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_7249672
_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         'C27 H23 B Co Fe N16, B F4, 2(C H4 O)'
_chemical_formula_sum            'C29 H31 B2 Co F4 Fe N16 O2'
_chemical_formula_weight         848.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-22
_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                90
_cell_angle_beta                 106.52
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1471(8)
_cell_length_b                   26.0291(14)
_cell_length_c                   12.1470(8)
_cell_measurement_reflns_used    7738
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      53.81
_cell_measurement_theta_min      2.95
_cell_volume                     3682.1(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 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 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.987
_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           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_av_unetI/netI     0.0840
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22017
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.964
_diffrn_reflns_theta_min         2.954
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           3.57
_diffrn_source_power             0.24947159999999996
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           69.88
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.074
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.5500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1248 before and 0.0685 after correction.
The Ratio of minimum to maximum transmission is 0.7327.
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    1.530
_exptl_crystal_description       plate
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.337
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         6682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_gt           0.0826
_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^)+(0.0721P)^2^+26.4093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2033
_refine_ls_wR_factor_ref         0.2145
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4894
_reflns_number_total             6682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01049c2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7249670--7249672.cif.'
_cod_original_cell_volume        3682.2(4)
_cod_database_code               7249672
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.786
_shelx_estimated_absorpt_t_min   0.415
_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
2.a Riding coordinates:
 O2(H2A), O1(H1B)
2.b Ternary CH refined with riding coordinates:
 C9(H9), B1(H1A)
2.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C24(H24), C6(H6), C27(H27), C26(H26), C23(H23), C5(H5),
 C11(H11), C22(H22), C12(H12), C13(H13), C25(H25), C20(H20), C10(H10), C7(H7),
 C1(H1), C3(H3), C21(H21), C2(H2), C19(H19)
2.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              61505
_shelx_hkl_checksum              10266
_olex2_submission_special_instructions 'No special instructions were received'