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_7063496
_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         'C64 H58 Cl Fe2 N4 P3, 3(C4 H8 O)'
_chemical_formula_sum            'C76 H82 Cl Fe2 N4 O3 P3'
_chemical_formula_weight         1339.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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
;
2024-10-06 deposited with the CCDC.	2024-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.105(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.770(2)
_cell_length_b                   12.4984(12)
_cell_length_c                   33.750(4)
_cell_measurement_reflns_used    9533
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      2.94
_cell_volume                     7453.2(14)
_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 0.956
_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  0.0829
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            297703
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.516
_diffrn_reflns_theta_min         2.783
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4945
_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    1.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1186
_refine_ls_number_reflns         18089
_refine_ls_number_restraints     1439
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1280
_refine_ls_R_factor_gt           0.0737
_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^)+(0.1053P)^2^+9.1673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1966
_refine_ls_wR_factor_ref         0.2369
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11060
_reflns_number_total             18089
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj03582h2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7063493--7063496.cif.'
_cod_original_cell_volume        7453.1(14)
_cod_database_code               7063496
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.896
_shelx_estimated_absorpt_t_min   0.891
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O1-C68 = O1-C65 = O2-C72 = O2-C69 = O3-C73 = O3-C76 = O4-C77 = O4-C80
 1.43 with sigma of 0.01
 C72-C71 = C70-C69 = C71-C70 = C68-C67 = C67-C66 = C66-C65 = C74-C73 = C75-C74
 = C76-C75 = C78-C77 = C79-C78 = C80-C79
 1.54 with sigma of 0.01
 O1-C66 = O1-C67 = O2-C70 = O2-C71 = O3-C74 = O3-C75 = O4-C78 = O4-C79
 2.426 with sigma of 0.02
 C68-C66 = C67-C65 = C72-C70 = C71-C69 = C73-C75 = C76-C74 = C77-C79 = C80-C78
 2.515 with sigma of 0.02
 C68-C65 = C72-C69 = C73-C76 = C77-C80
 2.336 with sigma of 0.02
3. Restrained planarity
 C42A, C40A, C39, C43A, C41A, C44A, N4
 with sigma of 0.01
 C64A, C62A, C61A, C59A, C63A, C60A, P3
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C73 \\sim C74 \\sim C75 \\sim C76 \\sim O3 \\sim C73A \\sim C74A \\sim C75A
\\sim C76A \\sim O3A: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
C65 \\sim C66 \\sim C67 \\sim C68 \\sim O1 \\sim C65A \\sim C66A \\sim C67A
\\sim C68A \\sim O1A: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
C77 \\sim C78 \\sim C79 \\sim C80 \\sim O4 \\sim C77A \\sim C78A \\sim C79A
\\sim C80A \\sim O4A: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
C69 \\sim C70 \\sim C71 \\sim C72 \\sim O2 \\sim C69A \\sim C70A \\sim C71A
\\sim C72A \\sim O2A: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C40A \\sim C41A
\\sim C42A \\sim C43A \\sim C44A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
P3 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim
C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C53A \\sim C54A \\sim C55A
\\sim C56A \\sim C57A \\sim C58A \\sim C59A \\sim C60A \\sim C61A \\sim C62A
