An unprecedented trigonal coordination geometry for the uranyl ion in its complex with p-tert-butylhexahomotrioxacalix[3]arene
Thuéry, Pierre; Nierlich, Martine; Masci, Bernardo; Asfari, Zouhair; Vicens, Jacques; Journal of the Chemical Society, Dalton Transactions  (1999) 3151–; doi:10.1039/a905939c

data_7027724
_publ_section_title
;
 An unprecedented trigonal coordination geometry for the uranyl ion in its
 complex with p-tert-butylhexahomotrioxacalix[3]arene
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3151
_journal_paper_doi               10.1039/a905939c
_journal_year                    1999
_chemical_formula_sum            'C42 H67 N O11 U'
_chemical_formula_weight         1000.00
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.844(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.464(3)
_cell_length_b                   14.203(2)
_cell_length_c                   19.590(2)
_cell_measurement_reflns_used    21286
_cell_measurement_temperature    270(2)
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      3.49
_cell_volume                     4578.5(12)
_computing_cell_refinement       'HKL package (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD software (Nonius, 1997)'
_computing_data_reduction        'HKL package (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, 1990)'
_diffrn_ambient_temperature      270(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'area detector'
_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  0.085
_diffrn_reflns_av_sigmaI/netI    0.087
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21286
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         3.49
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    3.600
_exptl_absorpt_correction_T_max  0.371
_exptl_absorpt_correction_T_min  0.303
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'MULABS (Spek, 1997)'
_exptl_crystal_colour            'translucent dark orange'
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.319
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         6299
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1384
_refine_ls_R_factor_gt           0.0816
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+20.3268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1720
_refine_ls_wR_factor_ref         0.2008
_reflns_number_gt                3733
_reflns_number_total             6299
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            905939Csup1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        4579(4)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7027724