Accessing bimetallic complexes through a variable bridging ligand strategy.
Liyanage, Hansani T Lekam Wasam; Smith, Mark D.; Wheeler, Kraig A.; Semeniuc, Radu F.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 1063–1078; doi:10.1039/d4dt02903h

data_7717576
_publ_section_title
;
 Accessing bimetallic complexes through a variable bridging ligand
 strategy.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1063
_journal_page_last               1078
_journal_paper_doi               10.1039/d4dt02903h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C27 H24 Cu N10 O3, 0.566(C H2 Cl2)'
_chemical_formula_sum            'C27.56 H25.13 Cl1.13 Cu N10 O3'
_chemical_formula_weight         648.08
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-11-11
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-13 deposited with the CCDC.	2024-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                69.659(4)
_cell_angle_beta                 81.772(4)
_cell_angle_gamma                89.586(4)
_cell_formula_units_Z            2
_cell_length_a                   7.9593(6)
_cell_length_b                   12.0730(9)
_cell_length_c                   15.9301(11)
_cell_measurement_reflns_used    9089
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.083
_cell_measurement_theta_min      2.993
_cell_volume                     1419.04(18)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'SMART (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2002) and XPREP (Bruker, 2001)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30909
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.617
_diffrn_reflns_theta_min         2.992
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.489
_exptl_absorpt_correction_T_max  0.2721
_exptl_absorpt_correction_T_min  0.2046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0716 before and 0.0467 after correction.
The Ratio of minimum to maximum transmission is 0.7519.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       plate
_exptl_crystal_F_000             665
_exptl_crystal_size_max          0.263
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.0008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         5069
_refine_ls_number_restraints     300
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0455P)^2^+1.1128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4408
_reflns_number_total             5069
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02903h2.cif
_cod_data_source_block           17rfs01a_rev
_cod_depositor_comments
'Adding full bibliography for 7717572--7717578.cif.'
_cod_database_code               7717576
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl1A-C28A = Cl2B-C28B = Cl1B-C28B = Cl2A-C28A
 1.75 with sigma of 0.01
 C20A-C19 \\sim C20-C19 \\sim C24A-C19 \\sim C24B-C19
 with sigma of 0.01
 N9B-C24B \\sim N9C-C24C \\sim N9A-C24A \\sim N7-C20 \\sim N7A-C20A
 with sigma of 0.01
 C24B-C19 \\sim C24C-C19 \\sim C24A-C19 \\sim C20-C19 \\sim C20A-C19
 with sigma of 0.01
 C11A-C10 \\sim C11-C10
 with sigma of 0.01
 N3-C11A \\sim N3-C11 \\sim N5A-C11A \\sim N5-C11
 with sigma of 0.01
3. Restrained planarity
 C24C, N9C, C25C, C26C, C27C, N10C
 with sigma of 0.01
4. Rigid bond restraints
 C24B, N9B, N10B, C27B, C26B, C25B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(N7A) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C21A) \\sim Ueq, Uanis(C21)
\\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C22A) \\sim Ueq, Uanis(C23) \\sim Ueq,
