Slow magnetic relaxation in Fe(II) m-terphenyl complexes
Valentine, Andrew James; Geer, Ana M.; Blundell, Toby; Tovey, Will; Cliffe, Matthew; Davies, Edward Stephen; Argent, Stephen; Lewis, William; McMaster, Jonathan; Taylor, Laurence John; Reta, Daniel; Kays, Deborah Lorraine; Dalton Transactions  (2022) –; doi:10.1039/D2DT03531F

data_7711709
_publ_section_title
;
 Slow magnetic relaxation in Fe(II) m-terphenyl complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT03531F
_journal_year                    2022
_chemical_formula_moiety         'C50 H58 Fe Si2'
_chemical_formula_sum            'C50 H58 Fe Si2'
_chemical_formula_weight         770.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-03-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-07-07 deposited with the CCDC.	2022-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.414(4)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   25.4389(10)
_cell_length_b                   11.5117(4)
_cell_length_c                   47.1469(18)
_cell_measurement_reflns_used    12436
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.8460
_cell_measurement_theta_min      4.1960
_cell_volume                     13483.9(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 4.2207
_diffrn_detector_type            'Agilent Diffraction Titan S2 detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.973
_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    -50.00  28.00   1.00    7.50    --  -43.06  38.00-180.00   78
  2  \w    -50.00  28.00   1.00    7.50    --  -43.06  38.00 -60.00   78
  3  \w      2.00  96.00   1.00    7.50    --   43.06-125.00-180.00   94
  4  \w     19.00 112.00   1.00    7.50    --   43.06  57.00-150.00   93
  5  \w     20.00 114.00   1.00    7.50    --   43.06  38.00  30.00   94
  6  \w     23.00 109.00   1.00   30.00    --  103.63 -94.00  60.00   86
  7  \w     73.00 175.00   1.00   30.00    --  103.63 125.00 120.00  102
  8  \w     31.00  91.00   1.00   30.00    --  103.63 -30.00-150.00   60
  9  \w     31.00  91.00   1.00   30.00    --  103.63 -30.00-120.00   60
 10  \w     81.00 172.00   1.00   30.00    --  103.63  45.00-180.00   91
 11  \w     32.00 122.00   1.00   30.00    --  103.63-125.00-120.00   90
 12  \w     35.00  98.00   1.00   30.00    --  103.63 -45.00  60.00   63
 13  \w     13.00 115.00   1.00    7.50    --   43.06  77.00  30.00  102
 14  \w     19.00 112.00   1.00    7.50    --   43.06  57.00 -90.00   93
 15  \w     19.00 112.00   1.00    7.50    --   43.06  57.00 120.00   93
 16  \w     80.00 176.00   1.00   30.00    --  103.63  30.00 120.00   96
 17  \w     68.00 178.00   1.00   30.00    --  103.63  15.00 -60.00  110
 18  \w     73.00 175.00   1.00   30.00    --  103.63  77.00-150.00  102
 19  \w     23.00  92.00   1.00   30.00    --  103.63 -94.00 -90.00   69
 20  \w     81.00 172.00   1.00   30.00    --  103.63  45.00 -30.00   91
 21  \w     80.00 176.00   1.00   30.00    --  103.63  30.00  30.00   96
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Titan S2'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0455248000
_diffrn_orient_matrix_UB_12      0.0605347000
_diffrn_orient_matrix_UB_13      0.0112986000
_diffrn_orient_matrix_UB_21      -0.0141486000
_diffrn_orient_matrix_UB_22      -0.1160624000
_diffrn_orient_matrix_UB_23      0.0128244000
_diffrn_orient_matrix_UB_31      0.0396527000
_diffrn_orient_matrix_UB_32      0.0280662000
_diffrn_orient_matrix_UB_33      0.0287497000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.1280
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            79133
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.656
_diffrn_reflns_theta_min         3.558
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.424
_exptl_absorpt_correction_T_max  0.826
_exptl_absorpt_correction_T_min  0.442
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_description       block
_exptl_crystal_F_000             4944
_exptl_crystal_recrystallization_method 'Recrystallised from hexane at 0'
_exptl_crystal_size_max          0.444
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     738
_refine_ls_number_reflns         13471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0844
_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^)+(0.0553P)^2^+89.0368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1951
_refine_ls_wR_factor_ref         0.2115
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9834
_reflns_number_total             13471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03531f2.cif
_cod_data_source_block           feajvb
_cod_database_code               7711709
_nottingham_internal_coll_name   FEAJVB
_nottingham_internal_coll_number 16218
_nottingham_internal_coll_client AJV/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'ofand \w scans'
_nottingham_internal_coll_frame_time 'degrees,, 7.50, 30.00'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_user   pcxav1
_nottingham_internal_coll_date   04/07/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVA, PL13110002'
_nottingham_internal_process_date 05/07/2016
_nottingham_internal_process_user pcxav1
_nottingham_internal_solution_date 05/07/2016
_nottingham_internal_solution_user pcxav1
_nottingham_internal_refinement_date 05/07/2016
_nottingham_internal_refinement_user pcxav1
_nottingham_internal_self_archive_date 05/07/2016
_nottingham_internal_self_validation_date 05/07/2016
_nottingham_internal_self_validation_user pcxav1
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50 H58 Fe Si2'
_chemical_oxdiff_usercomment
'FEAJVB #16218 GVA-1028 IN FOMBLIN ON A MICROMOUNT FOR AJV/DLK'
_reflns_odcompleteness_completeness 99.98
_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
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C17(H17), C18(H18), C19(H19),
 C25(H25), C27(H27), C31(H31), C32(H32), C33(H33), C39(H39), C40(H40), C41(H41),
  C53(H53), C55(H55), C59(H59), C60(H60), C61(H61), C67(H67), C68(H68), C69(H69)
2.b Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C14(H14a,H14b,H14c), C21(H21a,H21b,H21c), C22(H22a,H22b,
 H22c), C35(H35a,H35b,H35c), C36(H36a,H36b,H36c), C43(H43a,H43b,H43c), C44(H44a,
 H44b,H44c), C45(H45a,H45b,H45c), C46(H46a,H46b,H46c), C47(H47a,H47b,H47c),
 C48(H48a,H48b,H48c), C49(H49a,H49b,H49c), C50(H50a,H50b,H50c), C63(H63a,H63b,
 H63c), C64(H64a,H64b,H64c), C71(H71a,H71b,H71c), C72(H72a,H72b,H72c), C73(H73a,
 H73b,H73c), C74(H74a,H74b,H74c), C75(H75a,H75b,H75c)
;
_shelx_res_checksum              72603
_shelx_hkl_checksum              15617
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_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 3.837
_oxdiff_exptl_absorpt_empirical_full_min 0.408