First Actinide Complexes of the Nitrogen-Containing Ligands Dinitramide (N(NO2)2-), 4,5-Dicyano-1,2,3-triazolate (C4N5-), and Dicyanamide (N(CN)2-)
Margaret-Jane Crawford; Arkady Ellern; Konstantin Karaghiosoff; Franz Martin; Peter Mayer; Inorganic Chemistry 49 (2010) 2674–2683; doi:10.1021/ic901820b

data_4315135
_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_fax         +49-89-2180-77492
_publ_contact_author_name        'M.-J. Crawford'
_publ_section_title
;
 First Actinide Complexes of the Nitrogen-Containing Ligands Dinitramide
 (N(NO2)2-), 4,5-Dicyano-1,2,3-triazolate (C4N5-), and Dicyanamide
 (N(CN)2-)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2674
_journal_page_last               2683
_journal_paper_doi               10.1021/ic901820b
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'U O2, 3(P O C18 H15), 2(C4 N5)'
_chemical_formula_sum            'C62 H45 N10 O5 P3 U'
_chemical_formula_weight         1341.035
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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_C4N5_POPh3_jn457_klapoetke
_audit_creation_date             31-Oct-05
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             10-Aug-09
_cell_angle_alpha                90.00
_cell_angle_beta                 111.4449(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.9970(2)
_cell_length_b                   31.9500(3)
_cell_length_c                   20.1133(2)
_cell_measurement_reflns_used    22494
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.134
_cell_volume                     11362.7(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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       phi/omega-scan
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0491846
_diffrn_orient_matrix_UB_12      -0.0042501
_diffrn_orient_matrix_UB_13      0.0066113
_diffrn_orient_matrix_UB_21      -0.0270734
_diffrn_orient_matrix_UB_22      0.0146042
_diffrn_orient_matrix_UB_23      -0.0463254
_diffrn_orient_matrix_UB_31      -0.0068121
_diffrn_orient_matrix_UB_32      -0.0273546
_diffrn_orient_matrix_UB_33      -0.0257596
_diffrn_radiation_collimation    0.25
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_sigmaI/netI    0.1212
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43753
_diffrn_reflns_theta_full        26.09
_diffrn_reflns_theta_max         26.09
_diffrn_reflns_theta_min         3.15
_diffrn_source_current           45.00
_diffrn_source_power             2.250
_diffrn_source_type              'FR 591 generator'
_diffrn_source_voltage           50.00
_exptl_absorpt_coefficient_mu    3.001
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.56785(3)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             5312
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.204
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1459
_refine_ls_number_reflns         22368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0129P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0661
_reflns_number_gt                13639
_reflns_number_total             22368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901820b_si_002_3.cif
_cod_data_source_block           jn457
_cod_original_cell_volume        11362.69(19)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4315135