Regioisomers of singly bridged calix[6]crown-6 and their heavy alkali metal complexes: a molecular baseball glove for caesium(I)
Kim, Seulgi; Jung, Jong Hwa; Lee, Shim Sung; Park, In-Hyeok; IUCrJ 9 (2022) 43–48; doi:10.1107/S2052252521010563

data_1565847
_publ_section_title
;
 Regioisomers of singly bridged calix[6]crown-6 and their heavy alkali
 metal complexes: a molecular baseball glove for caesium(I)
;
_journal_issue                   1
_journal_name_full               IUCrJ
_journal_page_first              43
_journal_page_last               48
_journal_paper_doi               10.1107/S2052252521010563
_journal_volume                  9
_journal_year                    2022
_chemical_formula_moiety         'C52 H50 Cs O10, 3(C H Cl3)'
_chemical_formula_sum            'C55 H53 Cl9 Cs O10'
_chemical_formula_weight         1325.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 106.172(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1773(15)
_cell_length_b                   20.344(2)
_cell_length_c                   22.581(3)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.86
_cell_measurement_theta_min      2.31
_cell_volume                     5814.0(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    "'Bruker SHELXTL"
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            57934
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.313
_diffrn_reflns_theta_min         1.372
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.106
_exptl_absorpt_correction_T_max  0.8174
_exptl_absorpt_correction_T_min  0.7117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2684
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.190
_refine_diff_density_max         1.382
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         14416
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0628P)^2^+6.6900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1388
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9852
_reflns_number_total             14416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yc5035.cif
_cod_data_source_block           2
_cod_original_cell_volume        5814.2(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1565847
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.712
_shelx_estimated_absorpt_t_max   0.817
_shelx_res_checksum              30339
_shelx_hkl_checksum              20915