Magnetic and electrical properties of a cyanide-bridged CoCu₃ cluster featuring square pyramidal Cu(II) centers
Zhang, Yang-Lu; Cai, Meng-Tan; Chen, Yi; Shen, Fuxing; Yang, Jiong; Zhu, Junlun; Shao, Dong; CrystEngComm  (2025) –; doi:10.1039/D5CE00957J

data_7251249
_publ_section_title
;
 Magnetic and electrical properties of a cyanide-bridged CoCu&#x2083;
 cluster featuring square pyramidal Cu(II) centers
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D5CE00957J
_journal_year                    2025
_chemical_formula_moiety         'C48 H96 Co Cu3 N18, C6 Co N6, 14(H2 O)'
_chemical_formula_sum            'C54 H124 Co2 Cu3 N24 O14'
_chemical_formula_weight         1642.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-07-10
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-07-18 deposited with the CCDC.	2025-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.598(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.834(2)
_cell_length_b                   29.952(5)
_cell_length_c                   12.453(2)
_cell_measurement_reflns_used    5899
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.06
_cell_measurement_theta_min      2.33
_cell_volume                     4013.4(12)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT V8.40B (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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'Bruker PHOTON-II area detector'
_diffrn_detector_area_resol_mean 7.4
_diffrn_detector_type            'CMOS-PHOTONII area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON-II area detector'
_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  0.0420
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            24734
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.280
_diffrn_reflns_theta_min         1.360
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0997 before and 0.0486 after correction.
The Ratio of minimum to maximum transmission is 0.7873.
The \l/2 correction factor is 0.00150.
;
_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    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1738
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         8238
_refine_ls_number_restraints     389
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0734P)^2^+7.4387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1607
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6209
_reflns_number_total             8238
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00957j2.cif
_cod_data_source_block           a_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_cell_volume        4013.8(13)
_cod_database_code               7251249
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.854
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N14-C24 = N14-C26 = N14-C25 = N15-C28 = N15-C29 = N15-C30 = N16-C31 = N16-C33
 = N13-C35 = N13-C23 = N16-C32 = N13-C22
 1.47 with sigma of 0.01
 C24-C23 = C28-C27 = C27-C26 = C31-C30 = C34-C33 = C35-C34
 1.54 with sigma of 0.01
 C33-C35 = C28-C26
 2.515 with sigma of 0.2
 C24-C25 \\sim C24-C25 \\sim C25-C26
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O2 \\sim O2A \\sim O2B: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O1A \\sim O1 \\sim O1B: within 3A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 3A
Cu2 \\sim C25 \\sim N14 \\sim N15 \\sim C26 \\sim C28 \\sim C35 \\sim C24 \\sim
C27 \\sim C22 \\sim C32 \\sim N16 \\sim C30 \\sim N13 \\sim C34 \\sim C29 \\sim
C33 \\sim C31 \\sim C23: within 3A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 3A
O3A \\sim O3: within 3A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 3A
4. Others
 1*[Sof(O1)+Sof(H1A)+Sof(H1B)]+1*[Sof(O1A)+Sof(H1AA)+Sof(H1AB)]+1*[Sof(O1B)+
 Sof(H1BA)+Sof(H1BB)]=1 with esd of 0
 1*[Sof(O2)+Sof(H2A)+Sof(H2B)]+1*[Sof(O2A)+Sof(H2AA)+Sof(H2AB)]+1*[Sof(O2B)+
 Sof(H2BA)+Sof(H2BB)]=1 with esd of 0
 Sof(O2)=Sof(H2A)=Sof(H2B)=FVAR(1)
 Sof(O1)=Sof(H1A)=Sof(H1B)=FVAR(2)
 Sof(O1A)=Sof(H1AA)=Sof(H1AB)=FVAR(3)
 Sof(O1B)=Sof(H1BA)=Sof(H1BB)=FVAR(4)
 Sof(O2A)=Sof(H2AA)=Sof(H2AB)=FVAR(5)
 Sof(O2B)=Sof(H2BA)=Sof(H2BB)=FVAR(6)
 Sof(O3A)=Sof(H3AA)=Sof(H3AB)=1-FVAR(7)
 Sof(O3)=Sof(H3A)=Sof(H3B)=FVAR(7)
 Fixed Sof: C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5) N14(0.5) N15(0.5) C26(0.5)
 H26A(0.5) H26B(0.5) C28(0.5) H28A(0.5) H28B(0.5) C35(0.5) H35A(0.5) H35B(0.5)
 C24(0.5) H24A(0.5) H24B(0.5) C27(0.5) H27A(0.5) H27B(0.5) C22(0.5) H22A(0.5)
 H22B(0.5) H22C(0.5) C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5) N16(0.5) C30(0.5)
 H30A(0.5) H30B(0.5) N13(0.5) C34(0.5) H34A(0.5) H34B(0.5) C29(0.5) H29A(0.5)
 H29B(0.5) H29C(0.5) C33(0.5) H33A(0.5) H33B(0.5) C31(0.5) H31A(0.5) H31B(0.5)
 C23(0.5) H23A(0.5) H23B(0.5)
5.a Riding coordinates:
 O8(H8A,H8B), O5(H5A,H5B), O7(H7A,H7B), O6(H6A,H6B), O2(H2A,H2B), O3A(H3AA,
 H3AB), O1(H1A,H1B), O2A(H2AA,H2AB), O1A(H1AA,H1AB), O1B(H1BA,H1BB), O2B(H2BA,
 H2BB), O3(H3A,H3B)
5.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C21(H21A,H21B), C20(H20A,H20B), C11(H11A,H11B), C19(H19A,
 H19B), C10(H10A,H10B), C16(H16A,H16B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), C26(H26A,H26B), C28(H28A,H28B), C35(H35A,H35B), C24(H24A,H24B),
  C27(H27A,H27B), C30(H30A,H30B), C34(H34A,H34B), C33(H33A,H33B), C31(H31A,
 H31B), C23(H23A,H23B)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C12(H12A,H12B,H12C), C014(H01A,H01B,
 H01C), C25(H25A,H25B,H25C), C22(H22A,H22B,H22C), C32(H32A,H32B,H32C), C29(H29A,
 H29B,H29C)
;
_shelx_res_checksum              56531
_olex2_submission_special_instructions 'No special instructions were received'