Ferromagnetically coupled single-chain magnets exhibiting a magnetic hysteresis of 0.42 Tesla in cyano-bridged FeIII2MII (M = Ni, Fe) coordination polymers
Wang, Jin-Hua; Javed, Mohammad Khurram; Li, Jia-Xin; Zhang, Yi-Quan; Li, Zhaoyang; Yamashita, Masahiro; Dalton Transactions  (2023) –; doi:10.1039/D3DT01043K

data_7713660
_publ_section_title
;
 Ferromagnetically coupled single-chain magnets exhibiting a magnetic
 hysteresis of 0.42 Tesla in cyano-bridged FeIII2MII (M = Ni, Fe)
 coordination polymers
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01043K
_journal_year                    2023
_chemical_formula_moiety         'C48 H56 B2 Fe3 N22 O2, 4[H2O]'
_chemical_formula_sum            'C48 H64 B2 Fe3 N22 O6'
_chemical_formula_weight         1234.38
_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_Hall           '-I 2 2c'
_space_group_name_H-M_alt        'I b a m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-07-25
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-27 deposited with the CCDC.	2023-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4590(8)
_cell_length_b                   26.826(2)
_cell_length_c                   14.0720(7)
_cell_measurement_reflns_used    6031
_cell_measurement_temperature    300.0(3)
_cell_measurement_theta_max      73.2590
_cell_measurement_theta_min      3.2080
_cell_volume                     5835.7(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -37.00  37.00   0.50    5.00    --    0.00 -57.00  90.00  148
  2  \w    -87.00 -44.00   0.50    5.00    --    0.00 -57.00  90.00   86
  3  \w     18.00  43.00   0.50    5.00    --    0.00  57.00-120.00   50
  4  \w     17.00  69.00   0.50   45.00    --   98.20 -61.00-180.00  104
  5  \w     76.00 135.00   0.50   45.00    --   98.20 -61.00-180.00  118
  6  \w     36.00 134.00   0.50   45.00    --   98.20 -82.00-180.00  196
  7  \w    138.00 188.00   0.50   45.00    --   98.20 -15.00 -60.00  100
  8  \w     64.00  89.00   0.50   45.00    --   98.20  61.00-180.00   50
  9  \w      9.00  76.00   0.50   45.00    --   98.20 -15.00 -60.00  134
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0056672000
_diffrn_orient_matrix_UB_12      0.0486303000
_diffrn_orient_matrix_UB_13      -0.0501048000
_diffrn_orient_matrix_UB_21      0.0143436000
_diffrn_orient_matrix_UB_22      -0.0865061000
_diffrn_orient_matrix_UB_23      -0.0274251000
_diffrn_orient_matrix_UB_31      -0.1083520000
_diffrn_orient_matrix_UB_32      -0.0090014000
_diffrn_orient_matrix_UB_33      -0.0061532000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8809
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.467
_diffrn_reflns_theta_min         3.295
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    6.448
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       block
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         2980
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1480P)^2^+9.8594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2039
_refine_ls_wR_factor_ref         0.2082
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2760
_reflns_number_total             2980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01043k2.cif
_cod_data_source_block           2
_cod_original_cell_volume        5835.8(6)
_cod_database_code               7713660
