"Choose-a-size" control in the synthesis of sucrose based urea and thiourea macrocycles.
Łęczycka-Wilk, Katarzyna; Ulatowski, Filip; Cmoch, Piotr; Jarosz, Sławomir; Organic & biomolecular chemistry 16 (2018) 6063–6069; doi:10.1039/c8ob01340c

data_7156354
_publ_section_title
;
 &quot;Choose-a-size&quot; control in the synthesis of sucrose based urea
 and thiourea macrocycles.
;
_journal_issue                   33
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              6063
_journal_page_last               6069
_journal_paper_doi               10.1039/c8ob01340c
_journal_volume                  16
_journal_year                    2018
_chemical_absolute_configuration rm
_chemical_formula_sum            'C55 H58 N2 O9 S'
_chemical_formula_weight         923.09
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-11-07 deposited with the CCDC.
2018-08-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1611(7)
_cell_length_b                   18.4375(11)
_cell_length_c                   23.2735(12)
_cell_measurement_reflns_used    2957
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      27.2720
_cell_measurement_theta_min      3.4300
_cell_volume                     4789.3(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.862
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_sigmaI/netI    0.1170
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16160
_diffrn_reflns_theta_full        29.21
_diffrn_reflns_theta_max         29.21
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.128
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.18(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         9844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1795
_reflns_number_gt                6643
_reflns_number_total             9844
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c8ob01340c2.cif
_cod_data_source_block           kl544_01
_cod_depositor_comments          'Adding full bibliography for 7156354.cif.'
_cod_original_sg_symbol_H-M      P212121
_cod_original_formula_sum        'C55 H58 N2 O9 S1'
_cod_database_code               7156354