\\sim C63A \\sim C64A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C76)
\\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C73A) \\sim Ueq, Uanis(C74A) \\sim Ueq,
Uanis(C75A) \\sim Ueq, Uanis(C76A) \\sim Ueq, Uanis(O3A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C77) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C80)
\\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C77A) \\sim Ueq, Uanis(C78A) \\sim Ueq,
Uanis(C79A) \\sim Ueq, Uanis(C80A) \\sim Ueq, Uanis(O4A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
5. Same fragment restrains
{C39, C40A, C41A, C42A, C43A, C44A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C39, C40, C41, C42, C43, C44}
{P3, C53A, C54A, C55A, C56A, C57A, C58A, C59A, C60A, C61A, C62A, C63A, C64A}
sigma for 1-2: 0.01, 1-3: 0.02
as in
{P3, C53, C54, C55, C56, C57, C58, C59, C60, C61, C62, C63, C64}
{C65A, C66A, C67A, C68A, O1A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C65, C66, C67, C68, O1}
{C69A, C70A, C71A, C72A, O2A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C69, C70, C71, C72, O2}
{C73A, C74A, C75A, C76A, O3A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C73, C74, C75, C76, O3}
{C77A, C78A, C79A, C80A, O4A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C77, C78, C79, C80, O4}
6. Others
 Sof(C65A)=Sof(H65C)=Sof(H65D)=Sof(C66A)=Sof(H66C)=Sof(H66D)=Sof(C67A)=
 Sof(H67C)=Sof(H67D)=Sof(C68A)=Sof(H68C)=Sof(H68D)=Sof(O1A)=1-FVAR(1)
 Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(C67)=Sof(H67A)=
 Sof(H67B)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(O1)=FVAR(1)
 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(O2A)=1-FVAR(2)
 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(O2)=FVAR(2)
 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(O3A)=0.5*(1-FVAR(4))
 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(O3)=0.5*FVAR(4)
 Sof(C77A)=Sof(H77C)=Sof(H77D)=Sof(C78A)=Sof(H78C)=Sof(H78D)=Sof(C79A)=
 Sof(H79C)=Sof(H79D)=Sof(C80A)=Sof(H80C)=Sof(H80D)=Sof(O4A)=0.5*(1-FVAR(5))
 Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(C79)=Sof(H79A)=
 Sof(H79B)=Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(O4)=0.5*FVAR(5)
 Sof(C53A)=Sof(C54A)=Sof(H54A)=Sof(C55A)=Sof(H55A)=Sof(C56A)=Sof(H56A)=
 Sof(C57A)=Sof(H57A)=Sof(C58A)=Sof(H58A)=Sof(C59A)=Sof(C60A)=Sof(H60A)=
 Sof(C61A)=Sof(H61A)=Sof(C62A)=Sof(H62A)=Sof(C63A)=Sof(H63A)=Sof(C64A)=
 Sof(H64A)=1-FVAR(5)
 Sof(C53)=Sof(C54)=Sof(H54)=Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56)=Sof(C57)=
 Sof(H57)=Sof(C58)=Sof(H58)=Sof(C59)=Sof(C60)=Sof(H60)=Sof(C61)=Sof(H61)=
 Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63)=Sof(C64)=Sof(H64)=FVAR(5)
 Sof(C40A)=Sof(H40A)=Sof(C41A)=Sof(H41A)=Sof(C42A)=Sof(H42A)=Sof(C43A)=
 Sof(H43A)=Sof(C44A)=Sof(H44A)=1-FVAR(6)
 Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42)=Sof(C43)=Sof(H43)=
 Sof(C44)=Sof(H44)=FVAR(6)
7.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C26(H26A,H26B), C45(H45A,H45B), C52(H52A,H52B), C65(H65A,H65B),
 C66(H66A,H66B), 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), C65A(H65C,H65D), C66A(H66C,H66D), 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), C79A(H79C,H79D), C80A(H80C,H80D)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41),
  C42(H42), C43(H43), C44(H44), C47(H47), C48(H48), C49(H49), C50(H50),
 C51(H51), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61),
  C62(H62), C63(H63), C64(H64), C54A(H54A), C55A(H55A), C56A(H56A), C57A(H57A),
 C58A(H58A), C60A(H60A), C61A(H61A), C62A(H62A), C63A(H63A), C64A(H64A),
 C40A(H40A), C41A(H41A), C42A(H42A), C43A(H43A), C44A(H44A)
;
_shelx_res_checksum              3198
_olex2_submission_special_instructions 'No special instructions were received'