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_7111264
_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            'C65 H99 N3 O4 U'
_chemical_formula_weight         1224.50
_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                 90.188(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.737(3)
_cell_length_b                   15.0416(12)
_cell_length_c                   26.266(2)
_cell_measurement_temperature    228(2)
_cell_volume                     14119(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      228(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0730
_diffrn_reflns_av_sigmaI/netI    0.0869
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            58665
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    2.340
_exptl_absorpt_correction_T_max  0.7997
_exptl_absorpt_correction_T_min  0.5923
_exptl_absorpt_correction_type   'SADABS (BrukerAXS SaintPlus Program Suite)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       recatangular
_exptl_crystal_F_000             5072
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.918
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.266
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         15962
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.514
_refine_ls_shift/su_mean         0.048
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0721P)^2^+0.0000P] where 
P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1380
_reflns_number_gt                10202
_reflns_number_total             15962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b208473bsup1.cif
_cod_data_source_block           aryloxide
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      C2/c
_cod_database_code               7111264