Simple synthetic protocol to obtain 3d-4f-heterometallic carboxylate complexes of N-heterocyclic carbenes
Nikolaevskii, Stanislav A.; Petrov, Pavel A.; Sukhikh, Taisiya S.; Yambulatov, Dmitriy S.; Kiskin, Mikhail A.; Sokolov, Maxim N.; Eremenko, Igor L.; Inorganica Chimica Acta 508 (2020) 119643–; doi:10.1016/j.ica.2020.119643

data_1564584
_publ_section_title
;
 Simple synthetic protocol to obtain 3d-4f-heterometallic carboxylate
 complexes of N-heterocyclic carbenes
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119643
_journal_paper_doi               10.1016/j.ica.2020.119643
_journal_volume                  508
_journal_year                    2020
_chemical_formula_moiety         'C72 H102 N5 O15 Tb Zn2, C4 H8 O'
_chemical_formula_sum            'C76 H110 N5 O16 Tb Zn2'
_chemical_formula_weight         1639.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.0878(10)
_cell_length_b                   26.4673(14)
_cell_length_c                   27.3749(14)
_cell_measurement_reflns_used    9361
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.56
_cell_measurement_theta_min      2.32
_cell_volume                     16728.0(14)
_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(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            187737
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.776
_diffrn_reflns_theta_min         1.387
_exptl_absorpt_coefficient_mu    1.467
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5925
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             6832
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.139
_refine_diff_density_min         -1.108
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     968
_refine_ls_number_reflns         15979
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+56.1573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1294
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12050
_reflns_number_total             15979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-508-119643.cif
_cod_data_source_block           pe715
_cod_database_code               1564584
_shelx_estimated_absorpt_t_max   0.789
_shelx_estimated_absorpt_t_min   0.643
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C71) \\sim Ueq, Uanis(C71A) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C55A) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56A) \\sim Ueq, Uanis(C56)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
3. Others
 Sof(C70A)=Sof(H70D)=Sof(H70E)=Sof(H70F)=Sof(C71A)=Sof(H71D)=Sof(H71E)=
 Sof(H71F)=Sof(C72A)=Sof(H72D)=Sof(H72E)=Sof(H72F)=1-FVAR(1)
 Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=
 Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=FVAR(1)
 Sof(C55A)=Sof(H55D)=Sof(H55E)=Sof(H55F)=Sof(C57A)=Sof(H57D)=Sof(H57E)=
 Sof(H57F)=Sof(C56A)=Sof(H56D)=Sof(H56E)=Sof(H56F)=1-FVAR(2)
 Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=
 Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,H5SB)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C8(H8), C15(H15), C17(H17), C23(H23), C24(H24),
 C27(H27), C29(H29), C36(H36), C38(H38)
4.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C55(H55A,
 H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C60(H60A,H60B,H60C),
 C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C65(H65A,H65B,H65C), C66(H66A,H66B,
 H66C), C67(H67A,H67B,H67C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C72(H72A,
 H72B,H72C), C70A(H70D,H70E,H70F), C71A(H71D,H71E,H71F), C72A(H72D,H72E,H72F),
 C55A(H55D,H55E,H55F), C57A(H57D,H57E,H57F), C56A(H56D,H56E,H56F)
;