Magnetic Exchange Coupling in Chloride-Bridged 5f-3d Heterometallic Complexes Generated via Insertion into a Uranium(IV) Dimethylpyrazolate Dimer
Stosh A. Kozimor; Bart M. Bartlett; Jeffrey D. Rinehart; Jeffrey R. Long; Journal of the American Chemical Society 129 (2007) 10672–10674; doi:10.1021/ja0725044

data_4109848
_publ_section_title
;
 Magnetic Exchange Coupling in Chloride-Bridged 5f-3d Heterometallic
 Complexes Generated via Insertion into a Uranium(IV) Dimethylpyrazolate
 Dimer
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10672
_journal_page_last               10674
_journal_paper_doi               10.1021/ja0725044
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C29 H42.67 K N10 O U'
_chemical_formula_weight         824.53
_chemical_name_systematic
; 
 ? 
;
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_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   11.813(2)
_cell_length_b                   18.933(4)
_cell_length_c                   46.577(9)
_cell_measurement_reflns_used    6262
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      24.44
_cell_measurement_theta_min      3.27
_cell_volume                     10417(3)
_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      113(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_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  0.0674
_diffrn_reflns_av_sigmaI/netI    0.1216
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            42274
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         3.27
_exptl_absorpt_coefficient_mu    4.831
_exptl_absorpt_correction_T_max  0.7942
_exptl_absorpt_correction_T_min  0.4302
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            plate
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_meas      0
_exptl_crystal_description       brown
_exptl_crystal_F_000             4868
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.983
_refine_diff_density_min         -3.588
_refine_diff_density_rms         0.193
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.507(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         19545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0697
_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^)+(0.0233P)^2^+80.5529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1333
_reflns_number_gt                14420
_reflns_number_total             19545
_reflns_threshold_expression     >2sigma(I)
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_cod_data_source_block           freds
_cod_database_code               4109848