Uanis(C23A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N5) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(N5A) \\sim Ueq, Uanis(N6A) \\sim Ueq,
Uanis(C15A) \\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C17A) \\sim Ueq: with sigma
of 0.0075 and sigma for terminal atoms of 0.015
Uanis(C28A) = Uanis(C28B)
Uanis(C24B) = Uanis(C24C) = Uanis(C24A)
Uanis(Cl2B) = Uanis(Cl1A)
Uanis(N6) = Uanis(N6A)
Uanis(N5) = Uanis(N5A)
Uanis(C16) = Uanis(C16A)
Uanis(C15) = Uanis(C15A)
Uanis(C11) = Uanis(C11A)
Uanis(C17) = Uanis(C17A)
Uanis(N10A) = Uanis(N10C)
Uanis(N9C) = Uanis(N9A)
Uanis(C27A) = Uanis(C27C)
Uanis(C20) = Uanis(C20A)
Uanis(N7) = Uanis(N7A)
Uanis(N8) = Uanis(N8A)
Uanis(C21) = Uanis(C21A)
Uanis(C22A) = Uanis(C22)
Uanis(C23A) = Uanis(C23)
6. Rigid body (RIGU) restrains
 N5, N5A, C15, C15A, C16A, C16, C17, C17A, N6, N6A, C11, C11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Same fragment restrains
{N3, N4, C12, C13, C14} sigma for 1-2: 0.015, 1-3: 0.04
as in
{N7, N8, C21, C22, C23}
{C24A, N9A, N10A, C25A, C26A, C27A} sigma for 1-2: 0.01, 1-3: 0.04
as in
{C24B, N9B, N10B, C25B, C26B, C27B}
{C24A, N9A, N10A, C25A, C26A, C27A} sigma for 1-2: 0.01, 1-3: 0.04
as in
{C24C, N9C, N10C, C25C, C26C, C27C}
{N3, N4, C12, C13, C14} sigma for 1-2: 0.015, 1-3: 0.04
as in
{N7A, N8A, C21A, C22A, C23A}
8. Others
 1*[Sof(C24A)+Sof(H24A)+Sof(H24B)+Sof(N9A)+Sof(N10A)+Sof(C25A)+Sof(H25A)+
 Sof(C26A)+Sof(H26A)+Sof(C27A)+Sof(H27A)]+1*[Sof(C24B)+Sof(H24C)+Sof(H24D)+
 Sof(N9B)+Sof(N10B)+Sof(C25B)+Sof(H25B)+Sof(C26B)+Sof(H26B)+Sof(C27B)+
 Sof(H27B)]+1*[Sof(C24C)+Sof(H24E)+Sof(H24F)+Sof(N9C)+Sof(N10C)+Sof(C25C)+
 Sof(H25C)+Sof(C26C)+Sof(H26C)+Sof(C27C)+Sof(H27C)]=1 with esd of 0.00001
 Sof(C11A)=Sof(H11A)=Sof(N5A)=Sof(N6A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=
 Sof(C17A)=Sof(H17A)=1-FVAR(1)
 Sof(C11)=Sof(H11)=Sof(N5)=Sof(N6)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=
 Sof(C17)=Sof(H17)=FVAR(1)
 Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(N9A)=Sof(N10A)=Sof(C25A)=Sof(H25A)=
 Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=FVAR(2)
 Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(N7A)=Sof(N8A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=
 Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(H19A)=1-FVAR(3)
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(N7)=Sof(N8)=Sof(C21)=Sof(H21)=Sof(C22)=
 Sof(H22)=Sof(C23)=Sof(H23)=Sof(H19)=FVAR(3)
 Sof(Cl1A)=Sof(Cl2A)=Sof(C28A)=Sof(H28A)=Sof(H28B)=FVAR(4)
 Sof(Cl1B)=Sof(Cl2B)=Sof(C28B)=Sof(H28C)=Sof(H28D)=FVAR(5)
 Sof(C24B)=Sof(H24C)=Sof(H24D)=Sof(N9B)=Sof(N10B)=Sof(C25B)=Sof(H25B)=
 Sof(C26B)=Sof(H26B)=Sof(C27B)=Sof(H27B)=FVAR(6)
 Sof(C24C)=Sof(H24E)=Sof(H24F)=Sof(N9C)=Sof(N10C)=Sof(C25C)=Sof(H25C)=
 Sof(C26C)=Sof(H26C)=Sof(C27C)=Sof(H27C)=FVAR(7)
9.a Ternary CH refined with riding coordinates:
 C11(H11), C11A(H11A), C19(H19), C19(H19A)
9.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C20A(H20C,H20D), C24A(H24A,H24B), C24B(H24C,H24D), C24C(H24E,
 H24F), C28A(H28A,H28B), C28B(H28C,H28D)
9.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C15A(H15A), C16A(H16A), C17A(H17A), C21(H21),
 C22(H22), C23(H23), C21A(H21A), C22A(H22A), C23A(H23A), C25A(H25A), C26A(H26A),
  C27A(H27A), C25B(H25B), C26B(H26B), C27B(H27B), C25C(H25C), C26C(H26C),
 C27C(H27C)
;
_shelx_res_checksum              10959
_shelx_hkl_checksum              93384
_olex2_submission_special_instructions 'No special instructions were received'