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_7249670
_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         'C39 H33 B2 Co Fe2 N25, 4(C H4 O), 5(H2 O)'
_chemical_formula_sum            'C43 H59 B2 Co Fe2 N25 O9'
_chemical_formula_weight         1262.40
_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
_audit_creation_date             2024-07-24
_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                75.334(2)
_cell_angle_beta                 83.4110(10)
_cell_angle_gamma                74.951(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5164(4)
_cell_length_b                   16.3636(6)
_cell_length_c                   16.3579(6)
_cell_measurement_reflns_used    9221
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      26.26
_cell_measurement_theta_min      2.30
_cell_volume                     2875.96(18)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            58468
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.480
_diffrn_reflns_theta_min         2.296
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.857
_exptl_absorpt_correction_T_max  0.835
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_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    1.458
_exptl_crystal_description       block
_exptl_crystal_F_000             1306
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.211
_refine_diff_density_max         1.464
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         11845
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0629
_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^)+(0.0890P)^2^+9.9408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1696
_refine_ls_wR_factor_ref         0.1872
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9389
_reflns_number_total             11845
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01049c2.cif
_cod_data_source_block           lqy3282_0m
_cod_depositor_comments
'Adding full bibliography for 7249670--7249672.cif.'
_cod_database_code               7249670
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.840
_shelx_estimated_absorpt_t_min   0.827
_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, All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Riding coordinates:
 O1(H1B), O4(H4), C39(H39A,H39B,H39C), O6(H6), C41(H41A,H41B,H41C), O8(H8A,
 H8B), O9(H9A,H9B), O5(H5D,H5E), O3(H3A,H3B), O7(H7A), O2(H2B,H2C), C21(H21A,
 H21B,H21C)
3.b Ternary CH refined with riding coordinates:
 C12(H12), B2(H2A), B1(H1A)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C8(H8), C10(H10), C14(H14), C20(H20), C24(H24), C26(H26), C28(H28),
 C30(H30), C34(H34), C38(H38), C40(H40), C42(H42), C43(H43), C11(H11), C23(H23),
  C3(H3), C25(H25), C13(H13), C7(H7), C29(H29), C15(H15), C31(H31), C2(H2),
 C33(H33), C17(H17), C35(H35), C9(H9), C37(H37), C19(H19)
3.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_shelx_res_checksum              3961
_shelx_hkl_checksum              50099
_olex2_submission_special_instructions 'No special instructions were received'