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_7711707
_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         'C52 H58 Fe'
_chemical_formula_sum            'C52 H58 Fe'
_chemical_formula_weight         738.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-06-22
_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                 96.822(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9745(14)
_cell_length_b                   16.9307(18)
_cell_length_c                   20.1943(15)
_cell_measurement_reflns_used    6211
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      75.2590
_cell_measurement_theta_min      4.2620
_cell_volume                     4404.6(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41n (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41n (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41n (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            'PILATUS3 R 200K Hybrid Pixel Array Detector'
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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    -83.00  23.00   1.00   20.00    --    0.00 -38.00 150.00  106
  2  \w    -32.00  27.00   1.00   20.00    --    0.00 -82.00  30.00   59
  3  \w    -33.00  31.00   1.00   20.00    --    0.00 -82.00 -90.00   64
  4  \w    -43.00   9.00   1.00   20.00    --    0.00 -77.00  90.00   52
  5  \w     78.00 133.00   1.00   80.00    --   99.90 -82.00-120.00   55
  6  \w     11.00 122.00   1.00   80.00    --   99.90 -82.00 -30.00  111
  7  \w    148.00 182.00   1.00   80.00    --   99.90   0.00-180.00   34
  8  \w     74.00 110.00   1.00   80.00    --   99.90 -77.00 120.00   36
  9  \w     91.00 118.00   1.00   80.00    --   99.90 -82.00  30.00   27
 10  \w     10.00  68.00   1.00   80.00    --   99.90 -30.00 -60.00   58
 11  \w     41.00  67.00   1.00   80.00    --   99.90 -82.00 -60.00   26
 12  \w     10.00  69.00   1.00   80.00    --   99.90 -30.00-180.00   59
 13  \w    127.00 189.00   1.00   80.00    --   99.90  15.00 -90.00   62
 14  \w     27.00  53.00   1.00   80.00    --   99.90 -45.00 120.00   26
 15  \w     31.00 115.00   1.00   80.00    --   99.90 -82.00   0.00   84
 16  \w     23.00  49.00   1.00   80.00    --   99.90 -77.00 120.00   26
 17  \w     11.00 114.00   1.00   80.00    --   99.90 -82.00-180.00  103
 18  \w    100.00 126.00   1.00   80.00    --   99.90 -77.00-120.00   26
 19  \w     40.00 118.00   1.00   80.00    --   99.90 -82.00-150.00   78
 20  \w     71.00  97.00   1.00   80.00    --   99.90 -82.00  90.00   26
 21  \w     10.00 121.00   1.00   80.00    --   99.90 -82.00 -90.00  111
 22  \w     10.00 117.00   1.00   80.00    --   99.90 -82.00 150.00  107
 23  \w     42.00  76.00   1.00   80.00    --   99.90 -45.00  30.00   34
 24  \w     87.00 131.00   1.00   80.00    --   99.90 -82.00 -60.00   44
 25  \w     10.00 128.00   1.00   80.00    --   99.90 -82.00  60.00  118
 26  \w     62.00 106.00   1.00   80.00    --   99.90  15.00 -90.00   44
 27  \w     45.00  74.00   1.00   80.00    --   99.90 -45.00-120.00   29
 28  \w     17.00 104.00   1.00   80.00    --   99.90 -82.00 120.00   87
 29  \w     10.00  69.00   1.00   80.00    --   99.90 -30.00 -30.00   59
 30  \w     21.00  70.00   1.00   80.00    --   99.90 -77.00-120.00   49
 31  \w     27.00  75.00   1.00   80.00    --   99.90 -82.00  30.00   48
 32  \w     64.00 110.00   1.00   80.00    --   99.90 -77.00-150.00   46
 33  \w     76.00 115.00   1.00   80.00    --   99.90 -77.00  30.00   39
 34  \w     23.00  61.00   1.00   80.00    --   99.90 -45.00 -90.00   38
 35  \w     88.00 138.00   1.00   80.00    --   99.90   0.00-180.00   50
 36  \w    104.00 130.00   1.00   80.00    --   99.90 -77.00   0.00   26
 37  \w     16.00  83.00   1.00   80.00    --   99.90   0.00-180.00   67
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'XtalLAB PRO MM007, PILATUS3 R 200K'
_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      -0.0209121000
_diffrn_orient_matrix_UB_12      0.0894448000
_diffrn_orient_matrix_UB_13      0.0002613000
_diffrn_orient_matrix_UB_21      -0.1172278000
_diffrn_orient_matrix_UB_22      -0.0157663000
_diffrn_orient_matrix_UB_23      -0.0165091000
_diffrn_orient_matrix_UB_31      -0.0111154000
_diffrn_orient_matrix_UB_32      -0.0037611000
_diffrn_orient_matrix_UB_33      0.0749119000
_diffrn_radiation_collimation    'VariMax VHF mirror optic'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0949
_diffrn_reflns_av_unetI/netI     0.0785
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20637
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        54.526
_diffrn_reflns_theta_max         54.526
