Functional heterocyclic molecular inclusion in p-sulfonatocalix[5]arene and lanthanide(iii) complexes
Ling, Irene; Sobolev, Alexandre N.; Raston, Colin L.; RSC Adv. 6 (2016) 102695–; doi:10.1039/C6RA23283C

data_7226965
_publ_section_title
;
 Functional heterocyclic molecular inclusion in p-sulfonatocalix[5]arene
 and lanthanide(iii) complexes
;
_journal_issue                   104
_journal_name_full               'RSC Adv.'
_journal_page_first              102695
_journal_paper_doi               10.1039/C6RA23283C
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety
'4(C35 H27 O20 S5), 2(Cl), 4.67(Yb), 2(C18 H16 O5), C2 H6 O, C H4 O, 43(H2 O)'
_chemical_formula_sum            'C179 H236 Cl2 O135 S20 Yb4.67'
_chemical_formula_weight         6067.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-11-19 deposited with the CCDC.
2016-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                77.93(2)
_cell_angle_beta                 70.96(1)
_cell_angle_gamma                75.49(2)
_cell_formula_units_Z            1
_cell_length_a                   17.214(3)
_cell_length_b                   18.887(7)
_cell_length_c                   20.574(3)
_cell_measurement_reflns_used    12051
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.99
_cell_measurement_theta_min      2.43
_cell_volume                     6062(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Oxford Diffraction Gemini-R Ultra, Ruby CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_unetI/netI     0.0805
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            66742
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        65.002
_diffrn_reflns_theta_max         65.002
_diffrn_reflns_theta_min         2.770
_exptl_absorpt_coefficient_mu    5.947
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       needle
_exptl_crystal_F_000             3071
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.288
_refine_diff_density_min         -2.033
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1496
_refine_ls_number_reflns         20449
_refine_ls_number_restraints     344
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1989
_refine_ls_R_factor_gt           0.1470
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1600P)^2^+80.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3627
_refine_ls_wR_factor_ref         0.3914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10133
_reflns_number_total             20449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra23283c2.cif
_cod_data_source_block           complex2
_cod_database_code               7226965
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.297
_shelx_estimated_absorpt_t_max   0.842
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              53987