Cryptands with 1,3,5-Tris(1',3'-dioxan-2'-yl)-benzene Units: Synthesis and Structural Investigations
Monica Cîrcu; Albert Soran; Niculina Daniela Hădade; Monica Rednic; Anamaria Terec; Ion Grosu; Journal of Organic Chemistry 78 (2013) 8722–8729; doi:10.1021/jo401432y

data_4028568
_publ_section_title
;
 Cryptands with 1,3,5-Tris(1',3'-dioxan-2'-yl)-benzene Units: Synthesis
 and Structural Investigations
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8722
_journal_page_last               8729
_journal_paper_doi               10.1021/jo401432y
_journal_volume                  78
_journal_year                    2013
_chemical_formula_moiety         'C36 H48 O9, C H Cl3'
_chemical_formula_sum            'C37 H49 Cl3 O9'
_chemical_formula_weight         744.11
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   12.5910(7)
_cell_length_b                   12.5910(7)
_cell_length_c                   43.157(5)
_cell_measurement_reflns_used    4056
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      25.15
_cell_measurement_theta_min      2.66
_cell_volume                     5925.2(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            14367
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.282
_exptl_absorpt_correction_T_max  0.9202
_exptl_absorpt_correction_T_min  0.8884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker, 2001.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       block
_exptl_crystal_F_000             2364
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0871
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+24.3483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1650
_refine_ls_wR_factor_ref         0.1734
_reflns_number_gt                1924
_reflns_number_total             2325
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo401432y_si_002.cif
_cod_data_source_block           122alb
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4028568