Charge transfer and slow magnetic relaxation in a series of cyano-bridged FeIII4MII2 (M = FeII, CoII, NiII) molecules
Wang, Jin-Hua; Vignesh, Kuduva R.; Zhao, Jia; Li, Zhao-Yang; Dunbar, Kim R.; Inorganic Chemistry Frontiers 6 (2019) 493–; doi:10.1039/C8QI01245H

data_4349961
_publ_section_title
;
 Charge transfer and slow magnetic relaxation in a series of cyano-bridged
 FeIII4MII2 (M = FeII, CoII, NiII) molecules
;
_journal_issue                   2
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              493
_journal_paper_doi               10.1039/C8QI01245H
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         'C108 H112 B4 Fe4 N48 Ni2'
_chemical_formula_sum            'C108 H112 B4 Fe4 N48 Ni2'
_chemical_formula_weight         2466.51
_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
_audit_creation_date             2018-04-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-05-01 deposited with the CCDC.
2018-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                88.2190(10)
_cell_angle_beta                 85.2320(10)
_cell_angle_gamma                65.8640(10)
_cell_formula_units_Z            1
_cell_length_a                   15.0634(2)
_cell_length_b                   16.0649(2)
_cell_length_c                   17.2995(2)
_cell_measurement_reflns_used    25320
_cell_measurement_temperature    99.97(12)
_cell_measurement_theta_max      73.1180
_cell_measurement_theta_min      3.9210
_cell_volume                     3807.12(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(12)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.971
_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    -41.00  30.00   0.50    0.50    --    0.00 -38.00 -30.00  142
  2  \w     -8.00  28.00   0.50    0.50    --    0.00  57.00-150.00   72
  3  \w     52.00  88.00   0.50    0.50    --    0.00  57.00-150.00   72
  4  \w     26.00  89.00   0.50    0.50    --    0.00  57.00 -60.00  126
  5  \w    -74.00  29.00   0.50    0.50    --    0.00 -77.00-120.00  206
  6  \w     17.00  42.00   0.50    1.50    --   98.20 -82.00  30.00   50
  7  \w     69.00 108.00   0.50    1.50    --   98.20 -82.00  60.00   78
  8  \w     76.00 102.00   0.50    1.50    --   98.20 -82.00 -90.00   52
  9  \w     22.00  48.00   0.50    1.50    --   98.20 -82.00-150.00   52
 10  \w     71.00 134.00   0.50    1.50    --   98.20  45.00  30.00  126
 11  \w      9.00 122.00   0.50    1.50    --   98.20 -30.00   0.00  226
 12  \w     28.00  81.00   0.50    1.50    --   98.20  15.00 150.00  106
 13  \w     88.00 188.00   0.50    1.50    --   98.20  15.00 150.00  200
 14  \w     28.00 106.00   0.50    1.50    --   98.20 -61.00-180.00  156
 15  \w     59.00 114.00   0.50    1.50    --   98.20 -45.00-180.00  110
 16  \w     19.00 135.00   0.50    1.50    --   98.20 -82.00-180.00  232
 17  \w     81.00 106.00   0.50    1.50    --   98.20 -82.00-120.00   50
 18  \w     63.00 104.00   0.50    1.50    --   98.20 -82.00  90.00   82
 19  \w     94.00 120.00   0.50    1.50    --   98.20 -82.00 -30.00   52
 20  \w     26.00  99.00   0.50    1.50    --   98.20 -82.00 120.00  146
 21  \w     79.00 111.00   0.50    1.50    --   98.20 -82.00  30.00   64
 22  \w     77.00 102.00   0.50    1.50    --   98.20 -82.00-150.00   50
 23  \w     18.00 127.00   0.50    1.50    --   98.20 -61.00 -60.00  218
 24  \w     10.00 131.00   0.50    1.50    --   98.20 -82.00 -60.00  242
 25  \w     28.00 185.00   0.50    1.50    --   98.20  15.00-120.00  314
;
_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      -0.0638576000
_diffrn_orient_matrix_UB_12      -0.0343355000
_diffrn_orient_matrix_UB_13      0.0546379000
_diffrn_orient_matrix_UB_21      -0.0270780000
_diffrn_orient_matrix_UB_22      -0.0391836000
_diffrn_orient_matrix_UB_23      -0.0701093000
_diffrn_orient_matrix_UB_31      0.0884525000
_diffrn_orient_matrix_UB_32      -0.0912593000
_diffrn_orient_matrix_UB_33      0.0092163000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42660
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.485
_diffrn_reflns_theta_min         3.952
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.671
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_description       block
_exptl_crystal_F_000             1276
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         14874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0444P)^2^+8.7434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1306
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13852
_reflns_number_total             14874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi01245h2.cif
_cod_data_source_block           171126-2-100k_sq
_cod_database_code               4349961
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Ternary CH refined with riding coordinates:
 B1(H1), B2(H2)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C12(H12), C17(H17), C22(H22), C27(H27), C36(H36), C37(H37),
 C38(H38), C39(H39), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51),
  C52(H52), C53(H53)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C29(H29A,H29B,H29C), C56(H56A,
 H56B,H56C)
;
_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 1.349
_oxdiff_exptl_absorpt_empirical_full_min 0.851