Uranium complexes supported by an aryloxide functionalised triazacyclononane macrocycle: synthesis and characterisation of a six-coordinate U(III) species and insights into its reactivity
Castro-Rodriguez, Ingrid; Olsen, Kristian; Gantzel, Peter; Meyer, Karsten; Chemical Communications (Cambridge, United Kingdom)  (2002) 2764–2765; doi:10.1039/b208473b

data_7111263
_publ_section_title
;
 Uranium complexes supported by an aryloxide functionalised
 triazacyclononane macrocycle: synthesis and characterisation of a
 six-coordinate U(III) species and insights into its reactivity
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   23
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom) 
;
_journal_page_first              2764
_journal_page_last               2765
_journal_paper_doi               10.1039/b208473b
_journal_year                    2002
_chemical_formula_sum            'C55 H88 N3 O4.5 U'
_chemical_formula_weight         1101.31
_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-97
_cell_angle_alpha                60.832(2)
_cell_angle_beta                 74.682(2)
_cell_angle_gamma                66.580(2)
_cell_formula_units_Z            2
_cell_length_a                   14.8550(17)
_cell_length_b                   15.0174(17)
_cell_length_c                   15.2609(17)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      2.24
_cell_volume                     2717.3(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0891
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22661
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    3.032
_exptl_absorpt_correction_T_max  0.6940
_exptl_absorpt_correction_T_min  0.5823
_exptl_absorpt_correction_type   'SADABS (BrukerAXS SaintPlus Program Suite)'
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1134
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         5.185
_refine_diff_density_min         -3.406
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         11787
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0646
_refine_ls_shift/su_max          0.078
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0993P)^2^+0.0000P] where 
P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1525
_refine_ls_wR_factor_ref         0.1674
_reflns_number_gt                8803
_reflns_number_total             11787
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b208473bsup1.cif
_cod_data_source_block           oxo
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C55 H88 N3 O4.50 U'
_cod_database_code               7111263