Calixarenes as Scaffolds: Introduction of Tridentate Rare Earth Metal Binding Units into Calix[4]arene
Pascal Froidevaux; Jack M. Harrowfield; Alexander N. Sobolev; Inorganic Chemistry 39 (2000) 4678–4687; doi:10.1021/ic000353z

data_4321467
_publ_section_title
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 Calixarenes as Scaffolds: Introduction of Tridentate Rare Earth Metal
 Binding Units into Calix[4]arene
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4678
_journal_page_last               4687
_journal_paper_doi               10.1021/ic000353z
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         'C70 H86 N2 O14, H2O'
_chemical_formula_sum            'C70 H88 N2 O15'
_chemical_formula_weight         1197.42
_chemical_name_common
'1,3-dialkyl derivative of p-t-Butylcalix[4]arene, 1,2-alternate conformation'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-93
_cell_angle_alpha                90.0
_cell_angle_beta                 108.57(3)
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   14.190(3)
_cell_length_b                   13.444(3)
_cell_length_c                   18.258(4)
_cell_measurement_reflns_used    12
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      11.1
_cell_volume                     3301.7(14)
_computing_cell_refinement       'Siemens P3/P4-PC software, rev. 4.27, 1991'
_computing_data_collection       'Siemens P3/P4-PC software, rev. 4.27, 1991'
_computing_data_reduction        'PROFIT (Streltsov & Zavodnik, 1989)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1983)'
_computing_publication_material  'SHELXTL (Sheldrick, 1983)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P3/P4'
_diffrn_measurement_method       '\w-2\q scan'
_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  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8397
_diffrn_reflns_theta_max         22.57
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        3
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       Rhombic
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.0027(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.247
_refine_ls_goodness_of_fit_obs   1.322
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         4323
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.290
_refine_ls_restrained_S_obs      1.315
_refine_ls_R_factor_all          0.1238
_refine_ls_R_factor_obs          0.0811
_refine_ls_shift/esd_max         0.008
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0740P)^2^+3.0440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2389
_refine_ls_wR_factor_obs         0.1953
_reflns_number_observed          2892
_reflns_number_total             4352
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000353z_2.cif
_cod_data_source_block           L2A
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0740P)^2^+3.0440P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'.
New tag '_refine_ls_weighting_details' was created. The value of the
new tag was set to 'w=1/[s^2^(Fo^2^)+( 0.0740P)^2^+3.0440P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        3301.7(12)
_cod_database_code               4321467