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_1564583
_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         'C52 H94 Co2 La N5 O15, C4 H8 O'
_chemical_formula_sum            'C56 H102 Co2 La N5 O16'
_chemical_formula_weight         1358.19
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.2082(7)
_cell_length_b                   18.6630(8)
_cell_length_c                   18.4793(11)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.13
_cell_measurement_theta_min      2.20
_cell_volume                     6969.4(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28119
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.415
_diffrn_reflns_theta_min         1.485
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.133
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6338
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       plate
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         7136
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+7.3326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5497
_reflns_number_total             7136
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-508-119643.cif
_cod_data_source_block           pe707
_cod_database_code               1564583
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.742
_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. Restrained distances
 C4S-C3S = C4S-C5S = O1S-C5S = C2S-O1S = C2S-C3S
 1.45 with sigma of 0.002
 C4S-O1S
 2.35 with sigma of 0.004
 C4S-C2S
 2.35 with sigma of 0.004
 C5S-C3S
 2.35 with sigma of 0.004
 C5S-C2S
 2.35 with sigma of 0.004
 O1S-C3S
 2.35 with sigma of 0.004
3. Others
 Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C20A)=Sof(H20D)=Sof(H20E)=
 Sof(H20F)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1)
 Fixed Sof: O1S(0.5) C2S(0.5) H2SA(0.5) H2SB(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5)
 C4S(0.5) H4SA(0.5) H4SB(0.5) C5S(0.5) H5SA(0.5) H5SB(0.5)
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)
4.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C),
 C19A(H19D,H19E,H19F), C20A(H20D,H20E,H20F), C21A(H21D,H21E,H21F)
;
_shelx_res_checksum              99182
_shelx_hkl_checksum              90198