A cyanide-bridged Fe-Co pearl-chain-like single-chain magnet containing 4-coordinate cobalt(II) ions
Cheng, Yue; Liu, Qi; Chen, Zi-Yi; Zhang, Yuan-Zhu; Dalton Transactions  (2021) –; doi:10.1039/D1DT02844H

data_7708839
_publ_section_title
;
 A cyanide-bridged Fe-Co pearl-chain-like single-chain magnet containing
 4-coordinate cobalt(II) ions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02844H
_journal_year                    2021
_chemical_formula_moiety         'C42 H60 B2 Cl4 Co3 Fe2 N22 O4, C3 H7 N O'
_chemical_formula_sum            'C45 H67 B2 Cl4 Co3 Fe2 N23 O5'
_chemical_formula_weight         1462.12
_chemical_name_systematic        ([(Tp4-Me)Fe(CN)3CoCl2]2Co(DMF)4).1DMF
_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     iterative
_audit_creation_date             2021-10-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-01 deposited with the CCDC.	2021-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                115.446(2)
_cell_angle_beta                 108.234(2)
_cell_angle_gamma                98.006(2)
_cell_formula_units_Z            1
_cell_length_a                   11.5345(6)
_cell_length_b                   13.2546(7)
_cell_length_c                   13.4018(7)
_cell_measurement_reflns_used    9777
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.82
_cell_volume                     1665.37(16)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       APEX3
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      99.98
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8-Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            47978
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         2.196
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.376
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1080 before and 0.0726 after correction.
The Ratio of minimum to maximum transmission is 0.8912.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       block
_exptl_crystal_F_000             749
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         6533
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0854
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+25.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2045
_refine_ls_wR_factor_ref         0.2051
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6331
_reflns_number_total             6533
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02844h2.cif
_cod_data_source_block           1
_cod_original_cell_volume        1665.37(15)
_cod_database_code               7708839
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.770
_shelx_estimated_absorpt_t_min   0.725
_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. Uiso/Uaniso restraints and constraints
C23 \\sim C24 \\sim N12 \\sim C22 \\sim O3: within 2A with sigma of 0.0051 and
sigma for terminal atoms of 0.0102
C12 \\sim C5 \\sim C4 \\sim C2 \\sim C3 \\sim C8 \\sim C13 \\sim C1 \\sim C14
\\sim C19 \\sim C6 \\sim C7 \\sim C16 \\sim C15 \\sim C10 \\sim C9 \\sim C11
\\sim C20 \\sim C17 \\sim C21 \\sim C18 \\sim C22 \\sim C24 \\sim C23: within
2A with sigma of 0.05 and sigma for terminal atoms of 0.1
3. Others
 Fixed Sof: Co1(0.65) Cl1(0.65) Cl2(0.65) Cl2A(0.35) Co1A(0.35) Cl1A(0.35)
 N12(0.5) O3(0.5) C22(0.5) H22(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5)
 C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5)
4.a Ternary CH refined with riding coordinates:
 B1(H1)
4.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C4(H4), C8(H8), C14(H14), C19(H19), C6(H6), C16(H16), C10(H10),
 C22(H22)
4.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C11(H11A,H11B,H11C), C20(H20A,H20B,
 H20C), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C), C18(H18A,H18B,H18C), C24(H24A,
 H24B,H24C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              59692
_shelx_hkl_checksum              58199
_olex2_submission_special_instructions 'No special instructions were received'