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_7043435
_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         'C55 H43 Co N7 O4 U, 2(C5 H5 N)'
_chemical_formula_sum            'C65 H53 Co N9 O4 U'
_chemical_formula_weight         1321.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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     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                90
_cell_angle_beta                 104.034(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6829(2)
_cell_length_b                   23.5857(4)
_cell_length_c                   20.1120(4)
_cell_measurement_reflns_used    30933
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.3910
_cell_measurement_theta_min      3.6680
_cell_volume                     5376.44(17)
_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 2014/5 (Sheldrick, 2014)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.913
_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    -10.00  16.00   1.00   27.00    --   10.47  77.00 -90.00   26
  2  \w     62.00  87.00   1.00   27.00    --   10.47  77.00 -90.00   25
  3  \w     51.00  81.00   1.00   27.00    --   10.47 178.00  30.00   30
  4  \w    -64.00  39.00   1.00   27.00    --   10.47 -77.00-150.00  103
  5  \w    -46.00 -17.00   1.00   27.00    --   10.47 -77.00 -90.00   29
  6  \w     52.00  78.00   1.00   27.00    --   10.47 178.00-180.00   26
  7  \w    -12.00  83.00   1.00   27.00    --   10.47  37.00   0.00   95
  8  \w     10.00  35.00   1.00   27.00    --   10.47 -37.00 -90.00   25
  9  \w    -21.00  84.00   1.00   27.00    --   10.47  77.00  90.00  105
;
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            70018
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.509
_diffrn_reflns_theta_min         3.325
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.377
_exptl_absorpt_correction_T_max  0.776
_exptl_absorpt_correction_T_min  0.724
_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            red
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       prism
_exptl_crystal_F_000             2628
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         13687
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0176P)^2^+8.9402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0543
_refine_ls_wR_factor_ref         0.0572
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11871
_reflns_number_total             13687
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01993a2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        5376.44(18)
_cod_database_code               7043435
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              60141