Ligand redistribution reactions for the synthesis of heterobimetallic rare-earth metal complexes of Co(ii) and Fe(ii)
Du, Jun; Shi, Zhi-Qiang; Wang, Cong; Cui, Peng; New Journal of Chemistry 48 (2024) 18695–18699; doi:10.1039/D4NJ03582H

data_7063494
_publ_section_title
;
 Ligand redistribution reactions for the synthesis of heterobimetallic
 rare-earth metal complexes of Co(ii) and Fe(ii)
;
_journal_issue                   44
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18695
_journal_page_last               18699
_journal_paper_doi               10.1039/D4NJ03582H
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         '2(C52 H66 Cl3 Co N2 O2 P2 Y), C4 H8 O'
_chemical_formula_sum            'C108 H140 Cl6 Co2 N4 O5 P4 Y2'
_chemical_formula_weight         2206.49
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-09-16
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-10-09 deposited with the CCDC.	2024-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.2208(10)
_cell_length_b                   21.2208(10)
_cell_length_c                   20.8628(12)
_cell_measurement_reflns_used    9313
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.93
_cell_volume                     8136.3(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            476259
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.754
_diffrn_reflns_theta_min         2.929
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    1.619
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3450
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.945
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     848
_refine_ls_number_reflns         12585
_refine_ls_number_restraints     872
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0712P)^2^+9.4859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1610
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9468
_reflns_number_total             12585
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj03582h2.cif
_cod_data_source_block           added_by_encifer
_cod_depositor_comments
'Adding full bibliography for 7063493--7063496.cif.'
_cod_original_cell_volume        8136.3(9)
_cod_database_code               7063494
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.738
_shelx_estimated_absorpt_t_min   0.717
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O3-C53 = O3-C56
 1.43 with sigma of 0.01
 O4-C57 = O4-C60
 1.43 with sigma of 0.01
 C58-C57 = C59-C58 = C60-C59
 1.54 with sigma of 0.01
 C54-C53 = C55-C54 = C56-C55
 1.54 with sigma of 0.01
 C60-C57
 2.336 with sigma of 0.02
 C57-C59 = C60-C58
 2.515 with sigma of 0.02
 O4-C58 = O4-C59
 2.426 with sigma of 0.02
 O3-C54 = O3-C55
 2.426 with sigma of 0.02
 C53-C55 = C56-C54
 2.515 with sigma of 0.02
 C53-C56
 2.336 with sigma of 0.02
3. Restrained planarity
 C22A, C20A, C19A, C17A, C21A, C18A, P1
 with sigma of 0.01
 C21, C19, C18, C22, C20, C17, P1
 with sigma of 0.01
 C20A, C18A, C17A, C21A, C19A, C22A, P1
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
P1 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim
C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim P2 \\sim Y1 \\sim C45 \\sim
C46 \\sim C47 \\sim C48 \\sim O1 \\sim C11A \\sim C12A \\sim C13A \\sim C14A
\\sim C15A \\sim C16A \\sim C17A \\sim C18A \\sim C19A \\sim C20A \\sim C21A
\\sim C22A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C57 \\sim C58 \\sim C59 \\sim C60 \\sim O4: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
O2 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim C49A \\sim C50A \\sim C51A
\\sim C52A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Y1 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim O1 \\sim C45A \\sim C46A \\sim
C47A \\sim C48A \\sim O1A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C53 \\sim C54 \\sim C55 \\sim C56 \\sim O3: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Uanis(O4) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C58)
\\sim Ueq, Uanis(C59) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C54) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(C55) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
5. Same fragment restrains
{O2, C49A, C50A, C51A, C52A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{O2, C49, C50, C51, C52}
{P1, C11A, C12A, C13A, C14A, C15A, C16A, C17A, C18A, C19A, C20A, C21A, C22A}
sigma for 1-2: 0.01, 1-3: 0.02
as in
{P1, C11, C12, C13, C14, C15, C16, C17, C18, C19, C20, C21, C22}
{Y1, C45A, C46A, C47A, C48A, O1A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{Y1, C45, C46, C47, C48, O1}
6. Others
 Sof(C45A)=Sof(H45C)=Sof(H45D)=Sof(C46A)=Sof(H46C)=Sof(H46D)=Sof(C47A)=
 Sof(H47C)=Sof(H47D)=Sof(C48A)=Sof(H48C)=Sof(H48D)=Sof(O1A)=1-FVAR(1)
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C47)=Sof(H47A)=
 Sof(H47B)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(O1)=FVAR(1)
 Sof(C49A)=Sof(H49C)=Sof(H49D)=Sof(C50A)=Sof(H50C)=Sof(H50D)=Sof(C51A)=
 Sof(H51C)=Sof(H51D)=Sof(C52A)=Sof(H52C)=Sof(H52D)=1-FVAR(2)
 Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(C51)=Sof(H51A)=
 Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=FVAR(2)
 Sof(C11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14A)=
 Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(C18A)=Sof(H18A)=
 Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=
 Sof(H22A)=1-FVAR(3)
 Sof(C11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(C15)=
 Sof(H15)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=
 Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=FVAR(3)
 Fixed Sof: C53(0.33333) H53A(0.33333) H53B(0.33333) C54(0.33333)
 H54A(0.33333) H54B(0.33333) C55(0.33333) H55A(0.33333) H55B(0.33333)
 C56(0.33333) H56A(0.33333) H56B(0.33333) O3(0.33333) C57(0.16667)
 H57A(0.16667) H57B(0.16667) C58(0.16667) H58A(0.16667) H58B(0.16667)
 C59(0.16667) H59A(0.16667) H59B(0.16667) C60(0.16667) H60A(0.16667)
 H60B(0.16667) O4(0.16667)
 Fixed X: C59(-0.07199) C60(-0.03142)
7.a Ternary CH refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C25(H25), C27(H27), C30(H30)
7.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,
 H10B), C24(H24A,H24B), C26(H26A,H26B), C28(H28A,H28B), C29(H29A,H29B),
 C31(H31A,H31B), C32(H32A,H32B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B),
  C52(H52A,H52B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,
 H48B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B),
 C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C45A(H45C,
 H45D), C46A(H46C,H46D), C47A(H47C,H47D), C48A(H48C,H48D), C49A(H49C,H49D),
 C50A(H50C,H50D), C51A(H51C,H51D), C52A(H52C,H52D)
7.c Aromatic/amide H refined with riding coordinates:
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41),
 C42(H42), C43(H43), C44(H44), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16),
  C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C12A(H12A), C13A(H13A),
 C14A(H14A), C15A(H15A), C16A(H16A), C18A(H18A), C19A(H19A), C20A(H20A),
 C21A(H21A), C22A(H22A)
;
_shelx_res_checksum              12546