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_7063493
_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         'C78 H99 Cl Co2 K N3 O6 P3, 2(C4 H8 O)'
_chemical_formula_sum            'C86 H115 Cl Co2 K N3 O8 P3'
_chemical_formula_weight         1604.12
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-10-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-10-12 deposited with the CCDC.	2024-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.91(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.202(3)
_cell_length_b                   22.359(4)
_cell_length_c                   27.450(5)
_cell_measurement_reflns_used    9339
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.38
_cell_measurement_theta_min      2.91
_cell_volume                     9191(3)
_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)'
_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 0.991
_diffrn_measured_fraction_theta_max 0.998
_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_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            16144
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.058
_diffrn_reflns_theta_max         25.058
_diffrn_reflns_theta_min         2.835
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5375
_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    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3404
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.319
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1558
_refine_ls_number_reflns         16144
_refine_ls_number_restraints     2456
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0738
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1279P)^2^+16.0044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2248
_refine_ls_wR_factor_ref         0.2483
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12743
_reflns_number_total             16144
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj03582h2.cif
_cod_data_source_block           3_tw
_cod_depositor_comments
'Adding full bibliography for 7063493--7063496.cif.'
_cod_database_code               7063493
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.895
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.64(4)
 0.157(8) 0.20(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 O9-C90 = O9-C87 = O8-C83 = O8-C86 = O7-C79 = O7-C82
 1.43 with sigma of 0.01
 C82-C81 = C81-C80 = C80-C79 = C84-C83 = C85-C84 = C86-C85 = C88-C87 = C89-C88
 = C90-C89
 1.54 with sigma of 0.01
 C87-C90 = C83-C86 = C82-C79
 2.336 with sigma of 0.02
 C82-C80 = C79-C81 = C86-C84 = C83-C85 = C87-C89 = C90-C88
 2.515 with sigma of 0.02
 O7-C80 = O7-C81 = O8-C84 = O8-C85 = O9-C88 = O9-C89
 2.426 with sigma of 0.02
4. Restrained planarity
 C64A, C62A, C61A, C65A, C63A, C66A, P3
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
K1 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim
C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim O1 \\sim O2 \\sim O3 \\sim O4
\\sim O5 \\sim O6 \\sim C67A \\sim C68A \\sim C69A \\sim C70A \\sim C71A \\sim
C72A \\sim C73A \\sim C74A \\sim C75A \\sim C76A \\sim C77A \\sim C78A \\sim
O1A \\sim O2A \\sim O3A \\sim O4A \\sim O5A \\sim O6A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim
C53 \\sim C54 \\sim C46A \\sim C47A \\sim C48A \\sim C49A \\sim C50A \\sim C51A
\\sim C52A \\sim C53A \\sim C54A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A
\\sim C9A \\sim C10A: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
P3 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim
C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C55A \\sim C56A \\sim C57A
\\sim C58A \\sim C59A \\sim C60A \\sim C61A \\sim C62A \\sim C63A \\sim C64A
