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_4349959
_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 Co2 Fe4 N48'
_chemical_formula_sum            'C108 H112 B4 Co2 Fe4 N48'
_chemical_formula_weight         2466.95
_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             2018-04-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-05-01 deposited with the CCDC.
2018-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                87.5760(10)
_cell_angle_beta                 72.944(2)
_cell_angle_gamma                77.779(2)
_cell_formula_units_Z            1
_cell_length_a                   12.2908(2)
_cell_length_b                   15.6215(2)
_cell_length_c                   15.9090(3)
_cell_measurement_reflns_used    13710
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      73.0290
_cell_measurement_theta_min      4.0300
_cell_volume                     2853.38(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      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.966
_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    -22.00  24.00   0.50    0.50    --    0.00 -57.00  90.00   92
  2  \w    -35.00  15.00   0.50    0.50    --    0.00  77.00 150.00  100
  3  \w    -21.00  29.00   0.50    0.50    --    0.00 -57.00 -60.00  100
  4  \w     32.00  72.00   0.50    0.50    --    0.00  57.00-150.00   80
  5  \w    -89.00 -51.00   0.50    0.50    --    0.00 -57.00  90.00   76
  6  \w    -83.00 -35.00   0.50    0.50    --    0.00 -57.00 -60.00   96
  7  \w     30.00  88.00   0.50    0.50    --    0.00  77.00 150.00  116
  8  \w     97.00 187.00   0.50    4.64    --   98.20  45.00-150.00  180
  9  \w     10.00 131.00   0.50    4.64    --   98.20 -82.00 150.00  242
 10  \w     80.00 106.00   0.50    4.64    --   98.20 -82.00-120.00   52
 11  \w     70.00  96.00   0.50    4.64    --   98.20 -82.00 120.00   52
 12  \w     16.00 136.00   0.50    4.64    --   98.20 -82.00 -60.00  240
 13  \w    140.00 188.00   0.50    4.64    --   98.20  15.00  90.00   96
 14  \w     17.00  42.00   0.50    4.64    --   98.20 -61.00  30.00   50
 15  \w      9.00 130.00   0.50    4.64    --   98.20 -61.00 150.00  242
 16  \w     47.00 108.00   0.50    4.64    --   98.20 -82.00  60.00  122
 17  \w     93.00 137.00   0.50    4.64    --   98.20  77.00 -30.00   88
 18  \w     14.00 130.00   0.50    4.64    --   98.20 -61.00 -60.00  232
 19  \w     67.00 103.00   0.50    4.64    --   98.20 -61.00  30.00   72
 20  \w     29.00 100.00   0.50    4.64    --   98.20  15.00  90.00  142
 21  \w     27.00  65.00   0.50    4.64    --   98.20 -45.00-150.00   76
 22  \w     90.00 116.00   0.50    4.64    --   98.20 -82.00   0.00   52
 23  \w     11.00  39.00   0.50    4.64    --   98.20 -82.00  60.00   56
 24  \w     16.00  41.00   0.50    4.64    --   98.20 -82.00-120.00   50
 25  \w     73.00  98.00   0.50    4.64    --   98.20 -82.00-180.00   50
 26  \w     13.00 159.00   0.50    4.64    --   98.20 -15.00  30.00  292
;
_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      -0.0645282000
_diffrn_orient_matrix_UB_12      -0.0180542000
_diffrn_orient_matrix_UB_13      -0.0648765000
_diffrn_orient_matrix_UB_21      0.1174376000
_diffrn_orient_matrix_UB_22      -0.0371429000
_diffrn_orient_matrix_UB_23      -0.0680190000
_diffrn_orient_matrix_UB_31      -0.0040628000
_diffrn_orient_matrix_UB_32      -0.0920910000
_diffrn_orient_matrix_UB_33      0.0378005000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29239
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.428
_diffrn_reflns_theta_min         4.060
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.766
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62830
_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_colour            red
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       block
_exptl_crystal_F_000             1274
_refine_diff_density_max         0.992
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         11088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0695P)^2^+2.4231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1382
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9612
_reflns_number_total             11088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi01245h2.cif
_cod_data_source_block           171209-2_sq
_cod_database_code               4349959
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.53
_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), C13(H13), C21(H21), C26(H26), C31(H31), C37(H37), C38(H38),
 C39(H39), C40(H40), C46(H46), C47(H47), C48(H48), C49(H49), C51(H51), C52(H52),
  C53(H53), C54(H54)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C33(H33A,
 H33B,H33C)
;
_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 1.625
_oxdiff_exptl_absorpt_empirical_full_min 0.768