Spectroscopic Evidence for the Direct Coordination of the Pertechnetate Anion to the Uranyl Cation in [UO2(TcO4)(DPPMO2)2]+
Andrew D. Sutton; Gordon H. John; Mark J. Sarsfield; Joanna C. Renshaw; Iain May; Leigh R. Martin; Andrew J. Selvage; David Collison; Madeleine Helliwell; Inorganic Chemistry 43 (2004) 5480–5482; doi:10.1021/ic049588r

data_4311515
_publ_contact_author
;
    Madeleine Helliwell and Mark Sarsfield
;
_publ_section_title
;
 Spectroscopic Evidence for the Direct Coordination of the Pertechnetate
 Anion to the Uranyl Cation in [UO2(TcO4)(DPPMO2)2]+
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5480
_journal_page_last               5482
_journal_paper_doi               10.1021/ic049588r
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C50.75 H50 Cl2 O8.25 P4 U'
_chemical_formula_weight         1224.72
_chemical_name_systematic
; 
 ? 
;
_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                73.868(2)
_cell_angle_beta                 87.715(2)
_cell_angle_gamma                81.923(2)
_cell_formula_units_Z            4
_cell_length_a                   14.5893(16)
_cell_length_b                   19.282(2)
_cell_length_c                   19.991(2)
_cell_measurement_reflns_used    5882
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.53
_cell_measurement_theta_min      2.22
_cell_volume                     5348.7(10)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0713
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28032
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    3.304
_exptl_absorpt_correction_T_max  0.609
_exptl_absorpt_correction_T_min  0.488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pale
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2426
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.446
_refine_diff_density_min         -1.181
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1178
_refine_ls_number_reflns         18595
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+14.5358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1356
_reflns_number_gt                14347
_reflns_number_total             18595
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049588rsi20040709_010833_2.cif
_cod_data_source_block           s1452abs
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        5348.8(10)
_cod_database_code               4311515