\\sim C65A \\sim C66A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C83 \\sim C84 \\sim C85 \\sim C86 \\sim O8 \\sim C83A \\sim C84A \\sim C85A
\\sim C86A \\sim O8A: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
C79 \\sim C80 \\sim C81 \\sim C82 \\sim O7 \\sim C79A \\sim C80A \\sim C81A
\\sim C82A \\sim O7A: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
C87 \\sim C88 \\sim C89 \\sim C90 \\sim O9 \\sim C87A \\sim C88A \\sim C89A
\\sim C90A \\sim O9A: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
Uanis(C83) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C86)
\\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(C83A) \\sim Ueq, Uanis(C84A) \\sim Ueq,
Uanis(C85A) \\sim Ueq, Uanis(C86A) \\sim Ueq, Uanis(O8A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7) \\sim Ueq, Uanis(O7A) \\sim Ueq, Uanis(C79A) \\sim Ueq, Uanis(C82)
\\sim Ueq, Uanis(C82A) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C80) \\sim Ueq,
Uanis(C80A) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C81A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C90A) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O9A)
\\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C87A) \\sim Ueq, Uanis(C87) \\sim Ueq,
Uanis(C89A) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C88A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
6. Same fragment restrains
{C1, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A} sigma for 1-2: 0.01, 1-3:
0.02
as in
{C1, C2, C3, C4, C5, C6, C7, C8, C9, C10}
{C45, C46A, C47A, C48A, C49A, C50A, C51A, C52A, C53A, C54A} sigma for 1-2:
0.01, 1-3: 0.02
as in
{C45, C46, C47, C48, C49, C50, C51, C52, C53, C54}
{K1, C67A, C68A, C69A, C70A, C71A, C72A, C73A, C74A, C75A, C76A, C77A, C78A,
O1A, O2A, O3A, O4A, O5A, O6A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{K1, C67, C68, C69, C70, C71, C72, C73, C74, C75, C76, C77, C78, O1, O2, O3,
O4, O5, O6}
{P3, C55A, C56A, C57A, C58A, C59A, C60A, C61A, C62A, C63A, C64A, C65A, C66A}
sigma for 1-2: 0.01, 1-3: 0.02
as in
{P3, C55, C56, C57, C58, C59, C60, C61, C62, C63, C64, C65, C66}
{C79A, C80A, C81A, C82A, O7A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C79, C80, C81, C82, O7}
{C83A, C84A, C85A, C86A, O8A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C83, C84, C85, C86, O8}
{C87A, C88A, C89A, C90A, O9A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C87, C88, C89, C90, O9}
7. Others
 Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=
 Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=
 Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10C)=Sof(H10D)=1-
 FVAR(1)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=
 Sof(H5)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8)=
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=Sof(H10B)=FVAR(1)
 Sof(C46A)=Sof(H46C)=Sof(H46D)=Sof(C47A)=Sof(H47A)=Sof(C48A)=Sof(H48C)=
 Sof(H48D)=Sof(C49A)=Sof(H49A)=Sof(C50A)=Sof(H50C)=Sof(H50D)=Sof(C51A)=
 Sof(H51C)=Sof(H51D)=Sof(C52A)=Sof(H52A)=Sof(C53A)=Sof(H53C)=Sof(H53D)=
 Sof(C54A)=Sof(H54C)=Sof(H54D)=1-FVAR(2)
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C47)=Sof(H47)=Sof(C48)=Sof(H48A)=Sof(H48B)=
 Sof(C49)=Sof(H49)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(C51)=Sof(H51A)=Sof(H51B)=
 Sof(C52)=Sof(H52)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C54)=Sof(H54A)=Sof(H54B)=
 FVAR(2)
 Sof(C55A)=Sof(C56A)=Sof(H56A)=Sof(C57A)=Sof(H57A)=Sof(C58A)=Sof(H58A)=
 Sof(C59A)=Sof(H59A)=Sof(C60A)=Sof(H60A)=Sof(C61A)=Sof(C62A)=Sof(H62A)=
 Sof(C63A)=Sof(H63A)=Sof(C64A)=Sof(H64A)=Sof(C65A)=Sof(H65A)=Sof(C66A)=
 Sof(H66A)=1-FVAR(3)
 Sof(C55)=Sof(C56)=Sof(H56)=Sof(C57)=Sof(H57)=Sof(C58)=Sof(H58)=Sof(C59)=
