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_7063495
_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         'C66 H75 Cl Fe2 N3 P3, C4 H8 O'
_chemical_formula_sum            'C70 H83 Cl Fe2 N3 O P3'
_chemical_formula_weight         1222.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                94.167(2)
_cell_angle_beta                 97.369(2)
_cell_angle_gamma                92.465(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3337(4)
_cell_length_b                   12.3700(6)
_cell_length_c                   24.6238(12)
_cell_measurement_reflns_used    9690
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      2.89
_cell_volume                     3109.0(2)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2016)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT v8.38A (Bruker, 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 0.995
_diffrn_measured_fraction_theta_max 0.972
_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  0.0905
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            117552
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.629
_diffrn_reflns_theta_min         2.895
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4937
_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    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.866
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         14060
_refine_ls_number_restraints     500
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1207
_refine_ls_R_factor_gt           0.0766
_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^)+(0.0352P)^2^+12.1167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1753
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9656
_reflns_number_total             14060
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj03582h2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7063493--7063496.cif.'
_cod_database_code               7063495
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.911
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O1-C70 = O1-C67
 1.43 with sigma of 0.01
 C68-C67 = C69-C68 = C70-C69
 1.54 with sigma of 0.01
 C70-C68 = C67-C69
 2.515 with sigma of 0.02
 O1-C68 = O1-C69
 2.426 with sigma of 0.02
 C67-C70
 2.336 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
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
C67 \\sim C68 \\sim C69 \\sim C70 \\sim O1 \\sim C67A \\sim C68A \\sim C69A
\\sim C70A \\sim O1A: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
4. 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}
{C67A, C68A, C69A, C70A, O1A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C67, C68, C69, C70, O1}
5. Others
 Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=
 Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C9A)=Sof(H9A)=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(H5A)=Sof(H5B)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=
 Sof(H8B)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10A)=Sof(H10B)=FVAR(1)
 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(O1A)=1-FVAR(2)
 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(O1)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C3(H3), C6(H6), C9(H9), C25(H25), C27(H27), C30(H30), C47(H47), C49(H49),
 C52(H52), C3A(H3A), C6A(H6A), C9A(H9A)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B), 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), C67A(H67C,H67D), C68A(H68C,H68D),
 C69A(H69C,H69D), C70A(H70C,H70D), C2A(H2AA,H2AB), C4A(H4AA,H4AB), C5A(H5AA,
 H5AB), C7A(H7AA,H7AB), C8A(H8AA,H8AB), C10A(H10C,H10D)
6.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)
;
_shelx_res_checksum              88747
_olex2_submission_special_instructions 'No special instructions were received'