A versatile route to homo- and hetero-bimetallic 5f‒5f and 3d‒5f complexes supported by a redox active ligand framework
Camp, Clément; Toniolo, Davide; Andrez, Julie; Pécaut, Jacques; Mazzanti, Marinella; Dalton Trans.  (2017) –; doi:10.1039/C7DT01993A

data_7043434
_publ_section_title
;
 A versatile route to homo- and hetero-bimetallic 5f--5f and 3d--5f
 complexes supported by a redox active ligand framework
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01993A
_journal_year                    2017
_chemical_formula_moiety         'C48 H44 Cl2 N4 O6 U2, C4 H8 O'
_chemical_formula_sum            'C52 H52 Cl2 N4 O7 U2'
_chemical_formula_weight         1391.93
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2016/6
_audit_update_record
;
2017-03-20 deposited with the CCDC.
2017-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                76.376(3)
_cell_angle_beta                 77.185(3)
_cell_angle_gamma                78.707(3)
_cell_formula_units_Z            4
_cell_length_a                   11.7350(5)
_cell_length_b                   19.9970(7)
_cell_length_c                   22.9587(9)
_cell_measurement_reflns_used    17291
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.0370
_cell_measurement_theta_min      4.0190
_cell_volume                     5046.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1333
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -66.00  29.00   1.00    4.00    --  -42.20  37.00 -90.00   95
  2  \w   -113.00 -17.00   1.00    4.00    --  -42.20 -57.00 -30.00   96
  3  \w    -67.00  28.00   1.00    4.00    --  -42.20  57.00 120.00   95
  4  \w     35.00  63.00   1.00    4.00    --   42.20-125.00-180.00   28
  5  \w     47.00  83.00   1.00    4.00    --   42.20 -99.00-120.00   36
  6  \w     37.00 115.00   1.00   16.00    --  109.26 -61.00  90.00   78
  7  \w     76.00 111.00   1.00   16.00    --  109.26-111.00-150.00   35
  8  \w    113.00 178.00   1.00   16.00    --  109.26  49.00 -61.00   65
  9  \w     76.00 102.00   1.00   16.00    --  109.26 178.00 150.00   26
 10  \w     33.00 125.00   1.00   16.00    --  109.26 -30.00-150.00   92
 11  \w     50.00 134.00   1.00   16.00    --  109.26 -45.00 -30.00   84
 12  \w     58.00  86.00   1.00   16.00    --  109.26 178.00-180.00   28
 13  \w    112.00 139.00   1.00   16.00    --  109.26 178.00-180.00   27
 14  \w     33.00  66.00   1.00   16.00    --  109.26 -30.00  60.00   33
 15  \w     71.00 115.00   1.00   16.00    --  109.26-111.00  30.00   44
 16  \w     98.00 138.00   1.00   16.00    --  109.26 -30.00  60.00   40
 17  \w     27.00  74.00   1.00   16.00    --  109.26 -94.00-120.00   47
 18  \w     84.00 109.00   1.00   16.00    --  109.26 -94.00-120.00   25
 19  \w     37.00 141.00   1.00   16.00    --  109.26 -77.00-120.00  104
 20  \w     85.00 178.00   1.00   16.00    --  109.26  30.00  30.00   93
 21  \w     61.00 106.00   1.00   16.00    --  109.26-111.00 120.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            38801
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.444
_diffrn_reflns_theta_min         3.908
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.340
_exptl_absorpt_correction_T_max  0.401
_exptl_absorpt_correction_T_min  0.199
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_description       plate
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.079
_refine_diff_density_max         1.543
_refine_diff_density_min         -2.638
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1207
_refine_ls_number_reflns         20295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0466P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0931
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17233
_reflns_number_total             20295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01993a2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        5046.6(3)
_cod_database_code               7043434
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              9455
_shelx_fab_checksum              90468