Synthesis, Structural and Computational Investigations of UO2I42-: A Structurally Characterized U(VI)-I Anion
Margaret-Jane Crawford; Peter Mayer; Inorganic Chemistry 44 (2005) 5547–5549; doi:10.1021/ic050231c

data_4309322
_publ_contact_author_address
;
Department Chemie
Ludwig-Maximilians Universit\"at
Butenandtstra\&se 5-13 (Haus D)
D-81377 M\"unchen
Bundesrepublik Deutschland
;
_publ_contact_author_email       mjc@cup.uni-muenchen.de
_publ_contact_author_name        'Margret-J. Crawford'
_publ_contact_author_phone       +49-89-2180-77501
_publ_section_title
;
Synthesis, Structural and Computational Investigations of UO2I42-: A
Structurally Characterized U(VI)-I Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5547
_journal_page_last               5549
_journal_paper_doi               10.1021/ic050231c
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'U O2 I4, 2(P C24 H20), 2(C2 H3 N)'
_chemical_formula_sum            'C52 H46 I4 N2 O2 P2 U'
_chemical_formula_weight         1538.528
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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_author_name               'Mayer, P.'
_audit_block_code                UO2_I4_PPh4_CH3CN_jn015_klapoetke
_audit_creation_date             19-Jan-05
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             08-Feb-05
_cell_angle_alpha                90.00
_cell_angle_beta                 114.2659(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.4148(5)
_cell_length_b                   7.9560(2)
_cell_length_c                   28.5906(6)
_cell_measurement_reflns_used    30197
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.134
_cell_volume                     5270.3(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution
;
A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A.
Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for
crystal structure determination and refinement; J. Appl. Crystallogr. 1999,
32, 115-119.
;
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0283544
_diffrn_orient_matrix_UB_12      -0.0675894
_diffrn_orient_matrix_UB_13      -0.0081245
_diffrn_orient_matrix_UB_21      0.0111454
_diffrn_orient_matrix_UB_22      0.1029420
_diffrn_orient_matrix_UB_23      -0.0138500
_diffrn_orient_matrix_UB_31      0.0305718
_diffrn_orient_matrix_UB_32      0.0251579
_diffrn_orient_matrix_UB_33      0.0348445
_diffrn_radiation_collimation    0.35
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            22604
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         3.21
_diffrn_source_current           75.00
_diffrn_source_power             4.125
_diffrn_source_type              'FR 591 generator'
_diffrn_source_voltage           55.00
_exptl_absorpt_coefficient_mu    5.523
_exptl_absorpt_correction_T_max  0.7951
_exptl_absorpt_correction_T_min  0.4329
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Crystal faces optimized with XShape, rev. 1.02, STOE (Darmstadt, Germany)
Absorption correction with XRed, rev 1.09, STOE (Darmstadt, Germany)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.93903(7)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.435
_refine_diff_density_min         -1.182
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         5192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0328P)^2^+6.3647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0821
_reflns_number_gt                3787
_reflns_number_total             5192
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050231csi20050214_042938.cif
_cod_data_source_block           jn015
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4309322