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_7043438
_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         'C70 H58 N10 O4 U2, 2(I), 3(C5 H5 N)'
_chemical_formula_sum            'C85 H73 I2 N13 O4 U2'
_chemical_formula_weight         2070.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-06-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-06-06 deposited with the CCDC.
2017-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.910(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3578(11)
_cell_length_b                   15.3976(7)
_cell_length_c                   38.2404(17)
_cell_measurement_reflns_used    5366
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      32.3929
_cell_measurement_theta_min      3.3532
_cell_volume                     7864.2(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   73.00  100.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051  179.0000 -180.0000 27

  2 omega   42.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051  179.0000  -90.0000 48

  3 omega  -96.00   -7.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -57.0000  -30.0000 89

  4 omega  -58.00    6.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -19.0000   30.0000 64
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0053506000
_diffrn_orient_matrix_UB_12      -0.0421397000
_diffrn_orient_matrix_UB_13      -0.0072598000
_diffrn_orient_matrix_UB_21      -0.0527766000
_diffrn_orient_matrix_UB_22      -0.0048918000
_diffrn_orient_matrix_UB_23      -0.0004064000
_diffrn_orient_matrix_UB_31      -0.0018420000
_diffrn_orient_matrix_UB_32      0.0180043000
_diffrn_orient_matrix_UB_33      -0.0170679000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_unetI/netI     0.1169
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            31445
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.360
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.958
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3984
_exptl_crystal_size_max          0.433
_exptl_crystal_size_mid          0.338
_exptl_crystal_size_min          0.056
_refine_diff_density_max         2.350
_refine_diff_density_min         -2.296
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     955
_refine_ls_number_reflns         16050
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.1183
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+47.1959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1494
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11157
_reflns_number_total             16050
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01993a2.cif
_cod_data_source_block           cc335
_cod_database_code               7043438
_chemical_oxdiff_formula         'U2 N4 O4 C100 H100 I2'
_shelx_estimated_absorpt_t_max   0.769
_shelx_estimated_absorpt_t_min   0.223
_reflns_odcompleteness_completeness 98.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
N47 \\sim C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C14(H14), C27(H27)
3.b Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), 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), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34),
 C36(H36), C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C43(H43), C44(H44),
  C45(H45), C46(H46), C47(H47), C49(H49), C50(H50), C51(H51), C52(H52),
 C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60),
  C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67),
 C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75),
  C76(H76), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81), C82(H82),
 C83(H83), C84(H84), C85(H85)
;
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'