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_7052317
_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            'C81 H81 Cl4 N9 O4 U2'
_chemical_formula_weight         1862.41
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.604(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.2822(9)
_cell_length_b                   12.0928(3)
_cell_length_c                   21.8206(12)
_cell_measurement_reflns_used    115077
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.11
_cell_volume                     3767.2(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 four \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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            115077
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.11
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.491
_exptl_absorpt_correction_T_max  0.698
_exptl_absorpt_correction_T_min  0.420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light orange'
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1828
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.374
_refine_diff_density_min         -1.561
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         7153
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0470P)^2^+25.7376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1160
_reflns_number_gt                5783
_reflns_number_total             7153
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b606035h.txt
_cod_data_source_block           2.3py
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7052317