Structural regulation of three Fe–Co cyanometallate complexes: reactant ratio issue
Li, Qiuyu; Cao, Qiuyue; Xi, Jing; Zhang, Ziyi; Yao, Binling; Shao, Dong; Deng, Yi-Fei; Zhang, Yuan-Zhu; CrystEngComm 27 (2025) 407–414; doi:10.1039/D4CE01049C

data_7249671
_publ_section_title
;
 Structural regulation of three Fe--Co cyanometallate complexes: reactant
 ratio issue
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              407
_journal_page_last               414
_journal_paper_doi               10.1039/D4CE01049C
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety
'C54 H46 B2 Co2 Fe2 N32, 2(Cl O4), 2(H2 O), 2(C2 H3 N)'
_chemical_formula_sum            'C58 H56 B2 Cl2 Co2 Fe2 N34 O10'
_chemical_formula_weight         1711.44
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-30
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-10-12 deposited with the CCDC.	2024-12-03 downloaded from the CCDC.
;
_cell_angle_alpha                69.317(3)
_cell_angle_beta                 75.823(3)
_cell_angle_gamma                69.273(3)
_cell_formula_units_Z            1
_cell_length_a                   10.9427(11)
_cell_length_b                   13.2533(14)
_cell_length_c                   14.3559(15)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    101.42
_cell_measurement_theta_max      25.41
_cell_measurement_theta_min      2.35
_cell_volume                     1804.5(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      101.42
_diffrn_detector                 'Bruker PHOTO 100 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43382
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.444
_diffrn_reflns_theta_min         2.353
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.001
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6433
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1631 before and 0.0650 after correction.
The Ratio of minimum to maximum transmission is 0.8633.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         6641
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0410P)^2^+1.3140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0819
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5690
_reflns_number_total             6641
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01049c2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7249670--7249672.cif.'
_cod_database_code               7249671
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.788
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), B1(H1A)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C1(H1), C2(H2), C20(H20), C25(H25), C3(H3), C23(H23), C18(H18),
 C10(H10), C13(H13), C11(H11), C9(H9), C19(H19), C21(H21), C4(H4), C6(H6),
 C14(H14), C24(H24), C22(H22), C5(H5)
2.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C)
;
_shelx_res_checksum              33491
_shelx_hkl_checksum              85238
_olex2_submission_special_instructions 'No special instructions were received'