 Sof(H59)=Sof(C60)=Sof(H60)=Sof(C61)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63)=
 Sof(C64)=Sof(H64)=Sof(C65)=Sof(H65)=Sof(C66)=Sof(H66)=FVAR(3)
 Sof(C67A)=Sof(H67C)=Sof(H67D)=Sof(C68A)=Sof(H68C)=Sof(H68D)=Sof(C69A)=
 Sof(H69C)=Sof(H69D)=Sof(C70A)=Sof(H70C)=Sof(H70D)=Sof(C71A)=Sof(H71C)=
 Sof(H71D)=Sof(C72A)=Sof(H72C)=Sof(H72D)=Sof(C73A)=Sof(H73C)=Sof(H73D)=
 Sof(C74A)=Sof(H74C)=Sof(H74D)=Sof(C75A)=Sof(H75C)=Sof(H75D)=Sof(C76A)=
 Sof(H76C)=Sof(H76D)=Sof(C77A)=Sof(H77C)=Sof(H77D)=Sof(C78A)=Sof(H78C)=
 Sof(H78D)=Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=1-FVAR(4)
 Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(C69)=Sof(H69A)=
 Sof(H69B)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(C72)=
 Sof(H72A)=Sof(H72B)=Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(C74)=Sof(H74A)=Sof(H74B)=
 Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(C77)=Sof(H77A)=
 Sof(H77B)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(O5)=
 Sof(O6)=FVAR(4)
 Sof(C79A)=Sof(H79C)=Sof(H79D)=Sof(C80A)=Sof(H80C)=Sof(H80D)=Sof(C81A)=
 Sof(H81C)=Sof(H81D)=Sof(C82A)=Sof(H82C)=Sof(H82D)=Sof(O7A)=1-FVAR(5)
 Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(C81)=Sof(H81A)=
 Sof(H81B)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(O7)=FVAR(5)
 Sof(C83A)=Sof(H83C)=Sof(H83D)=Sof(C84A)=Sof(H84C)=Sof(H84D)=Sof(C85A)=
 Sof(H85C)=Sof(H85D)=Sof(C86A)=Sof(H86C)=Sof(H86D)=Sof(O8A)=0.5*(1-FVAR(7))
 Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(C85)=Sof(H85A)=
 Sof(H85B)=Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(O8)=0.5*FVAR(7)
 Sof(C87A)=Sof(H87C)=Sof(H87D)=Sof(C88A)=Sof(H88C)=Sof(H88D)=Sof(C89A)=
 Sof(H89C)=Sof(H89D)=Sof(C90A)=Sof(H90C)=Sof(H90D)=Sof(O9A)=0.5*(1-FVAR(8))
 Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(C89)=Sof(H89A)=
 Sof(H89B)=Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(O9)=0.5*FVAR(8)
8.a Ternary CH refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C25(H25), C27(H27), C30(H30), C47(H47), C49(H49),
 C52(H52), C3A(H3A), C5A(H5A), C8A(H8A), C47A(H47A), C49A(H49A), C52A(H52A)
8.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), C46(H46A,H46B), C48(H48A,H48B), C50(H50A,H50B),
  C51(H51A,H51B), C53(H53A,H53B), C54(H54A,H54B), C67(H67A,H67B), C68(H68A,
 H68B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B),
 C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B),
  C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,
 H82B), C83(H83A,H83B), C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B),
 C87(H87A,H87B), C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B), C79A(H79C,
 H79D), C80A(H80C,H80D), C81A(H81C,H81D), C82A(H82C,H82D), C83A(H83C,H83D),
 C84A(H84C,H84D), C85A(H85C,H85D), C86A(H86C,H86D), C87A(H87C,H87D), C88A(H88C,
 H88D), C89A(H89C,H89D), C90A(H90C,H90D), C2A(H2AA,H2AB), C4A(H4AA,H4AB),
 C6A(H6AA,H6AB), C7A(H7AA,H7AB), C9A(H9AA,H9AB), C10A(H10C,H10D), C46A(H46C,
 H46D), C48A(H48C,H48D), C50A(H50C,H50D), C51A(H51C,H51D), C53A(H53C,H53D),
 C54A(H54C,H54D), C67A(H67C,H67D), C68A(H68C,H68D), C69A(H69C,H69D), C70A(H70C,
 H70D), C71A(H71C,H71D), C72A(H72C,H72D), C73A(H73C,H73D), C74A(H74C,H74D),
 C75A(H75C,H75D), C76A(H76C,H76D), C77A(H77C,H77D), C78A(H78C,H78D)
8.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
  C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C56(H56), C57(H57),
 C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66),
  C56A(H56A), C57A(H57A), C58A(H58A), C59A(H59A), C60A(H60A), C62A(H62A),
 C63A(H63A), C64A(H64A), C65A(H65A), C66A(H66A)
;
_shelx_res_checksum              97514
_olex2_submission_special_instructions 'No special instructions were received'