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_7043436
_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_sum            'C54 H56 N4 Ni O7.5 U'
_chemical_formula_weight         1177.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-03-20 deposited with the CCDC.
2017-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.858(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.2314(8)
_cell_length_b                   12.9229(3)
_cell_length_c                   27.1920(7)
_cell_measurement_reflns_used    5233
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.4928
_cell_measurement_theta_min      3.3009
_cell_volume                     9151.7(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega   76.00  102.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051  179.0000 -150.0000 26

  2 omega -103.00  -34.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239 -179.0000  150.0000 69

  3 omega  -97.00   14.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -19.0000   30.0000 111

  4 omega  -97.00  -43.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000  -60.0000 54

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w 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  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0835
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            28607
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    4.008
_exptl_absorpt_correction_T_max  0.7478
_exptl_absorpt_correction_T_min  0.5439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'long block'
_exptl_crystal_F_000             4704
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.114
_refine_diff_density_min         -1.166
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         13862
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0846
_reflns_number_gt                9591
_reflns_number_total             13862
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt01993a2.cif
_cod_data_source_block           ja065
_cod_original_cell_volume        9151.8(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C54 H56 N4 Ni O7.50 U'
_cod_database_code               7043436