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_4109847
_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            'C54 H88 Cl10 N20 U2 Zn'
_chemical_formula_weight         1913.37
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.156(2)
_cell_angle_beta                 76.694(2)
_cell_angle_gamma                73.785(2)
_cell_formula_units_Z            1
_cell_length_a                   11.4596(14)
_cell_length_b                   12.2197(15)
_cell_length_c                   14.9748(18)
_cell_measurement_reflns_used    2100
_cell_measurement_temperature    165(2)
_cell_measurement_theta_max      20.55
_cell_measurement_theta_min      2.18
_cell_volume                     1892.6(4)
_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      165(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0768
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12016
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    4.983
_exptl_absorpt_correction_T_max  0.7542
_exptl_absorpt_correction_T_min  0.4069
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            plate
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_meas      0
_exptl_crystal_description       green
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.362
_refine_diff_density_min         -1.072
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         7272
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0374P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0941
_reflns_number_gt                5991
_reflns_number_total             7272
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0725044si20070410_071945.cif
_cod_data_source_block           sak30a
_cod_database_code               4109847