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_7708838
_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
'2(C57 H87 B2 Cl4 Co3 Fe2 N23 O5), 5(C3 H7 N O), 4(C1.5 H1.5 N0.5 O0.5)'
_chemical_formula_sum            'C135 H215 B4 Cl8 Co6 Fe4 N53 O17'
_chemical_formula_weight         3756.41
_chemical_name_systematic        ([(Tp*Me)Fe(CN)3CoCl2]2Co(DMF)4).4.5DMF
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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
;
2021-10-25 deposited with the CCDC.	2021-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.968(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.9177(11)
_cell_length_b                   14.1062(7)
_cell_length_c                   33.8098(19)
_cell_measurement_reflns_used    9286
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      2.39
_cell_volume                     10262.2(9)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       APEX3
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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      100.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0727
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            54472
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.140
_diffrn_reflns_theta_max         25.140
_diffrn_reflns_theta_min         2.454
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.911
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6200
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1315 before and 0.0839 after correction.
The Ratio of minimum to maximum transmission is 0.8320.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       block
_exptl_crystal_F_000             3908
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.286
_refine_diff_density_min         -1.121
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.205
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         9134
_refine_ls_number_restraints     234
_refine_ls_restrained_S_all      1.212
_refine_ls_R_factor_all          0.1252
_refine_ls_R_factor_gt           0.1131
_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^)+(0.0988P)^2^+166.4974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2952
_refine_ls_wR_factor_ref         0.3025
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7750
_reflns_number_total             9134
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02844h2.cif
_cod_data_source_block           2
_cod_database_code               7708838
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.875
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O5-C36 = C35-O5B = O4-C33 = O4A-C33
 1.2 with sigma of 0.02
 N14-C35 = N14-C34 = N14-C36
 1.4 with sigma of 0.02
 N13-C32
 1.47 with sigma of 0.02
 N5-C8
 1.47 with sigma of 0.02
 N15-C37 = N15-C38
 1.47 with sigma of 0.02
 N5A-C8A = N5A-C9A
 1.47 with sigma of 0.02
 C21-C18 = C20-C17 = C19-C16
 1.51 with sigma of 0.01
 C27-C24 = C26-C23 = C25-C22
 1.51 with sigma of 0.01
 C17-C16 = C18-C17 = C24-C23 = C23-C22
 1.38 with sigma of 0.01
 C7A-C9A
 2.35 with sigma of 0.04
 C32-C33
 2.35 with sigma of 0.04
 C37-C38
 2.35 with sigma of 0.04
 C33-C31
 2.2 with sigma of 0.04
 C34-C36
 2.35 with sigma of 0.01
 N14-O5B
 2.22 with sigma of 0.01
 N14-O5
 2.22 with sigma of 0.01
 N12-O3A
 2.22 with sigma of 0.01
 O4A-N13
 2.22 with sigma of 0.04
 O4-N13
 2.22 with sigma of 0.04
 O6-N15
 2.3 with sigma of 0.04
 O2-C7 \\sim O2-C7A
 with sigma of 0.02
3. Restrained planarity
 O2, C7A, C9A, C8A, N5A
 with sigma of 0.1
 O2, C7, C8, C9, N5
 with sigma of 0.1
 C38, C38_$1, N15, C37_$1, O6_$1
 with sigma of 0.1
 C38, N15, C37, O6
 with sigma of 0.01
4. Rigid bond restraints
 Cl2, Cl2A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl1, Cl1A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C31 \\sim C32 \\sim C33 \\sim N13 \\sim O4 \\sim O4A: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04
C28 \\sim C29 \\sim C30 \\sim N12 \\sim O3A \\sim O3: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04
C4 \\sim C5 \\sim C6 \\sim N4 \\sim O1: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C38 \\sim C38 \\sim N15 \\sim C37 \\sim C37 \\sim O6 \\sim O6: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C7) \\sim Ueq, Uanis(C7A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O3A) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(N12) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.05 and
sigma for terminal atoms of 0.1
Uanis(C7A) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C36) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O5B) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.05 and
sigma for terminal atoms of 0.1
Uanis(Cl2) = Uanis(Cl2A)
Uanis(Cl1) = Uanis(Cl1A)
Uanis(C7) = Uanis(C7A)
Uanis(C9A) = Uanis(C9) = Uanis(C8A) = Uanis(C8)
Uanis(N5A) = Uanis(N5)
Uanis(O4A) = Uanis(O4)
6. Others
 Fixed Sof: C7A(0.5) H7A(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5) H9AC(0.5) C8A(0.5)
 H8AA(0.5) H8AB(0.5) H8AC(0.5) Cl1(0.8) Cl2(0.8) N5A(0.5) C7(0.5) H7(0.5)
 C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5) C9(0.5) H9A(0.5) H9B(0.5) H9C(0.5)
 Cl1A(0.2) Cl2A(0.2) N5(0.5) C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) C29(0.5)
 C30(0.5) N12(0.5) O3A(0.25) O3(0.25) H33(0.5) H33A(0.5) O4(0.5) O4A(0.5)
 C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5) C35(0.5) C36(0.5) N14(0.5) O5(0.3)
 O5B(0.2) C38(0.5) H38A(0.5) H38B(0.5) H38C(0.5) N15(0.25) C37(0.25) H37(0.25)
 O6(0.25)
7.a Ternary CH refined with riding coordinates:
 B1(H1)
7.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7A(H7A), C7(H7), C33(H33), C33(H33A), C37(H37)
7.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C9A(H9AA,
 H9AB,H9AC), C8A(H8AA,H8AB,H8AC), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C28(H28A,
 H28B,H28C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C),
 C38(H38A,H38B,H38C)
;
_shelx_res_checksum              78466
_shelx_hkl_checksum              46778
_olex2_submission_special_instructions 'No special instructions were received'