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_7713661
_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 Fe2 N22 Ni O2, 2(H4 O2)'
_chemical_formula_sum            'C48 H64 B2 Fe2 N22 Ni O6'
_chemical_formula_weight         1237.24
_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     dual
_audit_creation_date             2023-07-05
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2023-07-14 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                   15.2745(5)
_cell_length_b                   26.0846(15)
_cell_length_c                   13.8740(4)
_cell_measurement_reflns_used    2858
_cell_measurement_temperature    126(9)
_cell_measurement_theta_max      71.3080
_cell_measurement_theta_min      3.4370
_cell_volume                     5527.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      126(9)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -88.00  36.00   1.00   24.21    --    0.00 -57.00 -60.00  124
  2  \w    -29.00   0.00   1.00   24.21    --    0.00 -57.00  90.00   29
  3  \w     59.00 119.00   1.00  100.00    --   98.20 -61.00  30.00   60
  4  \w     16.00  42.00   1.00  100.00    --   98.20 -61.00  30.00   26
  5  \w    106.00 188.00   1.00  100.00    --   98.20  61.00-150.00   82
  6  \w     63.00  88.00   1.00  100.00    --   98.20 -77.00  60.00   25
  7  \w     62.00 186.00   1.00  100.00    --   98.20  61.00 -30.00  124
  8  \w    104.00 134.00   1.00  100.00    --   98.20 -77.00-120.00   30
  9  \w     15.00  65.00   1.00  100.00    --   98.20 -77.00-120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0259016000
_diffrn_orient_matrix_UB_12      -0.0905601000
_diffrn_orient_matrix_UB_13      -0.0042419000
_diffrn_orient_matrix_UB_21      -0.0493693000
_diffrn_orient_matrix_UB_22      0.0426774000
_diffrn_orient_matrix_UB_23      -0.0386817000
_diffrn_orient_matrix_UB_31      0.0194684000
_diffrn_orient_matrix_UB_32      -0.0122037000
_diffrn_orient_matrix_UB_33      -0.1040203000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8772
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.570
_diffrn_reflns_theta_max         66.570
_diffrn_reflns_theta_min         3.353
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.125
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
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    1.487
_exptl_crystal_description       needle
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         2550
_refine_ls_number_restraints     226
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0693
_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^)+(0.1255P)^2^+12.7549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1919
_refine_ls_wR_factor_ref         0.2043
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2027
_reflns_number_total             2550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01043k2.cif
_cod_data_source_block           1
_cod_database_code               7713661
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.748
_shelx_estimated_absorpt_t_min   0.361
_reflns_odcompleteness_completeness 99.96
_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, All O(H,H) groups
2. Restrained distances
 N7-C17 \\sim N7-C13
 with sigma of 0.02
3. Restrained planarity
 C13, N7, C17, C16, C15, C14
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim N8 \\sim O1: within
8.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 8.7A
N3 \\sim N4 \\sim N3' \\sim N4': within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 2A
O1 \\sim N8 \\sim C18 \\sim C15 \\sim C16 \\sim N7 \\sim C17 \\sim C13 \\sim
C14: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C7') \\sim Ueq, Uanis(C8') \\sim Ueq, Uanis(C12') \\sim Ueq, Uanis(N3')
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) = Uanis(C1')
Uanis(N2') = Uanis(C2')
Uanis(C3') = Uanis(C4')
5. Others
 Sof(N5')=Sof(N6')=Sof(C1')=Sof(C8')=Sof(H8'A)=Sof(H8'B)=Sof(H8'C)=Sof(C9')=
 Sof(C10')=Sof(H10')=Sof(C11')=Sof(C12')=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(Fe1')=Sof(N2')=Sof(N3')=Sof(N4')=Sof(C2')=Sof(C3')=Sof(H3'A)=Sof(H3'B)=
 Sof(H3'C)=Sof(C4')=Sof(C5')=Sof(H5')=Sof(C6')=Sof(C7')=Sof(H7'A)=Sof(H7'B)=
 Sof(H7'C)=0.5*(1-FVAR(2))
 Sof(Fe1)=Sof(N2)=Sof(N3)=Sof(N4)=Sof(C2)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=
 Sof(C4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=0.5*FVAR(2)
 Sof(N5)=Sof(N6)=Sof(C1)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(C10)=
 Sof(H10)=Sof(C11)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
 Fixed Sof: H1WA(0.5) H1WB(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) C18(0.5) H18(0.5) N8(0.5) O1(0.5) H1A(0.5)
6.a Riding coordinates:
 C7'(H7'A,H7'B,H7'C), C12'(H12D,H12E,H12F), O1W(H1WA,H1WB), O2W(H2WA,H2WB)
6.b Me refined with riding coordinates:
 C3(H3A,H3B,H3C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C),
 C3'(H3'A,H3'B,H3'C), C8'(H8'A,H8'B,H8'C)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C10(H10), C5'(H5'), C10'(H10'), C13(H13), C14(H14), C16(H16),
 C17(H17), C18(H18)
6.d Tetrahedral OH refined with riding coordinates:
 O1(H1A)
;
_shelx_res_checksum              21425
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.411
_oxdiff_exptl_absorpt_empirical_full_min 0.730