Practical Synthetic Routes to Solvates of U(OTf)3: X-ray Crystal Structure of [U(OTf)3(MeCN)3]n, a Unique U(III) Coordination Polymer
Louise Natrajan; Marinella Mazzanti; Jean-Philippe Bezombes; Jacques Pécaut; Inorganic Chemistry 44 (2005) 6115–6121; doi:10.1021/ic0505652

data_4309438
_publ_section_title
;
Practical Synthetic Routes to Solvates of U(OTf)3: X-ray Crystal Structure
of [U(OTf)3(MeCN)3]n, a Unique U(III) Coordination Polymer
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6115
_journal_page_last               6121
_journal_paper_doi               10.1021/ic0505652
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C23 H20 F9 N4 O9.5 S3 U'
_chemical_formula_weight         1009.64
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 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                 110.751(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.055(4)
_cell_length_b                   13.973(4)
_cell_length_c                   18.653(6)
_cell_measurement_temperature    223(2)
_cell_volume                     3425.6(18)
_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      223(2)
_diffrn_measured_fraction_theta_full 0.906
_diffrn_measured_fraction_theta_max 0.906
_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  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0700
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21179
_diffrn_reflns_theta_full        28.90
_diffrn_reflns_theta_max         28.90
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    5.024
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1932
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         5.425
_refine_diff_density_min         -1.689
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         8173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0642P)^2^+23.4219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1537
_reflns_number_gt                5817
_reflns_number_total             8173
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0505652si20050412_092311_2.cif
_cod_data_source_block           struc_[{U(OTf)2(py)3}2{m-O}{m-OTf}2](2).2py
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3425.7(18)
_cod_original_formula_sum        'C23 H20 F9 N4 O9.50 S3 U'
_cod_database_code               4309438