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_7226966
_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
'6(C35 H26 O20 S5), 4(Gd), 4(Na), 8(C10 H19 N2), 39(H2 O)'
_chemical_formula_sum            'C290 H386 Gd4 N16 Na4 O159 S30'
_chemical_formula_weight         8322.88
_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                97.634(2)
_cell_angle_beta                 95.167(2)
_cell_angle_gamma                100.468(2)
_cell_formula_units_Z            1
_cell_length_a                   11.1318(2)
_cell_length_b                   17.7181(4)
_cell_length_c                   52.0066(12)
_cell_measurement_reflns_used    15404
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.478
_cell_measurement_theta_min      3.309
_cell_volume                     9928.5(4)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Oxford Diffraction Gemini-R Ultra, Ruby CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0099381
_diffrn_orient_matrix_UB_12      -0.0252611
_diffrn_orient_matrix_UB_13      0.0270788
_diffrn_orient_matrix_UB_21      -0.0104913
_diffrn_orient_matrix_UB_22      -0.0852949
_diffrn_orient_matrix_UB_23      -0.0123225
_diffrn_orient_matrix_UB_31      0.1409729
_diffrn_orient_matrix_UB_32      0.0095143
_diffrn_orient_matrix_UB_33      0.0045363
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            78155
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.638
_diffrn_reflns_theta_max         67.638
_diffrn_reflns_theta_min         3.357
_exptl_absorpt_coefficient_mu    6.558
_exptl_absorpt_correction_T_max  0.645
_exptl_absorpt_correction_T_min  0.277
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       needle
_exptl_crystal_F_000             4290
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_refine_diff_density_max         4.306
_refine_diff_density_min         -1.887
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2186
_refine_ls_number_reflns         35236
_refine_ls_number_restraints     927
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.1650
_refine_ls_R_factor_gt           0.1409
_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^)+(0.1200P)^2^+90.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3344
_refine_ls_wR_factor_ref         0.3502
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26185
_reflns_number_total             35236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra23283c2.cif
_cod_data_source_block           complex3
_cod_database_code               7226966
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.236
_shelx_estimated_absorpt_t_max   0.590
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              78249