Synthesis of homooxacalixarenes with 5 and 10 phenol units and crystal structure of their complexes with uranyl ions
Bernardo Masci; Pierre Thuéry; New Journal of Chemistry 29 (2005) 493–; doi:10.1039/b413827a

data_7050049
_publ_section_title
;
 Synthesis of homooxacalixarenes with 5 and 10 phenol units and crystal
 structure of their complexes with uranyl ions
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              493
_journal_paper_doi               10.1039/b413827a
_journal_volume                  29
_journal_year                    2005
_chemical_formula_sum            'C141.5 H183.5 N7.5 O14 U'
_chemical_formula_weight         2451.49
_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     patter
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.325(6)
_cell_angle_beta                 96.207(5)
_cell_angle_gamma                108.071(6)
_cell_formula_units_Z            2
_cell_length_a                   16.0169(17)
_cell_length_b                   16.2046(10)
_cell_length_c                   27.024(3)
_cell_measurement_reflns_used    39820
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.74
_cell_volume                     6551.9(11)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD software (Nonius B.V., 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full 0.873
_diffrn_measured_fraction_theta_max 0.873
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '\f scans'
_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  0.0833
_diffrn_reflns_av_sigmaI/netI    0.0928
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            39820
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.74
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    1.302
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent dark orange'
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2578
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.930
_refine_diff_density_min         -1.623
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1522
_refine_ls_number_reflns         21721
_refine_ls_number_restraints     342
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1717
_refine_ls_R_factor_gt           0.0867
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1017P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1842
_refine_ls_wR_factor_ref         0.2307
_reflns_number_gt                11742
_reflns_number_total             21721
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b413827a.txt
_cod_data_source_block           18
_cod_original_cell_volume        6552.0(11)
_cod_original_formula_sum        'C141.50 H183.50 N7.50 O14 U'
_cod_database_code               7050049