Complexes of uranium(IV) with acyclic polyphenoxides resulting from cleavage of homooxacalixarenes
Lionel Salmon; Pierre Thuéry; Michel Ephritikhine; Bernardo Masci; Dalton Trans.  (2003) 2405–2410; doi:10.1039/b302809g

data_7012938
_publ_section_title
;
 Complexes of uranium(IV) with acyclic polyphenoxides resulting from
 cleavage of homooxacalixarenes
;
_journal_issue                   12
_journal_name_full               'Dalton Trans.'
_journal_page_first              2405
_journal_page_last               2410
_journal_paper_doi               10.1039/b302809g
_journal_year                    2003
_chemical_formula_sum            'C91 H101 Cl4 N9 O4 U'
_chemical_formula_weight         1764.64
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 112.651(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.390(3)
_cell_length_b                   15.5898(16)
_cell_length_c                   20.2637(11)
_cell_measurement_reflns_used    27657
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.83
_cell_volume                     8859.9(14)
_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_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_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  0.0728
_diffrn_reflns_av_sigmaI/netI    0.1088
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27657
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.83
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    2.006
_exptl_absorpt_correction_T_max  0.818
_exptl_absorpt_correction_T_min  0.444
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent dark yellow'
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             3608
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.988
_refine_diff_density_min         -1.164
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.00107(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         7909
_refine_ls_number_restraints     188
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.1831
_refine_ls_R_factor_gt           0.0848
_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^)+(0.0925P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1726
_refine_ls_wR_factor_ref         0.2278
_reflns_number_gt                3751
_reflns_number_total             7909
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b302809g.txt
_cod_data_source_block           2
_cod_original_cell_volume        8859.9(13)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7012938