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_4349960
_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 Fe6 N48'
_chemical_formula_sum            'C108 H112 B4 Fe6 N48'
_chemical_formula_weight         2460.79
_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                82.9140(10)
_cell_angle_beta                 71.8690(10)
_cell_angle_gamma                84.3630(10)
_cell_formula_units_Z            1
_cell_length_a                   11.73660(10)
_cell_length_b                   15.9647(2)
_cell_length_c                   17.5474(2)
_cell_measurement_reflns_used    18397
_cell_measurement_temperature    298.5(2)
_cell_measurement_theta_max      73.1500
_cell_measurement_theta_min      3.9680
_cell_volume                     3094.51(6)
_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      air
_diffrn_ambient_temperature      298.5(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_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    -76.00 -49.00   0.50    0.50    --    0.00 -77.00 150.00   54
  2  \w     -4.00  41.00   0.50    0.50    --    0.00  57.00-150.00   90
  3  \w    -19.00   6.00   0.50    0.50    --    0.00  38.00-180.00   50
  4  \w    -38.00  89.00   0.50    0.50    --    0.00  82.00  90.00  254
  5  \w    -58.00 -32.00   0.50    0.50    --    0.00 -57.00 -30.00   52
  6  \w    -39.00 -12.00   0.50    0.50    --    0.00 -77.00 150.00   54
  7  \w    -36.00  89.00   0.50    0.50    --    0.00  77.00 -90.00  250
  8  \w     10.00  44.00   0.50    0.50    --    0.00  38.00-180.00   68
  9  \w     37.00 115.00   0.50    1.61    --   98.20 -82.00 -60.00  156
 10  \w     80.00 125.00   0.50    1.61    --   98.20 -82.00 120.00   90
 11  \w     19.00 105.00   0.50    1.61    --   98.20 -15.00 150.00  172
 12  \w    142.00 168.00   0.50    1.61    --   98.20 -15.00 150.00   52
 13  \w     14.00 102.00   0.50    1.61    --   98.20 -61.00   0.00  176
 14  \w     10.00 104.00   0.50    1.61    --   98.20 -61.00 -60.00  188
 15  \w     58.00  86.00   0.50    1.61    --   98.20 -82.00 150.00   56
 16  \w     29.00  54.00   0.50    1.61    --   98.20 -82.00 150.00   50
 17  \w     10.00 124.00   0.50    1.61    --   98.20 -30.00 150.00  228
 18  \w     91.00 137.00   0.50    1.61    --   98.20 -82.00   0.00   92
 19  \w     53.00 102.00   0.50    1.61    --   98.20 -82.00-120.00   98
 20  \w     70.00 119.00   0.50    1.61    --   98.20  61.00   0.00   98
 21  \w     69.00 178.00   0.50    1.61    --   98.20  45.00  90.00  218
 22  \w      9.00  40.00   0.50    1.61    --   98.20 -82.00-180.00   62
 23  \w      9.00 128.50   0.50    1.61    --   98.20 -82.00  60.00  239
 24  \w     13.00  97.00   0.50    1.61    --   98.20 -61.00 150.00  168
 25  \w     72.00 187.00   0.50    1.61    --   98.20  45.00 120.00  230
;
_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      0.1097204000
_diffrn_orient_matrix_UB_12      -0.0627792000
_diffrn_orient_matrix_UB_13      -0.0042664000
_diffrn_orient_matrix_UB_21      0.0786750000
_diffrn_orient_matrix_UB_22      0.0742537000
_diffrn_orient_matrix_UB_23      -0.0077659000
_diffrn_orient_matrix_UB_31      -0.0304257000
_diffrn_orient_matrix_UB_32      -0.0062619000
_diffrn_orient_matrix_UB_33      0.0924048000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32897
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.437
_diffrn_reflns_theta_min         3.667
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.019
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44972
_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            black
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         12058
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0477P)^2^+0.6631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0905
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10716
_reflns_number_total             12058
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi01245h2.cif
_cod_data_source_block           171030-4_sq
_cod_original_cell_volume        3094.52(6)
_cod_database_code               4349960
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.37
_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 1.891
_oxdiff_exptl_absorpt_empirical_full_min 0.555