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_7043437
_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 Co N4 O6 U, 1.5(C4 H8 O)'
_chemical_formula_sum            'C54 H56 Co N4 O7.5 U'
_chemical_formula_weight         1177.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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_date             2017-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_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                 96.065(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.2903(17)
_cell_length_b                   12.927(7)
_cell_length_c                   27.0396(12)
_cell_measurement_reflns_used    1794
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      32.4411
_cell_measurement_theta_min      3.4266
_cell_volume                     9138(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   39.00   81.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  179.0000 -120.0000 42

  2 omega  -69.00  -33.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  179.0000  120.0000 36

  3 omega  -93.00   -6.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -37.0000  -30.0000 87

  4 omega  -89.00  -10.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -57.0000  -90.0000 79
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0069756000
_diffrn_orient_matrix_UB_12      -0.0282330000
_diffrn_orient_matrix_UB_13      -0.0221722000
_diffrn_orient_matrix_UB_21      0.0261610000
_diffrn_orient_matrix_UB_22      -0.0104177000
_diffrn_orient_matrix_UB_23      -0.0021740000
_diffrn_orient_matrix_UB_31      -0.0016096000
_diffrn_orient_matrix_UB_32      -0.0458977000
_diffrn_orient_matrix_UB_33      0.0141484000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0839
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            26327
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.43
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.965
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73373
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4696
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.272
_refine_diff_density_max         2.382
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         13941
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+14.5136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1203
_reflns_number_gt                9624
_reflns_number_total             13941
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt01993a2.cif
_cod_data_source_block           cc398_2
_cod_original_formula_sum        'C54 H56 Co N4 O7.50 U'
_cod_database_code               7043437
_chemical_oxdiff_formula         'U Co N4 O6 C50 H50'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 O61-C61 = O61-C64
 1.45 with sigma of 0.02
 C61-C62 = C62-C63 = C63-C64
 1.52 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C42B) \\sim Ueq, Uanis(C44B) \\sim Ueq, Uanis(C62) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
4. Others
 Sof(H43C)=Sof(H43D)=Sof(C41B)=Sof(H41C)=Sof(H41D)=Sof(C42B)=Sof(H42C)=
 Sof(H42D)=Sof(C44B)=Sof(H44C)=Sof(H44D)=1-FVAR(1)
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H43A)=Sof(H43B)=
 Sof(C44)=Sof(H44A)=Sof(H44B)=FVAR(1)
 Fixed Sof: O61(0.5) C61(0.5) H61A(0.5) H61B(0.5) C62(0.5) H62A(0.5) H62B(0.5)
 C63(0.5) H63A(0.5) H63B(0.5) C64(0.5) H64A(0.5) H64B(0.5)
5.a Ternary CH refined with riding coordinates:
 C14(H14), C34(H34)
5.b Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C41B(H41C,
 H41D), C42B(H42C,H42D), C44B(H44C,H44D), C45(H45A,H45B), C46(H46A,H46B),
 C47(H47A,H47B), C48(H48A,H48B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B),
  C54(H54A,H54B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25),
  C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C36(H36), C37(H37),
 C38(H38), C39(H39)
;
_olex2_submission_special_instructions 'No special instructions were received'