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.537
_shelx_estimated_absorpt_t_min   0.390
_reflns_odcompleteness_completeness 99.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C15-C18
 1.5 with sigma of 0.01
 N8-O1
 1.38 with sigma of 0.01
 C18-N8
 1.32 with sigma of 0.01
 C15-N8
 2.444 with sigma of 0.04
 C18-O1
 2.205 with sigma of 0.04
 C18-C14 \\sim C18-C16
 with sigma of 0.02
3. Restrained planarity
 N7, N8, C13, C14, C15, C16, C17, C18
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O1 \\sim N7 \\sim N8 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim
C18: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.001 within
2A
5. Rigid body (RIGU) restrains
 Fe1, O1, N7, N8, C13, C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H8A(0.5) H8B(0.5) H8C(0.5) H12A(0.5) H12B(0.5) H12C(0.5) O1(0.5)
 H1A(0.5) N7(0.5) C13(0.5) H13(0.5) C14(0.5) H14(0.5) C15(0.5) C16(0.5)
 H16(0.5) C17(0.5) H17(0.5) N8(0.5) C18(0.5) H18(0.5)
 Fixed U11: Fe1(0.03691) Fe2(0.03739) N1(0.04574) N2(0.03752) N3(0.0519)
 N4(0.05635) N5(0.05356) N6(0.0437) C1(0.03762) C2(0.0476) C3(0.07504)
 C4(0.05315) C5(0.07048) C6(0.05858) C7(0.09487) C8(0.04546) C9(0.04374)
 C10(0.04997) C11(0.05423) C12(0.07943) B1(0.06397) N7(0.03588) C13(0.05561)
 C14(0.05483) C15(0.05932) C16(0.04757) C17(0.0468)
 Fixed U12: Fe1(0) Fe2(0.00179) N1(0.00297) N2(-0.00384) N3(0.00662)
 N4(0.00381) N5(-0.00486) N6(-0.00344) C1(0.00017) C2(-0.00101) C3(0.0117)
 C4(0.01267) C5(0.01503) C6(0.01258) C7(0.00762) C8(0.00611) C9(-0.00067) C10(-
 0.0083) C11(-0.01001) C12(-0.01931) B1(0.00282) N7(0) C13(-0.00037)
 C14(0.00665) C15(-0.00051) C16(0.00224) C17(-0.00285)
 Fixed U13: Fe1(0) Fe2(0) N1(0.00053) N2(0) N3(-0.00395) N4(0.00263) N5(0)
 N6(0) C1(-0.00152) C2(0) C3(-0.01938) C4(-0.00408) C5(-0.00256) C6(0.00443)
 C7(0.00635) C8(0) C9(0) C10(0) C11(0) C12(0) B1(0) N7(0) C13(-0.01001) C14(-
 0.00944) C15(-0.00254) C16(0.0041) C17(0.0054)
 Fixed U22: Fe1(0.02428) Fe2(0.02498) N1(0.03281) N2(0.04691) N3(0.03408)
 N4(0.03282) N5(0.03025) N6(0.03064) C1(0.03194) C2(0.04515) C3(0.0648)
 C4(0.05203) C5(0.05826) C6(0.04685) C7(0.04676) C8(0.05039) C9(0.04442)
 C10(0.05136) C11(0.0441) C12(0.0467) B1(0.04204) N7(0.0345) C13(0.0498)
 C14(0.08134) C15(0.06137) C16(0.07745) C17(0.05198)
 Fixed U23: Fe1(0) Fe2(0) N1(-0.0043) N2(0) N3(0.00481) N4(0.00844) N5(0)
 N6(0) C1(0.00161) C2(0) C3(-0.00748) C4(0.0052) C5(0.01657) C6(0.01936)
 C7(0.02816) C8(0) C9(0) C10(0) C11(0) C12(0) B1(0) N7(0.00019) C13(-0.00491)
 C14(-0.0008) C15(-0.00449) C16(-0.00637) C17(-0.00741)
 Fixed U33: Fe1(0.02547) Fe2(0.02696) N1(0.03234) N2(0.05598) N3(0.0383)
 N4(0.04543) N5(0.0469) N6(0.03891) C1(0.02962) C2(0.04473) C3(0.04608)
 C4(0.0357) C5(0.05197) C6(0.05777) C7(0.09469) C8(0.06563) C9(0.0386)
 C10(0.04765) C11(0.04918) C12(0.11643) B1(0.06144) N7(0.05901) C13(0.06714)
 C14(0.08133) C15(0.08965) C16(0.0859) C17(0.06664)
7.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C10(H10), C13(H13), C14(H14), C16(H16), C17(H17), C18(H18)
7.b Fitted hexagon refined as free rotating group:
 N7(C13,C14,C15,C16,C17)
7.c Tetrahedral OH refined with riding coordinates:
 O1(H1A)
7.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              16890
_shelx_fab_checksum              71646
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.199
_oxdiff_exptl_absorpt_empirical_full_min 0.472