First Structurally Characterized Actinide Isocyanates
Margaret-Jane Crawford; Peter Mayer; Heinrich Nöth; Max Suter; Inorganic Chemistry 43 (2004) 6860–6862; doi:10.1021/ic049078x

data_4311883
_publ_contact_author
;
      Margaret-Jane Crawford
      Institut f\"ur anorganische Chemie
      Universit\"at M\"unchen
      Butenandtstr. 5-13 (Haus D)
      81377 M\"unchen
      Bundesrepublik Deutschland
;
_publ_contact_author_email       mjc@cup.uni-muenchen.de
_publ_contact_author_fax         '089 2180 77492'
_publ_contact_author_phone       '089 2180 77503'
_publ_section_title
;
 First Structurally Characterized Actinide Isocyanates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6860
_journal_page_last               6862
_journal_paper_doi               10.1021/ic049078x
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety
'4(U O2), O2, 10(N C O), 6(N C8 H20), 2(C2 H3 N), H2 O'
_chemical_formula_sum            'C62 H128 N18 O21 U4'
_chemical_formula_weight         2413.904
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_cell_angle_alpha                90.00
_cell_angle_beta                 94.0849(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2787(2)
_cell_length_b                   15.56100(10)
_cell_length_c                   32.7619(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.134
_cell_volume                     8786.44(16)
_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    'SHELXS-97 (Sheldrick, 1990)'
_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_type  KappaCCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0858
_diffrn_reflns_av_sigmaI/netI    0.0628
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            106430
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    7.422
_exptl_absorpt_correction_T_max  0.8015
_exptl_absorpt_correction_T_min  0.4573
_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            yellow
_exptl_crystal_density_diffrn    1.82483(3)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             4648
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.505
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     873
_refine_ls_number_reflns         15478
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0581
_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^)+(0.0348P)^2^+107.2743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1245
_reflns_number_gt                10343
_reflns_number_total             15478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049078xsi20040713_061156_2.cif
_cod_data_source_block           Hn157
_cod_database_code               4311883