Synthesis and Structural Characterization of Unprecedented Bis-Asymmetric Heteroscorpionate U(III) Complexes: [U{κ3-H2B(pztBu,Me)(pzMe,tBu)}2I] and [U{κ3-H2B(pztBu,Me)(pzMe2)}2I]
Leonor Maria; Ângela Domingos; Isabel Santos; Inorganic Chemistry 42 (2003) 3323–3330; doi:10.1021/ic026210p

data_4313640
_publ_section_title
;
 Synthesis and Structural Characterization of Unprecedented Bis-Asymmetric
 Heteroscorpionate U(III) Complexes: [U{\k3-H2B(pztBu,Me)(pzMe,tBu)}2I]
 and [U{\k3-H2B(pztBu,Me)(pzMe2)}2I]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3323
_journal_page_last               3330
_journal_paper_doi               10.1021/ic026210p
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         '[UI{k3-H2B(pztBu,Me)(pzMe2)}2]'
_chemical_formula_sum            'C26 H44 B2 I N8 U'
_chemical_formula_weight         855.24
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 110.810(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.762(2)
_cell_length_b                   10.2865(10)
_cell_length_c                   19.579(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.9
_cell_measurement_theta_min      7.7
_cell_volume                     3343.9(7)
_computing_cell_refinement       'CAD4 sofware(Enraf-Nonius,1989)'
_computing_data_collection       'CAD4 sofware(Enraf-Nonius,1989)'
_computing_data_reduction        process-MoLEN(Fair,1990)
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  CAD4-Enraf-Nonius
_diffrn_measurement_method       \w/2\qscans
_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  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0773
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7081
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        3.6
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.805
_exptl_absorpt_correction_T_max  0.100
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   'empirical via \y-scan North et al(1968)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.453
_refine_diff_density_min         -1.342
_refine_diff_density_rms         0.167
_refine_ls_extinction_coef       0.00105(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6878
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0559
_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^)+(0.0337P)^2^+14.4155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.1139
_reflns_number_gt                4398
_reflns_number_total             6878
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026210psi20030121_040124_2.cif
_cod_data_source_block           ulassim
_cod_database_code               4313640