A General Method for High-Pressure-Promoted Postfunctionalization of Unclosed Cryptands: Potential Phase-Transfer Catalysts.
Tyszka-Gumkowska, Agata; Jurczak, Janusz; The Journal of organic chemistry  (2019) –; doi:10.1021/acs.joc.9b02985

data_4037743
_publ_section_title
;
 A General Method for High-Pressure-Promoted Postfunctionalization of
 Unclosed Cryptands: Potential Phase-Transfer Catalysts.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.9b02985
_journal_year                    2019
_chemical_formula_moiety         'C32 H44 N7 O8 1+, Cl 1-, 0.13(H2 O)'
_chemical_formula_sum            'C32 H44.26 Cl N7 O8.13'
_chemical_formula_weight         692.53
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                100.298(2)
_cell_angle_beta                 103.162(2)
_cell_angle_gamma                93.773(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5128(3)
_cell_length_b                   11.4465(3)
_cell_length_c                   16.0517(4)
_cell_measurement_reflns_used    19405
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      70.7210
_cell_measurement_theta_min      3.9390
_cell_volume                     1664.13(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01(10)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'micro-focus sealed X-ray tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0124
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29398
_diffrn_reflns_theta_full        70.68
_diffrn_reflns_theta_max         70.68
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    1.542
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             735
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.415
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         6343
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0854P)^2^+2.1604P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1405
_reflns_number_gt                6290
_reflns_number_total             6343
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jo9b02985_si_001.cif
_cod_data_source_block           p34_01
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4037743