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_4321466
_publ_section_title
;
 Calixarenes as Scaffolds: Introduction of Tridentate Rare Earth Metal
 Binding Units into Calix[4]arene
;
_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
'C78 H106 N6 O10, (H2 O), 0.5(C2 H6 O), 0.5(C H2 Cl2)'
_chemical_formula_sum            'C79.5 H112 Cl N6 O11.5'
_chemical_formula_weight         1371.20
_chemical_name_common
'1,3-dialkyl derivative of p-t-Butylcalix[4]arene, cone conformation'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-93
_cell_angle_alpha                86.45(3)
_cell_angle_beta                 79.09(3)
_cell_angle_gamma                74.87(3)
_cell_formula_units_Z            2
_cell_length_a                   12.395(2)
_cell_length_b                   18.021(4)
_cell_length_c                   18.763(4)
_cell_measurement_reflns_used    12
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.40
_cell_measurement_theta_min      11.75
_cell_volume                     3972.3(15)
_computing_cell_refinement       'Local diffractometer control software'
_computing_data_collection       'Local diffractometer control software'
_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_type  'Huber 512 goniometer'
_diffrn_measurement_method       '\w-2\q scan'
_diffrn_radiation_monochromator  none
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10864
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.0055(14)
_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   1.004
_refine_ls_goodness_of_fit_obs   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         10476
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.000
_refine_ls_restrained_S_obs      1.134
_refine_ls_R_factor_all          0.1411
_refine_ls_R_factor_obs          0.1098
_refine_ls_shift/esd_max         -1.353
_refine_ls_shift/esd_mean        0.022
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.1799P)^2^+7.2939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3314
_refine_ls_wR_factor_obs         0.2982
_reflns_number_observed          6780
_reflns_number_total             10476
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000353z_1.cif
_cod_data_source_block           L4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.1799P)^2^+7.2939P] 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^)+( 0.1799P)^2^+7.2939P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3972.3(14)
_cod_original_formula_sum        'C79.50 H112 Cl N6 O11.50'
_cod_database_code               4321466