reflns_number_total             6079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol5b02324_si_002.cif
_cod_data_source_block           7c-DMSO
_cod_database_code               1555300
_shelx_res_checksum              47277
_shelx_hkl_checksum              73154