Synthesis, structure and magnetic behaviour of dinuclear uranium(<small>IV</small>) complexes with a ‘calixsalophen’ type macrocycle
Lionel Salmon; Pierre Thuéry; Eric Rivière; Shinpei Miyamoto; Takehiko Yamato; Michel Ephritikhine; New Journal of Chemistry 30 (2006) 1220–; doi:10.1039/b606035h

data_7052319
_publ_section_title
;
 Synthesis, structure and magnetic behaviour of dinuclear
 uranium(<small>IV</small>) complexes with a
 &#x2018;calixsalophen&#x2019; type macrocycle
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1220
_journal_paper_doi               10.1039/b606035h
_journal_volume                  30
_journal_year                    2006
_chemical_formula_sum            'C91 H102 N6 O14 U2'
_chemical_formula_weight         1979.85
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.591(2)
_cell_angle_beta                 81.494(3)
_cell_angle_gamma                68.004(2)
_cell_formula_units_Z            2
_cell_length_a                   15.5199(4)
_cell_length_b                   16.7753(6)
_cell_length_c                   18.1932(8)
_cell_measurement_reflns_used    158460
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.98
_cell_volume                     4277.3(3)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'two \f and seven \w scans with 2\% steps'
_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  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            158460
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.98
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.847
_exptl_absorpt_correction_T_max  0.707
_exptl_absorpt_correction_T_min  0.421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light orange'
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1972
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.899
_refine_diff_density_min         -1.861
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1040
_refine_ls_number_reflns         16208
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0405P)^2^+2.2489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0739
_reflns_number_gt                13016
_reflns_number_total             16208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b606035h.txt
_cod_data_source_block           4.2py
_cod_database_code               7052319