_diffrn_reflns_theta_min         3.417
_diffrn_source                   'rotating anode'
_diffrn_source_current           30
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'MicroMax 007 HF'
_diffrn_source_voltage           40
_exptl_absorpt_coefficient_mu    2.971
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.604
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41n (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 greenish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_recrystallization_method 'Recrystallised from hexane at -30'
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.218
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         5295
_refine_ls_number_restraints     1170
_refine_ls_restrained_S_all      0.861
_refine_ls_R_factor_all          0.1147
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0838P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1296
_refine_ls_wR_factor_ref         0.1494
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2922
_reflns_number_total             5295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03531f2.cif
_cod_data_source_block           feajva
_cod_database_code               7711707
_nottingham_internal_coll_name   FEAJVA
_nottingham_internal_coll_number 15766
_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,, 20.00, 80.00'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_user   pcxav1
_nottingham_internal_coll_date   11/03/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'XtalLAB PRO, A00000876'
_nottingham_internal_process_date 14/03/2016
_nottingham_internal_process_user pcxav1
_nottingham_internal_solution_date 02/06/2016
_nottingham_internal_solution_user pcxav1
_nottingham_internal_refinement_date 24/06/2016
_nottingham_internal_refinement_user 'pcxav1 PCXHRS pczlt pczspa'
_nottingham_internal_self_archive_date 24/06/2016
_nottingham_internal_self_validation_date 24/06/2016
_nottingham_internal_self_validation_user 'pcxav1 PCXHRS'
_nottingham_internal_validation_date 22/06/2022
_nottingham_internal_validation_user pczspa
_nottingham_internal_archive_date 22/06/2022
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C52 H58 Fe1'
_chemical_oxdiff_usercomment
'FEAJVA #15766 MM-116 IN FOMBLIN FILM ON A MICROMOUNT FOR AJV/DLK'
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.514
_reflns_odcompleteness_completeness 99.06
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_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. Restrained distances
 C51A-C49 \\sim C51B-C49 \\sim C52A-C49 \\sim C50A-C49 \\sim C50B-C49 \\sim
C52B-C49
 with sigma of 0.02
 C16B-C15B \\sim C16A-C15A \\sim C20B-C15B \\sim C20A-C15A
 with sigma of 0.02
 C17B-C16B \\sim C17A-C16A \\sim C20B-C19B \\sim C20A-C19A
 with sigma of 0.02
 C18B-C17B \\sim C18A-C17A \\sim C19B-C18B \\sim C19A-C18A
 with sigma of 0.02
 C21A-C16A \\sim C21B-C16B \\sim C22B-C20B \\sim C22A-C20A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C51B \\sim C51A: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
Uanis(C51B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C50B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C50B)=Sof(H50d)=Sof(H50e)=Sof(H50f)=Sof(C51B)=Sof(H51d)=Sof(H51e)=
 Sof(H51f)=Sof(C52B)=Sof(H52d)=Sof(H52e)=Sof(H52f)=1-FVAR(1)
 Sof(C50A)=Sof(H50a)=Sof(H50b)=Sof(H50c)=Sof(C51A)=Sof(H51a)=Sof(H51b)=
 Sof(H51c)=Sof(C52A)=Sof(H52a)=Sof(H52b)=Sof(H52c)=FVAR(1)
 Fixed Sof: C15A(0.69) C16A(0.69) C17A(0.69) H17A(0.69) C18A(0.69) H18A(0.69)
 C19A(0.69) H19A(0.69) C20A(0.69) C21A(0.69) H21a(0.69) H21b(0.69) H21c(0.69)
 C22A(0.69) H22a(0.69) H22b(0.69) H22c(0.69) C15B(0.31) C16B(0.31) C17B(0.31)
 H17B(0.31) C18B(0.31) H18B(0.31) C19B(0.31) H19B(0.31) C20B(0.31) C21B(0.31)
 H21d(0.31) H21e(0.31) H21f(0.31) C22B(0.31) H22d(0.31) H22e(0.31) H22f(0.31)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C25(H25), C27(H27), C31(H31),
 C32(H32), C33(H33), C39(H39), C40(H40), C41(H41), C17A(H17A), C18A(H18A),
 C19A(H19A), C17B(H17B), C18B(H18B), C19B(H19B)
6.b Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C14(H14a,H14b,H14c), C35(H35a,H35b,H35c), C36(H36a,H36b,
 H36c), C43(H43a,H43b,H43c), C44(H44a,H44b,H44c), C46(H46a,H46b,H46c), C47(H47a,
 H47b,H47c), C48(H48a,H48b,H48c), C50A(H50a,H50b,H50c), C51A(H51a,H51b,H51c),
 C52A(H52a,H52b,H52c), C50B(H50d,H50e,H50f), C51B(H51d,H51e,H51f), C52B(H52d,
 H52e,H52f), C21A(H21a,H21b,H21c), C22A(H22a,H22b,H22c), C21B(H21d,H21e,H21f),
 C22B(H22d,H22e,H22f)
;
_shelx_res_checksum              68816
_shelx_hkl_checksum              76556
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.423
_oxdiff_exptl_absorpt_empirical_full_min 0.157